Smart Sensors, Measurement and Instrumentation 23

Subhas Chandra Mukhopadhyay
Octavian Adrian Postolache
Krishanthi P. Jayasundera
Akshya K. Swain Editors

Sensors for
Everyday
Life
Environmental and Food Engineering
Smart Sensors, Measurement
and Instrumentation

Volume 23

Series editor
Subhas Chandra Mukhopadhyay
Department of Engineering, Faculty of Science and Engineering
Macquarie University
Sydney, NSW
Australia
e-mail: [email protected]
More information about this series at http://www.springer.com/series/10617
Subhas Chandra Mukhopadhyay
Octavian Adrian Postolache
Krishanthi P. Jayasundera
Akshya K. Swain
Editors

Sensors for Everyday Life

Environmental and Food Engineering

123
Editors
Subhas Chandra Mukhopadhyay Krishanthi P. Jayasundera
Department of Engineering, Faculty of Institute of Fundamental Sciences
Science and Engineering Massey University
Macquarie University Palmerston North
Sydney, NSW New Zealand
Australia
Akshya K. Swain
Octavian Adrian Postolache Department of Electrical and Computer
Instituto de Telecomunicações Engineering
Lisbon University of Auckland
Portugal Auckland
New Zealand
and

ISCTE-IUL
Lisbon
Portugal

ISSN 2194-8402 ISSN 2194-8410 (electronic)

Smart Sensors, Measurement and Instrumentation
ISBN 978-3-319-47321-5 ISBN 978-3-319-47322-2 (eBook)
DOI 10.1007/978-3-319-47322-2
Library of Congress Control Number: 2016953322

© Springer International Publishing AG 2017

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Preface

Sensors play a pivotal role in our everyday life. They gather data on environment,
and information on weather, traffic congestion, air pollution, water pollution, etc. is
obtained; they gather data on human body, and information on health, treatment or
therapy outcomes is obtained; they gather data on objects, and information for
monitoring and control of these objects is obtained; they gather data on subjects or
objects functions, and information for better decisions, control and action is
obtained. For instance, the weather information is used to choose adequate clothes,
the battery level sensor permits smartphone power management optimization, and
the level of blood glucose allows better healthcare management. Data collected
through sensors enhance our lives and our connections to each other and with our
environment, allow real-time monitoring of many phenomena around us, provide
information about quality of products and services, improve the equipment control
based on sensorized interfaces and contribute to increase knowledge on physical
and chemical world.
The advances in electronics, embedded controller, technology for communica-
tion as well as the progress towards a better informed, knowledge based society
increase the demand for small size, affordable sensors that allow accurate and
reliable data recording, processing, storing and communication. The work contains
invited chapters from renowned experts, working in sensors’ field, and it is split into
two books that present several technologies and applications of sensors in Envi-
ronmental and Food Engineering (ISBN 978-3-319-47322-2) and for Healthcare
Settings (ISBN 978-3-319-47319-2).
The book Sensors for Everyday Life—Environmental and Food Engineering
describes novel sensors and sensing systems developed for environment monitoring
and food production and quality assessment.
Environmental quality refers to characteristics from natural environment as well
as from the built environment (i.e. city air and/or water pollution, concentration of
nitrate from the soil in cultivated fields). Environmental quality plays an important
role in health and well-being of the populations. Degraded environmental quality as
produced by air and water pollution may affect our lives, directly or through the
food we eat. In food engineering various sensors are used for assessment of

v
vi Preface

contaminants, adulterants, naturally occurring toxins or any other substance that

may make food injurious to health on an acute or chronic basis as well as sensors
that contribute for quality improvement of food. New developed sensors and
technology trend related air, water, food quality monitoring as well as for modern
agronomy and food production are presented in this book.

How This Book is Organized

In Chap. 1, a novel method for the simultaneous determination of NOx and soot in
the exhaust of diesel engines during the periodical technical inspection roadwor-
thiness test is presented. A multi-wavelength light extinction measurement, in a
setup similar to an opacimeter with high sensitivity, and a mathematical inversion
algorithm are used to obtain the concentrations from the extinction readings.
Analytical technique of the fine particles using atomic emission spectroscopy
system for an environmental pollution monitoring is presented in Chap. 2.
Laser-induced breakdown spectroscopy (LIBS) system and the helium-microwave-
induced plasma-atomic emission spectroscopy (He-MIP-AES) system are used for
characterizations and real-time measurement of the air chemical compositions and
particle size.
Chapter 3 presents sensors and method for automatic fault detection in heating
ventilating and air conditioning (HVAC) systems. This is important mainly in smart
buildings context as the indoor condition in these buildings is mainly related with
the capabilities and reliability of HVAC systems.
New optical fiber humidity sensor is described in Chap. 4. Different humidity
sensors that have been developed by now are presented focusing in the different
optical structures and materials that have been used for improving sensitivity and
resolutions of these sensors.
The measurement of air gas concentration represents an important field of
application of sensing technologies. In Chap. 5 of the book, a review on the oxygen
gas sensing technologies is presented with focus on potentiometric, amperometric,
paramagnetic and tunable diode laser spectroscopy (TDLS) sensors. Theoretical
aspects and operational basic of these technologies, system requirements as well as
limitations of the methods are discussed in this chapter.
A low-cost sensor node based on interdigital capacitive sensor for nitrate and
nitrite in surface and ground water concentration detection is presented in Chap. 6.
This sensor is important for agronomy as well as for water pollution assessment.
Nitrates may be present in high concentration in ground and surface water as a
result of intensive agriculture, disposal of human and animal sewage and industrial
wastes.
In Chap. 7 an intelligent wireless sensor network system designed to monitor
various parameter in palm oil plantation for improvement in the controlled polli-
nation process is presented. The system helps in making decision related to best
time for pollination process. The inaccuracy in determining pollination readiness
Preface vii

of the oil palm flower could potentially cause a detrimental effect on the palm oil
industry in the long run.
The following two chapters present sensors for determination of quality and
quantity of water for drinking purpose. In Chap. 8, a reflectometer and a Doppler
radar systems for detection of water level in septic tank is described. A novel S3
(Small Sensor System) nanowire device for the detection of complex mixtures of
bacteria in potable water is presented in Chap. 9.
Next three chapters describe sensors used in food productions and quality
assessment. A novel approach to monitor the quality of milk products, based on
electromagnetic wave spectroscopy is presented in Chap. 10. The system use vector
network analyser to capture spectral signatures in the form of scattering parameters
from electromagnetic wave sensors. Data on reliability testing is presented. A new,
rapid, portable, easy-to-use, economic and non-destructive fouling based on
nanowire technology device to control the presence of false grated Parmigiano
Reggiano cheese is described in Chap. 11. A review on the conventional techniques
and dielectric spectroscopy for analyzing food products is presented in Chap. 12,
focusing on the application of dielectric spectroscopy in fats and oils adulteration
detection.
Different wireless sensor network architecture is implemented nowadays to
perform distributed measurement tasks for environment monitoring with increase in
space resolution. Big challenge in these implementations continues to be wireless
interference and radio-frequency (RF) spectrum crowding. Chapter 13 focuses on a
technique for optical-based RF interference cancellation. In this chapter several
system architectures are presented and a sample of their experimental performance
and the key characteristics of this technique and the future prospects for this
technology, focusing specifically on photonic integrated circuits are discussed.
A scheme is proposed in Chap. 14 that can reduce the performance difference
between cluster heads (CHs) involved in inter-cluster communication on IEEE 802.
15.4 cluster-based wireless sensor networks (WSNs) under spatial non-uniform
traffic condition where the CHs have various amount of traffic. This reduced the
energy consumption and simplified processing mechanism to achieve long WSNs
lifetime under limited network resource condition.
We do sincerely hope that the readers will find this special issue interesting and
useful in their research on sensors and wireless sensor networks for environment
monitoring, food production and quality assessment.
We want to acknowledge all the authors for their contribution and for sharing
of their knowledge. We hope that the works presented in this book will stimulate
further research related to sensors for everyday life.

Sydney, Australia Subhas Chandra Mukhopadhyay

Lisbon, Portugal Octavian Adrian Postolache
Palmerston North, New Zealand Krishanthi P. Jayasundera
Auckland, New Zealand Akshya K. Swain
About the Editors

Dr. Subhas Chandra Mukhopadhyay (M’97,

SM’02, F’11) graduated from the Department of
Electrical Engineering, Jadavpur University, Calcutta,
India with a Gold medal and received the Master of
Electrical Engineering degree from Indian Institute of
Science, Bangalore, India. He has Ph.D. (Eng.) degree
from Jadavpur University, India and Doctor of Engi-
neering degree from Kanazawa University, Japan.
Currently he is working as Professor of
Mechanical/Electronics Engineering and Discipline
Leader of the Mechatronics Degree Programme of the
Department of Engineering, Macquarie University,
Sydney, Australia. He has over 26 years of teaching and research experiences.
His fields of interest include smart sensors and sensing technology, wireless
sensor networks, internet of things, electromagnetics, control engineering, magnetic
bearing, fault current limiter, electrical machines and numerical field calculation.
He has authored/co-authored over 400 papers in different international journals,
conferences and book chapter. He has edited thirteen conference proceedings. He
has also edited fifteen special issues of international journals as lead guest editor
and twenty-five books with Springer-Verlag.
He was awarded numerous awards throughout his career and attracted over NZ
$4.2 M on different research projects.
He has delivered 272 seminars including keynote, tutorial, invited and special
seminars.
He is a Fellow of IEEE (USA), a Fellow of IET (UK) and a Fellow of IETE
(India). He is a Topical Editor of IEEE Sensors Journal and an Associate Edi-
tor IEEE Transactions on Instrumentation. He has organized many international
conferences either as general chair or technical programme chair. He is the

ix
x About the Editors

Ex-Chair of the IEEE Instrumentation and Measurement Society New Zealand

Chapter. He chairs the IEEE IMS Technical Committee 18 on Environmental
Measurements.
Dr. Octavian Adrian Postolache (M’99, SM’2006)
graduated in Electrical Engineering at the Gh. Asachi
Technical University of Iasi, Romania, in 1992 and he
received the Ph.D. degree in 1999 from the same
university, and university habilitation in 2016 from
Instituto Superior Tecnico, Universidade de Lisboa,
Portugal. In 2000 he became principal researcher of
Instituto de Telecomunicações where he is now Senior
Researcher. Since 2012 he joined Instituto Universi-
tario de Lisboa/ISCTE-IUL Lisbon where he is cur-
rently Aux. Professor.
His fields of interests include smart sensors for
biomedical and environmental applications, pervasive sensing and computing,
wireless sensor networks, signal processing with application in biomedical and
telecommunications, non-destructive testing and diagnosis based on eddy currents
smart sensors, computational intelligence with application in automated measure-
ment systems.
He is active member of national and international research teams involved in
Portuguese and EU and International projects. He was principal researcher of dif-
ferent projects including EHR-Physio regarding the implementation of Electronic
Health Records for Physiotherapy and he is currently principal researcher of Tai-
lorPhy project Smart Sensors and Tailored Environments for Physiotherapy.
Dr. Postolache is author and co-author of 9 patents, 4 books, 16 book chapters,
66 papers in international journals with peer review, more than 220 papers in
proceedings of international conferences.
He is IEEE Senior Member I&M Society, Distinguished Lecturer of IEEE IMS,
chair of IEEEI&MSTC-13 Wireless and Telecomunications in Measurements,
member of IEEEI&MSTC-17, IEEEI&MSTC-18, IEEEI&MSTC-25, IEEE EMBS
Portugal Chapter and chair of IEEE IMS Portugal Chapter. He is Associate Editor
of IEEE Sensors Journal, and IEEE Transaction on Instrumentation and Measure-
ments, he was general chair of IEEE MeMeA 2014, and TPC chair of ICST 2014,
Liverpool and ICST 2015 in Auckland. He received IEEE best reviewer and the
best associate editor in 2011 and 2013 and other awards related to his research
activity in the field of smart sensing.
About the Editors xi

Dr. Krishanthi P. Jayasundera graduated from

University of Peradeniya, Sri Lanka with honors degree
in Chemistry. She obtained her both Master and Ph.D.
in Organic Chemistry from Kanazawa University,
Japan. She worked as postdoctoral researcher at Mas-
sey University nearly 14 years in New Zealand
involving various projects focused on the chemical
synthesis of architecturally interesting molecules which
have biological, environmental and/or medicinal sig-
nificance. Currently, she is an independent research
consultant. She specializes in organic chemistry, bio-
sciences, sensitivity analysis using NMR, HPLC, SPR
and so on. She has published over 30 papers in different international journals and
conference proceedings.

Akshya K. Swain received the B.Sc. degree in

Electrical Engineering and the M.Sc. degree in Elec-
tronic Systems and Communication from Sambalpur
University, Sambalpur, India, in 1985 and 1988,
respectively, and the Ph.D. degree from the Depart-
ment of Automatic Control and Systems Engineering,
University of Sheffield, Sheffield, U.K., in 1997. From
1994 to 1996, he was a Commonwealth Scholar in the
United Kingdom. Since September 2002, he has been
with the Department of Electrical and Computer
Engineering, the University of Auckland, Auckland,
New Zealand. He has published over 150 papers in
International Journals and conferences. His current research interests include non-
linear system identification and control, fault tolerant control, biomedical signal
processing, sensor networks, and control applications to power system and wireless
power transfer system. Dr. Swain is an Associate Editor of IEEE Sensors Journal
and Member of the Editorial Board of International Journal of Automation and
Control and International Journal of Sensors, Wireless Communications and
Control.
Contents

Determination of NOX and Soot Concentrations

Using a Multi-wavelength Opacimeter . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
H. Axmann, A. Bergmann and B. Eichberger
Development of the Atomic Emission Spectroscopy System
Using Helium-Microwave-Induced Plasma for Fine Particles
on Environmental Monitoring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
Satoshi Ikezawa, Jun Yamamoto and Toshitsugu Ueda
Real-Time HVAC Sensor Monitoring and Automatic Fault
Detection System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
Ying Guo, Josh Wall, Jiaming Li and Sam West
High Sensitivity Optical Structures for Relative Humidity Sensing . . . . . 55
Joaquin Ascorbe, Jesus Corres, Francisco J. Arregui, Ignacio R. Matias
and Subhas Chandra Mukhopadhyay
Oxygen Gas Sensing Technologies Application: A Comprehensive
Review . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81
P. Shuk
Application of Practical Nitrate Sensor Based
on Electrochemical Impedance Spectroscopy . . . . . . . . . . . . . . . . . . . . . . 109
Md Eshrat E. Alahi, Xie Li, Subhas Mukhopadhyay and L. Burkitt
Using Wireless Sensor Networks to Determine Pollination
Readiness in Palm Oil Plantation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 137
Mohamed Rawidean Mohd Kassim and Ahmad Nizar Harun
Time Domain Reflectometer for Measuring Liquid Waste
Levels in a Septic System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 157
Shreya Reddy Mamidi, Kaushik Bukka, Michael Haji-Sheikh,
Martin Kocanda, Donald Zinger and Mansour Taherinezahdi

xiii
xiv Contents

Nanowire (S3) Device for the Quality Control of Drinking Water . . . . . 179
Estefanía Núñez Carmona, Matteo Soprani and Veronica Sberveglieri
Milk Quality Monitoring Using Electromagnetic Wave Sensors . . . . . . . 205
Keyur H. Joshi, Alex Mason, Olga Korostynska
and Ahmed Al-Shamma’a
Grated Parmigiano Reggiano Cheese: Authenticity Determination
and Characterization by a Novel Nanowire Device (S3)
and GC-MS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 229
Veronica Sberveglieri, Manohar P. Bhandari, Andrea Pulvirenti
and Estefania Núñez Carmona
Lard Detection in Edible Oil Using Dielectric Spectroscopy . . . . . . . . . . 245
Masyitah Amat Sairin, Samsuzana Abd Aziz,
Nina Naquiah Ahmad Nizar, Nurul Adilah Abdul Latiff,
Alyani Ismail, Dzulkifly Mat Hashim and Fakhrul Zaman Rokhani
Optical-Based Interference Cancellation in Wireless
Sensor Networks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 273
Matthew P. Chang, Jingyi (Jenny) Sun, Monica Lu, Eric Blow
and Paul R. Prucnal
Traffic Adaptive Channel Access Scheme for IEEE802.15.4
Cluster-Based WSNs Under Spatial Non-uniform
Traffic Condition . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 303
Akiyuki Yamauchi, Kazuo Mori and Hideo Kobayashi
Author Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 323
Determination of NOX and Soot
Concentrations Using a Multi-wavelength
Opacimeter

H. Axmann, A. Bergmann and B. Eichberger

Abstract A novel approach to measure both the particle and the NO2 concentra-
tion in the exhaust of diesel engines during the roadworthiness test in the periodical
technical inspection is presented. It is based on a multi-wavelength extinction
measurement and a mathematical inversion algorithm to obtain the concentrations
from the extinction readings. Such individual concentration values can deliver
valuable insight into the cause of engine or exhaust aftertreatment defects. Fur-
thermore the extended opacimeter provides future-proofness, if nitrous gas emis-
sions are incorporated in the roadworthiness regulations. In addition to a detailed
description of the multi-wavelength approach this chapter provides an overview of
particle and nitrous gas emissions by diesel engines, the related legislation, the
extinction measurement using standard opacimeters, and the physical background
for this optical measurement method. The applicability of the multi-wavelength
method is derived mathematically and validated with first experimental results as
well as with simulations.

1 Introduction

The emissions of vehicles equipped with internal combustion engines pose a sig-
nificant environmental problem and cause severe health effects. A big portion of the
engines run on diesel fuel. In some European countries they even surpass the amount
of gasoline vehicles with a relation of 70 to 30 % [1]. Across Europe the average
fraction of newly registered diesel cars reached 58 % in 2011 [2]. While the main
pollutant in the exhaust of gasoline engines is carbon dioxide (CO2), the most

H. Axmann (✉)
AVL DiTEST GmbH, Alte Poststraße 156, 8020 Graz, Austria
e-mail: [email protected]
A. Bergmann ⋅ B. Eichberger
Institute of Electronic Sensor Systems, University of Technology,
Inffeldgasse 10/II, 8010 Graz, Austria

© Springer International Publishing AG 2017 1

S. Mukhopadhyay et al. (eds.), Sensors for Everyday Life, Smart Sensors,
Measurement and Instrumentation 23, DOI 10.1007/978-3-319-47322-2_1
2 H. Axmann et al.

relevant pollutants of diesel engines are particulate matter (PM) and nitrous gases
(NOX). CO2 is a green house gas, whereas particles and NO2 are toxic components.
Diesel particulate matter consists mainly of carbonaceous particles, ashes and
unburned fuel and oil droplets [3]. It has been lately proven to be carcinogenic [4].
Furthermore the black carbon (BC) fraction of the particles contributes to global
warming, and when deposited on snowpacks the particles lead to accelerated
melting through absorption of the sunlight [5].
Nitrous gases consist of nitrogen monoxide (NO) and nitrogen dioxide (NO2).
During the combustion process of diesel fuel mostly NO is produced. By the
catalyzed particle filter systems in modern vehicles a significant amount of NO is
oxidized to NO2 [6–8]. NO2 is a brown, toxic gas, which may lead to mucosal
irritation. It is a main contributor to smog in big cities [9] and is—in aqueous
solution—a strong acid leading to acid rain [10].
Governments all over the world reacted to this threat by introducing limits for
the allowed concentration of said pollutants in the exhaust of internal combustion
engines. Since the first emission regulations in the early 1970s the limit values have
been significantly reduced [10–12]. This is shown in Fig. 1 using the European
Emission Standards (EURO 1-6) as an example. To conform to these emission
limits the engine manufacturers have to optimize the combustion process and to add
new exhaust aftertreatment systems. Still the efficiency of these measures can
deteriorate over time. Accordingly periodic emission checks are necessary to ensure
the compliance of the vehicles to the emission limits. Such emission checks are
typically performed during the periodical technical inspection (PTI) in garages or
vehicle inspection institutions.
For the case of diesel vehicles the regulation-compliant functionality of the
engine and the exhaust system is determined from the opacity of the exhaust gases.
The corresponding measurement device is the opacity meter, commonly just called
opacimeter, which is based on an optical measurement. Just as the first emission

Fig. 1 PM and NOX limits of 0.16

EURO 1-6
0.14
EURO 1

0.12
PM limit [g/km]

0.1

0.08
EURO 2
0.06
EURO 3
0.04

0.02 EURO 4
EURO 5/6
0
0 0.2 0.4 0.6 0.8 1
NOx limit [g/km]
Determination of NOX and Soot Concentrations Using … 3

limits its measurement principle dates back to the 1970s [13]: A measurement
chamber of defined length is filled with exhaust gas, and the attenuation of light by
the sample is measured. While this was working perfectly for the older diesel
vehicles emitting tight black clouds of soot, it is reaching its limits for modern
models [14]. Equipped with diesel particle filters (DPFs) they emit much less, very
small particles. Accordingly the exhaust plumes are effectively transparent, only
with a very small amount of opacity. Therefore updated or new measurement
technologies are needed in order to perform meaningful and reliable measurements.
An example for a new technology is light scattering. It is also an optical mea-
surement method, measuring the amount of light deflected by the particles in the
exhaust gases. Due to its measurement principle it is mainly sensitive to particles
[15]. Although it proved to be well applicable for PTI exhaust measurements, it has
not been approved by the governments yet. Some other new measurement methods
have been proposed, but without success [16, 17]. As an alternative researchers
focused on updated versions of the opacimeter featuring an increased sensitivity.
Generally it is possible to lower the detection limit by at least one order of mag-
nitude with moderate means.
However opacimeters measure the combinational absorbing effect of all exhaust
components within the green wavelength range, where the human eye has its
maximum sensitivity. Originally this was by intention. It was the goal to measure an
overall visual obstruction produced by the vehicle. Besides, for older vehicles, most
of the effect could be attributed to the PM part. With the reduction of the particle
emissions the attenuating effect of the brown NO2 can surpass that of the particles.
In such a case it might often be desirable to obtain additional information about the
source of the measured signal in order to quickly identify the related defects in the
exhaust system. Furthermore getting individual figures for PM and NOX or NO2
can be advantageous regarding the individual limitation of these two criteria pol-
lutants. A one year study performed by the International Motor Vehicle Inspection
Committee (CITA) in 2011 already investigated PTI test equipment for individual
measurement of said components [13].
As shown in the following sections such extended measurement results can be
achieved by an opacimeter enhanced with a multi-wavelength light source.

2 The Opacimeter

A standard opacimeter consists of a measurement chamber of defined length, a

single-color, typically green light source on one side of the chamber and a light
detector on the opposite side (see Fig. 2). As long as the measurement chamber
contains clean air, the light emitted by the light source (e.g. a light emitting diode,
LED) does not get attenuated and a nominal light intensity I0 is measured on the
detector (e.g. a photo diode). During the measurement the chamber is filled with the
exhaust sample, which attenuates the light, resulting in a decreased light intensity
4 H. Axmann et al.

Fig. 2 Measurement particles/NO 2

principle of an opacimeter

light source measurement chamber detector

430 mm

I at the detector. By relating the two intensities I and I0 to each other the opacity
N can be calculated as

N = 1 − ðI ̸I0 Þ. ð1Þ

The opacity N is given in %. It depends on the length of the measurement

chamber. Typically a length of 430 mm is used, but differing values are possible.
Generally a length-independent measurement value is preferred. Therefore the
so-called extinction coefficient k is typically determined along with or instead of the
opacity. It is given in 1/m and can be calculated from I, I0 and the effective
measurement length Leff using Lambert’s Law [19]:

I ̸I0 = expð − kLeff Þ ð2Þ

In the literature this equation is also often called Lambert-Beer or Beer-Lambert

law. However the name Lambert-Beer law designates a slightly different variation
of (2), where the extinction coefficient is replaced by the product of the concen-
tration c of the absorbing material and its extinction efficiency σ ext [18]:

I ̸I0 = expð − cσ ext Leff Þ ð3Þ

Accordingly one can determine the concentration of the absorbing material from
the opacity measurement, if the extinction coefficient σ ext is known and constant.
The following section describes the physical background of said values and shows
typical values for PM and NO2.

3 Absorption of Particles and Gases

When light travels through a medium, energy is partly removed from the light beam
by the obstacles (particles, gas molecules and atoms) in the medium. This results in
an attenuation of the light beam. Such an effect is called extinction [19]. It is the
combination of absorption, where energy is transferred from the incident beam to
the obstacles, and scattering, where some parts of the light beam are deflected from
the original path and thereby also removed from the incident beam. Mathematically
this can be described in terms of the cross sections
Determination of NOX and Soot Concentrations Using … 5

σ ext = σ abs + σ sca , ð4Þ

where σ abs and σ sca are the absorption and the scattering cross sections respectively
[20]. The concept of a cross section is used to describe the ability of an obstacle to
remove light from an incident beam in a simple way. It can be understood as the
area shadowed from the incident beam. For the case of exhaust the main contributor
to extinction is absorption. This is attributable to the strong absorbing effects of the
primary components of the exhaust. Soot particles have a scattering share of only
10–30 % [21, 22]. Gases like NO2 even have a negligible scattering effect [23]. This
is the reason why, although physically incorrect, it has become customary to call
k absorption coefficient rather than extinction coefficient.
The total extinction coefficient of a mixture of substances with differing
extinction coefficients ki can be determined by summation [24]. As in (3) ki can be
expressed by the products of the individual cross sections σ ext, i and the respective
concentrations ci . Accordingly the total extinction coefficient k can be calculated as

k = ∑i ki = ∑i ci σ ext, i . ð5Þ

In principal the extinction cross section of the essential components in the

exhaust of diesel engines, PM and NO2, can be calculated with well-known for-
mulas. For species very small compared to the incident wavelength, e.g. gas
molecules, the shape of the object can be approximated as a sphere. In such a case
the Rayleigh model can be used to calculate scattering, absorption and extinction
effects. The Rayleigh model is valid, as long as the elements are smaller than
approximately one tenth of the wavelength. For bigger elements, like accumulation
mode exhaust particles [3], the shape must be taken into account. The behavior of
spherical objects can be calculated using the Mie theory, which is applicable for any
sphere diameter. Exact formulas also exist for some other well-defined shapes. For
irregular objects like the fractal-like soot particles, one typically uses approximative
models like the Rayleigh-Debye-Gans model for fractal aggregates (RDG-FA) [15].
For the purpose of this work it is important to understand the influence of the
wavelength on the extinction behavior. Accordingly the extinction spectrum over a
wide wavelength range is needed. The exact quantum-chemical calculation of such
a spectrum is yet not possible [25]. Fortunately especially for gases there exists
elaborate measurement data of the absorption behavior. For diesel soot particles
there exists extinction data, too, though not to the same amount.

3.1 Absorption of NO2

As said before the scattering effect of gases like NO2 is negligible. Its extinction
cross section is therefore almost identical to the absorption cross section, which is
shown in Fig. 3 for the wavelength range from 250 to 800 nm, given in
6 H. Axmann et al.

Absorption cross section σNO2 [cm2/molecule]

Fig. 3 Absorption cross 1 · 10
-18

section of NO2

8 · 10 -19

6 · 10 -19

4 · 10
-19

2 · 10
-19

0
300 400 500 600 700 800
Wavelength λ [nm]

cm2/molecule [26]. It has been measured at a pressure of 1000 mbar and a tem-
perature of 293 K.
Generally the uncertainty is in the order of a few percent. Near 250 nm the
uncertainty increases, as oscillations occur that are physically implausible. The peak
around 316 nm seems to be an artefact, too. Both phenomena are not of importance
for the actual work. The high oscillations around the peak at approximately 400 nm
however are factious. Thus it is crucial to utilize data with high wavelength reso-
lution in this area in order to achieve proper results. Temperature and pressure also
have a notable influence on the absorption behavior. Those influences can be
compensated using empirical models [25, 27].

3.2 Extinction of Soot Particles

The extinction behavior of particles is shown in Fig. 4 based on the example of a

Volkswagen turbo diesel engine (TDI Type 1Z, 1.9 l, 66 kW). It is given for the
wavelength range from 230 to 1000 nm in m2/g [28, 29]. In contrast to NO2 the
spectrum is rather smooth. According to their black color the soot particles absorb
light quite equally in the whole visible wavelength range. The measurement
uncertainty of the given data is in the order of 5 %. It has however not been
measured directly at the tailpipe. The particles had already grown to a median
mobility diameter (MMD) of 250–300 nm due to coagulation, which is approxi-
mately three times bigger than the MMD of tailpipe particles. The actual effect of
particle size on the extinction is rather small. The bigger particles will result in a
slightly stronger extinction. This is due to an increased scattering cross section, the
absorption cross section of fractal-like soot aggregates with constant volume is
independent of the particle size [30]. Simulations performed with typical particle
Determination of NOX and Soot Concentrations Using … 7

Fig. 4 Extinction cross 20

Extinction cross section σsoot [m2/g]

section of diesel soot

15

10

0
200 400 600 800 1,000
Wavelength λ [nm]

size distributions of diesel exhaust [3, 31] predict deviations in the order of a few
percent.
The absorption spectrum of NO2 and the extinction spectrum of soot are very
different, as obvious from Figs. 3 and 4. Accordingly their corresponding extinction
effects differ substantially for e.g. red, green and blue light. This is used in the
multi-wavelength approach presented in the following section.

4 The Multi-wavelength Approach

An examination of smoke samples using light at multiple wavelengths has already

been performed in the past. Aspey and Brazier for example have investigated the
particle mass fraction and mean particle size in exhaust [32]. Sharma et al. per-
formed optical characterizations of aerosols using a multi-wavelength
photoacoustic-nephelometer spectrometer [33]. Haisch and Niessner presented a
photoacoustic analyzer for the simultaneous quantification of soot and NO2 in
engine exhaust [34]. In this work a similar approach is adopted for an opacimter:
Using a multi-wavelength light source the individual contributions of soot and NO2
to the opacity are determined and the respective concentration values are derived.
For this purpose the extended opacimeter performs multiple consecutive mea-
surements of the smoke sample using different wavelengths. Any wavelengths for
which the extinction differs sufficiently could be used. Standard opacimeters are
equipped with a green light source. To support normal opacity measurements the
green light source can be retained and a red and blue light source added. The
according measurement setup is shown in Fig. 5. In each measurement i, where one
of the light sources is enabled at a time, the equation
8 H. Axmann et al.

Fig. 5 Three wavelength

measurement setup R detected signal
G led currents (particles + NO2)
B
t t
RGB led particles/NO2 RGB

reference measurement chamber detector

detector
430 mm

ki = kNO2 ðλi Þ + ksoot ðλi Þ + kother ðλi Þ ð6Þ

holds. Herein λi is the wavelength of each light source, kNO2 , ksoot , kother and ki are
the individual extinction coefficients of NO2, soot particles and other components
and the total extinction coefficient at the given wavelength λi respectively. The
equation can be rewritten as in (5) using the product of the concentrations cx and the
extinction cross sections σ x , leading to

ki = cNO2 σ NO2 ðλi Þ + csoot σ soot ðλi Þ + cother σ other ðλi Þ. ð7Þ

When performing three measurements of the same sample (i.e. the concentra-
tions cx remain constant during the whole measurement time) an equation system
with three equations and also three unknowns is obtained. This of course requires
knowledge of all extinction cross sections. In such a case, the matrix equation
0 1 0 10 1
k1 σ NO2 ðλ1 Þ σ soot ðλ1 Þ σ other ðλ1 Þ cNO2
@ k2 A = @ σ NO2 ðλ2 Þ σ soot ðλ2 Þ σ other ðλ2 Þ A@ csoot A ð8Þ
k3 σ NO2 ðλ3 Þ σ soot ðλ3 Þ σ other ðλ3 Þ cother

can ideally be solved by simple matrix inversion.

For σ other a representative absorber besides soot and NO2 should be chosen. In
practice the composition of the exhaust samples might vary to such a degree that the
selection of a single representative absorber is not possible. In that case it can be
omitted, leading to an over-determined system. Such a system can be solved using a
least-squares algorithm to calculate the best fit for the remaining two components.

5 Technical Realization

5.1 Physical Setup

The multi-wavelength opacimeter is built from the basis of a highly sensitive

single-pass opacimeter, as depicted in Fig. 5. In order to achieve a sufficiently high
Determination of NOX and Soot Concentrations Using … 9

sensitivity in the order of Δk = 0.001 m-1 the optical path length and hence the
measurement chamber should not be too small. We used a cylindrical cell with a
diameter of 2.4 cm and a length of 400 mm, where the axis of the cylinder coin-
cides with the optical axis of the system. The inlet for the smoke sample is placed in
the middle of the chamber. The exhaust is filled into the chamber by the dynamic
pressure in the exhaust pipe. It leaves the chamber through the in-/outlet for the
light beam.
A flow of sheath air transports the exhaust sample to the smoke outlet. The
sheath air flow is produced from ambient air by filtration using a high-efficiency
particulate air (HEPA) filter. On the one hand the sheath air protects the optical
setup from contamination, on the other hand it defines the length of the optical path.
As the optical path length directly influences the measurement value, it is crucial to
keep the optical path length constant. Therefore the sheath air flow needs proper
fluid dynamical considerations.
In Fig. 6 a multiphysical complex fluid dynamic simulation result is shown. The
ratio of exhaust gas entering through the middle section of the measurement cell to
the air flow rate through the sheath air channels defines the optical path. In order to
quantify a representative exhaust gas sample within the measurement cell, the
distribution of the analytes should be homogeneous, independently of the dynamic
pressure in the exhaust pipe. A proper fluid dynamic design and hence an iterative
optimization approach by means of complex fluid dynamics is a necessary pre-
requisite to obtain meaningful measurement results.
For the light source it is advantageous to use a realization that combines the three
colors into a single housing. That ensures comparable optical behavior of the

68.847
Particle velocity [m/s]

63.162
57.478
51.793
46.108
40.423
34.739
29.054
23.369
17.684
12.000
6.315
0.630

Fig. 6 Multiphysical complex fluid dynamic simulation of the measurement cell. The points
represent particle ensembles with particle velocities scaled by the color. A homogeneous velocity
distribution within the optical path guarantees representative samples of the exhaust gas portion to
be quantified
10 H. Axmann et al.

Fig. 7 Relative intensities of 1

the used multi-color LED
0.8

Relative intensity
0.6

0.4

0.2

0
400 450 500 550 600 650 700
Wavelength λ [nm]
Blue Green Red

different colors due to their proximity. To increase signal-to-noise ratio and reduce
the challenges for amplification on the receiver side, the light source should have a
high intensity. This is achievable with a commercially available high power LED,
like for instance the OSRAM LRTB. Its three dominant wavelengths are at 632,
523 and 455 nm for the red, the green and the blue color respectively (see Fig. 7).
The incident light is collimated by means of an aspherical lens (optical
parameters: d = 18 mm, f = 15 mm, bfl = 11.10 mm, Md = 6 mm), resulting in a
beam divergence of typically less than 8°. If needed the beam divergence can be
adapted by changing the distance between the lens and the LED.
On the receiver side an optical detector converts the incident light into the
electrical domain. For this purpose a PIN photodiode with a large optical area of
7 mm2 is used. A collimating lens, identical to the one on the transmitter side, is
placed in front of the photodiode, to maximize the incident intensity and overcome
losses due to misalignments produced by vibrations and shocks. As the measure-
ment signal is directly proportional to the source light intensity, a stable source is of
high importance. Nevertheless if fluctuations occur they can be compensated via a
reference photodiode, measuring the current source intensity.

5.2 Electronic Measurement Circuitry

The optical measurement principle is based on the attenuation of light in the

measurement chamber. An absence of particles or light absorbent gases corresponds
to a full scale reading at the optical receiver. As a consequence, any gain or offset
error/drift of the optical measurement directly and significantly influences the
reading.
Determination of NOX and Soot Concentrations Using … 11

Numerical post-processing involves the subtraction of the actual optical output

level from the reference output level and scaling this difference by the appropriate
sensitivity coefficient. Both resolution and accuracy of the optical detector, its
associated transconductance amplifier and the analog-to-digital converter
(ADC) have to be adequately high, such as to compensate for the loss of significant
digits in the following calculations.
The opacity as a ratio of I ̸I0 is a dimensionless quantity, which naturally sug-
gests a fully ratiometric measurement setup. Second order effects would still have
an influence, such as gain and offset errors of the amplifiers or nonlinearities of the
ADC. However, these can be kept well within allowable limits by careful circuit
design.
Figure 8 shows an idealistic approach of a fully ratiometric light absorption
measurement setup. The light emitted by the LED at the transmitter side is divided
into two paths: The first illuminates the measurement cell containing the analyte,
the second serves as a reference. An optical multiplexer at the receiver side alter-
nately lets one of the two signals pass to the optical receiver diode. Errors related to
the electronic instrumentation would largely cancel out, since the measurement and
reference phase use the same optical detector and signal conditioning circuitry.
Some nonlinearity would still remain, in the first instance related to the ADC.
Such an approach is not feasible for some reasons: the mechanical construction
including the optical multiplexer is costly and moderately reliable, and both the
optical transmitter and the optical receiver have a linear relationship between optical
power and electrical current, not voltage. In contrast, the electrical signal condi-
tioning is based on a reference voltage. It is the reference for the ADC at the
receiver side and the digital-to-analog converter (DAC) for adjusting the LED

exhaust sample

TX RX
LED photodiode

measurement path
ITX IRX

Transmitter Receiver
optical reference path
side side

reference
I

measurement

0 t

Fig. 8 Ideal approach of a fully ratiometric light absorption measurement

12 H. Axmann et al.

power at the transmitter side. As a consequence, at least two precision resistors are
needed: one is part of the voltage controlled current source for the transmitter LED,
another one is part of the transimpedance amplifier, converting the current output of
the photodiode into a voltage output for the ADC.
Figure 9 represents the actual setup. The electronic instrumentation relies on the
ratiometric principle to a great extent. A set of two identical optical receivers
replaces the optical chopper of Fig. 8, each one including its dedicated tran-
simpedance converter. A total of three precision resistors (RREF, TX , RREF, RX, 1 and
RREF, RX, 2 ) are required, which is acceptable because these parts are available with
excellent specifications for tolerance, temperature coefficient and long-term
stability.
The optical output power of the LED correlates with its forward current. It is
adjusted by the setting of the DAC, its reference voltage and the transconductance
of the voltage controlled current source. A digital control loop, implemented in the
firmware of the microcontroller, uses the output voltage VRX, 2 of the optical ref-
erence path to set the LED current ITX and keep it at the desired set level.
At the receiver side there are two photodiodes, each with its dedicated tran-
simpedance amplifier for the current-to-voltage conversion. A critical part for the
overall performance of the measurement setup is the matching of the optical
receivers and their interface electronics. The photodiodes operate in current (short
circuit) mode. Their light-to-current transfer ratio is therefore highly linear over
several decades of intensity. Thermal influences are low and further reduced by
keeping both photodiodes at the same temperature.
The influence of dark current and bias currents at the receiver side are com-
pensated by a reference measurement with the transmitter LED turned off. Minor
deviations are canceled out by digital post processing; abnormally high deviations
indicate a fault situation and are handled by self-diagnostic functions.

REF
RREF,RX,1 voltage
exhaust sample

VRX,1
V+
REF IRX,1
voltage RREF,RX,2 ADC
measurement path
ITX
DAC
optical reference path VRX,2
Voltage IRX,2
micro- RREF,TX controlled
micro-
processor current source
processor
control VCTL (transconductance Photo detectors & control
amplifier) transimpedance amplifiers

Fig. 9 Actual measurement setup

Determination of NOX and Soot Concentrations Using … 13

5.3 Mathematical Model

The measurement setup provides three extinction coefficients, each for one of the
three used wavelengths λi . Equation (8) provides the equation system for deter-
mining the concentrations of three absorbing species from such a measurement. As
mentioned above there is generally no exact solution for this equation system.
Furthermore the third typical absorber in addition to soot and NO2 can often not
easily be identified. We therefore use the reduced equation system
0 1 0 1
k1 σ NO2 ðλ1 Þ σ soot ðλ1 Þ  
@ k2 A = @ σ NO2 ðλ2 Þ c
σ soot ðλ2 Þ A NO2 , ð9Þ
csoot
k3 σ NO2 ðλ3 Þ σ soot ðλ3 Þ

which focusses on the two criteria pollutants particles and NO2. In the discussion
section we will show that this generally delivers good results for diesel engine
exhaust.
The concentrations can be determined from (9) by inversion. This can be most
easily achieved by multiplication with the pseudo inverse

A + = ðAT AÞ − 1 AT , ð10Þ

where A denotes the cross section matrix and AT its transpose. It will yield the best
fit for the solution in a least squares sense.
The cross section values σ x ðλi Þ for NO2 and soot can be taken from Figs. 3 and 4
respectively, as long as monochromatic light sources are used. The graphs however
use different units for the cross section values. So a conversion of one of the cross
sections to the unit of the other one is needed. We chose to use the unit m2/g and
converted the cross section for NO2 as follows:
     
m2 1 cm2 NA molecules ̸mol
σ NO2 = 4 σ NO2 ð11Þ
g 10 molecule MNO2 g ̸mol

Herein MNO2 = 46.005 g/mol is the molar mass of NO2 and NA = 6.022
1023 molecules/mol is the Avogadro constant.
Since we use a LED as a light source, the single colors are clearly not
monochromatic. In this case the corresponding nominal intensities I0 at the
wavelengths λi have to be replaced by continuous nominal intensity spectra I0 ðλÞ
from Fig. 7, where at each wavelength λ (2) holds:

IðλÞ = I0 ðλÞexpð − kLeff Þ ð12Þ

On the detector the single intensities IðλÞ are integrated with respect to the
spectral efficiency γðλÞ of the detector:
14 H. Axmann et al.

Z Z
I= γðλÞIðλÞdλ = γðλÞI0 ðλÞexpð − kLeff Þdλ ð13Þ

The total nominal light intensity I0 can be calculated accordingly. By relating

̄ i Þ can be determined, as before, for each
I and I0 a mean extinction coefficient k ðλ
color λi :
R
̄ i ÞLeff Þ = γðλÞI0 ðλÞ
expð − k ðλ R
expð − kðλÞLeff Þdλ
ð14Þ
γðλÞI0 ðλÞdλ

In order to set up the equation system, the extinction coefficient is again replaced
by the product of cross section and concentration, now denoted as σ x ðλi Þ and ĉ
respectively. However in the case of a polychromatic light source the strict pro-
portionality does not hold for the mean values. This is obvious from the following
equation:
R
γðλÞI0 ðλÞexpð − cσ x ðλÞLeff Þdλ
expð − ĉσ x ðλi ÞLeff Þ = R ð15Þ
γðλÞI0 ðλÞdλ

Despite the limited proportionality the model in (9) provides a good approxi-
mation to the real behavior, as shown by the simulations in the following discussion
section.

6 Results and Discussion

The multi-wavelength approach has been evaluated using simulations and basic
measurements. The results are presented and discussed in the following sections.

6.1 Sensitivity Measurements

Our first measurements have been performed with a new, highly sensitive
opacimeter, to ensure that reliable measurements of the extinction produced by NO2
are possible even at low concentrations. The opacimeter was equipped with a single
color light source (green light with Gaussian intensity spectrum, μ = 560 nm,
σ = 8 nm). The resolution was 0.001 m-1. The results are shown in Fig. 10.
Conforming to theory the measured extinction value is linearly related to the
NO2 concentration. The smallest resolvable NO2 concentration is in the order of
10 ppm. Compared to simulations the measured extinction coefficient is a bit lower.
The simulated value at 1000 ppm was approximately 0.2 m-1, whereas the
Determination of NOX and Soot Concentrations Using … 15

Fig. 10 NO2 measurements 0.12

with a new opacimeter

Extincion coefficient k [1/m]

0.1

0.08

0.06

0.04

0.02
Measurement
Linear fit
0
0 200 400 600 800 1,000
NO2 concentration [ppm]

measured value is 0.12 m-1. The deviations can probably be attributed to different
ambient conditions (pressure and temperature).

6.2 Mathematical Simulations

The simulations have been performed in MATLAB using the model from (9) with
the cross section spectra presented in Figs. 3 and 4. Combinations of NO2 at
concentrations from 100 to 1000 ppm and soot particles at concentrations from 1 to
1000 mg/m3 have been tested. The results for the estimation of the NO2 concen-
tration from the simulated values are depicted in Fig. 11 for the noise-free case in
the form of the relative deviation from the actual concentration.

Fig. 11 Error in calculated

NO2 concentrations
(simulation without noise)

1.5
NO2 error [%]

0.5
1
0 10
20
0 5
10 00 10 0
2 00
3 00 20 0
4 00 40 0
5 00
6 00 60 0
80 0
NO2 concentration 7 800 00 10
00
0 soot concentration
9 00
[ppm] 10 [mg/m3]
16 H. Axmann et al.

Fig. 12 Mean error in 10 0

calculated NO2 and soot
concentrations (simulation
with 1 % of noise)

Mean relative error ε

10 1

10 2

NO2
soot
10 3
10 −2 10 −1 10 0 10 1 10 2 10 3
Cross section ratio σsoot(λg)/σNO2(λg)

For most combinations the error is below 1 %. Only if the contribution of one
component is very low, e.g. 100 ppm of NO2, the error can increase to almost 2 %.
The reason for this error in the noise-free system is the limited proportionality due
to polychromatic light. Consequently the systematic error can be reduced, when
light sources with a narrow wavelength spectrum or quasi-monochromatic light
sources like lasers are used.
If noise is applied the errors generally rise to a few percent. The relative error for
1 % of noise is depicted in Fig. 12. Larger errors between 10 % to 40 % for the NO2
concentrations are only found when the contribution of soot is at least twenty times
higher than that of NO2. Solely if the share of NO2 is smaller than 1/100 and hence
negligible the mean error rises above 40 %. For the particle concentration small
errors below 2.5 % can be achieved for all combinations where csoot ≥ 10 mg/m3.

6.3 Discussion

Both preliminary measurements and simulations indicate a good applicability of the

described multi-wavelength approach. Further measurements are planned for the
future to investigate the performance on both laboratory mixtures of particles and
NO2 and real-world exhaust samples.
As our measurements have shown so far, it is advantageous to perform cali-
bration measurements to acquire the cross section matrix for concentration mea-
surements. The simulations can be a great tool for evaluating the method in theory
but may result in somewhat deviating numbers.
With a calibration based on practical measurements we except good results for
the determination of the concentrations of NO2 and particles, as long as they are the
Determination of NOX and Soot Concentrations Using … 17

primary contributors to the extinction. Other strong absorbers present in the exhaust
sample might lead to deteriorated results. For diesel exhaust this is a rare case.
Known examples of additional absorbers are white and blue smoke. White smoke,
produced by condensed water, can be eliminated by proper conditioning of the
engine prior to the PTI and by heated sample lines. By keeping the exhaust tem-
perature above the due point of exhaust gases, which is in the area of 45–55 °C
[14], water is hindered from condensing. When using a temperature above 100 °C
already condensed droplets can be evaporated again. Blue smoke is typically related
to an engine defect. It can occur for instance, if oil leaks into the cylinder [35–38].
If required, such hydrocarbon emissions can be eliminated by integration of an
oxidation catalyst (“catalytic stripper”) into the heated sample line [39]. Hence,
when implementing such measures, an overall good applicability to real engine
emissions can be assumed.
For the real-world exhaust samples comparison measurements with dedicated
NO2 sensors are planned to gain insights into the quality of the measurement
results. Although such dedicated devices will of course yield more accurate results
[40], the proposed method can provide at least valuable qualitative results without
the need for extra measurement equipment. Furthermore little or no additional
conditioning of the exhaust sample is needed in comparison to a standard
opacimeter. Finally the main functionality of the opacimeter, i.e. measuring the
exhaust opacity, is not degraded in any way.

7 Conclusion

Emission regulation covering the whole lifetime of vehicles is a key for a clean and
healthy environment. Two of the main pollutants of combustion engines, namely
soot and nitrous oxides, depend strongly on the state of health of the combustion
engine as well as of the exhaust aftertreatment system. Within this chapter a novel
method for the simultaneous determination of NO2 and soot in the exhaust of diesel
engines with emphasis on periodical technical inspection (PTI) was elaborated in
detail. It is based on a spectroscopic multi-wavelength light extinction measurement
in a setup similar to an opacimeter with high sensitivity. Preliminary experimental
results have proven its ability to reliably detect small concentrations of NO2 with a
limit of detection (LOD) as low as 10 ppm. The experimental research with the
focus on the simultaneous determination of the second pollutant soot is ongoing.
The overall results are promising and indicate the potential to gain further infor-
mation on the pollutants contained in exhaust without the need for an additional
dedicated sensor in PTI applications.
18 H. Axmann et al.

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Development of the Atomic Emission
Spectroscopy System Using
Helium-Microwave-Induced Plasma
for Fine Particles on Environmental
Monitoring

Satoshi Ikezawa, Jun Yamamoto and Toshitsugu Ueda

Abstract This chapter describes the elemental analytical technique of the fine
particles using atomic emission spectroscopy system for an environmental pollution
monitoring. Based on our previous measurement reports, differences of the usage
between the laser-induced breakdown spectroscopy (LIBS) system and the
helium-microwave-induced plasma-atomic emission spectroscopy (He-MIP-AES)
system are explained. Both systems were developed to allow to fulfil the criteria
prescribed by the Ministry of Environment, Japan, for measuring the chemical
components of particulate matter (PM) by introducing additional original sampling
systems. In current environmental monitoring systems, PMs are typically collected
on trapping filters placed across Japan and classified as either suspended particulate
matter (SPM) or PM2.5 depending on the size. The collected PMs are subsequently
analysed with automated measurement instruments such as a piezo balance and
with methods such as beta ray attenuation and light scattering. While these mea-
surement methods allow the mass concentration of PMs in the air to be obtained at
hourly intervals, the chemical composition of individual particles is analysed with
time-intensive laboratory procedures. In contrast, the LIBS and He-MIP-AES
measurement system allow the chemical compositions and particle sizes to be
measured simultaneously in real time.

1 Introduction

Recently, regional atmospheric environment issues around Japan have produced an

increase in particulate matter (PM), which is considered to be a transboundary
pollutant [1]. While domestically produced PM that is less than 2.5 µm in size

S. Ikezawa (✉) ⋅ J. Yamamoto ⋅ T. Ueda

Graduate School of Information Production and Systems, Waseda University,
Kitakyushu, Japan
e-mail: [email protected]

© Springer International Publishing AG 2017 21

S. Mukhopadhyay et al. (eds.), Sensors for Everyday Life, Smart Sensors,
Measurement and Instrumentation 23, DOI 10.1007/978-3-319-47322-2_2
22 S. Ikezawa et al.

(PM2.5) has been reported to be decreasing in cities [2], high concentrations of

PM2.5 that exceed the allowable limits set by the Ministry of Environment, Japan,
have been frequently observed in the western parts of the country. This PM is
considered to be transported through diffusion by the westerlies. The inhalation of
fine PM is known to cause a range of health problems [3–6]. PM2.5 can penetrate
the gas-exchange region of the lungs. Thus, information on the size of particulates
(e.g., distinguishing particulates based on size) is as important as information on
their elemental components and density. However, it is difficult to obtain real-time
information on the size and composition of nano-sized suspended particulate matter
(SPM) simultaneously. The beta-ray absorption system is the most commonly used
automatic measuring instrument for SPM in Japan. The main advantages of the
beta-ray absorption method are that the mass absorption coefficient is constant with
regard to the particulate composition, the method does not require frequent cleaning
like the piezo balance-type dust monitoring method, and it does not require standard
calibration steps that use a reference material like the light scattering method.
However, recent attention has been focused on designing environmental monitoring
systems that can detect particulates smaller than 2.5 µm. In order to meet the
requirement of being able to measure the chemical composition of fine particulates
in real time, we developed and proposed a laser-induced breakdown spectroscopy
(LIBS) system, laser-induced incandescence (LII) and helium-microwave-induced
plasma-atomic emission spectroscopy (He-MIP-AES) measuring system for envi-
ronmental monitoring [7–13]. The LIBS is a useful tool for determining the ele-
mental composition of various materials, and it does not require any chemical or
physical preprocessing steps. However, because the entire volume of the
laser-irradiation area is broken down without individually resolved particles, the
LIBS technique is not sufficient for obtaining information on specific particulate
sizes, just on the intensity value. The quantitative values obtained by LIBS only
relate to the total volume of particulates per unit volume; in other words, these
values relate to the weight/volume density. To overcome the weakness of the LIBS
system for fine particle quantitative measurement, the LII technique was introduced.
The most salient feature of the combined LIBS and LII system is its ability to
perform real-time measurements with noncontact and nonguiding particulates into
the measurement spot. He-MIP-AES system allows a larger and continuous volume
of atmospheric gases to be measured compared to LIBS and LII. The radiofre-
quency (RF) of a capacitively coupled plasma (CCP) operating at various fre-
quencies has long been used as an excitation source for analysis by optical emission
spectrometry (OES) [14–17] since Cristescu and Grigorovici experimented on the
discharge produced by the application of the output of a high-frequency oscillator to
two circular plates in 1941 [18]. Microwave-induced plasma (MIP) is formed in a
discharge tube placed in a cavity to which power is transmitted via a coaxial line
[19]. MIP supported by an inert gas has been applied as a versatile selective OES
detector in gas chromatography [20, 21]. Argon or helium is preferred as the plasma
support gas because of the absence of molecular background spectra. In typical
OES analysis like inductively coupled plasma (ICP), argon gas is frequently used
because argon plasma is more stable under atmospheric conditions or when the
Development of the Atomic Emission Spectroscopy System … 23

measurement sample is wet than helium plasma. However, helium is the ideal
support gas because the organic compounds eluted from the gas chromatograph are
then almost completely atomized in the plasma, which produces a line emission
spectrum. In contrast to the Ar-ICP system, the He-MIP-AES system employs
helium as the ionized gas for excitation. The metastable level of helium (19.8 eV) is
greater than argon (11.5 eV), and its high excitation energy allows the analysis of a
wide range of elements, including high-energy ionizing elements such as the
halogen family.

2 Motivation

With the rapid growth and industrialization of Asia’s economy, fossil fuel emis-
sions from factories, power plants and automobile are emitting into the atmosphere.
For preventing growing aerosol pollution and global climate change problems,
numerous organizations are actively involved in research programs for the
development of processes that utilize biodiesel sources. It is known that a diesel
engine is more fuel efficient than a gasoline engine, and further, electronically
controlled common-rail injection contribute to clean burning. Hence,
cleaner-burning engine often produce smaller soot; nanosized particles as a
byproduct. It is well known that inhalation of fine particle matter causes several
health problems. Particles that are smaller than 2.5 μm in size (PM2.5) can pene-
trate the gas-exchange region of the lung. However, it is difficult to obtain the size
and composition information of the fine particles in real time. We have developed
and conducted experiments using following measuring methods to overcome the
difficulty. Laser-induce breakdown spectroscopy (LIBS) is one of the useful
methods for the determination of the elemental composition of the fine particles.
Our research group has been developing LIBS techniques that have potential
applications in various fields. However LIBS itself is not enough to obtain the
particle size information. Figure 1 shows photograph of the MEMS fabrication
room and SEM images of the particles deposited on Si membrane porous filter
which gathered in the clean room.
Figure 2 illustrates for one example of the reason why LIBS particle size
measurement with the range smaller than laser spot size is hard to do. In case LIBS
measurement are conducted for fine particles, we only know the plasma intensity
information. Because of the intensity means total amount of the particles, it may be
only one particle, otherwise the plasma emission irradiated from number of
particles.
Based on the requirement for particle size information, we applied laser-induced
incandescence (LII) technique with LIBS. In previous our researches, the LII decay
simulation model was based on one of the most detailed studies provided by
Michelsen [22] (Fig. 3).
24 S. Ikezawa et al.

Fig. 1 Fine particles in the air and disadvantage of LIBS measurement

Fig. 2 Difficulty of the particle size information detection on LIBS measurement

When using the LII technique, laser pulse was irradiated on particles then
thermal radiation was recorded. LII technique is based on the analysis of cooling
behaviour of particles after irradiation with the laser pulse. By using
Stefan-Boltzmann law for a black body, the LII signal; profile of the intensity decay
time depending on the particle size. Figure 4 shows solution algorism to obtain the
LII signal as a function of time-temperature curve.
Development of the Atomic Emission Spectroscopy System … 25

Fig. 3 Difference of the radiation cooling time associated with the radiation rate as a function of
surface to volume ratio

Fig. 4 Solution algorism to obtain the LII signal as a function of time-temperature curve

According to the Michelsen’s model, the energy balance for the interaction of a
particle with laser is given by

QInt = Qabs − Qrad − Qcond − Qsub + Qann + Qox ð1Þ

where QInt represents the sensible energy storage in particle, Qabs is the rate of the
laser energy absorption, Qrad is the radiation rate by blackbody emission, Qcond
represents the energy dissipation rate by conduction, Qsub represents the rate of
energy loss by sublimation of carbon clusters and accounts for the energy con-
sumption during photodesorption of the annealed particle to form small carbon
clusters, Qann represents the energy production rate by particle annealing, and Qox
represents the energy generation rate by oxidation. Each terms of this energy flow
26 S. Ikezawa et al.

rate equation were accounted for by laser beam temporal intensity profile, time
dependence of the particle temperature, and initial states of the particle.
Time-derivative term of the particle temperature yields

dT 6
= ðQ − Qrad − Qcond − Qsub + Qann + Qox Þ ð2Þ
dt πD3 ρS cS abs

where T is the particle temperature, D is the primary particle diameter, ρs is density

of the particle cs is specific heat of solid carbon.
From Planck equation from blackbody, LII signal at wavelength λ′ is given by
Z
2πhc2
S = ΩπD2 ελ h   i Σλ ðλ′ Þdλ′ ð3Þ
′5
λ λ exp λ′ k T − 1
hc
B

where Ω is normalization constant, ελ is emissivity at wavelength λ for a Rayleigh

particle, h is Planck constant, c is speed of light, kB is Boltzmann constant, Σλ is
accounted for by including it in the integration of the Plank function over wave-
length. Solving the differential Eq. (2), each terms of energy flow ratio were cal-
culated from the laser beam intensity profile which obtained from actual
measurement.
Particle size measurement had been successfully accomplished with the help of
LII technique on our LIBS system. Despite the good agreement between calculation
and measured temporal profiles, calibrations using several size of particle are
required for the correction to the real particle size.
In our latest research, new measuring device using He-MIP-AES technique was
additionally introduced [13]. He-MIP-AES system allows a larger and continuous
volume of atmospheric gases to be measured compared to LIBS and LII.

3 Device Designs

A. LIBS and LII Analysis Method

Figure 5 represents the schematic of the LIBS and LII system. When using the
LIBS technique, a higher energy laser pulse was focused on particles to create
plasma then atomic specific emissions were dispersed by spectrograph and then
recorded with a streak camera by separating from predomination of bremsstrahlung
spectra. When using the LII technique, unfocused laser pulse was irradiated on
particles then thermal radiation was dispersed by spectrograph and then recorded
with a streak camera.
Development of the Atomic Emission Spectroscopy System … 27

Delay/pulse
Streak camera generator
Spectrograph

Condenser lens PC

Nd:YAG laser
Particle sample

Fig. 5 Schematic of the LIBS and LII combination system

Fig. 6 Schematic of the MIP system using Beenakker cavity and two-way spectroscopic analysis
system
28 S. Ikezawa et al.

B. He-MIP-AES Method
Figure 6 shows a schematic of the MIP system. The He-MIP-AES system is a
reconstruction of an existing particle analyzer system (PT1000, Yokogawa Electric
Co., Tokyo, Japan) [23]. The He-MIP system utilizes microwaves with a frequency
of 2.45 GHz in TM010 mode. The microwaves are introduced into a Beenakker-type
cylindrical cavity resonator. Electromagnetic energy at 70–200 W is condensed at
the quartz discharge tube, which is set at the center of the cavity. The plasma
stability depends on the temperature stability of the cavity. In order to keep the
cavity temperature at 20 °C, a laminar airflow at 20 L/min is formed on the surface
of the discharge tube for cooling, and a Peltier device is attached to the discharge
tube for fine control. Preventing the introduction of other gases into the cavity is
also important for plasma stability. Helium gas is introduced to the sampling
introduction system at 45 ± 10 mL/min and to the aspirator at 300 mL/min for
optimal operation. Contaminating gases lead to shrinking of the plasma and elec-
tromagnetic polarization. This may cause insufficient plasma processing of the
samples, which may lead to failure of the quantitative analysis from the matrix
effect, molecular ion effect, and quenching phenomenon. In order to maintain
plasma purity, special techniques need to be carefully applied to collecting samples
and introducing particulates. Therefore, the particle is exposed under a helium
atmosphere at the sample introduction area of the system.
The particle is then aspirated with helium gas, and the aggregate is unpacked at
the point of the inflow area into the fast-flowing helium gas. Considering the location
and velocity of the sample particles, the fastest helium flow of the centre axis for the
cylinder (inner diameter is 3.5 mm) reaches 1.108 m/s. The flow velocity at the
centre is twice the average flow speed at a 300 mL/min flow rate. This means that the
minimum transit time of particles inside the helium plasma over a distance of 10 mm
is about 9 ms. The minimum transit time requires the optical system to measure each
particle within 9 ms. The optical system employs an originally designed switching
module to detect particles in order to reveal their chemical composition at high
sensitivities (0.33 nm resolution) or to detecting particles with unknown chemical
compositions over broad wavelength ranges (250–680 nm, 3.3 nm resolution). The
optical system for the plasma emission spectrum combines a monochromator and
photomultiplier; these are used in the high-sensitivity detection mode. In the
high-sensitivity mode, the wavelength of the spectrum peak should be a narrow band
around a known spectral line when presetting the photomultiplier. The intensity
signal of the plasma emission produced from each particle is converted to the third
root value by the electrical circuit to obtain a diameter-equivalent value. When
detecting the chemical composition of the particles, a multi-channel spectrometer is
used, and the spectra are recorded with the charged-coupled device (CCD) array.
The trigger signal output has a delay at the oscilloscope of 20 ns. The CCD requires
8–9 µs to reset its operation and 1.9 ms to process data. Thus, if the gate time of the
spectrometer is 1 ms, one measuring cycle takes 2.909 ms (344 Hz). The system
operation time is clearly within 9 ms.
Development of the Atomic Emission Spectroscopy System … 29

4 Calibration and Evaluation

A. Wavelength Calibration of Monochromator

Wavelength calibration tests of the monochromator were conducted by using a
mercury lump with several spectrum wavelengths: 253.65, 313.16, 365.02, 435.84,
and 546.07 nm. In these calibration tests, the measurement scanning direction was
set from both wavelength sides to find the backlash effect between turning table
gears. The results are shown (Figs. 7, 8, 9, 10, and 11).
These experimental results for the monochromator indicate that spectrum peek
data obtained both direction have a certain of error toward true value, and these
error difference at comparable level means that the backlash had almost no effect at
these calibration wavelengths. Figure 12 shows the peak shift trend toward the
measured wavelength. It shows that the monochromator had a margin of error for
the wavelength of ±0.3 nm, and the peak shift showed a linear trend toward the
wavelength. Thus, the calibration curve allowed the correct value to be obtained in
actual measurements.

Fig. 7 Measurement results 15

at 253.65 nm wavelength
Output voltage [V]

From shorter
wavelength side
10
From longer
wavelength side
5
Calibration
wavelength

0
253.2 253.3 253.4 253.5 253.6 253.7 253.8 253.9 254.0 254.1 254.2
Wavelength [nm]

Fig. 8 Measurement results 0.5 From shorter

at 313.16 nm wavelength wavelength side
Output voltage [V]

0.4
From longer
0.3 wavelength side

Calibration
0.2 wavelength

0.1

0
312.6 312.7 312.8 312.9 313.0 313.1 313.2 313.3 313.4 313.5 313.6
Wavelength [nm]
30 S. Ikezawa et al.

Fig. 9 Measurement results 0.7

at 365.02 nm wavelength From shorter
0.6 wavelength side

Output voltage [V]

From longer
0.5 wavelength side
0.4 Calibration
wavelength
0.3
0.2
0.1
0
364.5 364.6 364.7 364.8 364.9 365.0 365.1 365.2 365.3 365.4 365.5
Wavelength [nm]

Fig. 10 Measurement results 1

at 435.84 nm wavelength From shorter
Output voltage [V]

0.8 wavelength side

From longer
0.6 wavelength side

0.4 Calibration
wavelength
0.2

0
435.4 435.5 435.6 435.7 435.8 435.9 436.0 436.1 436.2 436.3 436.4
Wavelength [nm]

Fig. 11 Measurement results 0.6

at 546.07 nm wavelength From shorter
Output voltage [V]

0.5 wavelength side

0.4 From longer

wavelength side
0.3
Calibration
0.2 wavelength

0.1
0
545.6 545.7 545.8 545.9 546.0 546.1 546.2 546.3 546.4 546.5 546.6
Wavelength [nm]

B. Equivalent Grain Size Identification

To evaluate the performance of the MIP system for quantitative particle size
analysis, the particle size was identified from the output intensity signal. Spherical
and uniform-size silicon dioxide particles were used as standard particles of a
known size (Fig. 13).
Development of the Atomic Emission Spectroscopy System … 31

Fig. 12 Peak shift trend 0.3

Peak wavelength shift

toward measurement
0.2
wavelength
0.1

[nm]
0
-0.1
-0.2
-0.3
200.0 300.0 400.0 500.0 600.0
Wavelength [nm]

Fig. 13 Silicon dioxide

standard particles

Four particle sizes (diameter: 2.5, 5.0, 10, and 20 µm) were used in the exper-
iment (Table 1). For conversion to the size of a pure silicon particle, the conversion
factor from the silicon dioxide particle was set to 0.7615 based on the volume
fractions of the constituent elements. The detection wavelength for silicon was set
to 288.18 nm.
C. Introduction of Intensity Correction Factor for Other Elements
The equivalent particle diameter D has a proportional relationship to the output
voltage of the third root amplifier V. However, the intensity correction factor K for
other elements with different wavelengths should be as given in (4) b
ased on previous research works [23].

D = KV ð4Þ

Table 1 Experimental results for output voltage at greatest frequency of third root amplifier and
particle diameter
Particle diameter variation
SiO2 (µm) 2.5 5.0 10.0 20.0
Si (µm) 1.9 3.8 7.6 15.2
Output voltage of third root amplifier (V) 1.7 3.8 7.5 14.7
32 S. Ikezawa et al.

D. Limit of Detection
The limit of detection (LOD) for a particle size in the system is defined according
to the relative intensity of the atomic spectrum (intensity correction factor) and the
ground noise level. Table 2 presents a reference chart for several elements.

Table 2 List of correction factors and LOD

Element Selected spectrum Intensity correction Noise level (V) He-MIP-AES
wavelength (nm) factor K LOD of particle
size (µm)
Si 288.18 1 0.76 0.98
Ag 328.07 0.270 0.66 0.23
Al 396.15 0.622 0.63 0.51
As 234.98 0.276 0.58 0.21
Au 267.60 0.360 0.65 0.30
B 294.77 0.421 0.62 0.34
Ba 493.41 0.355 0.59 0.27
C 247.86 0.631 0.51 0.42
Ca 393.37 0.103 2.47 0.33
Ce 401.24 1.550 0.61 1.24
Cl 479.45 2.494 0.23 0.75
Cr 520.84 0.426 0.60 0.33
Cu 324.75 0.293 0.70 0.27
F 685.60 4.704 0.54 3.28
Fe 238.20 0.257 2.63 0.88
Ga 294.36 0.158 0.67 0.14
K 766.49 1.905 0.50 1.25
Mg 285.21 0.278 0.84 0.30
Mn 293.31 0.492 0.70 0.45
Mo 277.54 0.483 0.65 0.41
N 744.26 2.450 0.50 1.58
Na 588.99 0.274 0.58 0.21
Ni 341.48 0.482 0.65 0.41
P 255.33 0.529 0.63 0.43
Pb 405.78 0.167 4.32 0.94
S 527.89 2.849 0.59 2.19
V 298.88 0.415 0.73 0.39
W 400.87 1.448 0.62 1.18
Zn 334.50 0.327 0.69 0.29
Zr 343.82 0.533 0.69 0.48
Development of the Atomic Emission Spectroscopy System … 33

5 Measurement and Analysis of Suspended Particles

in Atmosphere Using MIP System for Environmental
Monitoring

The measurements was taken on the rooftop deck of a building at our university
campus in Kitakyushu, Japan. The height of the roof top deck is about 10 m from
the ground. Suspended particles were collected over a 7-h period from 10:00 to
17:00 with a flow rate of 5 L/min and deposited on a filter with a pore diameter of
0.4 µm.
Figure 14 shows the premeasurement plasma spectrum of the He-MIP system
with a multi-channel spectrometer being used for wide-range spectrum finding.
Besides the helium carrier gas (He), hydrogen (H), oxygen (O) and hydroxyl radical
(•OH) were also observed. This is because of the measurement was conducted
under atmospheric pressure conditions, and moisture in the air or adhering to the
inner tube wall was introduced.
The measurement results for particles suspended in air using the He-MIP-AES
instrument are reported in Figs. 15, 16, 17, and 18. These figures show the event
number of plasma emissions with respect to individual particle sizes for elemental

Fig. 14 Plasma spectrum of He-MIP system using multi-channel spectrometer without measured
particles
34 S. Ikezawa et al.

Fig. 15 Counts of particles greater than 5 µm in size for elemental signals obtained from plasma
spectral emissions

Fig. 16 Counts of particles greater than 2 µm and less than 5 µm in size for elemental signals
obtained from plasma spectral emissions

signals classified by the equivalent grain size diameter D. The diameter was derived
from the output voltage of the third root amplifier with an intensity correction
factor.
Development of the Atomic Emission Spectroscopy System … 35

Fig. 17 Counts of particles greater than 1 µm and less than 2 µm in size for elemental signals
obtained from plasma spectral emissions

Fig. 18 Counts of particles less than 1 µm in size for elemental signals obtained from plasma
spectral emissions
36 S. Ikezawa et al.

6 Conclusions

Suspended particle measurement was demonstrated using the He-MIP system with
two-way spectroscopic analysis. The measurement results can be explained as
follows. For the particles with a diameter of over 5 µm, silicon (Si) was the most
often observed element followed by carbon (C) and potassium (K). For particles in
the size range of 2–5 µm, Si was the most often observed element followed by C,
K, zinc (Zn), iron (Fe), magnesium (Mg), and boron (B). In the size range of 1–
2 µm, C was the most often observed element followed by Fe, B, Si, sodium (Na),
phosphorus (P), Mg, zirconium (Zr), Zn, molybdenum (Mo), aluminum (Al),
nitrogen (N), silver (Ag), and manganese (Mn). Nanoparticles with diameters in the
sub-micrometer range were also detected. A large number of elements were
detected, e.g., Fe, Mg, Zn, B, C, Au, chromium (Cr), Na, copper (Cu), calcium
(Ca), Mo, chlorine (Cl), Ag, arsenic (As), vanadium (V), Si, Mn, lead (Pb), and
gallium (Ga). The results obtained with the He-MIP system confirmed that the
nanoparticles contained rare and precious metals that are not produced around the
location where measurements were conducted. This indicates that many of the
nanoparticles were either related to industrial activities or had been transported over
several thousands of kilometers. While primary particles remain suspended for a
few days and then diffuse over several kilometers, secondary particles remain in
suspension for a few weeks to a few months. Thus, it was inferred that the measured
nanoparticles had undergone reactions, in contrast to other micro-sized particles,
over repeated cycles of aggregation and disaggregation. The above method allows
the sizes and chemical compositions of the PM to be detected simultaneously; this
may aid in gaining an understanding regarding the interactions between yellow sand
and nanoparticles and the adhesive properties of carbonaceous materials in terms of
nanoparticles deposited on micro-sized particles.

Acknowledgment We are grateful to JGC Catalysts and Chemicals Ltd. for providing us with
silicon dioxide particles.

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Real-Time HVAC Sensor Monitoring
and Automatic Fault Detection System

Ying Guo, Josh Wall, Jiaming Li and Sam West

Abstract Real-time monitoring of heating, ventilation, and air conditioning

(HVAC) systems is crucial to maintaining optimal performance such as providing
thermal comfort and acceptable indoor air quality, guaranteeing energy saving, and
assuring system reliability. In a realistic situation, HVAC systems can degrade in
performance or even fail due to a variety of operational problems, such as stuck
open or closed air dampers and water valves, supply or exhaust air fan faults, hot or
chilled water pump faults, and inefficiencies in the way HVAC systems or pieces of
equipemnt are controlled. This paper presents automatic fault detection techniques,
as well as a key sensor sets selection approach that can help to maintain the
performance of HVAC systems, and optimise fault detection results. One key step
to make sure the approach succeeds is the sensor feature selection process. This
paper implements the ensemble rapid centroid estimation (ERCE) as the data-driven
sensor and feature selection algorithm, which is the core method to assure the
automatic fault detection can function correctly. Instead of choosing sensors
manually, ERCE method can automatically select representative features that are
unique and relevant to the faults in a HVAC system. The methodology presented is
implemented in real-world commercial buildings with experimental results showing
that different types of faults are detected successfully.

1 Introduction

Heating, ventilation, and air conditioning (HVAC) systems are designed to provide
thermal comfort and acceptable indoor air quality in a range of commercial buildings
[1]. HVAC systems consume a large amount of energy throughout the world. For

Y. Guo (✉) ⋅ J. Li
Data61, CSIRO (Commonwealth Scientific and Industrial Research Organisation),
Marsfield, NSW 2122, Australia
e-mail: [email protected]
J. Wall ⋅ S. West
Energy, CSIRO (Commonwealth Scientific and Industrial Research Organisation),
Mayfield West, NSW 2304, Australia

© Springer International Publishing AG 2017 39

S. Mukhopadhyay et al. (eds.), Sensors for Everyday Life, Smart Sensors,
Measurement and Instrumentation 23, DOI 10.1007/978-3-319-47322-2_3
40 Y. Guo et al.

example, in Australia, it is estimated that the installed base of non-residential HVAC

systems consumes 9 % of electricity produced, representing more than 3.6 % of
Australia’s greenhouse gas emissions; and they create more than 55 % of electrical
peak demand in commercial business district (CBD) buildings [2]. The Australia
government recognizes that large efficiency gains can be achieved through ongoing
maintenance and more optimal operation of HVAC systems in existing building
stock, and seeks to establish national system standards of documentation for design,
installation, operation and maintenance of HVAC equipment/systems.
As well as the mechanical and electrical components and pieces of equipement, a
HVAC system comprises some form of control logic to regulate the operation of the
components and system as a whole. Usually a sensing device is used to compare the
actual state (e.g. temperature or humidity) with a target state. Then the control logic
draws a conclusion of what action has to be taken (e.g. provide more heating or
cooling). Modern HVAC systems not only have fundamental sensors and actuating
devices in addition to some basic control logic to perform their required function, but
often include a more advanced building management and control system
(BMCS) that provides multiple levels of control, data monitoring and analytics,
user interfaces and even interfaces to other building energy systems.
A variety of sensing devices (such as temperature, humidity, velocity, or pres-
sure) are installed in the HVAC systems. Sensors measure the actual value of
a controlled variable such as temperature, humidity or flow and provides infor-
mation to the BMCS. In a realistic situation, the building HVAC system can fail to
satisfy performance expectations envisioned because of problems caused by
improper installation of sensors, inadequate maintenance, and equipment or sensor
failures. These problems, or “faults,” include mechanical failures such as stuck,
broken, or leaking valves, dampers, or actuators; control problems related to failed
or drifting sensors, poor feedback loop tuning or incorrect sequencing logic; fouled
heat exchangers; design errors; or inappropriate operator intervention. Such faults
often go unnoticed for extended periods of time until the deterioration in perfor-
mance becomes great enough to trigger comfort complaints, equipment failure or
excessive power consumption.
Automated fault detection and sensor monitoring techniques for HVAC systems
can identify these types of faults, with the potential energy-saving of avoiding these
faults is estimated at 10–40% of HVAC system energy consumption, depending on
the age and condition of the equipment, maintenance practices, climate, and
building use [3–6]. By sensing and identifying minor problems before they become
major problems, the useful service life of equipment can be extended. Also, repairs
can be scheduled when convenient, avoiding downtime and overtime work.
Depending on the building use, better control of the temperature, humidity, and
ventilation rate of the occupied spaces can improve employee productivity, occu-
pant comfort, and/or product quality control.
Most of the current commercially available solutions in HVAC sensor monitoring
and fault detection systems use rule-based methods, where most solutions integrate
and interpret incoming sensor data in accordance with the pre-determined set of rules,
produce a risk profile, and initiate a response to a breach of these rules [7–10].
Real-Time HVAC Sensor Monitoring … 41

Another class of solutions use model-based methods, which use analytical mathe-
matical models to compare and identify faults based on the sensor data sets [11–13].
Since every building is unique, it is not a simple task to set these rules or to
generate these analytical mathematical models. In addition, the task of setting these
thresholds used by such solutions to raise alarms is quite involved, and prone to
producing false alarms. Hence, we developed a statistical machine learning algo-
rithm based approach for the automated monitoring and fault detection in HVAC
systems [14–17]. Our approach uses probabilistic models that are constructed on
the probabilistic links between variables. Meanwhile, the probabilities are learnt
from the stored sensor monitoring data sets. It is an ideal representation for com-
bining prior knowledge and data, and can have much better flexibility and adapt-
ability when applied to HVAC system.
For a complex HVAC system, the number of sensors and actuators can number
in their thousands, and the selection of key sensors and actuators containing the
main feature of the system and reflect to important system faults, is crucial for the
success of our approach. This paper presents automated monitoring and fault
detection techniques, and a key sensor sets selection approach to optimise the fault
detection results. This methodology has been implemented and tested in
real-world commercial buildings and experimental results show that different types
of faults are detected successfully.

2 Overview on HVAC Systems, Sensor Monitoring

and Fault Detection

A HVAC system normally includes central plant consisting of a hydronic heater, a

hydronic chiller, a pump system, a valve system, a heat exchange system (which
includes dedicated heated and chilled water coils), and an air distribution system for
supplying occupants with conditioned air. It also includes a sensing system that
includes a number of sensors located throughout the system, such as temperature,
humidity, air velocity, volumetric flow, pressure, gas concentration, position, and
occupancy detection sensors. The BMCS includes a computing system which
interfaces with various sensory signals in the HVAC system. Using feedback from
various components and sensors of the HVAC system, the environmental condi-
tions for the inhabitancy or functional purpose of the building can be regulated.
Figure 1 shows a simple schematic of a HVAC system. It consists of three main
parts: air handling unit (AHU), the chiller (cooling) and boiler (heating) systems,
and the control system. When a HVAC system is operational, a supply air fan as
part of the AHU draws air from either outside, return air from the indoor area, or a
mix of both, and past the cooling/heating coil heat exchange to achieve the desired
temperature and humidity before being supplied to the indoor area. A trade off
among exhaust, fresh and recirculation air is decided by the BMCS, based on the
real-time sensor signals.
42 Y. Guo et al.

Fig. 1 General schematic diagram of a typical HVAC system

In a typical multiple storey commercial building, there can be tens to hundreds of

zones. A large high rise commercial office building needs to be divided into mul-
tiple zones, in order to satisfy and maintain desired temperature and air quality
conditions. Figure 2 shows a screenshot of a single zone from a BMCS interface.
Some sensors such as the damper positions, valve positions are marked in the
figure, while some other sensors’ readings are listed in the top right corner, such as
the supply air temperature set point, return fan speed set point, etc.
Thousands of sensors read real-time status of the equipment in a large HVAC
system. The abundance of sensor data makes it difficult and expensive for human
operators to continuously monitor the system and identify faults or operational
inefficienies quickly.
One solution is to develop an intelligent automated sensor monitoring and fault
detection system which can continuously monitor sensor data from various system
components and identify unusual or inefficient behaviours.
Our approach is to use statistic machine learning algorithms based on key sensor
selection and monitoring technique. Firstly, historical sensor data is logged during
normal operation of the HVAC system. Secondly, suitable sensor combinations and
their features are chosen to train HVAC system status models. These self-learnt
models can build up the time-varying relationships between monitored sensors
and/or sensor features of normal operation in a HVAC system.
Finally, ongoing real-time sensor data is read in, and the likelihood of this data
matching with learnt historical behaviour indicates whether the HVAC system is
running as normal or not. Figure 3 shows the overview of this real-time monitoring
and fault detection approach.
Real-Time HVAC Sensor Monitoring … 43

Fig. 2 The view of an Air Handling Unit (AHU) of a HVAC system from the Building
Management & Control System interface.

Fig. 3 Overview of the real-time sensor monitoring and fault detection approach
44 Y. Guo et al.

3 Sensor Monitoring and Fault Detection Approach

in Detail

To overcome or ameliorate some of the limitations of existing fault detection

methods, our approach is a combination of the state-of-the-art machine learning
algorithms, including dynamic Bayesian networks (DBNs), Hidden Markov Models
(HMMs), as well as swarm intelligence and consensus clustering methods. This
section overviews our approach in details. Subsection A will present the key sensor
selection for efficient real-time monitoring, the second subsection will show the
architecture of the machine learning based methods, and the third subsection will
list the main faults that are detected for HVAC systems.
Sensor and feature selection: As explained in Sect. 2, thousands of sensors are
sending data to the database, and some of them are very crucial for proper system
monitoring, modelling, and correct fault detection results. Proper sensor and/or
sensor feature selection is essential for the whole model-based approach.
The aim of sensor selection is minimising redundancies between sensors so that
the important system features are not undermined. HVAC system’s performance
may change dynamically depending on many conditions such as weather condition,
seasonal condition, and occupancy of the building. Hence the sensors and their
features need to be constantly monitored. Moreover, some sensors may contain
little dynamic information, and can adversely affect the final model to an extent that
some faults are missed. One way to decide the sensor combination is to depend on
the HVAC technician’s experience, but this is not an efficient way when it is
applied to different structured buildings.
In our approach, we applied the rapid centroid estimation (RCE) as the key
data-driven sensor and feature selection algorithm, which specifically performs well
under varying seasonal conditions [18]. The feature extraction process from the
sensor data involves statistical analysis [19–21] and dimensionality reduction [19,
21]. This is a crucial step, as inappropriate features could reduce the capability of
the fault detection result.
We implemented an approach for sensor/feature selection using an ensemble
clustering algorithm, which allows the natural recovery of clusters without having a
priori knowledge regarding the optimum number of clusters. The method is
Ensemble Rapid Centroid Estimation (ERCE) [22] based on the RCE algorithm
[23]. ERCE exploits the fact that the quality of a clustering ensemble depends on
the degree of diversity of the provided clusters. It shows better performance than
conventional clustering algorithms such as complete linkage, ensemble k-means
and ensemble fuzzy c-means.
The ERCE is a sequential process including clustering, fuzzification, and
ensemble aggregation. In the clustering stage, various unique voronoi tessellations
of the data is discovered; in the fuzzification stage, the voronoi tessellations are
converted into fuzzy partitions; and in the ensemble aggregation stage, the final
partition is recovered using the weighted fuzzy co-association-tree by hybrid
Real-Time HVAC Sensor Monitoring … 45

method [22, 23]. An overview of ERCE is presented as following, where a detailed

description is available in [22, 23].
Given a data matrix Y,
 
Y = y1 . . . yj . . . ynj ,

where j denotes the observation index, nj denotes the number of data (volume), and
a particle position matrix X

X = ½x1 . . . xi . . . xni ,

where i denotes the particle index, ni denotes the number of particles, high
dimensional voronoi tessellations are performed on the data such that each obser-
vation in Y is mapped to the nearest particle. In other words, each particle xi governs
a voronoi cell of the set Ci :

CX = ½C1 . . . Ci . . . Cni , ∅ ⊆ C1, ..., ni

which may contain empty sets. The clustered set,

CX = Cr, ..., nc ∩ Ci, ..., ni , ∅ ⊆ CX ,

is the sets in Ci, ..., ni which partitions Y to nc non-empty clusters.

The ERCE contains nm swarms working in parallel such that

CERCE = CX1 . . . CXnm .

Using the concept of charged particles [22], the possibility of creating duplicate
partitions is minimised. Ideally each CXm would then return a unique partition of the
data such that

CX1 ≠ C X2 ≠ . . . ≠ CXm ,

where each partition CXm denotes an optimal partition returned by the mth swarm.
After the clustering process, the label matrix is fuzzified based on the distance
between particles and data D = DðX, YÞ. The fuzzy membership value for the jth
observation with respect to the ith cluster, uij , can be calculated as followings:

e − dij ̸ð2λi Þ
uij = ð1Þ
∑ni =i 1e − dij ̸ð2λi Þ

where dij is the distance between the ith particle to the jth observation, and λi
denotes the ith bandwidth of the cluster centre. Here λ1, ..., n can be optimised using a
compromise between the partition’s fuzzified dissimilarity
46 Y. Guo et al.

Dij = uij dij ,

and Shannon entropy

H uij = − uij log uij

for each i and j. In other words, for each cluster, Ci , the optimum λi can be found by
solving a convex optimisation problem:

mins.t.∀i, λi > 0 kH − Dk2 , ð2Þ

which optimised λi for all cells, i = 1, . . . , ni , that the Gaussian probability distri-
bution of the data governed in each corresponding voronoi cell is best described. In
this approach, we use non-linear least square to optimise Eq. (2).
The examples in Sect. 4 will show that the feature selection is a powerful tool
which can not only determine the feature cluster number, but also rank each feature
within each cluster. The feature with the highest ranking in each cluster is then
chosen as the key feature for fault detection.
Intelligent fault detection methods: The main processes of fault detection
algorithm work as two steps, training process step (or called learning), and fault
detection step (or called testing).
The historical sensor data which measures the normal operation status of the
system was collected for training process. The intelligent sensor and feature
selection process (as in Sect. 3A) is firstly implemented to prepare the training
datasets. A statistical machine learning approach then learns the relativity between
sensor measurements and system performance through these data. This approach
uses probabilistic models that consist of variables and probabilistic links, which can
denote the physical relationship between the sensor readings. Because of the
complexity of the HVAC system, multiple models are learnt during the training
process. The training process can be done during nights or weekends, and it nor-
mally takes about ten minutes over one week’s datasets for one building. Because
the system performance might change slowly because of season, weather, or other
conditions, the training process can be repeated at a regular basis. For instance, the
current training process can be done every week on tested buildings.
The fault detection process is to detect whether there is a fault in the system or
not (binary classification problem). After the training process, a learnt normality
model of the HVAC system can be used to detect system faults automatically. The
collected sensor data is periodically detected with the models built based on the
sensor features, and the similarity between current measurement and the historical
feature is calculated. If the algorithm finds that the difference is obvious, a fault
alarm is raised.
As the training process is a binary classification problem on time-series sensor
features, we implemented a methodology which is based on a combination of the
HMMs and the Support Vector Machines (SVM) algorithms [24]. HMMs are used
Real-Time HVAC Sensor Monitoring … 47

to denote the physical relationship between the sensor data in a dynamic system.
Meanwhile, SVM can handle the nonlinear behavior very well, and requires small
amount of training samples [16, 25, 26].
Furthermore, while the faults are detected as deviations in the normal operation,
they can be the input data for training one or more of the fault detection models to
learn patterns of faulty operation of the HVAC system wherein normal operation is
detected as deviations in the faulty operation. As a dynamic process, the normality
model and the fault models are adapted while the HVAC BMS dataset increases,
hence the performance of real-time monitoring and fault detection improves.
The selected features of the sensor data are tested on different pre-trained HVAC
normality models. Then the likelihood matrix is calculated as the indicator of the
similarity between current sensor readings and normal system sensor readings.
A couple of methodologies such as clustering and data fusion algorithms are also
implemented as the final stage in the analysis of the likelihood matrix, and make the
final decision as a sequence of binary value (e.g. Yes for normal, and No for
abnormal). More details of the training methodologies are in [6, 15, 27].
Main faults for HVAC systems: It is reported that a few top listed faults are the
major faults for HVAC systems [28]. Properly detect these faults can avoid up to
30% of energy waste in HVAC systems [29]. A short description of each fault is
listed as following, and our sensor monitoring and fault detection approach will
mainly focus on them.
• Hot water valve leaking or stuck: If the hot water valve stuck, hot air cannot be
provided properly. If an internal valve leaks, it can be very difficult to trou-
bleshoot and is often confused with a compressor that is not pumping to
capacity. Both a leaking valve and a failing compressor have the same symp-
toms—both the heating and cooling capacity of the system are diminished. This
is because the compressor continues to pump the air around and around inside
the leaking valve.
• Supply-air fan belt slipping: The supply-air fan belt slipping can lead to the
supply-air fan not running at setting speed.
• Outside air damper leaking or stuck: Damper not in the proper position. Outside
air cannot circulate properly.
• Return air damper leaking or stuck: Return air cannot circulate properly.
• Individual zone temperature sensor fault: The temperature sensor reading in a
zone is wrong.

4 Experimental Results

The intelligent real-time sensor monitoring and fault detection system has been
tested on several buildings. In this section, we will show the results in one of these
buildings, a large commercial building in Newcastle, Australia. The sensors are
sending real-time data to the monitoring and fault detection system with a 1-min
48 Y. Guo et al.

interval which is typical of the resolution of trended sensor data from a BMS
database [13]. Figure 4 shows an example of 15 sensors for an air handling unit
(AHU).
Fault detection experimental results: During August and September 2013, 35
faults in four different fault types were generated for one AHU. Most faults last over
six hours.
Table 1 listed the summary of the experimental results. Two types of faults, hot
water valve stuck and individual zone air temperature failure are 100 % detected.
But the success rate for the slipping supply-air fan belt fault is low. The lowest,
though, is the return air/outdoor air damper point stuck fault, where only one third
faults are detected. One of the main reasons is the measurement of the effects of
each fault. For some faults, the return air qualities are affected directly, and cor-
responding sensor measurements are collected, such as return air temperature. For
the return air damper, when it stuck at 70 %, the main facts that can change
accordingly should be outdoor air fraction or indoor air CO2. These facts were not
measured or saved in the datasets for modelling.
Sensor monitoring and feature selection results: We have also analyzed the
sensitivity of the sensor features for the fault detection in HVAC systems. The
parameters that we judge include the data sample rate, training window size,

Fig. 4 An example of the sensor data for an air handling unit in the Newcastle building
Real-Time HVAC Sensor Monitoring … 49

Table 1 Summary of fault detection experimental results

Generated Detected Not Detection Comments
faults in detected rate (%)
Aug/Sep
2013
Hot water 11 0 100
valve stuck
Return 3 6 33 For the return air damper, when it
air/outdoor stuck at 70 %, the main facts that can
air damper change accordingly should be
stuck outdoor air fraction or indoor air
CO2. These data were not measured
or saved in the datasets hence not
selected for modelling
Slipping 7 4 63.6
supply-air fan
belt fault
Individual 4 0 100
zone air
temperature
failure

missing data tolerance, and minimal sensor subset performance. We chose the high
frequency datasets for comparison experiments. The original dataset’s sample rate
is at one reading per 5 s, which is higher than most real HVAC systems. From the
original trials, we observed that the training/testing window size is relevant to the
sample rate. Hence we analyze the effects of the combination of these two
parameters. We changed the sample rate to the following: 5 s, 20 s, 30 s, 40 s, 50 s,
60 s, 80 s, and 90 s. The training/testing window size changes between the fol-
lowing values: 10, 20, 50, 80, and 100. The combination of sensors is the same as
default (six sensors).
Table 2 summarize the performance of the combination of these two parameters.
Tick for successful detection, cross for unsuccessful detection. As we can see, when
the sample rate increases, the window size need to be shorter to get the successful
results. For the 90 s sample rate, the window size should be 20, which means that
the training and testing data covers a 30–min period.

Table 2 Sensitivity of the sample rate versus window size of the sensor monitoring rate. Ticks for
successful fault detection
Sample rate → 5s 20 s 30 s 40 s 50 s 60 s 80 s 90 s
Window size ↓
10 × × × × × × × ×
20 × × × √ √ √ √ √
50 × × √ √ √ √ √ ×
80 × √ √ × × × × ×
100 √ √ × × × × × ×
50 Y. Guo et al.

Case study for sensor selection and its effect on fault detection: In this
subsection, we will present one example to show the effect of sensor selection on
fault detection results. The detail of this fault is as following:
• Date: 20/11/2009
• Location: All AHUs for Newcastle building
• Description: This is an actual fault that occurred when the chilled water system
was under heavy load. Chiller 2 failed due to an overheating safety cut-out, and
Chiller 1 failed to ramp up due to some misconfigured set-points, causing the
chilled water temperature to rise to around 23 °, and in turn causing the chilled
water valves on many zones (AHU9 included) to open up to near 100 %.
This type of faults is relatively common for HVAC systems, and can lead to a
large waste of energy. The sensors that are selected to build the HMMs by the
intelligent algorithms described in Sect. 3. A are: hot water valve sensor, chilled
water valve sensor, supply air relative humidity sensor, supply air temperature
sensor, return air relative humidity sensor, return air temperature sensor.
HMMs are trained on normal fault-free historical data. Then the real-time sensor
monitoring data is fed in to calculate the likelihood. The lower the likelihood value,
the higher possibility a fault exists.
The fault detection results are shown in Figs. 5 and 6. Figure 5 is the likelihood
curves for the data on 20th Nov 2009, and the corresponding fault detection results
after a classification and clustering process is shown in Fig. 6. It is clear that the
fault, occurring after 12:00 pm, is convincingly detected, as shown by the likeli-
hood curves.

3000

2000

1000

-1000

-2000

-3000

-4000
0 500 1000 1500 2000 2500 3000 3500 4000 4500 5000

Fig. 5 A family of likelihood curves from a detected fault prior to clustering

Real-Time HVAC Sensor Monitoring … 51

2
class ID

0
09:00 12:00 15:00 18:00

Fig. 6 Detection results for the fault after clustering and classification on the likelihood curves

If we manually remove one sensor feature from the optimized sensor combi-
nation, the fault would then become difficult to be detected. One example is shown
in Figs. 7 and 8, for the same fault datasets—where the supply air temperature
sensor data is not used for the HMM learning process. The likelihood curves drop
to lower levels earlier that day, and the classified fault period is not correct. This
example shows the importance of proper sensor features. Our approach can auto-
matically select suitable sensor features rather than depend on domain expert, and
assure successful detection results.
The above example proves that ERCE, as the data-driven sensor and feature
selection algorithm, is crucial for the fault detection results. In fact, ERCE specifi-
cally performs well under varying seasonal conditions. The ERCE method selects
features that are unique and relevant to the faults in the HVAC system. For different
seasons, ERCE selects different combination of sensor data as the key features.
Pattern for the winter dataset is different from the pattern for the summer dataset. The
experimental results show that the sensor and feature selection process can ensure

Failed Chiller: removedSensor - SATemp

-1000

-1500

-2000

-2500
loglikehood

-3000

-3500

-4000

-4500

-5000

-5500

-6000
09:00 12:00 15:00 18:00

Fig. 7 A family of likelihood curves without using optimal sensor combination

52 Y. Guo et al.

Detection Result for Failed Chiller: removed Sensor - SATemp

3

2
class ID

0
09:00 12:00 15:00 18:00

Fig. 8 Corresponding fault detection results

the success of the fault detection results for the HVAC system. It is proven that the
ERCE method can improve the fault detection results, comparing to the results based
on other feature selection clustering method, such as EAC k-means [18].

5 Conclusion and Discussion

This paper presents dynamic, machine-learning based techniques for automated

sensor monitoring and fault detection in HVAC systems. This approach can be seen
as a good combination of model-based methods and data-based methods. The main
approaches are based on graphical modelling techniques such as HMMs, which
encode probabilistic relationships among variables of interest. This approach is an
ideal representation for combining prior knowledge and data. It does not need very
detailed understanding of the physical system as in model-based approaches. It also
does not need huge data sets as in the black-box approaches. Comparing with pure
model-based or data-based approaches, it combines the strengths in both areas and
can overcome their shortfalls by balancing the dependency on physical models and
datasets.
One critical step to ensure the approach succeeds is that of the sensor feature
selection process. This paper implements the ensemble rapid centroid estimation
(ERCE) as the data-driven sensor and feature selection algorithm, which is the core
method to ensure automated fault detection is achieved. Instead of choosing sensors
manually, the ERCE method can automatically select representative features that
are unique and relevant to the faults in the HVAC system. It also discards redundant
sensors that are less crucial or have less system features. The experimental results
show that this sensor and feature selection process can ensure the success of the
fault detection results for HVAC systems. It is proven that the ERCE method can
improve the fault detection results, comparing to the results based on other feature
selection clustering methods, such as EAC k-means.
Planned future work includes comparing the selected sensor features from dif-
ferent buildings, and identifing the common features for multiple types of buildings.
Real-Time HVAC Sensor Monitoring … 53

By improving the generalizability of the sensor monitoring and fault detection

approach, less modelling time can be saved, and more improvements in perfor-
mance, such as fault detection accuracy, can be achieved.

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High Sensitivity Optical Structures
for Relative Humidity Sensing

Joaquin Ascorbe, Jesus Corres, Francisco J. Arregui,

Ignacio R. Matias and Subhas Chandra Mukhopadhyay

Abstract This chapter is focused in the different optical structures and materials
that have been used for the development of optical fiber humidity sensors. First, we
will start with a short introduction of what relative humidity is, and why it has been
extensively investigated. We will make also a brief summary of the different
options that have been developed by now, showing the evolution of this research
field. Then we will look more closely at the most used structures, the most common
materials and the devices having greater sensitivity and resolution.

1 Introduction

Humidity constitutes one of the most commonly required physical parameters to be

measured. Humidity sensing and control is really important in several application
fields, such as semiconductor and electronic manufacturing, food, textile, wood or
paper industries, conservation and storage, chemical, biological and pharmaco-
logical industry among others.
Different terms related to humidity measurement can be found in the literature
and they are commented here before starting. While moisture refers to the water in
liquid form that may be present in solid materials, humidity is a measure of water in
gaseous state present in the environment and it can be measured as absolute
humidity (kg of water vapour per kg of dry air) or as relative humidity. The relative
humidity of an air mass is the ratio of water vapour contained and the maxi-
mum steam content that it would have if it were completely saturated. For higher
temperatures the air has more capacity of containing water so for a given absolute
humidity at certain temperature, the relative humidity will decrease if the temper-

J. Ascorbe ⋅ J. Corres (✉) ⋅ F.J. Arregui ⋅ I.R. Matias ⋅ S.C. Mukhopadhyay

Institute of Smart Cities, Public University of Navarra, Campus Arrosadia,
31006 Pamplona, Spain
e-mail: [email protected]
S.C. Mukhopadhyay
Macquarie University, 2109 Sydney, NSW, Australia

© Springer International Publishing AG 2017 55

S. Mukhopadhyay et al. (eds.), Sensors for Everyday Life, Smart Sensors,
Measurement and Instrumentation 23, DOI 10.1007/978-3-319-47322-2_4
56 J. Ascorbe et al.

Fig. 1 Evolution of the optical fiber humidity sensors contributions (Source Scopus)

ature is increased [1]. In this chapter we will always refer to relative humidity
although sometimes it will be mentioned only as humidity.
In Fig. 1, it is shown the evolution of the contributions found in Scopus, related
to optical fiber humidity sensors, from 1982 to 2015. As it can be seen, the number
of contributions has increased continuously since 1999 keeping today a number
worthy of consideration.
This increasing interest in optical fiber humidity sensors is due to the intrinsic
advantages of using optical fibers as the sensing structure. These advantages
include: small size, lightness, the possibility of working on flammable environ-
ments, the ability of working on greater pressure and temperature ranges and, the
most important, their electromagnetic immunity.

2 Materials

Several materials have been used for the development of optical fiber humidity
sensors, from polymers to metal oxides, from hydrophilic to hydrophobic materials.
Hydrophobic materials, which are composed of non-polar molecules, present
greater contact angles than the hydrophilic ones. Both of them have been used for
the development of humidity sensors [2, 3].
However, for the development of optical fiber sensors, there are other behaviors
which provide better performance from an optical point of view. These behaviors
are called swelling and adsorption. Swelling is a process whereby a material
increases in size when subjected to increasing humidity. This increased thickness
provokes that the light traveling through the core of an optical fiber found a greater
effective refractive index, which will affect at the transmitted light. The other
physical phenomena, adsorption, is defined by the IUPAC as an increase in the
concentration of a dissolved substance at the interface of a condensed and a liquid
phase due to the operation of surface forces. Adsorption can also occur at the
interface of a condensed and a gaseous phase [4]. For humidity measurements, the
High Sensitivity Optical Structures for Relative Humidity Sensing 57

result of adsorption is the generation of a thin film of water over the surface of the
material. Swelling is common for some polymers while adsorption is the pre-
dominant effect in metal oxides.
It does not mean that the previously commented physical phenomenon are the
only ones that can be used for measuring relative humidity by an optical set-up.
There are other phenomenon used for humidity sensing as it can be fluorescence
[5], but in this chapter we will focus on evanescent wave sensors, fiber gratings,
sensors based on Lossy Mode Resonances and Fabry-Pèrot interferometers, with
coatings based on adsorption and swelling.

3 Conventional Methods

There are conventional methods for measuring the relative humidity and we will
make a brief overview of those methods. Different physical phenomena have been
used for this methods and they can be classified on these categories:
• Wet and dry bulb psychrometer
• Mechanical
• Electrical
• Infrared (IR) optical absorption hygrometer
The wet and dry bulb psychrometer consists of two thermometers, one of which
is covered with a damp wick (wet bulb). The difference between the measured
temperatures is due to water evaporation and latent heat transfer [1, 6] and the
relative humidity can be calculated with the psychrometric diagram.
Mechanical humidity sensors are based on the expansion/contraction of certain
materials. A well-known humidity sensor based on mechanical behavior is the
mechanical hygrometer. Common materials used include synthetic fibres and
human hair. The first mechanical hygrometers were formed by linking the material
with a weak tension by a spring, and a mechanical linkage operates a needle. Other
mechanical hygrometers were formed by linking the material to strain gauges or
other devices to measure the displacement caused by the change in humidity [6].
Resistive and capacitive-type humidity sensors are included into the electrical
category. Resistive-type humidity sensors are based on changes on the electrical
resistivity of some materials as conductive polymers, semiconductors or compos-
ites. This behavior has been explained in [7–9] by the water adsorbed on the oxide
surface in the molecular and hydroxyl forms. Furthermore, Boyle and Jones [7]
established that water demonstrates donor properties at adsorption in the molecular
form while it shows acceptor properties in the hydroxyl form [10]. In the same way
capacitive-type sensors are based on the dielectric changes of a thin film. Common
materials used for capacitive sensors are ceramics like alumina [11] and polymers
[12]. The capacitive- and resistive-based humidity sensors are the most commonly
used, with capacitive-based sensors dominating and making up nearly 75 % of the
commercial humidity sensor market [13].
58 J. Ascorbe et al.

Fig. 2 a Mechanical humidity sensor, b wet and dry bulb psychrometer, c capacitive humidity
sensor, d IR optical absorption method and e resistive humidity sensor

Finally, the infrared (IR) optical absorption hygrometer is based on the optical
absorption of the water vapor. It works by emitting light at two different wave-
lengths. One of them has negligible absorption and it is used as reference. The
transmission ratio between those two wavelengths provides a direct measurement of
water absorption, making this technique insensitive to contaminants [6] (Fig. 2).

4 Optical Fiber Humidity Sensors

There are many ways of measuring the relative humidity by means of optical
set-ups, one of them has been mentioned before. Here, we are going to explain in
detail those based on optical fibers and most specifically, those involving coatings
onto an optical fiber. Among those devices we will focus on Fabry-Pèrot inter-
ferometers and Lossy Mode Resonances based devices although some other
structures will be mentioned to have a sight of the differences between them and the
evolution that optical fiber humidity sensors have suffered. Optical fiber humidity
sensors (OFHS) can be classified by the physical phenomena they used as:
• Evanescent wave sensors
High Sensitivity Optical Structures for Relative Humidity Sensing 59

– Optical absorption
– Change on the refractive index
– Lossy mode resonances (LMRs)
• Fluorescence sensors
• Interferometric sensors
• Fiber gratings

4.1 Evanescent Wave Sensors

First of all, we are going to introduce the earlier optical fiber humidity sensors,
classified as evanescent wave (EW) sensors. The evanescent field is created as a
result of the standing wave generated by the interference between the incident and
the reflected signals at the core/cladding interface, inside an optical fiber, due to the
Total Internal Reflection (TIR) phenomena [6]. The amplitude of the evanescent
field decays exponentially with the distance away from the core/cladding interface
and it can be calculated as:

EðzÞ = E0 expðz ̸dp Þ ð1Þ

where the penetration depth (dp) is defined as the depth at which the amplitude of
the evanescent field, E, has decayed to 1/e of the initial value E0 at the
core/cladding interface and this is given by

λ
dp = h i1 ̸2
ð2Þ
2πncore ðsin θ − ðnclad ̸ncore Þ2
2

where λ is the wavelength of the propagating signal in the optical fiber, θ is the
angle of incidence normal at the interface, ncore and nclad are the refractive indices
of the fiber core and cladding, respectively.
There are two different approaches: the first one based on changes on the optical
absorption and the second one based on changes of the refractive index. The main
difference between these two methods is that optical absorption causes changes at a
certain wavelength or in a wavelength range and when changing the refractive
index there are changes at all wavelengths. Earlier optical fiber humidity sensors
were developed by the first method since 1985 using, for example, cobalt chloride
[14] or other chemical reagents immobilized in a polymeric matrix, and cladding
removed optical fibers. The problem with these sensors is that the evanescent tail
has only a small fraction of power, and a long portion of fiber must be coated to
have a detectable change at the output end [15]. For that reason some other
structures have been developed to increase the amplitude of the evanescent field and
consequently the sensitivity of the device. For example U-bent fibers [15] or porous
60 J. Ascorbe et al.

Fig. 3 a Humidity sensor structure. Taper profile with ESA overlay and b Optical output
spectrum dependence with respect to the relative humidity with 23 bilayers deposited. Tapered
fiber waist diameter: 20 μm. Taper length: 2.2 mm. Nanofilm: [PDDA+/Poly-R−]. Reprinted from
Sens. Actuators B, vol. 122, no 2, Corres, J.M., Arregui, F.J., and Matías, I.R., Sensitivity
optimization of tapered optical fiber humidity sensors by means of tuning the thickness of
nanostructured sensitive coatings, pp. 442–449, (2007), with permission from Elsevier

fibers [16] have been used to develop more sensitive OFHS based on optical
absorption.
Several different approaches have been followed to develop evanescent wave
sensors by changing the refractive index of the coating. Removed plastic cladding
optical fibers [17], tapered single mode [18, 19] optical fibers or D-shape optical
fibers can be used for this kind of devices. Common materials used for these OFHS
are hydrogels as poly-hydroxyethyl methacrylate, poly-acrylamide, poly-N-vinyl
pyrrolidinone and agarose [17, 18]. As it can be seen in Fig. 3, extracted from [19]
changes are produced at all wavelengths with this method.

4.2 Lossy Mode Resonances

Optical fiber sensors based on Lossy Mode Resonances are a special case of
evanescent wave sensors and, more specifically, a special case of EW sensors based
on changes of the refractive index. Here, the material chosen for coating the optical
fiber has to meet two conditions: to be sensitive to the physical parameter for what
the sensor is developed and to meet the requirements to generate LMRs. This
method, which is included in the wavelength based techniques, overcome the
limitations of the previous EW methods, such as external noises or power fluctu-
ations [20].
Lossy Mode Resonances are a physical phenomenon which consists on the
absorption of the light at certain wavelength. It is important to remark that this
absorbed light is not related to the absorbed light mentioned before. For EW sensors
based on optical absorption, the absorption of the light is produced when the
coating is subjected to the physical parameter to be measured. However, once the
LMR has been generated, the optical absorption occurs without need of an external
High Sensitivity Optical Structures for Relative Humidity Sensing 61

parameter. The LMR will be located at different wavelengths depending on the

refractive index of the surrounding medium. This is due to coupling between a
waveguide mode and a particular lossy mode of the coating, which depends on two
conditions: there is a considerable overlap between the mode fields, and the
phase-matching condition (i.e. the equality of real parts of propagation constants) is
sufficiently satisfied [21–23]. LMR occurs when the real part of the thin-film per-
mittivity is positive and higher in magnitude than both its own imaginary part and
permittivity of the material surrounding the thin-film [23].
The wavelength where this absorption occurs depends on the refractive index of
the material, the thickness of the coating and the refractive index of the surrounding
medium. Several materials have been proved as LMR generators as ITO [23], In2O3
[24], SnO2 [25], PAH/PAA [26], TiO2/PSS [27, 28] …
It exists other kind of resonances called Surface Plasmon Resonances (SPRs)
which are generated by a few materials, generally metallic materials like silver and
gold, and they occur when the real part of the thin-film permittivity is negative and
higher in magnitude than both its own imaginary part and the permittivity of the
material surrounding the thin-film [22]. As contrast to LMRs, in SPRs the collective
coherent oscillations of free electrons in the conduction band of a metal is excited
by the interactive electromagnetic field at a metal/dielectric interface [29, 30]. There
is also a third type of resonances known as Long Surface Plasmon Resonances
(LSPRs). The spectral location of the LSPR is sensitive to the shape, size, and
composition of the nanostructure, as well as on the optical properties of the sur-
rounding dielectric [31]. Main differences between LMRs and SPRs are resumed in
Table 1 and a schema of how and when LMRs are generated is shown in Fig. 4.

4.2.1 Plastic Cladding Removed Multimode Optical Fiber

As it has been mentioned before, metallic oxides are good candidates for the
generation of LMRs and they are also a good choice for humidity sensing because
of their absorption capability. Most of the research done for LMRs has been
developed coating a 200/225 µm core/cladding plastic cladding optical fiber. This
optical fiber allows to transmit light in the range 400–2200 nm and the cladding can
be removed by simple chemical methods. First LMR devices were developed by
coating an optical fiber with ITO and they were characterized as humidity sensors
[32] and also as refractometers [33]. Then a typical transmission set-up, Fig. 5, was
used while the optical fiber was subjected to changes on the relative humidity and

Table 1 Comparison LMRs SPRs

between lossy mode
resonances and surface Number of absorption peaks >1 1
plasmon resonances Wavelength Tunable Fixed
Number of available materials Many Few
Visible for both TE and TM polarized light Yes No
62 J. Ascorbe et al.

Fig. 4 a Scheme of lossy mode resonances generation, b dielectric and refractive index
conditions for LRSEP, SPR and LMR generation and c graphic representation of previously
mentioned conditions

Fig. 5 Optical fiber transmission setup

the wavelength shift of the LMR was observed. A SEM image of the coating can be
seen in Fig. 6.
The wavelength shift of the LMR is caused by changes on the refractive index
(RI) of the coating. Due to the absorbed water on the ITO surface the effective
refractive index increases, and as the LMR wavelength depends on that, its
wavelength position shifts to greater wavelengths. It seems to be a general trend that
for an increase of the refractive index there is a redshift of the LMR, although there
might be exceptions. Main contribution for these OFHS is due to changes on the RI
of the coating, although it may be considered that the RI of the surrounding medium
is also altered, it is negligible by comparison. Figure 7 shows the dynamic beha-
viour of these kind of devices.
The previous situation uses the dependence of LMRs on the RI of the coating.
But OFHS can be also developed taking advantage of the dependence of LMRs on
High Sensitivity Optical Structures for Relative Humidity Sensing 63

Fig. 6 SEM image of a ITO coating and b In2O3 coating deposited onto the optical fiber core.
Reprinted from Lossy mode resonances toward the fabrication of optical fiber humidity sensors,
P. Sanchez et al., 2012, Meas. Sci. Technol. 23 014002 doi:10.1088/0957-0233/23/1/014002 with
permission from IOP Publishing

Fig. 7 Dynamical response of ITO sensors from 20 to 80 % of RH. Reprinted from Lossy mode
resonances toward the fabrication of optical fiber humidity sensors, P. Sanchez et al., 2012, Meas.
Sci. Technol. 23 014002 doi:10.1088/0957-0233/23/1/014002 with permission from IOP
Publishing

the RI of the surrounding medium. For that purpose, some devices have been
developed using ITO for the generation of LMRs and using other materials like
PAH/PAA as the sensitive layer [20, 28]. These devices combine the high sensi-
tivity of LMRs to changes on the external RI with the greater changes on the RI of
PAH/PAA when subjected to high humidity, improving the sensitivity of the device
to changes on the relative humidity. This combination of two different layers allows
to have the LMR located at greater wavelengths, which also enhances the sensi-
tivity of the device. Figure 8 shows the absorption spectrum for this device at two
different relative humidity values and its dynamic response.
64 J. Ascorbe et al.

Fig. 8 Spectral response of the a non-tuned and b tuned sensors for 20 and 90 % RH and
dynamical response of the sensors to changes in the RH of the external medium c non-tuned sensor
(20 PAH/PAA bilayers) and d tuned sensor (100 PAH/PAA bilayers). Reprinted from Sens.
Actuators B, vol. 146, no 1, Zamarreño, C.R., Hernaez, M., Del Villar, I., Matias, I.R., and
Arregui, F.J., Tunable humidity sensor based on ITO-coated optical fiber, pp. 414–417, (2010),
with permission from Elsevier and IOP Publishing

4.2.2 Single Mode Optical Fiber

Standard SMFs has some advantages respect plastic cladding multimode optical
fiber, and one of them is its price. On the other hand it is more difficult to make a
SMF sensitive to external parameters because its cladding it is made of silica
instead of plastic. But there are some methods to obtain access to the evanescent
field of a SMF. One of these methods consists on tapering the SMF by applying
heat and stretching. The heat can be applied by means of a flame or by an electric
arc [34–36]. When a single-mode fiber (SMF) is tapered, the core/cladding interface
is redefined in such way that the SMF in the tapered region acts as a multimode
fiber, sustaining several LP0 m modes. In this case, the light propagation in the
waist of the taper extends to the whole fiber, which plays the role of the new core,
and the new cladding is the external medium; this fact eases the interaction of the
evanescent field with the outer medium so that small changes of the outer medium
influence the transmitted optical power. Some OFHSs have been developed using
this structure [19, 34–36], most of them based on optical power measurements [19,
35] and others based on resonances [36]. As it can be seen in Fig. 9 from [36], a
tapered SMF can be sensitive to external parameters if coated with the appropriate
material, indium tin oxide for this case.
There are other ways to gain access to the evanescent field of a SMF as using a
D-shape optical fiber [27], but here we are going to focus on another structure that
has been recently used [37], which consists of a cladding etched single mode optical
fiber (CE-SMF) coated with a semiconductor oxide thin-film. As contrast to tapered
SMF, that keeps the ratio core/cladding, in the CE-SMF the core is not narrowed,
High Sensitivity Optical Structures for Relative Humidity Sensing 65

Fig. 9 a Evolution of the transmitted optical spectrum of a tapered SMF coated with ITO for
b some cycles of 20–90 % RH and c optical spectra for some values of RH [36]

Fig. 10 Cladding-etched single mode optical fiber. Reprinted from Sens. Actuators B, vol. 233,
Ascorbe, J., Corres, J.M., Matias, I.R., and Arregui, F.J., High sensitivity humidity sensor based on
cladding-etched optical fiber and lossy mode resonances, pp. 7–16, (2016), with permission from
Elsevier

only the cladding is partially removed by chemical methods. A common method to

remove the cladding is the use of hydrofluoric acid (HF) [38, 39] (Fig. 10).
But the sensitivity of the naked CE-SMF to external parameters is quite small
and it transmission spectra has not any absorption peak whose wavelength shift
could be measured. Changes of the transmitted optical power lower than 1 dBm are
achieved when immersing it in water. That is the reason why it is necessary to coat
the CE-SMF with a thin-film which provides a wavelength phenomenon that can be
tracked and which is sensitive to the external parameter to be measured at the same
time. The material chosen for this purpose has been indium oxide (In2O3) which
meets the requirements for LMR generation [25]. Indium oxide has been coated
onto a CE-SMF by means of Pulsed DC Sputtering System, a physical vapor
deposition method, which allows to coat metals and some semiconductor oxides,
providing homogeneous coatings and high control of the thickness deposited. In
Fig. 11 it is shown how the LMR is generated as the thickness of the coating
increases.
66 J. Ascorbe et al.

Fig. 11 a Some transmitted optical spectra for different thicknesses of In2O3 nano film coated
onto a cladding etched single mode optical fiber and b changes on the transmitted optical spectrum
for increasing thickness of In2O3 nano film

This coated CE-SMF was then connected to the light source and to an optical
spectrum analyzer (OSA). The light source was a super-luminescent emitting diode
(SLED) HP-83437A white light source which has four LEDs at 1200, 1310, 1430
and 1550 nm and the OSA was the HP-86142A, which has a wavelength range
between 600 and 1700 nm, although 1200–1600 nm range was used. The optical
fiber was introduced in a climatic chamber (Angelantoni ACS CH 250), as it can be
seen in Fig. 12.

Fig. 12 Experimental set-up for measuring changes on the transmitted optical spectrum while
relative humidity changes. Reprinted from Sens. Actuators B, vol. 233, Ascorbe, J., Corres, J.M.,
Matias, I.R., and Arregui, F.J., High sensitivity humidity sensor based on cladding-etched optical
fiber and lossy mode resonances, pp. 7–16, (2016), with permission from Elsevier
High Sensitivity Optical Structures for Relative Humidity Sensing 67

Fig. 13 a Optical spectra for some values of RH, b evolution of the transmitted optical spectrum
of a CE-SMF coated with ITO for c some cycles of 20–90 % RH

There, the relative humidity has been increased from 20 to 90 % at a constant

temperature of 25 °C. Due to previously commented phenomenon of absorption, the
effective refractive index of the coating increases. The LMR shifts to greater wave-
lengths as the relative humidity increases. Figure 13, shows the spectra for different
values of relative humidity and its evolution for some cycles 20–90 % RH.
The optical spectrum varies in several aspects: first of all, the attenuation of the
LMR increases, besides the LMR narrows, and finally there is a wavelength shift in
the wavelength of the resonance. By locating the wavelength of the resonance point
with a higher attenuation it could be possible to measure relative humidity by
registering the wavelength as a function of the relative humidity. This has been
done by means of MATLAB® software. By applying a simple algorithm, it has
been approached the spectrum to a parabola and then its vortex was calculated.
Plotting the wavelength position of the LMR and the relative humidity, obtained by
an electronic humidity sensor inside the climatic chamber we have obtained the
next graph. Changes greater than 30 nm have been obtained for RH varying from
20 to 90 %. High linearity and low hysteresis are some of the characteristics of this
device (Fig. 14).
The same structure has been proved with tin oxide as the LMR generator and as
the sensitive material in [40]. Tin oxide has greater refractive index than indium
oxide and it has also a great adsorption capability. It has proved good performance
as humidity sensor based on LMRs. Figure 15 shows different optical spectra for
different values of relative humidity. For this material wavelength shifts greater than
130 nm have been obtained, achieving a sensitivity of 1.9 nm/%RH. This increase
in sensitivity is due, in part, to the higher refractive index of tin oxide with respect
to indium oxide and it might be due also to differences in their adsorption
capability.
68 J. Ascorbe et al.

Fig. 14 Wavelength position of the LMR and relative humidity plotted simultaneously as a
function of time for previous device

Fig. 15 a Optical spectra for four cycles of 20–90 % RH, b relative humidity cycles inside the
climatic chamber and c optical spectra for some values of RH. Reprinted from Sens. Actuators B,
vol. 233, Ascorbe, J., Corres, J.M., Matias, I.R., and Arregui, F.J., High sensitivity humidity sensor
based on cladding-etched optical fiber and lossy mode resonances, pp. 7–16, (2016), with
permission from Elsevier
High Sensitivity Optical Structures for Relative Humidity Sensing 69

4.3 Interferometric Sensors

In this section of the chapter we are going to focus on optical fiber humidity sensors
based on Fabry-Pèrot interferometers (FPI). There are a lot of different ways to
generate interferometry. One of the most known interferometers is the
Mach-Zehnder interferometer, which measures the phase difference between light
propagating through two arms of different length [41]. These kind of interferom-
eters can be obtained by splitting the optical waveguide and recombining it later, by
splicing different kind of fibers [42] or by tapered optical fibers [43]. This inter-
ferometers [42, 43] are based on modal interferometry, which is generated between
core modes and cladding modes. But there is another kind of optical fiber inter-
ferometers which are called Fabry-Pèrot interferometers (FPIs). FPIs can be clas-
sified into extrinsic and intrinsic interferometers. In the intrinsic FPIs (IFPIs) the
cavity is contained within the fiber and in the extrinsic FPIs (EFPIs) sensors the
cavity is external to the fiber. Both of them are based on the interference caused by
multiple reflections of light between two reflecting surfaces. Constructive inter-
ference occurs if the transmitted beams are in phase, and this corresponds to a
high-transmission peak of the etalon. If the transmitted beams are out-of-phase,
destructive interference occurs and this corresponds to a transmission minimum.
Whether the multiply reflected beams are in phase or not depends on the wave-
length of the light, the angle the light travels through the etalon, the thickness of the
etalon and the refractive index of the material between the reflecting surfaces [44]
(Fig. 16).
Fabrication methods for EFPIs are inexpensive and simpler than those used for
the fabrication of IFPIs. Regarding the fabrication of EFPIs different approaches
have been followed to obtain the interferometer. Most used structure consists of an
air gap between two optical fibers [45, 46]. Hollow core fiber spliced to a
single-mode optical fiber (SMF) and filled with a sensitive material [47] has been
also used. But the most robust and reliable method for developing an EFPI is
generating a nano-cavity by coating the tip of the SMF [48–50]. Although we are
going to focus on a sputtered coating, other methods have been used for the
fabrication of Fabry-Pèrot interferometers, as dip-coating [47], e-beam evaporation
[51] or electrostatic self-assembly [49].
In an interferometric cavity the mirrors are formed by the refractive index dif-
ferences between the different optical media at either end. In this case by the
refractive index differences between the optical fiber and the SnO2 coating, and then
between the SnO2 coating and the external medium, which is air for this case. The
reflectance of each mirror will be approximately that determined by Fresnel’s law
for the case of normal incidence,

ðn1 − nÞ2
R1 = ð3Þ
ðn1 + nÞ2
70 J. Ascorbe et al.

Fig. 16 a Schematic representation of interference in an etalon, b scheme of an all-fiber

Fabry-Pèrot interferometer and c SEM image of the coating which will generate the interferometer

ðn2 − nÞ2
R2 = ð4Þ
ðn2 + nÞ2

where R1 is the reflection coefficient of the first interface (optical fiber/SnO2

coating) and R2 is the reflection coefficient of the second interface (coating/air). The
interferometric cavity functions exactly as an optical fiber Fabry–Perot etalon. The
expression of the reflectance for such a Fabry–Perot etalon is:
pffiffiffiffiffiffiffiffiffiffi
R1 + R2 + R1 R2 cosθ
RFP = pffiffiffiffiffiffiffiffiffiffi ð5Þ
1 + R1 R2 + R1 R2 cosθ

and

4πnL
θ= ð6Þ
λ

where L is the length of the etalon and λ is the wavelength of the excitation light
[48].
High Sensitivity Optical Structures for Relative Humidity Sensing 71

4.3.1 Fabry-Pèrot Interferometer as Humidity Sensor

Here we are going to show the behaviour of a FPI obtained by coating the tip of an
optical fiber with tin dioxide [52]. Tin dioxide is a good choice for humidity sensing
because of its absorption capability and it is also a good choice for the FPI gen-
eration because of its high refractive index. First of all, in Fig. 17 it is shown a
simulation of how the interferometry is generated and how it changes as the
thickness of the etalon increases.
First of all, just one interference peak appears, which shifts to greater wave-
lengths, then another peak appears which also shifts to greater wavelengths, but it
shifts more slowly than the previous one and so and so forth. This difference in the
speed of the wavelength displacement makes that, for greater thicknesses there were

Fig. 17 a Evolution of the simulated spectrum as the thickness of the coating increases and
b simulated optical spectra for different thickness of the coating
72 J. Ascorbe et al.

more interference peaks, which leads to an increase of the wavelength resolution of

the interferometer. The commented behaviour is due to changes on the length of the
cavity for a fixed refractive index. Once the length is fixed, it is subjected to
changes on the relative humidity using a reflection set-up. Now the optical changes
are caused by a change on the refractive index of the cavity.
As it can be seen in Fig. 18, the wavelength where a constructive interference
and also where the destructive interference occur shifts to greater wavelengths when
the relative humidity is increased. This is due to the adsorbed water onto the tin
oxide layer. The effect of the water adsorbed onto the tin oxide layer can be
modelled by the following phenomena. Since water is a polar molecule, the neg-
atively charged oxygen of the water molecule is electrostatically attracted to the
positively charged cationic side of the metal oxide surface. If the charge density of
the cationic side is low, then water remains physically adsorbed at the surface by a
weak electrostatic field [53]. When the cationic charge density is high, the elec-
trostatic force is high enough to form a chemical bond between hydrogen and
oxygen of a water molecule, which in turn may break the bond between oxygen and
one of the hydrogen atoms [54–56]. Mostly, the force is high enough to break the
bond in the initially adsorbed water vapour layer. Therefore, the initial monolayer is
generally chemisorbed [53]. As relative humidity (RH) increases, an additional
layer of water molecules starts to be formed, on the chemisorbed one. Many more
physisorbed layers will be joined as humidity gets higher [57]. These layers are
easily removed by decreasing the humidity [58, 59]. This layer of water causes an
increase of the effective refractive index of the coating, changing the interference
conditions.

Fig. 18 a Evolution of the reflected optical spectrum for b four cycles of 20–90 %RH, c some
optical spectra for different values of RH and d wavelength position of the interference peaks as a
function of the RH
High Sensitivity Optical Structures for Relative Humidity Sensing 73

Wavelength shifts of 100 nm have been achieved for changes on the relative
humidity from 20 to 90 %. The wavelength shifts have a dependence on the
wavelength, slightly greater displacements are obtained for interference peaks
located at greater wavelengths. This kind of devices have low hysteresis, high
linearity, good response time and high sensitivity. However, it must be carefully
selected the material which is going to be used for the development of this device. It
must meet the requirements to be sensitive to RH and to generate a good inter-
ferometer. Most semiconductors are sensitive to changes on relative humidity and
they will generate a better interferometer as its refractive index is greater.

4.4 Long Period Fiber Gratings

Long period fiber gratings (LPGs) has some desirable characteristics for their use as
optical fiber sensors. LPGs structure consists on a periodic modification of the
refractive index of the optical fiber. Several approaches have been followed to
develop LPGs. Modification of the refractive index of the optical fiber can be
obtained by exposing to UV radiation hydrogen-loaded germanosilicate fibers [60,
61], or by methods based on the physical deformation of the fiber [62], diffusion of
the core dopants in special nitrogen-doped Ge free fibers [63, 64], or refractive
index variation produced by CO2 lasers [65], CO laser [63, 64], ion implantation
[66], or electrical discharges [62, 63, 67, 68] (Fig. 19).

Fig. 19 Scheme of a LPG, indicating their parameters, and its characteristic spectrum when the
light goes through the grating. Reprinted from Sens. Actuators B, vol. 227, Urrutia A. et al.,
Simultaneous measurement of humidity and temperature based on a partially coated optical fiber
long period grating, pp. 135–141, (2016), with permission from Elsevier
74 J. Ascorbe et al.

LPGs have been also studied as humidity sensors [69–74]. Different materials
have been checked as the sensitive layer for humidity sensing purposes. In [69],
poly(ethylene oxide)/cobalt chloride (PEO/CoCl2) as a hybrid hygrosensitive
cladding coating. The material parameters associated with the sensing mechanism
may include those of refractive index, absorption, and morphological alterations of
the overlaid material. Relative humidity variations in the range from 50 to 95 %
have been detected with a resolution better than 0.2 %. The response time constant
of the fiber sensor is of the order of a few hundred milliseconds. Maximum
wavelength shift of 6 nm have been obtained, but the response of this hybrid
coating is nonlinear. In [70] a hydrogel has been used as the sensitive material
obtaining a linear wavelength shift of 12 nm for humidity changing from 30 to
100 %. Other approach has been followed in [73] where the LPG has been coated
by means of electrostatic self-assembly method with PAH, PAA and silica nano-
spheres. Wavelength shifts of 14 nm have been obtained for RH varying from 10 to
80 %. Optical spectra for different values of RH are shown in Fig. 20. It has been
also checked the influence of temperature on the sensitivity, which has not
noticeable effect.
Finally, in [74] a simultaneous measurement of temperature and RH has been
accomplished by a half-coated LPG. When half of the LPG coating was chemically
removed the main attenuation band was split into two different contributions, one of
them due to the grating and the other due to the coating. When this semi-coated
LPG was also exposed to RH and temperature tests, the new two attenuation bands
presented different behaviors for humidity and temperature. This novel
dual-wavelength based sensing method enables the simultaneous measurement of
RH and temperature using only one LPG (Fig. 21).

Fig. 20 LPG spectra: a theoretical simulation for different refractive index values of the overlay;
b experimental results for different relative humidity levels. Reprinted from A fibre optic humidity
sensor based on a long-period fibre grating coated with a thin film of SiO2 nanospheres, Viegas, D.
et al., 2012, Meas. Sci. Technol. 20 034002, doi:10.1088/0957-0233/20/3/034002 with permission
from IOP Publishing
High Sensitivity Optical Structures for Relative Humidity Sensing 75

Fig. 21 a Transmission spectra evolution of the partially-coated LPG as the RH is changed.

b Wavelength shift of both attenuation bands during the RH variation, c Transmission spectra
evolution of the partially-coated LPG as the temperature is changed. d Wavelength shift of both
attenuation bands with the temperature variations. Reprinted from Sens. Actuators B, vol. 227,
Urrutia A. et al., Simultaneous measurement of humidity and temperature based on a partially
coated optical fiber long period grating, pp. 135–141, (2016), with permission from Elsevier

5 Conclusions

There are several ways to measure relative humidity by optical set-ups and by
optical fiber humidity sensors. Here, we have delved into lossy mode resonances
and Fabry-Pèrot interferometers, and LPGs have been briefly commented. These
structures have been chosen for this review because each of them presents an
optimal feature to function as an optical fiber sensor. Although there are more
structures that have not been analysed, some interesting conclusions can be
extracted from those that have been explained here.
First of all, polymeric coatings and inorganic salts usually present nonlinear
behaviour, especially at high relative humidity values where they have their greatest
sensitivity. Metal oxides and semiconductors oxides are a good choice for obtaining
linear responses and good sensitivities in the 20–90 % RH range. Their response
times are usually smaller than those of hygroscopic materials.
With regard to optical structures, there should be an agreement between the
wanted spectral width of the attenuation band and its displacement. LPFGs need a
fabrication process to obtain the grating which requires a specific machine. They are
76 J. Ascorbe et al.

not sensitive to external parameters by themselves and they need an external

coating besides the grating. For lossy mode resonances generation, it is also need
some process for getting access to the evanescent field. This process is simpler than
that used for the development of a LPFG and usually consists on a chemical method
to remove partially or completely the cladding. LMRs are a physical phenomenon
which allows to generate the absorption peak with the same material that will act as
the sensitive layer simplifying the process to obtain an optical fiber humidity sensor.
Finally, Fabry-Pèrot interferometers, developed by coating the tip of an optical
fiber, seems to be a good choice to obtain optical fiber humidity sensors because of
their good performance and their relatively easy method to obtain them. They are
also the less invasive way to measure with optical fibers.

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Oxygen Gas Sensing Technologies
Application: A Comprehensive Review

P. Shuk

Abstract Different oxygen gas sensing technologies, i.e., potentiometric, amper-

ometric, paramagnetic and tunable diode laser spectroscopy (TDLS) are reviewed in
details. Special attention is given to the theoretical aspects and operation basics of
the technologies, application limits and analyzers or system requirements. A com-
prehensive technologies review is supported with the latest developments trends
especially on the potentiometric zirconia and tunable diode laser analyzers.

1 Introduction

Oxygen is the third most abundant chemical element in the universe, after hydrogen
and helium, and is one of the most important elements required to sustain the life
[1]. Oxygen is vitally important not only to the existence of the human and animal
life with ∼3 million tons daily of oxygen consumption just for the respiration [2]
but also very critical for any combustion process at power generation, chemicals
production, heating, process control, safety, and quality. A major oxygen gas
sensing application is for the combustion process optimization. The air required for
the oxidation of hydrocarbons (fossil or bio fuels) is optimized to ensure the fuel
complete combustion with the highest possible efficiency [3, 4]. Oxygen excess in
the combustion in normally measured in the flue gas not far away from the fire ball
or box and the fuel/air ratio supplied to the burner is controlled to the ideal mini-
mum of oxygen or air excess (Fig. 1). The oxygen is also measured to minimize
runaway combustion sometimes leading to the explosion and to control the product
formation and quality. Some oxygen sensors work at ambient conditions where
oxygen is either dissolved in liquid or solid or oxygen measurements have to be

P. Shuk (✉)
Rosemount Liquid and Combustion Analysis, Emerson Process Management, Emerson
Electric Corp. 2400 Barranca Pkwy, Irvine, CA 92606, USA
e-mail: [email protected]

© Springer International Publishing AG 2017 81

S. Mukhopadhyay et al. (eds.), Sensors for Everyday Life, Smart Sensors,
Measurement and Instrumentation 23, DOI 10.1007/978-3-319-47322-2_5
82 P. Shuk

made under ambient conditions. Mostly these sensors are applied in medical, food
processing and waste management industries. The oxygen sensors used under
ambient conditions include Clark type cells [5], paramagnetic [6] and optical
sensors [7, 8].
The high temperature oxygen sensors can be based on the potentiometric or
amperometric electrochemical cells and resistive semiconductors [9, 10]. Poten-
tiometric sensors measure the equilibrium voltage of the cells according to the
Nernst equation and would require the reference. The amperometric oxygen sensor
with fixed applied voltage and oxygen diffusion barrier is based on electrical current
dependence on oxygen concentration and can be only successfully applied to very
clean environment and this technology was discussed in many details elsewhere
[11, 12].
The resistive oxygen sensor is based on semiconductors with the defect
concentrations varying exponentially with the oxygen concentration [13]. The
sensitivity of the surface to the particular gas can be as low as parts per billion
(ppb) [14–17] and it is highly desirable that metal oxide semiconductor sensors
have a large surface area, so as to adsorb as much of the target analyte gas on the
surface as possible, giving a stronger and more reliable response especially at low
concentrations. The applications of the semiconductors oxygen sensors in severe
combustion process would be highly limited because of sensitivity, selectivity and
reproducibility issues [10].
Four major oxygen gas sensing technologies are applied in an in situ or
extractive mode to the combustion process environment and will be discussed in
more details.

30 80

N 70
25 2

Combustion
Gas concentration (%)

HO
Gas concentration (%)

2 control
20 60

15 50

CO
2
10 40

CO O 30
5 2

0 20
-5 0 5 10
% Deficiency % Excess
Oxygen concentration (%)

Fig. 1 Combustion flue gas concentration diagram

Oxygen Gas Sensing Technologies Application: A Comprehensive … 83

2 Zirconia Potentiometric Oxygen Gas Sensing

Technology

Zirconia potentiometric oxygen gas sensing technology widely used nowadays in

O2 analyzers for different industrial combustion applications and in automotive
Lambda sensors was invented in 1961 by Peters and Möbius [18] and Weissbart
and Ruka [19] and was rapidly accepted in the power industry traditionally more
conservative regarding the new technologies application. The first industrial zir-
conia oxygen analyser for the process gas application was developed early 70th by
Westinghouse Electric Co (Rosemount Analytical Inc.), and was based on the
advanced platinum cermet electrode and zirconia solid electrolyte technologies
developed initially for the application in solid oxide fuel cells.
All industrial zirconia oxygen sensors are based on an electrochemical cell with
solid electrolyte based mostly on yttrium on stabilized zirconia (YSZ) and two
platinum based electrodes printed and sintered on the opposite sides of the zirconia
ceramic and exposed to the process and reference gases:
0
O2 ðpO2 , Reference), PtjYSZjPt, O2 ðp′′O2 , ProcessÞ ð1Þ

The oxygen electrochemical reaction in the regular sensor with Pt-electrodes is

taking place on the triple phase boundary (TPB: electrode, electrolyte, and gas)
where oxygen molecules (O2), electrons (e-) and oxygen vacancies (VO..) are
available (Fig. 2a) and this electrochemical reaction would be expanding to the all
electrode bulk by using Pt-cermet electrode with electronic and oxygen ionic
conductivity (Fig. 2b). This reaction includes oxygen molecules absorption, dis-
sociation on the electrolyte/electrode surface, diffusion to the TPB and finally
oxygen electrochemical reaction:

(a) (b)

Pt-electrode Mixed conducting Process

Process
electrode
O2
e- O2 2- ..
O , V O, e
-

2- ..
O ,VO
2- ..
O , VO
Solid electrolyte Solid electrolyte

Fig. 2 Oxygen electrochemical reaction on TPB interface [20]

84 P. Shuk

O2 ðgas) ↔ O2 ðElectrolyte ̸Electrode)

O2 ðElectrolyte ̸ Electrode) ↔ 2O(Electrolyte ̸ Electrode)
ð2Þ
2O(Electrolyte ̸ Electrode) ↔ 2O(Electrolyte ̸Electrode ̸ Gas)
0
2O(TPB) + 4e ðElectrode) + 2V..O ðElectrolyte) ↔ OO ðElectrolyte)

The process side of the cell is gas tight separated from the reference side with the
special high temperature ceramic/metal/glass seals and zirconia ceramic is used in
the form of disc (Fig. 3), tube or thimble.
Differential oxygen chemical potentials on the oxygen cell electrodes would
develop electromotive force (EMF), E, according to the Nernstian equation:

RT pðO2 Þ′′Process
E= ln , ð3Þ
4F pðO2 Þ′Ref

with R universal gas constant, T the process temperature in Kelvin (K) and F the
Faraday number.
By using fixed oxygen partial pressure on the reference electrode, e.g., air with
20.9 % O2 and p(O2) = 2.1 * 104 Pa, the sensor signal of the thermally balanced
oxygen sensor will be only depending on the sensor temperature (Fig. 4). Oxygen
potentiometric gas analysis was established by Mӧbius [21] and is also permitting
measurements of not free but chemically bonded oxygen concentration <1 ppm
(part per million) or <1 ppb (parts per billion) O2 released in the reducing condi-
tions in the process and CO/CO2-ratio (Fig. 5) or H2/H2O-ratio (Fig. 6) can be also
calculated based on the oxygen sensor signal.
Pt electrode film microstructure is highly depending on the sintering temperature
and formation at lower temperatures would create much finer open porosity (Fig. 7)
contributing to the better oxygen molecules diffusion to TPB interface but the
electrode/electrolyte interface should be well established and lower temperature
sintered electrodes might not be reliable in the severe process environment with the

Fig. 3 Zirconia Ceramic or metal tube Zirconia Pt-electrodes

potentiometric oxygen gas disc
sensing cell

Reference gas Flue gas

air (20.9% O2 ) O2- p(O2)’’
p(O2 )’
Oxygen Gas Sensing Technologies Application: A Comprehensive … 85

0.1 0.25 0.5 0.75 1 c(O )

100 2
%

2
80

60 4
E (mV)

6
40
8

10
20

15

0 20
600 800 1000 1200 1400
o
T ( C)

Fig. 4 Potentiometric zirconia oxygen sensor signal-concentration-temperature diagram

significant temperature and pressure variation. A special, highly porous Pt-zirconia

cermet electrode formed at higher ∼1400 °C temperatures was developed at
Rosemount Combustion and Liquid Analysis with the special catalyst treatment to
refine and re-open TPB interface for the oxygen diffusion and oxygen electro-
chemical reaction (Fig. 8) improving zirconia oxygen sensor response and opera-
tion life.
Industrial zirconia oxygen sensors are operating at elevated temperatures with
oxygen ion migration in zirconia ceramics establishing oxygen equilibrium at the
process and reference electrodes and zirconia electrolyte interfaces at >300 °C
depending on the electrode composition and microstructure. Over 1400 °C oxygen
electrolytic permeability of the zirconia solid electrolyte ceramic might compromise
oxygen measurements. Higher application temperature will favour oxygen sensor
performance but would be highly limiting the high temperature ceramic/metallic
materials variety to be applied in the zirconia oxygen sensor packaging. Most
industrial zirconia oxygen sensors are operating at elevated temperatures around
700…800 °C. Disc-shape zirconia ceramics brazed into special metal alloy sup-
porting tube initially developed by Rosemount Analytical Inc. offer an advantage of
86 P. Shuk

10-20 c(O2)
1500
(%)
c(CO)/c(CO 2)
10-15
103
C
102
1000
10
10-10
E (mV)

10-1

500 10-5
10-2
10 -5
10 -4 10-4
10-3 10-3
CO2 10-2
0.1
0.4
1
8
0
700 800 900 1000 1100 1200 1300
T (oC)

Fig. 5 Potentiometric zirconia oxygen sensor signal dependence on CO/CO2 ratio

the much less differential temperature profile across the cell on the reference and
process sides compared to the tube or thimble ceramic shape and less thermal stress
considering a good thermal expansion coefficients (TEC) optimization of all
involved in the oxygen sensor packaging metallic and ceramic materials. The small
oxygen sensor is gas tight sealed at O2 analyzer probe end for in situ operation
(Fig. 9) or process flue gas can be alternatively delivered to the sensor using special
extractive gas guiding tube [22]. The special protective shield, internal calibration
line and reference gas line made from the special alloys like Inconel, Hastelloy or
stainless steel 316L were implemented in the probe design to resist severe high
temperature process environment. With these entire improvements zirconia probe
can very precise measure in situ oxygen concentration down to 10 ppm (Fig. 10).
A special oxygen cell with improved thermal balance and ceramic or metallic dif-
fuser for the process gas particulate filtration was designed to improve O2 analyzer
[20] delivering an excellent stability (<0.1 % O2) and reproducibility (±0.01 % O2)
in 2…5 % oxygen combustion concentration range (see Figs. 11 and 12).
Typical installation points of Zirconia O2-probe in a coal fired boiler as it can be
seeing from Fig. 13, would be located before or after heater exchanger
Oxygen Gas Sensing Technologies Application: A Comprehensive … 87

10-20 c(O2)
1400
%
c(H2)/c(H 2O)
103 10-15
1200 10 2

10
1000 1

10-1 10-10

800 10-2
E (mV)

10-3

600 10-4

10-5 10-5

400 H2O 10-4

10-3
10-2
200 0.1
0.4
1
8
0
700 800 900 1000 1100 1200 1300
o
T ( C)

Fig. 6 Zirconia oxygen sensor signal dependence on H2/H2O ratio

o
1400 C 1200 oC o
1000 C

Fig. 7 Pt electrode microstructure dependence on the temperature

(economizer). For the combustion control and higher efficiency single or multiple
probe systems might be used depending on the duct size and economizer outlet.
Additional probes may be mounted downstream monitoring the air entrance to
ensure efficient operation of fans and dampers. In the combustion process due to
88 P. Shuk

Fig. 8 SEM image of

Pt-cermet process electrode
[20]

Fig. 9 In-situ O2 analyzer

(Rosemount Liquid and
Combustion Analysis)

O2-cell

centrifugal forces, fly ash is concentrated towards the duct outer wall following
bends in the duct and the installation of Zirconia O2 analyzers in these locations
should be avoid to reduce the probe body erosion in the high velocity and high
concentration abrasive fly ash environment. There is a good Zirconia O2-probe
installation practice (Fig. 14) reducing very fine fly ash accumulation inside the
oxygen sensor on the process electrode and on the protection filter on the probe end.
In the oil and gas fired applications these problems are not present.
Zirconia O2 analyzer was applied with very good success in the combustion
control of power generation boilers, hot stoves for steelmaking, heating and com-
bustion exhaust gas control of coke ovens for steelmaking, lime and cement kilns
Oxygen Gas Sensing Technologies Application: A Comprehensive … 89

200 O -Analyzer with linearity ~0.9999:

10 ppm O2
2
±0.75% error or <±0.05% O 2 accuracy

150
E (mV)

100

50

0
0.0001 0.001 0.01 0.1 1 10
c (O ) (%)
2

Fig. 10 Zirconia O2 analyzer linearity

10
6888 O 2 probe drift at 0.41%, 2.0 and 8.0% O 2 (3/5...9/8/14)

8.0±0.1 % O2
8

6
c (O ) (%)
2

2.00±0.06 % O2
2

0.41±0.01% O2

0
Mar/19/14 Apr/12/14 May/6/14 May/30/14 Jun/24/14 Jul/18/14 Aug/11/14 Sep/4/14
Date

Fig. 11 Zirconia O2-analyzer stability

combustion control, incinerator combustion control, combustion control of heating

furnaces for oil refinery and petrochemical industry and many other applications.
After 45 years zirconia potentiometric oxygen gas sensing technology is still
90 P. Shuk

70
Zirconia O 2 Analyzer reproducibility at 2...5% O 2 :
<±0.01% O 2
60
2% O2 2% O 2
E (mV)

50
3% O2 3% O2

# 1
4% O 2 4% O 2 # 2
40 # 3
# 4
5% O 2 # 5

30

0 5 10 15 20
t (min)

Fig. 12 Zirconia O2-analyzer reproducibility

Secondary
600-700 C
o
combustion zone

Zirconia
O2-probe Primary
Economizer combustion zone
installation
options
o
~400 C

Flue gas

Fig. 13 Zirconia O2-probe installation locations in coal fired boiler

dominating the combustion market because of the high reliability, accuracy in the
most of applications and relative low price. Ametek, Rosemount Liquid and
Combustion Analysis, Yokogawa and ABB are the major players on the in situ
Oxygen Gas Sensing Technologies Application: A Comprehensive … 91

Zirconia
O2-probe

Flue gas

s
ga
ue
Fl
s
ga
ue
Fl

Fig. 14 Zirconia O2-probe recommended installation options in flue gas

Fig. 15 In-situ Zirconia O2-analyzers on the market

oxygen measurements market (Fig. 15). The performance of Zirconia O2-Analyzers

on the market is summarized in Table 1.
There have been numerous attempts to miniaturize oxygen sensor with innovative
reference like sealed chamber and oxygen pump [23] or glass sealed metal/metal
oxide references electrode [24–26] but the evaluation couldn’t confirm these designs
reliability in traditionally difficult stack gas or waste combustion gas analysis.
92 P. Shuk

Table 1 Standard zirconia in situ O2-analyzers performance and materials

Company In situ Accuracy Operation O2-sensor Materials
O2-probe temperature temperature
(°C) (°C)
Rosemount 6888 O2 ±0.75 % 704 or 825 736 316L SS
(USA) or ± 0.05 % E-Brite
O2
Yokogawa ZR202G ±1.0 % error up to 700 750 316 SS
(Japan) Hastelloy
ABB (Swiss) Endura ±0.75 % up to 800 700 316L SS
Z20 or ± 0.05 %
O2
Ametek (USA) WDG ±1.0 % up to 677…800 615 310 SS
In situ or ± 0.05 %
flue O2
Enotec (Germany) Oxitec ±0.2 % of up to 800 840 316 SS
5000 MV* 1400 (with
cooling tube)
Fuji (Japan) ZKF8 ±0.5 % up to 800 800 316 SS
of FS** 304 SS
GE-Panametric FGA311 ±3 % up to 650 700 316 SS
(USA) or ± 0.1 % up to 1050 (HT) Inconel
O2
Energy Support (Japan) TF-10 ±1.0 % up to 300 ∼800 305 SS
of FS** 308 SS
LamTec (Germany) LS2 ±2.0 % up to 300 ∼800 305 SS
or ± 0.2 % 308 SS
O2
Zirox (Germany) SS28 ±5.0 % up to 800 700…800 1.4841
(314 SS)
ETC (UK) ETC ±1 % of up to 540 ∼800 305 SS
2800 MV* 308 SS
Ceramic Oxide JS probe ±0.1 % O2 up to 600 70 316 SS
Fabricators (Australia)
Novatech (Australia) 1231 ±1.0 % up to 800 800 316 SS
* MV—Measured Value, ** FS—Full Scale

3 Tunable Diode Laser Spectroscopy (TDLS)

Tunable diode laser spectroscopy (TDLS) is an innovative optical measurement

technique utilizing semiconductor lasers to detect a variety of gases (Fig. 16),
including oxygen in the near infrared (IR) range to deliver part per millions
(ppm) level measurements [27–30].
Over the last ∼45 years, tunable diode laser (TDL) absorption sensing has
become an established method for non-intrusive measurements of gas properties in
Oxygen Gas Sensing Technologies Application: A Comprehensive … 93

Fig. 16 Diode laser types and combustion gases versus wavelength [30]

combustion environment due to the robust, compact, low-cost TDL sources, and the
convenient overlap of TDL wavelengths with absorption bands of O2. CO, NOx,
H2O, CO2 combustion gases. TDLS with the ability to interface directly with the
process gas and eliminating the need for the very high cost and high maintenance
sample handling systems would be ideal for the real time dynamic measurement of
the process conditions. With the federal, state and private companies multi billions
investments TDL analyzers have now comprehensively established themselves as a
core measurement technology within the portfolio of the gas analysis techniques
available on the market [29, 31–33].
The infrared absorption spectrum of the flue gases is like a fingerprint, providing
oxygen identification at ∼760 nm (Fig. 17) and measurements in a wide concen-
tration range down to ∼80…100 ppm as a detection limit.
With the longer optical path length a higher absorption and better sensitivity will
be achieved. Laser wavelength can be changed over a wide range by changing the
laser operation temperature and over a narrow range by changing the applied
current to the laser. Tunable lasers enabling the miniaturization of transmission and
receiving units, provide highly sensitive, quantitative measurements with the fast
response time without the need for the frequent calibration. TDL analyzers have
been shown to be capable of the effective, accurate measurement even loosing up to

CO
2330 nm
CO 2
1960 nm
NO
1800 nm
CO
1570nm
H 2O
1390nm
O2
760nm

500 1000 1500 2000 2500

IR wavelength (nm)

Fig. 17 Combustion gases near IR absorption lines used in TDLS detection

94 P. Shuk

Fig. 18 Partial spectrum of

oxygen at 760 nm [34]

90-95 % of the original signal in the dusty environment. TDL spectroscopy is

highly distinguishing from the conventional process photometry by the laser ability
to be scanned across the narrow oxygen absorption peaks (Fig. 18) many times per
second by trimming the current through the laser. Thus the baseline and peak are
continuously measured allowing recalculation of the background. While conven-
tional optical filter bandwidth is >5 nm, a laser scan (0.2…0.3 nm typical range)
would provide much better resolution and selectivity [35].
Wavelength-modulation spectroscopy (WMS) as a derivative form of absorption
spectroscopy has been increasingly applied to these measurements improving
sensitivity and selectivity over the direct absorption and would be especially
favourable in the harsh and noisy combustion environment [36–38]. Many of the
calibration-free WMS methods could be very useful for certain cases with known
and stable environmental conditions but would be difficult to employ in some
practical environments with the most of the environmental conditions unknown and
laser intensity rapidly varying due to the vibration, window-fouling, beam-steering
and some interfering species, elevated pressures and temperatures broadening the
absorption peaks [38]. The single gas adsorption line selection was found to be very
critical with some absorption lines changing less with the temperature and pressure
variation. To eliminate moisture (H2O) interference at high temperature for O2/CO
measurements a spectral survey was done to determine optimum adsorption lines
and baseline treatment algorithms were developed to minimize effects of the
overlaps. Balanced detector circuit developed by IBM (Hobbs) with a reference
detector to reduce or eliminate common mode laser noise was implemented after
TDL analyzer testing in the real process environment [32].
The use of the digital signal processing and increasingly sophisticated
methodologies continue to improve TDLS sensitivity and selectivity. Initially
0.70…1.70 µm wavelengths laser diodes were developed for telecommunications
helping to cover the most gases presented in the combustion environment (see
Fig. 1). At near IR wavelengths, molecular absorption band strengths are signifi-
cantly weaker than in the fundamental absorption region and high sensitivity
Oxygen Gas Sensing Technologies Application: A Comprehensive … 95

detection techniques such as Frequency Modulation Spectroscopy (FMS) and

Wavelength Modulation Spectroscopy (WMS) were employed to improve sensi-
tivity and selectivity. Higher sensitivity can be also achieved by using specific
microstructures such as Hollow-Core Photonic Bandgap Fibres (HC-PBFs) or high
Q cavities that provide longer absorption path lengths for the gases. In micro-sphere
based optical cavities, light can be confined by total internal reflection in a so-called
Whispering Gallery Mode (WGM) [39]. As the light is guided along the spherical
surface of the glass-gas interface, a significant part of the evanescent optical field
exists outside the micro-sphere and can be used to interact with gas and to measure
the optical absorption. Q factors in glass micro-spheres can be as high as 10 million
giving a huge increase in the effective path length and hence absorption sensitivity.
TDL O2 analyzer would provide near real time measurements with no cross
interference to other gases in the combustion environment with an advantage of
non-contacting procedure suitable for many aggressive applications.
Considering initially the alignment across the gas stream (Fig. 19) as a major
issue in the reliability of oxygen measurements there were some attempts to spread
the laser beam to keep the alignment but this would significantly reduce the signal
intensity and signal-to-noise ratio, making the measurement sometimes more
erratic. Another approach with flexible bellows improving the alignment reliability
in the vibration environment was implemented by Yokogawa (Fig. 20).
Highly promoted by Mettler-Toledo Process Analytics an in situ TDL O2-probe
(Fig. 21) with the deflector on the probe end would eliminate misalignment
problem but this in situ probe will be exposed to the severe process environment
and deflection mirror or prism would be limiting factor for the probe’s operation
temperature. TDL O2-probe would provide single point measurement like Zirconia
in situ O2-probe but at much higher cost.
Even TDL O2 analyzer is promoted to provide the most accurate average O2-
reading in the process, considering the flue gas stratification in the duct, with ∼1…
5 % oxygen concentration variation, a laser beam ∼5…20 cm in diameter shooting

Fig. 19 A typical installation of TDL O2-analyzer across the combustion duct [40]
96 P. Shuk

Fig. 20 Alignment
improvement with flexible
bellows without affecting the
process seal [41]

Fig. 21 An in situ TDL O2-

analyzer for the clean
(top) and dusty applications
[42]

across the duct, would be unlikely much more representative than zirconia O2-
analyzer single point measurement. With the increasing temperature oxygen
absorption intensity would be reduced [43] and this might bring some challenge in
the interpretation of weaker intensity at higher temperature and temperature vari-
ation compensation affecting oxygen concentration calculation and contributing to
signal to noise ratio reduction. Temperature and pressure variation in the process
even claimed to be compensated might bring an additional error in the oxygen
measurements. Calibration and validation of TDL O2 analyzer on line is still
waiting for a conclusive answer. Implemented in some TDL instrumentation a
reference cell has a different temperature compared to the process and is very short
to provide very reliable in situ validation. Alignment across the stack and IR light
reflection at high temperature combined with the process windows fouling and wide
background radiation from the fire ball or box would bring many challenges in the
application and might reduce service life of the TDL O2-analyzer. Fiber coupled
Oxygen Gas Sensing Technologies Application: A Comprehensive … 97

Fig. 22 TDL O2 analyzers on the market

laser solution increases the optical noise by a factor of 5–7 compared to the free air
lasers [43] and would reduce the sensitivity with detection limit ∼500 ppm. The
major players on TDL analyzers market are Neo Monitors (Norway), Yokogawa
(Japan), Focused Photonics Inc. (China) and Siemens (Germany) (Fig. 22).
One significant difference between traditional Zirconia O2-sensor single point
measurements and TDL O2 analyzer path average measurements is that the path
measurement does not provide spatial information [33]. Zirconia O2 probes are
providing a measurement at a particular point in the process with very useful
information identifying variations in O2 concentration levels caused by burner to
burner (unbalanced burners) and this information can be successfully used for the
burner diagnostics.
More details on TDLS theoretical background and application can be found in
the latest reviews [29, 30, 44–47]. Performance and application option of some of
TDL O2 analyzers on the market is summarized in Table 2.
With wide applicability, TDL O2 analyzers are enjoying great popularity but
being ∼4−5 times more expensive compared to the zirconia O2 analyzers and
additional, very expensive and sophisticated up to 4 months installation [32, 33] are
generally covering right now special chemicals production and very high temper-
ature (>1400 °C) applications where zirconia O2-analyzers would be rejected by
severe temperature environment or the probe might contaminate the chemicals in
the production. An extractive zirconia O2 analyzer might be considered as an
alternative less expensive option for these applications. Majority of the combustion
systems is still using zirconia oxygen O2 analyzers.
98 P. Shuk

Table 2 Tdl O2 analyzers performance and application options

Company Product Detection Accuracy Application
limit
Yokogawa TDLS8000 Application ±1.0 % Across the duct,
(Japan) dependent or ± 0.01 % Installation over the fire
O2 ball
Siemens SITRANS SL 0.02 % O2 ±1.0 % Across the duct
(Germany)
ABB (Swiss) LS4000 0.05 % O2 ±0.2 % Across the duct
No nitrogen purging
required
Ametek (USA) TDLAS 5100 0.01 % O2 ±1.0 % Extractive
or ±0.03 %
O2
Servomex SERVOTOUGH 0.01 % O2 ±1.0 % Across the duct
(UK) MiniLaser Oxy or ±0.01 %
O2
Sick Maihak TRANSIC151LP 0.01 % O2, ±0.2 % O2 In situ probe (<80 °C)
(Germany) O2
Mettler-Toledo TDLS GPro 500 0.01 % O2 ±2.0 % In situ probe (250 °C or
(USA-Swiss) or ±0.01 % 600 °C with thermal
O2 barrier)
Fuji Electric ZSS6 O2/CO N/A ±2.0 % of Across the duct,
(Japan) Analyzer (0.01 % O2?) FS Dual measurement
NEO Monitors LaserGas III SP 0.01 % O2 ±1 % Across the duct
(Norway)
Focused LGA-4100 0.01 % O2 ±1 % Across the duct &
Photonics Inc. (in situ) extractive
(China) LGA-4500
(extractive)
TDL Sensors LGM-CD 0.05 % N/A Across the duct
Ltd (UK) 20 ppm O2
Zolo ZoloBoss 0.01 % O2 ±0.5 % Across the duct
Technologies 4-channel unit (O2,
(USA) CO, CO2, H2O)
Oxigraf Inc. O2iL, O2iC, O2E, 0.01 % O2 ±0.2 % Extractive
(USA) O2E2, O2C, O2D,
O2L

4 Paramagnetic Oxygen Gas Sensing Technology

Oxygen with two unpaired electrons is well known paramagnetic gas and would be
attracted into a strong magnetic field. These paramagnetic properties enable rela-
tively selective oxygen measurements method used by industries over fifty years
and applied in three different methodologies: magnetodynamic, thermomagnetic or
magnetic wind and non-contact Quinke method [48]. The magnetodynamic oxygen
Oxygen Gas Sensing Technologies Application: A Comprehensive … 99

sensors are dumbbell or of the magnetic pressure type. In the dumbbell type O2-
sensor incorporates two nitrogen-filled glass spheres mounted on the rotating sus-
pension (Fig. 23). This assembly is in a strong magnetic field and with the gas
sample containing oxygen introduced into the magnetic field, the oxygen molecules
will tend to approach the strongest part of the magnetic field pushing the dumbbell
aside and causing the suspending wire to be twisted. This twist is detected as the
movement of the light from the reflective mirror located at the suspending wire
centre (Figs. 23 and 24). The output from the photo-sensor would be fed back to a
coil around the suspension assembly restoring torque to the original “zero” position.
The current would be directly proportional to the magnetic susceptibility of the
sample oxygen gas and oxygen partial pressure. The applied current will be pro-
portional to the oxygen concentration in the gas mixture and would be used for the
precise oxygen calculation. This method with the high linearity and good response
is however highly sensitive to the different mechanical shocks, like vibration. In the
magnetic pressure type O2-sensor a small amount of reference gas like pure
nitrogen or air is externally supplied through a small hole made on one of the
magnetic poles. When the sample gas is introduced into uneven magnetic field,
paramagnetic oxygen gas would be attracted toward the strongest part of the
magnetic field, in which the magnetic poles have come closer to each other. The
increase in pressure resulting from the attraction of oxygen can be detected with a
capacitor microphone type detector or a mass flow sensor. In order to ensure the
stable signals detection, the two magnetic poles are alternately excited to amplify
the alternating current. The selectivity of this method is pretty high but a reference
gas would be required for these measurements. Thermomagnetic O2-sensor (mag-
netic wind method) has two chambers with heating wire element located at the
centre. A magnetic field would be provided only on the measurement chamber.

Fig. 23 Paramagnetic O2-sensor schematically [49]

100 P. Shuk

Fig. 24 Paramagnetic O2-sensor operation [50]

After the analysing oxygen gas is entering the measurement chamber, oxygen
would be attracted by the magnetic field and then heated using the heating wire
element. The magnetic oxygen flow would be cooling the heating wire element as
its intensity varies proportional to the oxygen concentration. The resistance changes
during this process would be picked up as unbalanced voltage at the Wheatstone
bridge to measure the oxygen concentration. The magnetic wind type analyzer has
no movable parts and is more stable in the vibration environment. Carbon dioxide
with the some positive interference for oxygen by the small variation in the con-
centration can be compensated.
Quincke O2-detector utilizes a pneumatic Wheatstone bridge for the measure-
ments using a differential pressure or flow to determine the oxygen concentration.
Reference gas is used so the sample does not come in contact with the sensor. The
reference gas is divided into two flow paths recombining at the reference gas outlet,
where the sample gas is also introduced. A magnetic field is in one arm of the
reference gas outlet creating a back pressure related to the presence of the oxygen in
the gas sample.
Measurement range for the paramagnetic O2-sensor is typically between 0.05 %
and 100 % O2 and sensor can be very precise under certain conditions [48] but
would require quite expensive gas sample conditioning system to stabilize the
process gas flow, pressure and temperature and to remove hazardous gases and
dust. The major disadvantages of the paramagnetic oxygen sensors are the price,
low stability in the vibration environment and relative low accuracy (± 0.10…
0.25 % O2). Paramagnetic analyzers have been historically limited to the extractive
application with general use (Fig. 25) or intrinsically safe instrumentation version
(Fig. 26) and maximum external operation temperature up to 120−145 °C.
Oxygen Gas Sensing Technologies Application: A Comprehensive … 101

Fig. 25 Paramagnetic O2 analyzer [51]

Fig. 26 Intrinsically safe paramagnetic O2 analyzer [52]

Paramagnetic O2-sensor can be also implemented in Multicomponent gas

analyser like X-STREAM (Fig. 27) often used in a combination with gas condi-
tioning system (GCS) in Continuous Emission Monitoring System (CEMS).
With some good success paramagnetic O2-analyzers were used for the process
control and monitoring in the chemical and petrochemical industries, combustion
efficiency control, ceramic and cement industry, inert gas blanketing and industrial
safety in food and beverage industries. With gas handling design paramagnetic
oxygen analyzer will be well suiting for the precise (±0.2 ppm) atmospheric
oxygen measurements [54], can be miniaturized using MEMS [55] but can’t
overcome the technology weaknesses related to the not the strongest magnetic
102 P. Shuk

Fig. 27 Paramagnetic O2-sensor implemented in X-STREAM analyzer [53]

nature of the oxygen limiting the detection to >100 ppm O2 and moving parts in
the design highly limiting applications especially in high temperature and humid
vibration environment. Paramagnetic analyzers are lately often expelled by the new
advanced Tunable Diode Laser (TDL) analyzers (see Sect. 3 of this review) pro-
viding more expensive but likely more reliable and more precise measurements
according to TDLS publications.
Paramagnetic oxygen analyzers are applied to the measurement of trace oxygen
concentration in various manufacturing processes, city gas quality control, safety
control at various plants, oxygen concentration control of flammable gas containing
mixtures and coke dry quenching (CDQ) plants for the steelmaking.

5 Amperometric Oxygen Gas Sensing Technology

with Liquid Electrole (Clark Cell)

The electrochemical O2-sensors with liquid electrolyte date back to the 50th and
were used for the environmental oxygen monitoring providing warning of abnormal
conditions in industrial safety environments, i.e., mines, oil production facilities and
chemical plants. Oxygen measuring instruments containing electrochemical sensors
based on consumable lead anodes have been available for over 30 years [56]. These
type electrochemical oxygen sensors are metal-air battery type with the diffusion
limited barrier [56, 57] and oxygen sensor generates a current proportional to the
oxygen diffusion to the cathode limited by the diffusion film or capillary barrier
(Fig. 28). Such barriers are typically made of thin, low-porosity Teflon membranes.
Besides offering a mechanical protection to the sensor, the membrane performs the
additional function as a filter. Selecting the correct pore size of the membrane and
capillary is necessary to transfer the proper amount of gas molecules. The pore size
should be optimized to allow enough gas molecules to reach the sensing electrode
but be small enough to prevent liquid electrolyte from leaking out or drying too
quickly.
Oxygen Gas Sensing Technologies Application: A Comprehensive … 103

O2 O2

Diffusion film Capillary barrier

Cathode
Load resistor
Electrolyte

Anode

Fig. 28 Electrochemical O2-sensor with liquid electrolyte

Oxygen in contact with the cathode is reduced to hydroxyl ions, with a balancing
reaction of lead oxidation at the anode:

Cathode: O2 + 2H2 O + 4e − → 4OH

ð4Þ
Anode: 2Pb + 4OH − → 2PbO + 2H2 O + 4e −

This electrochemical reaction would be resulting in the lead anode oxidization

and with the cell electrochemical properties changes a periodic calibration would be
always required. The consumption of the lead anode would also limit the sensor life
therefore the major part of the oxygen electrochemical sensor with liquid electrolyte
should be constructed from lead anode (Fig. 29) to increase the operation life of the
sensor.
The lower would be the oxygen concentration to be measured the longer
operation life will be expected and these sensors are designed to last for not more

Fig. 29 Oxygen sensor schematic [58]

104 P. Shuk

Fig. 30 Oxygen sensor from

City Technology, Honeywell
Corp [59]

than one or two years. Some components of the flue gas like carbon dioxide (CO2)
and chlorine (Cl2) might increase the rate of the oxidation or would react with the
lead shortening the life of the sensor. A dust protector is normally installed on the
top of the sensor (Fig. 30) to reduce diffuser hole or film pluggage and a scrubber
filter is sometimes installed in the front of the sensor to improve the sensor
selectivity.
There is a limited selection of the filters with the different efficiency degrees. The
most commonly used filter medium is activated charcoal filtering most chemicals
except of carbon monoxide (CO) and hydrogen (H2).
This oxygen electrochemical technology with the liquid electrolyte has been one
of the key technologies enabling the availability of the small, compact instru-
mentation for different applications with the estimated over 50 million sensors sold
world-wide since 1980 [56] and this technology is still continuing to dominate
industrial safety application. Although lead was recognized as offering an attractive
combination of suitable properties some metals like cadmium, bismuth, antimony
and copper were identified as potential lead free candidates with only copper being
available in a high surface area wire form. With a number of alternative approaches
offering longer lifetime for lead-free oxygen sensors a little market penetration was
achieved so far. More details on the electrochemical oxygen gas sensing technology
with liquid electrolyte latest development can be found in the recent review [56].
These electrochemical oxygen sensors are mostly supplied by City Technology Ltd
(UK) and Drägerwerk AG (Germany) and are used primary for the industrial safety
or oxygen monitoring at room temperature in portable analyzers and Continuous
Emissions Monitoring Systems (CEMS) with the gas conditioning employed.

Acknowledgment The author would like to thank Rosemount Liquid and Combustion Analysis
for the research program support.
Oxygen Gas Sensing Technologies Application: A Comprehensive … 105

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Application of Practical Nitrate Sensor
Based on Electrochemical Impedance
Spectroscopy

Md Eshrat E. Alahi, Xie Li, Subhas Mukhopadhyay and L. Burkitt

Abstract Nitrate is a naturally occurring ionic compound that is part of nature’s

nitrogen cycle. Nitrates are readily lost to ground and surface water as a result of
intensive agriculture, disposal of human and animal sewage and industrial wastes
and the impact of elevated nitrate concentrations on water quality, has been iden-
tified as a critical issue facing New Zealand’s future. It is therefore, highly desirable
to monitor water quality to facilitate regional councils and central governments to
understand trends in concentrations and to develop a healthy water management
policy. Presently, water quality managers follow the traditional measurement sys-
tems that involve physically sampling water from remote sites and laboratory-based
testing. These methods are expensive, require trained people to analyze the data and
produce a lot of chemical waste. Due to the time and labor required, surface
samples are often only collected once per month and these risks missing significant
trends in nitrate loss. Therefore, it is of utmost important to develop low-cost,
robust embedded sensor nodes to detect the concentration of individual nutrients
like nitrate and nitrite in surface and ground water. The interdigital capacitive
sensor has been used to measure the different nitrate concentration. The sensor used
to measure also the temperature and humidity of the samples. The results have
shown that the sensor has high potential in a different application.

1 Introduction

Fresh water is an important part of New Zealand’s way of life and economy. The
water quality of lakes, rivers, streams, and aquifers in New Zealand is variable and
depends mainly on the dominant land use in the catchment. Water quality is good in
the areas of indigenous vegetation and less intensive use of land, however, it is
poorer where there are pressures from urban and agricultural land use [1]. Rivers in

M.E.E. Alahi ⋅ X. Li ⋅ S. Mukhopadhyay (✉) ⋅ L. Burkitt

Massey University, Palmerston North, New Zealand
e-mail: [email protected]

© Springer International Publishing AG 2017 109

S. Mukhopadhyay et al. (eds.), Sensors for Everyday Life, Smart Sensors,
Measurement and Instrumentation 23, DOI 10.1007/978-3-319-47322-2_6
110 M.E.E. Alahi et al.

New Zealand has reduced water clarity and aquatic life, and higher concentrations
of nutrients and Escherichia coli (E.coli) bacteria [1].
The growth of population and increasing agricultural land use have placed
increasing pressure on waterways. Between 1990 and 2012, the estimated amount
of nitrogen (N) that leached into the soil from agriculture increased 29 % [1]. The
reason for this was due to the numbers of livestock (6.4 million dairy cattle and 29.5
million sheep [2]) (and, therefore, urine contains high concentrations of nitrogen
(N)) and the use of N fertilizer. Between 1989 and 2013, total N concentrations in
rivers increased between 12 to 60 % in the 77 monitored sites around the country
which was monitored by NIWA, the National Institute of Water and Atmospheric
Research. The physical impact of excessive N concentrations in New Zealand rivers
can be nuisance plantopic algae (includes blue green algae), benthic algae (includes
periphyton) and macrophytes(rooted plants) growth. This growth reduces oxygen
levels in the water, hampers river flows, and smothers the riverbed and plant life,
which fish and other aquatic animals depend on for food and habitat. About 49 % of
monitored river sites currently have enough N to trigger periphyton growth. High
levels of N can also be harmful to fish [1]. A common form of nitrogen is nitrate,
nitrite, and ammonium. In the human body, nitrite can react with secondary or
tertiary amines forming nitrosamines, which are recognized as carcinogenic agents.
When existing in high concentrations in the blood, nitrite can also react with iron(II)
in hemoglobin to form methemoglobin, which has no ability to carry oxygen [3–5].
Nitrate can also have the same toxic effects because it can be reduced to nitrite by
bacterial colonies that reside within the mouth [6]. Anthropogenic actions, such as
agriculture, discharge of industrial and domestic wastewaters and vehicle emis-
sions, have caused the increases in the concentrations of inorganic nitrogenous
compounds in aquatic ecosystems [4, 6, 7]. Ingested nitrate from polluted drinking
waters can cause methemoglobinemia, particularly in young infants, and also have a
potential role in developing cancers of the digestive tract due to the formation of
nitrosamines [4]. The regular monitoring of the levels of nitrate in water is,
therefore, relevant because of their potentially harmful impact on both the envi-
ronment and human health.

2 Motivation

New Zealand’s lakes, rivers, and groundwater are regularly monitored by regional
councils, NIWA, and community interest groups. New Zealand’s river network has
a total stream length of 199,641 km. Regional councils monitor river water quality
to manage environmental impacts. NIWA also monitors water quality at 77 sites on
35 major river systems. Figure 1 indicates the different monitoring sites by NIWA.
These sites tend to be in catchments dominated by agricultural land use. Regional
councils measure a range of parameters at each of the sites they monitor. The
parameters include turbidity, rainfall, different nutrients (nitrate, nitrite, ammonium,
and phosphate), pH, Dissolved Oxygen (DO).
Application of Practical Nitrate Sensor Based … 111

Fig. 1 National River water quality network sites [1]

2.1 Present Status of Water Quality Study

Locally, a water quality monitoring study has been established at Massey

University’s Agricultural Experiment Station, called Tuapaka, to examine the
impact of hill country beef and sheep grazing on stream water quality. This farm is
located 15 km from the Massey University campus in Palmerston North and pro-
vides the resources for the testing and validation of a water quality sensor for nitrate
and nitrate. Currently, water samples are manually collected from Tuapaka every
two weeks and analysed for nitrate and ammonium concentrations measured using
the colorimeter method using a Technicon Auto-Analyzer in the laboratory.
112 M.E.E. Alahi et al.

Weirs (Fig. 2a) have been installed at various locations around Tuapaka
(Fig. 2b) to monitor stream flow and water quality. These sites will be used to test
and validate the sensors under field conditions. Stream and river water contain
sediment and organic material. Under the current manual sampling regime, samples
are filtered through a 0.45 µm filter prior to nitrate analysis. It will, therefore, be
important to test the sensors performance in the presence of sediments and organic
material. The sensors functionality and robustness will also need to be tested under
the harsh weather conditions experienced in the remote stream and river locations.

2.2 Current Laboratory Measurement System

Technicon Auto-Analyzer uses continuous flow system (CFS), which samples are
taken automatically from the sample tray and pump adds the appropriate reagents.
Samples are passed through manifold for mixing, filtering and heating. The col-
orimeter then measure the absorbance of color in the reaction of sample and is
displayed in the recorder [8].
Figure 3 shows the Technicon Auto Analyzer used to determine both of nitrate
and ammonium concentration in the laboratory using the current method. The Auto
analyzer is set up with a heating bath at 28–29 °C and uses 520 nm filters in the
colorimeter. A red azo dye and an indo-phenol prussian blue dye are used to
measure nitrate and ammonium respectively. Reagents used for nitrate-N detection
include catalyst solution, sodium hydroxide solution, hydrazinum sulphate solution
and so on (as shown in Fig. 3b). Reagents are pumped into the system for about
30 min to ensure the system is flushed completely. In the sample tray (Fig. 3a), the
prepared nitrate standard and water samples are put in the sample tray. The probe
will take each sample in the preset time interval into the system. The samples and
reagents are mixed in the system (Fig. 3c) and the measurement is done by a
colorimeter (Fig. 3d). The colorimeter analyzes the intensity of the color and the
results are displayed on a chart recorder in the computer. This recorder baseline
should be set along with the colorimeter baseline control before the measurement
starts by standard calibration. This method requires expensive equipment and
trained staff to conduct measurements in addition to the limitation on water samples
collection, which can only be collected periodically. This approach risks missing
key changes in nitrate-N concentration when river-flow rapidly rises or falls.
Although high-frequency nitrate sample equipment is available, these cost in the
order of $30–50,000.
Typically nutrient and sediment concentrations change with increasing and
decreasing stream or river flow rates (Fig. 4). Therefore, a monthly or fortnightly
sampling regime may not adequately represent the concentration nutrient profile.
This could influence our understanding of the seasonal effects on nutrient loss as
well as the total loads of nutrients (i.e. kg of nitrate/ha) estimated to be leaving a
catchment. This information is critical for reginal councils to implement policy and
management around water quality in their catchments.
Application of Practical Nitrate Sensor Based … 113

Fig. 2 Water sample

collection

(a) Paddock down the hill

(b) Monitoring sites in Tuapaka

114 M.E.E. Alahi et al.

Samples

Probe

(a) Sample Tray (b) Chemical Reagents

(c) Detection part (colorimeter) (d) Measured result

Fig. 3 Technicon Auto Analyzer currently used in the laboratory

2.3 Laboratory Based Measurement Technique

The maximum permissible levels of nitrate–N and nitrite–N in fresh waters at 10

and 1 mg L−1, respectively [9]. The determination of nitrite and nitrate has been
the study object of numerous researchers and a diversity of analytical methods have
been developed for this purpose [6]. These include kinetic methods [8], ion
chromatography [10, 11], gas chromatography–mass spectrometry [12], capillary
electrophoresis [13], electrochemical methods [14–18], luminescence [19] and
spectrophotometric methods [5, 20–26]. However, most of these methods have as a
disadvantage the employment of large volumes of toxic reagents, the application of
time-consuming procedures and complicated systems [27]. Therefore, the devel-
opment of simple, rapid and reliable methods for the quantification of nitrite and
nitrate is opportune.
Application of Practical Nitrate Sensor Based … 115

Fig. 4 Sampling date in comparison to flow rate

2.4 Market Research

Hach is well-known as suppliers of an analytical instrument and chemical reagents

for the laboratory-based purpose, especially for water quality and other liquid
solutions. Take IntelliCal ISENO3181 Nitrate Ion Selective Electrode (ISE) for
nitrate detection as an example; it is designed by the solid-state PVC membrane
with epoxy, and solid gel ion exchange eliminates the frequency of replacing
membrane. The ISE can only be used periodically in the lab or field and is not
suited to continual measurement. It can detect the nitrate-nitrogen concentration
from 0.1 to 14000 mg/L. It has an integrated temperature sensor which can measure
the temperature range from 0–50 °C. The price is at $2100. Hach Nitratax sc tank
sensor is being used extensively internationally and in New Zealand. It uses the UV
absorption measurement with reagent-free technique. There are three different
models with the different detection range: 0.1–100 mg/L by Nitratax plus sc; 1.0–
20 mg/L by Nitratax exo sc; and 0.5–20 mg/L by Nitratax clear sc. These models
cost around $40 k to 60 k.
“S::can” is Austria-based Company which provides varied product range for
water and environmental monitoring. All “s::can” instruments are operated fol-
lowed by the “plug & measure” principle, so all of them are ready to use with
pre-calibrated works. The “spectro::lyser” UV monitors can be used to NO3-N
detection. It is measured based on the UV-Vis spectrometry with the nitrate
detection range from 0–20 mg/L. This instrument is also being used extensively
116 M.E.E. Alahi et al.

internationally and in New Zealand. However, the whole set of the system is very
expensive (around $60–70 k).
Hanna Instruments is focused on developing electro-analytical instrumentation.
They provide the products like nitrate portable/benchtop photometer and nitrate ion
selective electrode. For example, Hanna HI96728 is a portable checker to detect
nitrate in freshwater based on the colorimetric method. A special Tungsten lamp is
used as the light source and silicon photocell with narrow band interference filter at
the wavelength of 525 nm used to detect the light. It uses the cadmium reduction
method to determine the nitrate-nitrogen concentration range from 0.0 to
30.0 mg/L. The price is at around $350 NZD.
Xylem is a world leader in providing compact instruments for water technology.
It has a broad range of products under different brands. YSI is one of Xylem brand,
which providing the environmental monitoring products. IQ SensorNet 182 is a
modular water quality terminal which allowed connecting additional sensors such
as 6884 Nitrate ISE sensor and it provides a continuously measurement of water
quality parameters like pH, Dissolved oxygen, temperature, conductivity, ammo-
nium, nitrate, potassium, TOC (total organic carbon), COD (chemical oxygen
demand), DOC (dissolved organic carbon share of TOC), BOD (biochemical
oxygen demand) and SAC (spectral absorption coefficient). It has an easy-to-read
digital display and wireless connection via radio transmission with a range of 100
meters. However, when it uses the nitrate sensor such as NitraLyt, the function of
real-time monitoring is disabled. Another Xylem brand—WTW, it provides online
measurement system—TresCon Analyzer which can monitor Ammonium, Nitrate,
and Nitrite continuously. A continuous water sample supply with low solids con-
tents is required for operating this system. For nitrate detection, the UV light is
absorbed by the nitrate ions and determines the nitrate concentration at a wave-
length of 254 nm.
ABB is a multinational corporation which mainly designs and manufactures
power and automation products, including flow measurement, gas and liquid ana-
lyzer and environmental monitoring systems. For example, UV Nitrate Monitor
AV455 provides a continuous analysis without chemical reagents. It can detect the
nitrate concentration at the range of 0–100 mg/L at a wavelength of 220 nm. It
requires low-maintenance and simple calibration with auto cleaning for the optical
component. It uses de-nitrification as a process to reduce the nitrate concentrations
for nitrate monitoring.
ASA Analytics Inc. specializes in the manufacture of the automatic chemical
analysis system. ChemScan 6101 Process Analyzer can monitor Ammonia,
Phosphate, Nitrate-Nitrite and Phosphate in surface water based on the
UV-spectrometric method. The light is absorbed by nitrate ions and into 256
wavelengths of 200–450 nm. The detection range of nitrate is from 0.5–20 mg/L.
Table 1 summarizes the commercially available nitrate detection product/system
in the market. Hanna HI 96728 is a portable device, but it still needs to collect the
sample and require the reagent for measurement of nitrate. The YSI IQ SensorNet
182 terminal provides the continuous monitoring, but it calls for an additional
sensor for nitrate measurement.
Application of Practical Nitrate Sensor Based … 117

Table 1 Summarize of commercially available sensors

Model Method of detection Detection range (Nitrate) (mg/L)
IntelliCal ISENO3181 Ion selective electrode 0.1–14000
Nitratax plus sc UV-photometric 0.1–100
S::can UV-spectrometric 0–20
Hanna HI96728 Colorimetric 0–30
YSI 6884 Nitrate Sensor Ion selective electrode 0.0–200.0
TresCon Analyzer UV-spectrophotometric 0.1–60
UV Nitrate Monitor AV455 Ion exchange 0–100
ChemScan 6101 Process Analyzer UV-spectrometric 0.5–20

3 Operating Principle of Interdigital Sensors

3.1 Interdigital Sensors

Interdigital sensors are made of comb-like or finger-like periodic pattern of parallel

electrodes on a solid phase substrate. These electrodes are used to build up the
capacitance which is related to the electric fields that penetrate into the test material
and carry useful information about the properties of the material sample [28]. One
of the most significant benefits of the planar interdigital sensors is the single-side
access to the Material Under Test (MUT). This property helps to penetrate the
sample with magnetic, electric, or acoustic fields from only one side. The strength
of the output signal can be controlled by changing the area of the sensor, the
number of fingers, and the spacing between them. The capability of being used for
non-destructive testing is another advantage of these sensors, which makes them
more useful for inline trial and process control applications [29].
Planar interdigital sensors follow the operating principle of parallel plate
capacitors. Figure 5 [30] shows a gradual transition from the parallel-plate capacitor
to a planar, fringing field capacitor, where electrodes open up to provide a
single-side access to the MUT.

Fig. 5 Gradual transition from the parallel-plate capacitor to a planar capacitor

118 M.E.E. Alahi et al.

Fig. 6 Geometric structure

of conventional planar
Interdigital sensor

Fig. 7 Electric field formed

for different pitch lengths [60]

The electrode pattern of the interdigital sensor can be repeated several times, to
get a stronger signal and keep the signal-to-noise ratio in an acceptable range [31].
The configuration of the conventional interdigital sensor is shown in Fig. 6.
When an AC signal is applied as an excitation voltage to the terminals, an
electric field is setup from positive to negative terminal. This electric field bulges
through the test sample via excitation electrode and is received by the sensing
electrode which carries useful information about the properties of MUT such as
impedance, density, chemical composition and so on.
Figure 7 shows the electric field formed between positive and negative elec-
trodes for different pitch lengths- the distance between two consecutive electrodes
of the same polarity. As it is illustrated in the figure, different pitch length (l1, l2 and
l3) shows different penetration depth. The penetration depth improves by increasing
the pitch length, at the cost of electric field strength that will get weaker with greater
distance between the electrodes at same potential (pitch length).

3.2 Novel Planer Interdigital Sensors

Novel interdigital sensors are designed with number of sensing electrodes as

compared to the excitation electrodes, to increase the penetration depth of the
Application of Practical Nitrate Sensor Based … 119

Fig. 8 Schematic excitation

patterns for multi-sensing
electrode interdigital sensors

Table 2 Geometric design parameters for four types of interdigital sensors

Sensor Pitch length Number of sensing Number of excitation Sensing area
type (µm) electrodes electrodes (mm2)
1-5-25 25 40 9 6.25
1-5-50 50 30 7 6.25
1-11-25 25 44 5 6.25
1-11-50 50 33 4 6.25

fringing electric field. Different geometries have been studied in research literature
[32–34]. Figure 8 shows the excitation pattern for a multi-sensing electrode in
interdigital sensor geometry.
The novel interdigital sensors have been fabricated based on different geometric
parameters. Table 2 shows geometric parameters of four different interdigital
sensors and Fig. 9 shows the schematic of 1-5-25 and 1-11-25 configuration of
newly designed planer interdigital sensors [35].

Fig. 9 1-5-25 and 1-11-25 configuration of novel interdigital sensors

120 M.E.E. Alahi et al.

A time-dependent sinusoidal electrical perturbation is applied to the excitation

electrodes of the interdigital sensor. The switching electric field bulges through the
test-sample via excitation electrode and is received by the sensing electrode which
carries useful information about the properties of the material under test nearby of
the sensing area [28, 29]. These sensors have several applications in manufacturing
process [36], environmental monitoring [34, 37–40], humidity and moisture sensing
system [41, 42], photosensitive detection [43] and gas sensor [44]. A sensing
system was developed based on the interdigital sensor to detect the dangerously
contaminated chemical in seafood [32, 40]. Another one was developed based on
the electrochemical impedance spectroscopy technique to monitor the presence of
phthalates in aqueous solution [37–39].

3.3 Electrochemical Impedance Spectroscopy (EIS)

Electrochemical Impedance Spectroscopy (EIS) is a popular and powerful method

to measure the resistive and capacitive properties of materials by applying a small
AC signal. EIS method can be applied in non-destructive testing, label-free
detection and single-sided access for different chemical analysis. Different appli-
cation of EIS had been reported such as the detection of fat contents in meat [45],
biotoxins in shellfish [32], bacterial endotoxin in food [46], phthalates in water and
juices [38], determination of the corrosive behavior of materials [47, 48] and
analysis of electrical properties for soymilk coagulation process [49]. EIS has
several applications in different research areas such as corrosion mechanisms [50],
coating evaluation [51, 52], optimization of batteries [53] and biosensing [30].
Among some methods available for impedance measurements, Frequency
Response Analysis (FRA) has become a de facto standard for EIS measurement
which is a rapid approach to evaluating the impedance variation in real-time. This
technique measures the impedance of the system over a wide frequency range and
compares the results with reference data. In order to ensure the system stability,
linearity, and repeatability, this method is rendered viable only for a stable and
reversible system in equilibrium [54–56].

3.4 Basic Principles of EIS

Electrochemical impedance can be measured by applying a small AC signal and

then measuring the phase shift in current signal on the applied potential. Electro-
chemical impedance is measured using a low excitation signal so that the cell’s
response is pseudo-linear. In a linear system, this current response to a sinusoidal
excitation potential will result in a sinusoidal current at the same frequency but
shifted in phase as shown in Fig. 10.
Application of Practical Nitrate Sensor Based … 121

Fig. 10 Phase shift in current

signal with reference to the
applied voltage

Impedance is defined as the measurement of the ability of a circuit to opposite

the flow of electrical current when a voltage is applied. In an AC circuit, impedance
is represented as a complex value which involves real part (resistance) and
imaginary part (reactance).
According to the basic Ohm’s law in Eq. 1, impedance is defined as the ratio of
potential, V and current, I;

V
R= ð1Þ
I

The excitation signal can be explained as a function of time;

Vt = V0 sin ωt ð2Þ

where Vt is the voltage difference at time t, V0 is the amplitude of the signal, and the
angular frequency is ω.It is given by (ω = 2πf) expressed in radians/second and
frequency, f, in hertz [57].
For a linear system, the response signal, It, has a phase shift, θ, with amplitude of
I0 which can be explained by

It = I0 sinðωt − θÞ ð3Þ

Equation 1 (Ohm’s Law) can be used to calculate the impedance of the system
given by;

Vt V0 sin ωt
Z= =
It I0 sinðωt − θÞ
ð4Þ
sinðωtÞ
= Z0
sinðωt − θÞ

The impedance, Z, now can be expressed in term of a magnitude of Z0 and a

phase shift, θ.
122 M.E.E. Alahi et al.

From Eq. 4, it can also be expressed in term of Euler’s relationship given by;

ejθ = cos θ + j sin θ ð5Þ

The impedance, Z, can be expressed in terms of potential, V, and current

response, I, given by;

Vt = V0 ejωt ð6Þ

It = I0 ejðωt − θÞ ð7Þ

Therefore the impedance, Z;

Vt V0 ejωt
ZðωÞ = = jðωt − θÞ = Z0 ejθ ð8Þ
It I0 e

= Z0 ðcos θ + j sin θÞ ð9Þ

The impedance now is in the form of real part (Z0 cosθ) and imaginary part
(Z0 sinθ).
Calculated impedance characteristics can be analysed using Nyquist plot and
Bode plot.

3.5 Data Presentation in the Form of Nyquist Plot and Bode

Plot

The Nyquist plot is a popular format for evaluating electrochemical impedance data
such as electrolytic solution resistance (Rs), electrode polarization resistance (Rp)
and double layer capacitance (Cdl). These parameters will be discussed in the
following sections. Nyquist plot represents imaginary impedance component
against real impedance component at each excitation frequency. The Nyquist plot
offers several advantages. The effects of solution resistance can be observed easily
using this format. One major drawback of the Nyquist plot is that there is no
information about the frequency in the Nyquist plot which makes it difficult to
calculate the double layer capacitance [55]. The Bode plot represents the absolute
impedance and the phase shift versus frequency.

3.6 Randle’s Electrochemical Cell Equivalent Circuit Model

Randle’s equivalent circuit is the most frequently discussed equivalent circuit [58]
used to interpret EIS experimental results in electrical form as shown in Fig. 11. It
Application of Practical Nitrate Sensor Based … 123

Fig. 11 Randle’s equivalent

circuit model

Fig. 12 The Nyquist plot for

the Randle’s equivalent
circuit

consists of solution resistance Rs in series connected to a parallel combination of

double layer capacitance Cdl to the charge transfer resistance Rct in series with
Warburg impedance Zw [30].
Randle introduced this model in 1947 [59] and it can be used to describe both
kinetics and diffusion processes taking place at the electrode-electrolyte interface.
The Nyquist plot from the equivalent circuit consists of a semi-circular region
followed by a 45º straight line, as shown in Fig. 12. In this model, the impedance of
a faradaic reaction consists of an active charge transfer resistance Rct, and a specific
electrochemical element of diffusion which is called Warburg element. The
semi-circular region represents a slower charge transfer at higher frequencies
whereas the straight line describes a faster mass-transfer at lower frequencies. Rct
can be calculated by extrapolating the semicircle to Zreal axis. Solution resistance Rs
can be calculated by reading the real axis value at the high-frequency intercept
which is the intercept near the origin of the Nyquist plot. Rct can be calculated by
extrapolating the semicircle to Zreal axis as illustrated in Fig. 11. Cdl can be
obtained from the frequency at the maximum of semicircle portion in the Nyquist
plot using ω = 1/Rct Cdl [58].
The absolute impedance as a function of frequency is given as;

Rct jωR2ct Cdl

ZðωÞ = Rs + − ð10Þ
1 + ω Rct Cdl 1 + ω2 R2ct Cdl
2 2 2 2

where the real part (Z′) is given by;

Rct
Z ′ ðωÞ = Rs + ð11Þ
1 + ω2 R2ct Cdl
2
124 M.E.E. Alahi et al.

moreover, the imaginary part (Z″) is given by;

ωR2ct Cdl
Z ′′ ðωÞ = − ð12Þ
1 + ω2 R2ct Cdl
2

The rate of an electrochemical reaction can be strongly influenced by diffusion of

reactants towards, or away from the electrode-electrolyte interface. This situation
can exist when the electrode is covered with adsorbed solution components or a
selective coating. An addition element called Warburg impedance, ZW, appears in
series with resistance Rct. Mathematically Warburg impedance is given by;
σw
ZW = pffiffiffiffiffi ð13Þ
jω

where, σw is Warburg diffusion coefficient. The diffusion of reactants to the elec-

trode surface is a slow-paced process which can happen at low frequencies only.
However, at higher frequencies, the reactants do not have enough time to diffuse.
The slope of this line gives Warburg diffusion coefficient.

4 Experimental Setup, Results and Discussion

The interdigital sensor is very sensitive to ambient temperature and humidity. The
first experiment was conducted to measure the impedance characterization in a
temperature range between 10 to 40 °C and obtain the linear relationship between
temperature and impedance. The second experiment was performed to get the
relationship between temperature and impedance by varying the humidity in dif-
ferent thermal condition. Then, the sensor was tested to observe the impedance
response in prepared diluted water samples from nitrates forms: ammonium nitrates
(NH4NO3) by commercial equipment-LCR meter.

4.1 Temperature Measurement

The sensor was tested in the Milli-Q water in the temperature range from 10 to
40 °C. The characteristics of the sensor can be extended to accommodate the
behavior of it outside the range. The objective of this experiment was to observe the
impedance response of the sensor to different temperatures.
Application of Practical Nitrate Sensor Based … 125

4.1.1 Experimental Setup

Figure 13 shows the experimental setup and it involved high precision Hioki
3522-50 LCR meter, Hioki 4-terminal probe 9140, mercury thermometer,
SCILOGEX MS 7-H550 Digital Hotplate and computer for data acquisition. The
hotplate had the maximum limit from ambient temperature to 550 °C. In order to
measure the water sample at a lower temperature (below room temperature), the
water sample was stored in the freezer initially to let its temperature fall close to
0 °C and then taken out for testing at room temperature. The mercury thermometer
was immersed in the water to obtain a continuous temperature reading. Meanwhile,
the sensing surface was also submerged in the water and starts to collect data when
the temperature reached to a certain degree. The heating plate was used to heat the
water sample to reach the desired temperature. The Parylene coated sensor
(1-5-50A) was used for this experiment.
The Hioki 3522-50 was used to obtain the measured parameters for investigating
the impedance values in the frequency range between 1 Hz to 100 kHz. The probe
9140 had two sets of terminals connected to the sensor and LCR meter. The HCUR
and LCUR were used to measure the current flowing through the sensor and HPOT
and LPOT were used to measure the voltage across the sensor. Table 4.4.1.1 illus-
trates the technical specifications of the Hioki 3522-50 LCR meter (Hioki 2001).

4.1.2 Results and Discussion

The parylene coated 1-5-50A sensor was immersed into the MilliQ water in varying
thermal conditions. The resistance (Rs) and reactance (X) part of the impedance

Thermometer

Computer

LCR Meter

Hotplate

Fig. 13 Lab setup for sensor response at different temperature

126 M.E.E. Alahi et al.

Fig. 14 Nyquist plot for testing MilliQ at various temperatures

were evaluated and plotted in Fig. 14. The X-axis shows resistance part of impe-
dance in Ω and the Y-axis shows the reactance part of the impedance in Ω. With the
increase in temperature, the total impedance is decreased. Each data point on the
plot indicates the impedance at a specific frequency.
Figure 15 shows the relationship between the resistance of impedance and the
frequency. The resistance is decreased with the increasing in temperature and the
sensitive range is significant till 400 Hz.
Figure 16 shows the reactance (X) of MilliQ to changing temperature plotted
against frequency. This parameter is used to measure the dielectric properties of the
MilliQ in different temperature.
The experiment was repeated at different times to observe impedance behavior
and to take average results for the measurement of temperature for Parylene coated
sensor. Table 3 shows the average measurement results for resistance (Rs) and

Fig. 15 Real part of impedance versus frequency in varying temperature

Application of Practical Nitrate Sensor Based … 127

Fig. 16 Imaginary part of impedance versus frequency in various temperature

Table 3 Temperature measurement

Sensor Pitch length Number of sensing Number of excitation Sensing area
type (µm) electrodes electrodes (mm2)
10 118037.7617 9.55 47125.9455 9.74
15 104281.2167 15.01 41141.9445 14.54
20 91693.88783 20.00 34318.99883 20.00
25 77142.05667 25.77 26339.72167 26.39
30 64181.38833 30.91 19565.99883 31.81
35 52901.83333 35.84 14054.88283 36.23
40 42392.83333 39.55 9658.2 39.75

reactance (X) at a different temperatures. As the linear relationship between the

impedance and temperature, the slope can be calculated by the Eq. 14:

ΔR R40 − R10
Slope = = ðEqu. 4.3.2.1Þ ð14Þ
ΔT T40 − T10

where:
• R40: Resistance value measured at 40 °C
• R10: Resistance value measured at 10 °C
• T40: Temperature at 40 °C
• T10: Temperature at 10 °C
Therefore, the slope for resistance part is (42392.83–118037.76)/(40–10) =
–2521.498. Similarly, replacing the ΔX with ΔR, the slope for reactance part is
(9658.2–47125.95)/(40–10) = –1248.92. Figure 17 shows the relationship between
the temperature and Rs. The resistance of impedance drops nearly linearly with the
increase in temperature.
128 M.E.E. Alahi et al.

Fig. 17 Relationship between the temperature and resistance part of impedance Therefore, the
temperature can be measured by Eq. 4.3.2.2

RT − R20
Tðo CÞ = + T20 ðEqu. 4.3.2.2Þ ð15Þ
slope

where:
• RT: Measured resistance value
• R20: Resistance value at 20 °C (which is the reference value)
• T20: Reference temperature is at 20 °C

4.2 Humidity Experiment and Result

This experiment observed the impedance characteristics as a function of humidity

and temperature. The experiment was tested at a temperature range from 20 to
40 °C with the step of 5 °C and the varied humidity was applied.
Figure 18 shows the experimental setup for obtaining the impedance of sensor in
the various temperature and humidity. It used the Thermo Scientific Heratherm
Compact Microbiological Incubator, LCR meter, Humidity and temperature por-
table sensor and computer.
The incubator can control the temperature between 17 to 40 °C but it cannot
monitor the humidity. Therefore, to vary the humidity, a small container with the
hot water was used to increase the humidity in the incubator.
However, this humidity rate could not be controlled exactly, so the humidity
range in this experiment depended on the volume of hot water in the container.
The LCR meter was used to obtain the parameters’ measurement for investigating
Application of Practical Nitrate Sensor Based … 129

Incubator

Sensor

LCR Meter

Portable Temperature
and Humidity Sensor

Fig. 18 Experiment setup for temperature and humidity measurement

the impedance value in the frequency range between 1 Hz to 100 kHz, and the
computer is used for data acquisition.
Figure 19 shows the Nyquist plot for the Parylene coated sensor test at 25 °C
with varying humidity. From the Fig. 19, the total impedance is reduced with the
increase in humidity. The relationship between the resistive part of impedance and
frequency at different humidity is shown in Fig. 20. The most sensitive area of the
sensor is from 1 Hz to 400 Hz.

Fig. 19 Nyquist plot for testing varying humidity at 25 °C

130 M.E.E. Alahi et al.

Fig. 20 Resistance part of Rs vs Frequency (25oC)

impedance versus frequency 300000
in varying humidity at 25 °C
250000

200000
54%

Rs (Ω)
150000
61%
100000
76%
50000
85%
0

1
2.257
5.094

25.95
58.57
132.2
298.4
673.4
1520
3430
7743
17480
39440
89020
11.5
Frequency (Hz)

Fig. 21 Resistance of impedance against humidity at 25 °C

Figure 21 illustrates when the increase in humidity, the resistance of impedance

reduces and it shows a good correlation with R2 = 0.9833.

4.3 Experimental Setup, Results and Discussion of Nitrate

Concentration

The first experiment was to test different concentration of Ammonium Nitrate

(NH4NO3) between 0.1 and 0.5 mg/L by using commercial measurement equip-
ment: LCR meter. The water samples were prepared using the serial dilution
Application of Practical Nitrate Sensor Based … 131

1.60E+05

1.40E+05

1.20E+05
0.1 mg/L
1.00E+05
0.2 mg/L
Zimag (Ω)

8.00E+04
0.3 mg/L
6.00E+04
0.4 mg/L
4.00E+04
0.5 mg/L

2.00E+04

0.00E+00
0.00E+00 5.00E+04 1.00E+05 1.50E+05 2.00E+05 2.50E+05 3.00E+05 3.50E+05 4.00E+05
Zreal (Ω)

Fig. 22 Nyquist plot for NH4NO3 at different concentration

method. Electrochemical impedance spectroscopy [38] was used to perform

impedance measurements based on different concentrations as represented by
Nyquist plot shown in Fig. 20. The frequency range considered for the experiment
was from 1 Hz to 100 kHz (setting from LCR meter). The Nyquist plot illustrates
that the impedance of the sensor is inversely related to the concentration of the
water samples.
Due to the presence of ionic salts in the solution, there was a significant change
in the real part of the impedance compared to the imaginary part. From Fig. 22, it is
seen that the real part of the impedance changes with the change in frequency.
Different concentrations of solution were considered to determine the sensitive
region (from 5 to 150 Hz) of the sensor under consideration (100 Hz is chosen in
this case) Fig. 23.
Figure 24 shows the corresponding change in the imaginary part of impedance
with the change in frequency. It is seen from the figure that there is not much
change in the reactance values for the complete frequency range as compared to the
change in the resistive (Real part of Impedance) values as shown in Fig. 24.
Equation 7 illustrates the chemical formula for the ionic equilibrium state for
ammonium nitrate. As the purpose is the detection of nitrate ions, the real part of the
impedance (R) shows a significant change compared to the imaginary part (X), R is
chosen as the reference for measurement.

NH4 NO3 ↔ NH4+ + NO3− ð16Þ

The NH4NO3 solution was used as a standard solution to calculate the nitrate
concentration in the collected water samples.
132 M.E.E. Alahi et al.

4.00E+05

3.50E+05

3.00E+05
0.1 mg/L
2.50E+05
Zreal (Ω)

0.2 mg/L
2.00E+05
0.3 mg/L
1.50E+05
0.4 mg/L
1.00E+05
sensitive area 0.5 mg/L
5.00E+04

0.00E+00
1.592
2.535
4.037
6.428
10.24
16.3
25.95
41.32
65.79
104.8
166.8
265.6
422.9
673.4
1

1072
1707
2719
4329
6893
10970
17480
27830
44310
70550
Frequency (Hz)

Fig. 23 Real part of impedance versus frequency at low concentration (NH4NO3)

Frequency (Hz)

10970
17480
27830
44310
70550
1.592
2.535
4.037
6.428
10.24

25.95
41.32
65.79
104.8
166.8
265.6
422.9
673.4
1072
1707
2719
4329
6893
16.3
1

0.00E+00

2.00E+04

4.00E+04
Z imagniary (Ω)

6.00E+04
0.1 mg/L
8.00E+04
0.2 mg/L
1.00E+05
0.3 mg/L
1.20E+05
0.4 mg/L
1.40E+05
0.5 mg/L
1.60E+05

Fig. 24 Imaginary part of impedance versus frequency at different concentration (NH4NO3)

R − R0.3
C= + C0.3 ð17Þ
− 115543

where R is the real impedance of water sample, R0.3 is the real part of the impe-
dance at 0.3 mg/L of NH4NO3, C0.3 represent the concentration of 0.3 mg/L, which
Application of Practical Nitrate Sensor Based … 133

is a reference. Substituting the value of R0.3 and C0.3 into Eq. (8), the concentration
was calculated by:

R − 48056.78
C= + 0.3 ð18Þ
− 115543

5 Conclusion

Electrochemical Impedance Spectroscopy was employed to detect and display

temperature, humidity and nitrate concentrations by evaluating the impedance
change read by the planar interdigital transducer. Calibration curve has also been
developed to measure the unknown parameters. The nitrate concentration has been
measured without the selectivity. The proper selectivity for the sensor that could
capture only the nitrate ions is necessary before an accurate assessment of NO3-N
concentration in the stream water will be explored. However, the interdigital sensor
has the potential to be used for testing temperature, humidity and nitrate concen-
tration in real-time applications for a rough estimation. For the in situ purpose, a
robust sensor node needs to develop to do the real-time monitoring of the sampling
site.

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Using Wireless Sensor Networks
to Determine Pollination Readiness
in Palm Oil Plantation

Mohamed Rawidean Mohd Kassim and Ahmad Nizar Harun

Abstract The Wireless Sensors Network (WSN) is nowadays widely used to build
decision support systems to solve many real-world problems. One of the most
interesting fields having an increasing need of decision support systems is
agricultural environment monitoring. Agricultural environment monitoring has
become an important field of control and protection, providing real-time system and
control communication with the physical world. An intelligent and smart WSN
system can collect and process large amount of data from the beginning of the
monitoring and manage air quality, soil conditions, to weather situations. Wireless
sensors are used in a palm oil plantation to monitor the humidity, temperature and
other parameters of a mother palm to find the best time to start a controlled
pollination process. Pollination is the process of transferring pollen from the male
reproductive organ to the female reproductive organ of a flower. The inaccuracy in
determining pollination readiness of the oil palm flower could potentially cause a
detrimental effect on the palm oil industry in the long run.

1 Introduction

Agricultural environmental monitoring applications can be broadly categorized into

indoor and outdoor monitoring [1]. Indoor monitoring applications typically
include buildings and greenhouses monitoring. Outdoor monitoring applications
include chemical hazardous detection, habitat monitoring, earthquake detection,
volcano eruption, flooding detection and weather forecasting. These applications
involve sensing temperature, light, humidity, moisture and air quality. This chapter
will explain in detail how a practical, cost-effective and user-friendly pollination
readiness of palm oil flower monitoring system was developed based on WSN
technology.

M.R.M. Kassim (✉) ⋅ A.N. Harun

Product and System Architecture, MIMOS, Ministry of Science, Technology and Innovation,
Kuala Lumpur, Malaysia
e-mail: [email protected]

© Springer International Publishing AG 2017 137

S. Mukhopadhyay et al. (eds.), Sensors for Everyday Life, Smart Sensors,
Measurement and Instrumentation 23, DOI 10.1007/978-3-319-47322-2_7
138 M.R.M. Kassim and A.N. Harun

Palm oil has become increasingly popular as it provides rich sources of α and
β-carotene and vitamin E, which play important roles in blood coagulation, sup-
pression of cholesterol production and cancer inhibition. Besides its nutritional
value, it is a well-known raw material for oleo chemical industry and bio-fuel for
automobiles. Around 85 % of the palm oil production is concentrated in Indonesia
and Malaysia, but its use is rapidly spreading in whole world as China and India are
the main importing countries, next to the EU.
At present, Malaysia accounts for an overwhelming contribution to world’s palm
oil production and export which is 39 % and 44 %, respectively. A massive 17.73
million tons of palm oil and 2.13 tons of palm kernel oil have been produced from
about 4.49 million hectares of land. Malaysia has a vital role to play in achieving
the rising global need for oils and fats, as Malaysia is one of the major producer and
exporter countries of palm oil and palm oil products.
Pollination is an important process in oil palm breeding as correct method
increases yield and quality of palm oil production. During pollination process the
conditions need to be monitored thoroughly within a time frame to ensure genetic
purity that will increase yield. Currently, this monitoring process of pollination is
very manual and labour intensive job. Workers need to climb an average height of 3
stories building only to check the conditions of the pollination. Climbing is dan-
gerous as risk of falling down can cause disability and deaths.
Advances in sensor and wireless radio frequency (RF) technologies and their
convergence with the Internet of Things (IoT) offer vast opportunities for appli-
cation of sensor systems for agriculture industry. Emerging wireless technologies
with low power needs and low data rate capabilities have been developed which
suit precision agriculture [1–5]. The WSNs have become the most suitable tech-
nology to monitor and control the agricultural environment.
Wireless Sensor Network (WSN) is the ideal candidate to provide effective and
economically viable solutions for a large variety of applications ranging from health
monitoring, agriculture, environmental monitoring to military operations. WSN is a
very important component in IoT and integrates the knowledge of sensors,
automation control, digital network transmission, information storage and infor-
mation processing. WSN market is forecast to rise from $0.45 billion in 2012 to $2
billion in 2022 [6, 7].
Current pollination processes for oil palm pollination relies heavily on human
dependence. It involves manual checking of trees for pollination readiness and is
more of a guessing game rather than an exact science. For the process of oil palm
pollination to be efficient and cost-effective, a logical solution would be to automate
the process and reduce dependence on human tacit knowledge by transferring it into
a system. Therefore, a remote monitoring system for pollination readiness using
WSN is introduced to help the field workers reduce the dangerous task load besides
improving the quality and productivity of yield. Figure 1 shows an oil palm
plantation in Malaysia.
Using Wireless Sensor Networks to Determine Pollination … 139

Fig. 1 An oil palm tree can reach up to 20 m

2 Agricultural Environmental Monitoring

Environmental monitoring applications can be broadly categorized into indoor and

outdoor monitoring [8]. Indoor monitoring applications typically include buildings
and greenhouses monitoring. These applications involve sensing temperature, light,
humidity, and air quality. Outdoor monitoring applications include chemical haz-
ardous detection, habitat monitoring, traffic monitoring, earthquake detection,
volcano eruption, flooding detection and weather forecasting. Sensor nodes also
have found their applicability in agriculture. Soil moisture and temperature moni-
toring is one of the most important application of WSNs in agriculture. When
monitoring the environment, it is not sufficient to have only technological knowl-
edge about WSN and their protocols. It is also necessary the knowledge about the
ecosystem.
Environmental Monitoring: WSNs have become an important tool in envi-
ronmental monitoring. The relatively low cost of the devices allows the installation
of a dense population of nodes that can adequately represent the variability present
in the environment. They can provide risk assessment information for example
140 M.R.M. Kassim and A.N. Harun

alerting farmers at the onset of frost damage and providing better microclimate
awareness.
Pierce and Elliot developed a regional and on-farm sensor network that provides
remote, real-time monitoring and control of farming operations in two agricultural
applications, a weather monitoring network and an on-farm frost monitoring net-
work [9].
Precision Agriculture: The development of WSN applications in precision
agriculture makes it possible to increase efficiencies, productivity and profitability
in many agricultural production systems, while minimizing unintended impacts on
wildlife and the environment. The real time information obtained from the fields
can provide a solid base for farmers to adjust strategies at any time. Instead of
making decisions based in some hypothetical average condition, a precision agri-
culture approach recognizes differences and adjusts management actions
accordingly.
Greenhouse: Greenhouse plants and crops can benefit a lot from the use of
WSNs, because inside the greenhouse the crop conditions such as climate and soil
do not depend on external factors and the implementations are thus easier than in
outdoor applications. The first application of WSN in a greenhouse was reported in
the year 2003. It was a monitoring and control system developed using Bluetooth
protocol. Since then, several applications have been developed, most of them
making use of IEEE 802.15.4/ZigBee protocol. Gonda and Cugnasca presented a
proposal of a distributed greenhouse control and monitoring system using ZigBee
[10]. Lea-Cox et al. developed a WSN in a greenhouse, that integrates a number of
sensors which can measure substrate water, temperature, electrical conductivity,
daily photosynthetic radiation and leaf wetness in real-time [11].

3 Environmental Monitoring System Applications

Habitat Monitoring: Habitat monitoring (HM) is one of the essential components

in environmental monitoring. HM is important to make sure there is no any eco-
logical disturbance for animals and plants. Pollution can cause a lot of negative
impacts to the eco system. A web-based system was developed to alert and manage
the data of pollution efficiently [12].
Greenhouse Monitoring: The greenhouse effect occurs when solar radiation is
trapped by the gases in the earth’s atmosphere and reflected back from the earth.
Greenhouse Monitoring system normally used to measure and monitor environ-
mental parameters such as temperature, pH, humidity, moisture etc. When the
temperature and humidity drops below threshold value the host system will trigger
misting, turn on fans etc. Figure 2 shows a greenhouse environment for growing
Capsicum Annum.
Climate Monitoring: Climate change have brought many effects such as
breaking of sea ice, heat waves, glazier melting and lake temperature warming.
Thus, there is a need to control and monitor the climate change. Flood prediction is
Using Wireless Sensor Networks to Determine Pollination … 141

Temperature

Humidity

Fig. 2 A greenhouse environment for growing Capsicum Annum

another example of climate monitoring, where wireless sensors can be used to

detect rainfall and water levels to trigger an alarm system.
Forest Monitoring: Forests are important sources for biodiversity and ecolog-
ical balance. Currently, the forest has been interrupted by unethical activities such
as illegal logging and development activities. Therefore, it is very important to
implement an effective forest monitoring system. The forest monitoring system also
includes fire monitoring and detection in forests.

4 Important Parameters in Agricultural Environment

Agricultural environment are complex systems where changes in one environmental

factors could have an adverse effect on another factor. Environment factors can
affect the growth of plants especially sprouting, pollination and fruit development.
Furthermore, these factors can also be used to indicate the risk of plant diseases and
future forecasting. Therefore, it is very important to monitor these environment
factors. Temperature, humidity, light intensity, rainfall level, air pressure, moisture,
electrical conductivity (EC) and pH are some of the important factors.
pH is a very important parameter for plants and crops growth. In general,
measurement of soil pH will indicate the soil acidity and soil alkalinity. The growth
of different types of plants and crops depends on soil pH. Some plants and crops
need acidic soil and some need alkaline soil. The pH also affect the availability of
nutrients in the soil, therefore the farmers need to know the pH level so that they
can use fertilizers at the right time.
142 M.R.M. Kassim and A.N. Harun

Soil moisture is the water that is held in the spaces between soil particles. Soil
moisture data will be used to determine when to irrigate and amount of water for
each irrigation. Based on observation, most of the time, the fields are over irrigated.
Over irrigation prevents the nitrogen to be used by roots, and lack of oxygen in the
root area. Different crops need different level of moisture to maximize the
productivity.
Temperature is another important parameter in agriculture field. Low tempera-
tures will slow down the photosynthesis process, thus growth is slowed and this
results lower yields. Different plants and crops grow best at different temperature.
Humidity is one of the very important parameter in agriculture field. Relative
humidity (RH) is the ratio of actual water vapour content to the saturated water
vapour content at a given temperature and pressure in percentage. RH indirectly
affects leaf growth, photosynthesis, pollination and generate pests and various types
of plant diseases.
Temperature and humidity are closely linked in a greenhouse environment. The
decrease of the relative humidity is a sign of increased air temperature because cold
air has a lower moisture-holding capability than warmer air. Humidity control is
very important to prevent plant diseases. The range of healthy RH for plants is from
50 to 70 % [13]. If humidity is below 50 % for longer duration, the plant growth
will be affected due to loss of water from leaves might be faster.
Electrical conductivity will determine the suitability of an environment for the
plants and crops. EC estimates the amount of total salts or ions in the soil. In
general, EC shows the level of ability of the soil water to carry an electrical current.
In other words, EC level is an indication of the amount of nutrients available for
plants and crops to absorb.
Figure 3 shows one of the wireless sensors developed by MIMOS that can be
used to measure the above environment parameters.

Fig. 3 Wireless Sensor for

environment monitoring
Using Wireless Sensor Networks to Determine Pollination … 143

5 Challenges in Palm Oil Industry

Malaysia’s position as the world’s leading palm oil country has allowed the
industry to flourish in the way it has never been before. The results in the churning
out of a wide variety of products as a result of continuous R&D efforts. With the
escalation in the volume of palm oil products and the fruit itself, it becomes nec-
essary to produce high quality seedlings from high yield trees by automating and
transforming the current process of pollination to meet growing demands.
The current methods of pollination involve tacit knowledge of checking whether
a palm is suitable for pollination and manual labour being deployed in fields of vast
sizes spanning over thousands of hectares in the nation itself. The drawbacks of
such a system is late bagging during the pollination process that ultimately impacts
overall yield and the process, being labour dependent, relies on a sizeable number
of foreign manpower to work the fields. The current gaps are:
• Human dependence to monitor trees for within the plantation and determine if
they are ready for pollination.
• Inaccurate human-based decision making based on the determining of the
pollination window.
• Vast plantation areas to be monitored to catch the pollination window to
maximise yield.

6 Oil Palm Flower Pollination Process

Controlled pollination consists of transferring pollen from one plant to the receptive
female reproductive organs of another plant while excluding all other pollen.
Controlled pollination plays an important role in the commercial crops production,
especially in oil palm production, as it facilitates producing progeny with favorable
genetic trait inherited from the parent plants.
Controlled pollination also contributes to offspring generation with more genetic
uniformity compared to the naturally pollinated plants. The success of the polli-
nation process depends greatly on the ability to determine the period at which the
flower or floral organs is receptive towards the pollens, namely the pollination
period. The introduction of pollens out of the pollination period, either too early or
too late, will result in the abortion of the unfertilized flowers or the development of
pathernocarpic fruits and thus resulted in a poorly pollinated bunch. Thus, the
pollination stage must be accurately determined for the pollination process to take
place. The ability to correctly determine the pollination readiness of an oil palm
flower provides a significant advancement in the oil palm industry.
Research has shown that the average receptive period of a female flower lasts
from 3 to 10 days, depending on the species of the flower. When a female flower is
found to be in its receptive period, pollination is usually repeated on three
144 M.R.M. Kassim and A.N. Harun

successive days. Conventional methods done in the agricultural industry to deter-

mine pollination readiness include examining the structure of the flower to deter-
mine its developmental state and its pollination readiness. The main limitation of
this method is the dependence on inspection by eye and the subjective nature of this
inspection. Observations alone may differ widely between different individuals, and
other factors such as quality of light, time of day, or experience of each individual
plays a role in influencing the accuracy of these inspections.
Amongst the many species of flowers, the oil palm flower is known for having a
shorter receptive period than average. Its receptive period lasts only for about 36–
48 h, with flowering starting at the base of the inflorescence and progressing to the
top. The shorter time frame of the receptive period of the oil palm flower increases
the complexity of being able to accurately determine the pollination readiness of the
flower, and performing pollination even a day too early or too late would result in
an unsuccessful pollination of the oil palm flower. The inaccuracy in determining
pollination readiness of the oil palm flower could potentially cause a detrimental
effect on the palm oil industry in the long run.
Therefore, the challenge to overcome the current conventional method to provide
a system and method to determine pollination readiness of a flower in an accurate and
time-efficient manner is vital in sustaining a successful production of commercial
crop. In this system, sensor node will send humidity value inside a pollination bag
every 1 h to server. Another sensor node will send humidity value of an empty
pollination bag as a reference. The difference between the two sensor reading will be
calculated to determine the best pollination time to start the pollination process.

7 Wireless Technologies and WSN

Many wireless technologies were developed over the last few decades to solve
many real-world problems. Wireless technologies and sensor networks have
become the most suitable technologies to monitor and control the agricultural
environment. These technologies are capable of providing greater level of flexi-
bility, mobility at an affordable cost and low power consumption. There are more
than 10 wireless technologies available for industrial applications however the most
exploited wireless technologies are Wi-Fi, ZigBee and Bluetooth. The selection of
these technologies dependents on the nature of the applications.
Bluetooth: Bluetooth is a short range wireless communication intended to
replace portable or fixed device. Bluetooth operates at 2.4 GHz ISM band. Blue-
tooth has the capability to simultaneously handle data and voice transmissions and
used in applications such as hands-free handsets for voice calls.
Wi-Fi: Wi-Fi requires high frequency radio waves, usually 2.4 or 5 GHz for data
transmissions and supports several hundred meters between two places. Wi-Fi was
initially used in mobile computing devices in LANs but now diversified to more
applications such as Internet and consumer electronics. There are few generations
of Wi-Fi standards available and carter for different applications.
Using Wireless Sensor Networks to Determine Pollination … 145

Fig. 4 WSN Node architecture [23]

ZigBee: ZigBee is used for short range wireless communications. ZigBee is

targeted for cost sensitive applications such as home and building automation.
ZigBee supports data transmission up to 100 meters and consumes less power and
most suitable for portable and low power consumption applications.
Figure 4 shows a general WSN node architecture. Each sensor network node
consists of a sensor module, processor module, communication module and power
module using battery. The rapid evolution of the Micro-Electro-Mechanical Sys-
tems (MEMS) has contributed to the development of small and smart sensors.
These sensors have become increasingly very small in terms of size, more intelli-
gent and less expensive. WSN is a network of small sensing devices known as
sensor nodes or motes, arranged in a distributed manner, which collaborate with
each other to gather, process and communicate over wireless channel about some
physical phenomena.
The selection of wireless technologies depends on their applications. For
example, ZigBee technology cannot be applied to high data transmission applica-
tions because of their high bandwidth requirements. Bluetooth and Wi-Fi are not
suitable for battery powered applications because of their high power consumption.

8 Platform Architecture

MIMOS PA solution comprise of three platforms; MIMOS Wireless Sensor net-

work called as MSCAN, Precision Agriculture Management System (PAMS) which
has MBPS parser engine and raw database, and Application Database (DB) and
Web-based Application Services.
146 M.R.M. Kassim and A.N. Harun

Figure 5a shows general MSCAN architecture which consists of sensor node,

router and gateway. Sensor node has two main parts; tip and mote. Gateway also
has two main parts; collector and main microcontroller unit (MCU). Cur-
rently MSCAN platform is using ZigBee as the wireless communication technol-
ogy. At application layer, MSCAN architecture use proprietary protocol named as
MBPS for application data communication.
MSCAN make use ZigBee technology to provide mesh network, self-organised
and self-healing network features. By making used of application specific profile,
MSCAN platform is allowed to implement application for MIMOS PA solution.
Products that had been developed for MSCAN Platform are Sensor Node, Router
and Gateway.
MSCAN Sensor Node: Fig. 5b shows MSCAN sensor node product. There are
two types of tip, sensor tip and actuator tip. Tip will has unique identification
number and version identification. Version identification will determine number of
difference sensors or actuators on the tip. Each sensor or actuator has a type ID to
identify type on sensor or actuator on the tip.
Mote is a wireless end device that has battery which also supply power to the tip
attached to the mote. Mote has unique MAC address and will be assigned a network
address when it joins the network. Mote has two push-button and two led for the
user interface. Mote implements power management that able to save battery for
long operation and longer life. Mote controls tip operation by controlling power and
using MBPS protocol for communication between mote and tip.
MSCAN Router: MSCAN Router provides hopping feature that allows Sensor
Node to be placed longer distance from the Gateway [14]. MSCAN architecture has
been configured to support maximum of 5 depth of hopping from Gateway to the
last Sensor Node in a network. Gateway and Router both can support maximum of
5 Routers child. Using multiple routers in a network will allow wide coverage of

(a) Sensor Node Gateway

MSCAN MSCAN MSCAN MSCAN Main
Mote Router Collector MCU

(b) (c) (d)

Fig. 5 MSCAN platform architecture

Using Wireless Sensor Networks to Determine Pollination … 147

Fig. 6 Maximum of 5 depth of hoping by routers

network with mesh network capability [15]. Router has to be powered up to ensure
network is always available for the sensor node to send sensor data to the Gateway
[16]. Router use external battery that has enough capacity to provide power longer
life. Figure 5c shows MSCAN router product that has cable to connect to the
external battery [17] Fig. 6.
MSCAN Gateway: MSCAN Gateway has two main module; Collector and
Main MCU board. Collector is a ZigBee coordinator that control router and Sensor
Node in the wireless sensor network. Collector interfaces to the main CPU using
serial interface. Main CPU board has GPS module, GSM module and other control
circuit for the gateway.
Collector forwards sensor data in MBPS packet format to the Gateway main
CPU which sends the packet to LSMS server using GPRS or SMS over GSM
network. Gateway is located in the field, powered by battery and solar panel.
Figure 5d shows MSCAN gateway product.

9 System Architecture

The system architecture of the Pollination Monitoring System consists of three

layers as shown in Fig. 7. The Physical Layer represents the physical sensors,
actuators and CCTV cameras. The Middle Layer represents the WSN interface,
CCTV interface, sensor and image manager, database, App server and Web server.
Finally, the Application Layer represents the Graphical User Interface (GUI),
monitoring services (sensor and image monitoring), alerting services and decision
making services.
The applications developed using this architecture can measure and analyse
external weather conditions such as temperature, humidity, rain fall, wind direction,
148 M.R.M. Kassim and A.N. Harun

ApplicaƟon
Layer PDA App Web App

Middle Web Server App Server

Layer
Database
Image Manager
Sensor Manager

Physical
Layer

CCTV Environmental & Soil Sensors

Fig. 7 System architecture

wind speed and also internal weather conditions in a greenhouse such as temper-
ature, pH, relative humidity, moisture, CO2, EC, and the intensity of light. The
information collected in real-time is then converted and stored into a database
through a web server, which provides critical information to users.
Physical Layer: The physical layer consists of wireless environmental, soil
sensors (temperature, humidity, moisture, EC, pH and CO2), actuators and CCTV
cameras. These sensors will collect environmental and soil information from indoor
(e.g. greenhouses) and outdoor environment periodically and sent the data to sensor
manager.
The measurement data include temperature, humidity, soil and water pH, soil
moisture, rainfall quantity, EC, wind speed and direction, water level, water con-
sumption, etc. The data is further analyzed and converted into appropriate formats
and finally sent to Middle Layer for storing in databases.
Middle Layer: The middle layer (ML) supports communication between
physical layer and application layer. Currently this architecture is using ZigBee as
the wireless communication technology. The ML converts the data received from
the physical layer and store it in a database. The ML will also support the data
request from the application layer. The Web server and App server allows users to
monitor data processed by the components through a Web browser, PDA or smart
phone at any time.
Using Wireless Sensor Networks to Determine Pollination … 149

The sensor manager converts and analyses this data and store it in a database.
The web server will fetch the sensing data stored in the database at a fixed interval
and send it to the GUI. The users can view the sensor data through the GUI in the
Application Layer. The GUI will also display and send emails and SMS if there is
any alerts and warnings. The CCTV cameras will collect real-time image infor-
mation (real-time streaming) on the indoors and outdoors and send it to image
manager. The image manager will store it in the database. The user can access the
image data at anytime and anywhere through the GUI using PDAs or Smart Phones.
The web server used to host sites and deliver web pages content to clients who
can access them through the Internet. Another use of web server is to connect any
component of the physical layer to browse any monitoring or actuating device in
real time.
Application Layer: The application layer consists of various GUIs to provide
suitable information and support user requests. The users can access environmental
information and status through various platforms such as smart phone, web and
PDA. This layer also consists of monitoring support, actuating support, alerting
support and decision making support.

10 Pollination Readiness Monitoring Process

A review of pollination studies conducted on palms by Henderson showed that

mainly insects are responsible for transferring pollen from anthers to stigma [18].
Henderson concluded that three major pollination syndromes exist in palms: beetle
pollination (cantharophily), bee pollination (mellitophily) and fly pollination
(myophily).
More particularly, in palm trees bearing inflorescences which will develop into
fruit bunches upon fertilization, specific procedure is adopted in the controlled
pollination system. Prior to the anticipated pollination occurrence, the inflorescence
is required to be covered with a tight bag fitted with a transparent window (refer
Fig. 11), so that unwanted pollens will not reach the inflorescences during the
receptive period of the inflorescence.
The transparent window is necessary to enable visual inspection on color and
structural developments of the inflorescence, according to the conventional way of
detecting pollination. Upon visual detection of pollination, controlled pollination is
carried out by applying pollens of a desired progeny directly onto the female
inflorescence using a hand puffer. Santos et al. [19] reported that the inflorescence
should be inspected daily or every alternate day, starting from the day of bagging,
to verify the onset of pollination of the inflorescence.
The pollination readiness monitoring process developed in this project starts
with identifying the female inflorescences which are going to be pollinated. The
complete process is described below and Fig. 3 represent the overview system for
determining pollination readiness.
150 M.R.M. Kassim and A.N. Harun

(a) The female inflorescences which are going to be pollinated are identified. The
female inflorescences which are anticipated to undergo pollination within
certain number of days are covered with a bag attached with a main humidity
sensor on the interior surface of the bag.
(b) A reference humidity sensor is installed inside another bag similar to the bag
covering the main humidity sensor. The bag containing the reference humidity
sensor is placed in a position similar to the bag containing the main humidity
sensor in terms of the height of the surrounding trees.
(c) The humidity value is taken by the main humidity sensor and the reference
humidity sensor at certain times of the day. Each reading of the humidity
detected will be compiled into a database in a matrix form, wherein the
humidity readings will be arranged in one row in the matrix. For each day, a
new row is added to the humidity matrixes of the main humidity [Hm] and the
reference humidity [Hr]. The humidity profiles are compared regularly to
determine whether pollination has occurred.
(d) A general formula for determining pollination is shown below, where polli-
nation is deemed to have occurred when:

½α ⋅ ½Hm  − ½β ⋅ ½Hr  > ½HR 

In which [α] and [β] are the coefficient matrixes and [HR] is the triggering
matrix. The meaning of the above equation is that if a predefined combination
of the humidity of the main bag is greater than a predefined combination of the
humidity of the reference bag by the triggering (threshold) value, then polli-
nation is deemed to have occurred. The threshold humidity values are based
on pre-existing information of humidity values emitted from flowers ready for
pollination that were collected over the years using sensors in different
plantations.
(e) Once pollination is determined to have occurred, the system will notify the
user regarding the event on the GUI (Web) and also by sending a message to
the user’s mobile phone. Upon receiving the notification, the user will intro-
duce the male pollen to the female inflorescence.
(f) The bag covering the inflorescence is opened and the pollens of the desired
progeny are transferred to the inflorescence. This can be carried out, for
example, by applying the pollens onto the inflorescence by using a hand
puffer. In a preferred embodiment, the pollination has to be performed on the
same day or the subsequent day of the receipt of the notification. This will
complete the controlled pollination process Fig. 8.
Using Wireless Sensor Networks to Determine Pollination … 151

Fig. 8 Overview system for determining pollination readiness

Fig. 9 GUI of pollination monitoring system

152 M.R.M. Kassim and A.N. Harun

(a) Gateway installation - fixed pole and (b) Router installation use portable pole.
powered by car battery & solar.

Fig. 10 Router and gateway installation at site

11 Pollination Monitoring Systems (PMS)

The above mentioned architecture in Fig. 7 has been deployed to monitor the
humidity of a mother palm to find the best time to start a pollination process. Sensor
Node will send humidity value inside pollination bag at a predefine interval and
forward by Gateway to PMS using SMS/GPRS over GSM.
The GUI of PMS present important information such as list of data from sensor
node, sensor status, pollination alert list and sensor battery level. Figure 9 shows
the GUI for PMS. Each of the node in the GUI represent a sensor node installed at

(b)

(a)

(a) Pollination bag with humidity sensor

(b) Sensor Node

Fig. 11 Sensor node installed at palm oil frond

Using Wireless Sensor Networks to Determine Pollination … 153

palm oil frond. The colour of each node represent the pollination status of each
palm tree. The trees which are ready for pollination is represented in blue colour.
Figure 10 shows the router and gateway installed at the palm oil plantation.
Figure 11 shows the sensor node and pollination bag with main humidity sensor.

12 Results and Discussion

In Phase 1 of this project, 200 palm oil trees are deployed with wireless sensors.
Each palm oil tree will be tagged for identification purposes. The initial threshold
value for pollination readiness are based on values obtained from manual obser-
vation. In Phase 2, another 300 palm oil trees are deployed. The improved threshold
value from Phase 1 was used in this phase. The final results show that the threshold
value from Phase 1 is very consistent throughout this project.
The data collection after the certain days of bagging will be carefully monitored
to see whether any pollination readiness has taken place. Figure 12 shows a set of
data (humidity from a pollination bag) collected on the nth day after bagging.
Figure 13 shows the graph of humidity difference between the humidity value
from main sensor and reference sensor. This graph will help us to determine
whether pollination has taken place or not.
Once pollination have occurred, the system will notify the user regarding the
event on the GUI (Web) and also by sending a message to the user’s mobile phone.
Upon receiving the notification, the user will introduce the male pollen to the
female inflorescence on the same day of receipt of the notification to complete the
controlled pollination process.
In an oil palm plantation, 69 palm oil trees were selected randomly to install with
sensors. The purpose is to test pollination readiness (CP) success rate. In this test,
PMS manage to detect a total number of 64 trees means these oil palm trees are
ready for pollination. We can conclude that the IPMS success rate in detecting
pollination readiness is 93 %.

Fig. 12 Humidity form main Humidity (Main Sensor)

sensor node 82.00
80.00
78.00
76.00
74.00
72.00
70.00
68.00
66.00
64.00
62.00
9:59:10am
12:00:52am
1:00:32am
1:00:33am

2:00:35am
4:00:01am
4:00:02am
6:59:08am
6:59:09am
7:59:07am
8:59:06am
8:59:07am

9:59:11am
2:00:34am

10:59:15am
154 M.R.M. Kassim and A.N. Harun

Fig. 13 Humidity (Main)— Humidity (Difference)

25.00
Humidity (Reference)
20.00

15.00

10.00

5.00

0.00

13 Conclusions

Using the key elements of information, technology, and management, PMS can be
used to increase production efficiency, improve product quality, conserve energy
and protect the environment. Moreover, PMS with minor customization can also be
applied to other agricultural environmental applications.
Some of the benefits of using smart agriculture system for oil palm pollination
are as follows:
• To be able to trigger pollination period within certain days.
• To increase yield.
• To increase productivity.
• Possible reduction of labour dependency.
• To be able to directly communicate with the sensor nodes to get real time data
using WSN.
WSN ecosystem can be deployed in various sectors provided that the end-to-end
devices and solutions are properly configured. WSN is the key for deployment of
IoT as it provides large pool of sensors to be configured to the end devices. Among
the critical issues in palm oil pollination readiness monitoring is the RF range due to
the coverage of palm leaves and also terrain of the plantation area [20, 21]. The
second issue is on the power management for the sensor node which uses battery to
operate. However, in this project we only target sensor node battery life up to
2 years due to battery life time limitation [22]. We can conclude that the PMS
success rate in detecting pollination readiness is more than 90 %. The network data
security and power management with efficient algorithms will also be given higher
priority in our future work.
Using Wireless Sensor Networks to Determine Pollination … 155

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Time Domain Reflectometer
for Measuring Liquid Waste Levels
in a Septic System

Shreya Reddy Mamidi, Kaushik Bukka, Michael Haji-Sheikh,

Martin Kocanda, Donald Zinger and Mansour Taherinezahdi

Abstract The objective of this study was to determine the level of water in a septic
tank by inserting a waveguide at the top of the tank. A TDR (i.e. waveguide) probe is
immersed in the water tank, through which a pulse signal is launched. The impe-
dance mismatch occurs at the air-water interface and the bottom of the tank, which
results in the reflection of the signal. This reflected signal is algebraically added to
the incident signal. From the time difference between the incident and reflected
signal, the distance between the TDR and the surface of water is calculated. The
distance is generally twice the time traveled by the wave. Thus, the calculated
distance helps in finding out the length of water in the tank. Additionally, the TDR
was compared with a Doppler radar system to determine if the Doppler system
would be a feasible non-contact measurement system as compared to the TDR.

1 Introduction

A Time Domain Reflectometer (TDR) level measurement device capable of gen-

erating and receiving electromagnetic waves for the measurement of waste water is
demonstrated. Waste water in a septic system is a mixture of solids and liquids
along with various levels of acidic compounds of urea. Disinfectants and other
additive chemicals also effect the melange that are in the human waste-water sys-
tems. Typical measurement systems for these type storage containers often are float
based and or they use ultrasonic transceivers. Septic systems that could use this
type of measurement system are, but not limited to, transportation systems. These
transportation systems are buses, planes, and trains. If the system cost is low
enough, the application space can be expanded to recreational vehicles. These
vehicles have extremely large storage tanks and a measurement system can help

S.R. Mamidi ⋅ K. Bukka ⋅ M. Haji-Sheikh (✉) ⋅ M. Kocanda ⋅ D. Zinger ⋅

M. Taherinezahdi
Department of Electrical Engineering, Micro-Electronic Research an Development Center,
Northern Illinois University, Dekalb, IL 60115, USA
e-mail: [email protected]

© Springer International Publishing AG 2017 157

S. Mukhopadhyay et al. (eds.), Sensors for Everyday Life, Smart Sensors,
Measurement and Instrumentation 23, DOI 10.1007/978-3-319-47322-2_8
158 S.R. Mamidi et al.

prevent accidental spillage and localized environmental damage. The primary

objective, though, is to measure the height of waste water in a tank and design an
efficient measuring device. The TDR is based on the reflection mechanism, in
which the time delay between the transmitted and reflected signals helps to deter-
mine the distance from the source to the surface of water, which is later used to
calculate the height of water in the tank. The TDR is built using a 74AC14 IC,
which is capable of producing pulse signals with very low rising and falling times
that provide greater accuracy. Thus, the generated pulse signals are transmitted into
the probe inserted in a tank. The total time taken by the pulse to travel the path to
and from is calculated, which in return helps in calculating the height of the liquid
in the tank. The functioning of the proposed TDR circuit and the bi-axial probe is
also tested in the laboratory.
Level estimation is used to determine the linear vertical separation between a
reference point and the surface of the liquid or top of a pile of divided solids [1].
The water level in a tank such as underground septic tank or overhead water tank or
airplane septic tank has to be estimated. If the sewage overflows a groundwater tank
it could cause a shutdown of drinking water systems. If it reads full in an aircraft the
regulators force an unplanned landing not to mention that the passengers will have
to deal with unpleasentness. It is necessary to know the level of water in the tank to
avoid problems, like overflow and leakage. There are many ways to estimate the
water level in tanks, such as sight glasses, hydrostatic devices, capacitive level
sensors and microwave sensors. Sight glasses are susceptible to leakage and also
conceal visible level of water due to the sediment buildup on it. Hydrostatic devices
such as displacers, bubblers and differential pressure transmitters have reduced
measurement accuracy, due to the shift in the liquid’s gravity based on change in
temperature. In case of capacitive sensors, long conductive cables suffer cable
breakage due to extreme mechanical tension. Radar systems through-air are affected
by divergence problems. In order to estimate the level of water in the tank, engi-
neers have to come up with a technique, which is more efficient than the above
mentioned procedures. The trending technology these days is measurement of
distance between the source and liquid level by time-based measurement, which
replaced mechanical and pressure-based measurement tools. One such method is
Time Domain Reflectometry where the probe provides the focused path [2].
The TDR system does require contact to the liquid which may be an issue in some
applications. Unlike, ultrasonic measurement systems which may be fooled by
floating debris that absorbs ultrasonic energy (materials such as water logged
paper), the TDR is immune to those effects.
Time Domain Reflectometer (TDR) is fundamentally a radar in which a voltage
pulse is launched along a co-axial cable. Whenever distortion (or defect) occurs
along the cable, a reflection of the transmitted wave happens. The location of the
cable defect is determined by the reflection travel time, and the reflection magnitude
is proportional to the magnitude of the defect. In case of water level measurement, a
hollow co-axial cable can be installed in a monitoring tank, and it is observed that
the reflection occurs at the air-water interface. This strong reflection makes it
possible to monitor changes in water level. A common component in sewage is the
Time Domain Reflectometer for Measuring Liquid … 159

presence of toilet tissue. Some of this material breaks down readily and some of the
material floats. Since this material is saturated with water is should not significantly
affect the reflection from the air water interface.
The TDR technique was introduced in the early 1980s. Since its introduction, it
has gained interest by many fields of science for various applications [3]. TDR has
wide variety of applications and is very efficient compared to other measurement
techniques. TDR is also used for measuring impedance of the transmission lines,
dielectric constant of the medium of transmission, electrical conductivity and types
and position of faults in the transmission lines. A brief mention of some of the
previous work performed in the area. Tomi Engdahl designed a simple TDR using
74AC14 IC, which was primarily used to detect faults along the cable. He also
analyzed the outputs and classified them into different types of distortions [4]. Jim
Bartling worked on a “Low cost, high resolution Time Domain Reflectometer”
which was designed using a 16-bit microcontroller and a Charge Time Measurement
Unit (CTMU) peripheral on-chip that is used to measure time with a high degree
precision and resolution. The main goal of his work was to find out transmission-line
length, location of faults due to opens and location of faults due to shorts [5]. Jim
Bartling also developed a “Time Domain Reflectometer for liquid level measure-
ment”. He has designed a TDR using PIC microcontroller and used it with a probe to
measure the level of liquid. Time measurement is again accomplished using CTMU.
It provides information of the fluid composition as well [6]. Brian Kenner and John
Wettroth designed a TDR using Intel 87C51 microcontroller to measure length and
termination impedance of co-axial cables commonly used in computer networks,
like Ethernet, Arcnet etc. A high-speed comparator is enabled to measure the length.
The software consists of approximately 3 K of 8051 assembly language [7].
James R. Andrews analyzed “Time Domain Reflectometry and Timer Domain
Transmission Measurement fundamentals” in 2004. The main aim of his study was
to identify the nature of the Device Under Test (DUT) [8]. Scott B. Jones, Jon M.
Wraith and Dani Or discussed “Time domain reflectometry measurement principles
and applications” in 2002. Their main motive was to determine the porous media
water content based on dielectric properties and electrical conductivity of the
medium [3]. Kevin M O’Conner and Charles H. Dowding worked on “Real-Time
monitoring of infrastructure using TDR technology”. His study reveals the summary
of principles involved in various applications of TDR. This work was primarily
intended to provide background on the principles involved in geotechnical and
infrastructure applications of TDR [9]. Xinbao Yu and Xiong Yu studied on
“Measurement of simulated scour by Time domain reflectometry” in 2006. “TDR
instrument and analyses framework can be potentially refined into a useful tool for
bridge scour surveillance”. Their study shows the determination of dielectric con-
stant, electrical conductivity, the depth of the scour and properties of the soil sedi-
ments (porosity, density) [10]. A. Thomsen, B. Hansen and K. Schelde proposed a
TDR technique for measuring water level in tanks collecting surface water runoff
and soil moisture in their paper “Application of TDR to water level measurement” in
2000. They designed a two-wire closed loop TDR probe with balun transformer for
transforming impedance from 50 to 200 Ω. The water level calibration depended on
160 S.R. Mamidi et al.

time-based measurements [11]. D. Moret, M. V. Lopez, J. L. Arrue worked on water

level measurement and volumetric water content of the soil in Mariotte reservoir
using TDR method. Their work was published as “TDR application for automated
water level measurement from Mariotte Reservoirs in tension disc infiltrometers”.
A three-rod TDR probe was designed that was used for simultaneous measurements
of both water flow and volumetric water content of soil below the infiltrometer disc,
placed at the bottom of the reservoir. The measurement was done considering the
summation of pulse travel times [12]. W.F. Kane studied “Embankment monitoring
with time domain reflectometry”, where the slope movement and peizometric levels
were determined. The work proposed the use of coaxial cable which was embedded
in the vertical hole to locate shear failure in the embankment, rate of ground
movement and water levels. It was the first application of TDR in civil engineering in
1998 [13].

2 Scope of Work

The objective of this study is to determine the level of water in a septic tank by
placing a waveguide at the top of the tank. A TDR (i.e. waveguide) probe is
immersed in the water tank, through which a pulse signal is launched. The impe-
dance mismatch occurs at the air-water interface and the bottom of the tank, which
results in the reflection of the signal. This reflected signal is algebraically added to
the incident signal. From the time difference between the incident and reflected
signal, the distance between the TDR and the surface of water is calculated. The
distance is generally twice the time traveled by the wave. Thus, the calculated
distance helps in finding out the length of water in the tank. Additionally, the TDR
was compared with a Doppler radar system to determine if the Doppler system
would be a feasible non-contact measurement system as compared to the TDR.

2.1 TDR Measurement System

TDR was basically developed to check for faults in cables. That where it got its
name as ‘cable tester’ [3]. TDR is also called guided-wave RADAR, i.e. the pos-
itive pulse generated by TDR, travels along the cable or a metal rod under test. The
signal waveform is seen on the Oscilloscope, which is connected at the source and
DUT connection. This explains the basic TDR setup. It generates a step signal or an
impulse with fast rising and falling edges. The rise and fall time of the pulse
matters, the steeper the slope the greater the resolution [10].
Once the incident pulse is fed into the DUT, the waveform displayed by the
Oscilloscope is monitored. If the load impedance matches the characteristic
impedance of the line, no reflection is seen. Since the whole signal transmitted is
absorbed at the load. The only thing seen on the Oscilloscope screen is the incident
pulse. But, if the load impedance does not match the characteristic impedance of the
Time Domain Reflectometer for Measuring Liquid … 161

Fig. 1 (Top) Oscilloscope display when load impedance matches characteristic impedance.
(Bottom) Oscilloscope display when load impedance mismatches characteristic impedance [14]

line, part of the incident pulse is reflected back to the source, which is recorded by
the Oscilloscope as in the Fig. 1. This reflected pulse can be easily noticed as there
is a time difference between incident and reflected pulses [14].
For cable testing, a cable of known length with velocity of propagation, Vp, is
taken, and reflections from discontinuities are observed on the Oscilloscope screen.
The time difference and the voltage difference between the incident and the
reflected peaks are noted, from which the distance of the discontinuity from the
source can be calibrated. The time difference is the time taken by the wave to travel
the round trip (i.e. two times the length, L) between source and discontinuity.
Therefore the time difference is:

2L
t= ð1Þ
v

where, L is the length of the discontinuity from the source, t is the time difference
(total time taken from source to discontinuity and again back to source) and v is the
velocity of light in the medium. TDR is also used to measure the properties of the
materials surrounded by the probe. Typical properties are impedance, dielectric
constant, its conductivity and velocity of propagation.

2.2 Advantages and Disadvantages of TDR

TDR has many advantages compared to other measurement techniques.

1. It has the ability to measure reliably even in temperature and pressure fluctua-
tions, dust and noise, condensation and steam generation.
2. TDR can be used to measure the level of any kind of liquid. It is immune to
different properties of liquids like dielectric constant.
3. Multiple discontinuities can be measured at same time unlike other techniques.
4. It is a non-destructive method of testing.
5. It has the ability to provide thorough time series measurements at multiple
locations.
162 S.R. Mamidi et al.

6. It provides simultaneous measurement recording. The TDR probe is resistant to

corrosion and also immune to mechanical shock, TDR parts do not wear out,
circuitry is simple and operates at low voltage and better resolution compared to
other techniques.
There are also few limitations and disadvantages in TDR.
1. Discontinuities that are either small or closely spaced are mathematically
smoothed into single irregularity. This effect does not show up all the discon-
tinuities and also leads to inaccurate impedance readings. If the distance
between the two neighboring discontinuities is less than half the rise time of
TDR, then the discontinuities are merged into one signal [14].
2. TDR system’s resolution can be affected by rise time, settling time and pulse
aberrations.
3. By the time the incident pulse reaches the end of the cable, the rise time and
settling time might be degraded, which affects the resolution and accuracy of the
system.
4. Internal reflections from the mismatches and random noise induce error.
5. The electrical interface from coaxial cable to probe might cause localized
disturbance.
But the advantages of TDR technique outweigh the disadvantages when using
with wastewater.

2.3 Proposed Circuit

In the previous section, TDR basics and transmission line basics were discussed.
Their functions and various applications have been analyzed. In this chapter the
proposed circuit and the experimental setup for measuring the water level in the
tank will be studied.
The TDR circuit discussed starts Wolke’s [15] TDR circuit. This simple circuit
comprises of a Schmitt trigger for generation of a square wave which acts as the
source of incident voltage pulse.
The Fig. 2 shows the block diagram of the experimental setup. The setup is
divided into three main parts. The signal generation, TDR probe and Oscilloscope.
The signal generation is carried out by the simple TDR circuit built in the labo-
ratory. The Oscilloscope is used to check the waveforms and also to extract the data
in the digital form. The probe used here is a bi-axial probe built using two brass
rods. All these three parts are inter-connected using a BNC Tee-connector.
In the sections below, all the parts will be discussed. The Oscilloscope used here
is Agilent Technologies Digital Storage Oscilloscope DSO1102B. It is a 2-channel,
100 MHz Input bandwidth oscilloscopes with a sample rate of 500 MSa/s–1 GSa/s
[16]. Signal generation is done by a simple TDR circuit, built using 74AC14 IC as
shown in the Fig. 3. It generates a square wave with fast rising and falling edges,
Time Domain Reflectometer for Measuring Liquid … 163

Fig. 2 Block diagram of the TDR system used in this study

Fig. 3 Schematic of TDR circuit [15]. Signal generation is done by a simple TDR circuit, built
using 74AC14 IC
164 S.R. Mamidi et al.

which is transmitted to the biaxial cable that is immersed in the water tank.
This TDR circuit has the Schmitt trigger in the circuit which yields the square wave.
The TDR probe used here is a bi-axial probe (i.e. 2-wire transmission line). It is
made out of two 3/32 brass rods which are 36 inches long and have 2.38 mm
diameter. These two brass rods which have to be immersed in water and are
connected to a coaxial cable at one end. First, the outer conductor of the coaxial
cable is unbraided and connected to one of the brass rods, and the inner conductor is
connected to the other rod using crimp connectors. The main stretch of the bi-axial
cable in targeted to be at 50 Ω in air to minimize the reflections when the tank has
no water in it. The connections to the bi-axial cable create a static reflection node
which does not change.

3 Experimental Procedure

The TDR circuit and probe built are now used to calibrate the level of water in the
tank. Firstly, the TDR launches the voltage pulse into the probe. This incident pulse
reflects at the bottom of the tank and the air-water interface, due to change in
impedance. As the probe is open at the end, reflection happens at the end of the
probe. At air-water interface, due to large difference in the dielectric constants of air
and water (i.e. 1 and 80.4 respectively) impedance mismatch occurs. The incident
and reflected signals are captured on the Oscilloscope screen. The time difference
between the two peaks (i.e. the incident and reflected peaks) is found out, which in
return helps to find out the height of water in the tank.
The Fig. 4 shows the setup in the water tank. The propagation velocity of the
probe inserted in the medium must be known to find out the height of water. The
wave propagates through coaxial cable, air and water mediums. The velocity of
propagation is different in each section. The total time will be the summation of
travel times in all the phases (coaxial cable, air and water). Then from the measured
travel time, it will be easy to find out the level of water in the tank [12].
The coaxial cable used here has a solid polyethylene dielectric with dielectric
constant 2.23, and characteristic impedance 50 Ω. The velocity factor of coaxial
cable is 67 %, i.e. the velocity of propagation of wave in coaxial cable is 0.67 times
the velocity of propagation in air (3 × 108 m/s). Therefore, the velocity of prop-
agation of wave in coaxial cable is 2 × 108 m/s.
The relative dielectric constant of water is 80.4. The speed of EM wave prop-
agating through a dielectric medium is given by:

V = c ̸ðε1r ̸2 Þ, ð2Þ

where, V is the velocity of wave in medium, c is the velocity of wave in vac-

uum = 3 × 108 m/s, εr is the relative permittivity.
Time Domain Reflectometer for Measuring Liquid … 165

Fig. 4 Probe setup in the tank describing the various reflection points

Vw = 3 × 108 m ̸s ̸ 80.41 ̸2 = 3.33 × 107 m ̸s ð3Þ

where, Vw is the velocity of wave in water. The velocity of propagation of a wave

in water column is equal to 0.33 × 108 m/s. The velocity of the TDR pulse in
water to air is in the ratio of 1:9 [11]. The sum of all the travel times in different
media will be equal to the total measured time. The wave travels the total length
twice, i.e., to and from the discontinuity.
166 S.R. Mamidi et al.

2*Length
time = ð4Þ
velocity
 
x ðl − hÞ h
t=2 + + ð5Þ
Vc Va Vw

where, t is the total time taken to travel the probe

h is the height of the water in the tank
x is the length of coaxial cable
l is the length of the bi-axial cable
Vc is the velocity of wave in coaxial cable = 2 × 108 m/s
Va is velocity of wave in air = 3 × 108 m/s
Vw is velocity of wave in water = 0.33 × 108 m/s
For a given tank, by substituting all the known values and constants into the
above equation, the relation between time and height can be derived. In this way the
height of water can be found out.

4 Results and Discussion

The experiment was carried out under laboratory conditions to simplify the
experimental environment. Below is the Fig. 5, which shows experimental setup
and TDR circuit. During initial testing of the TDR circuit, a square wave which did
not have clean edges was obtained. There was little bit ringing on the edges, which
will be used to identify the location of the reflected signal in order to calculate the
distance between the source and surface of water. The square wave generated by the
TDR circuit has amplitude of about 5.2 V and frequency 2.84 kHz.
The waveform, in Fig. 6, is the screen-shot of the Oscilloscope. Here, the x-axis
represents time and y-axis represents voltage. The first peak here is the incident
peak, whereas the second peak is the sum of incident and reflected peaks. The other
peaks are the ringing at the edge of the square wave. Later, water is added into the
tank, and the readings are noted at regular intervals (for every 100 ml addition of
water). The time difference between the incident and reflected peaks is observed.
The height of the water in the tank is also noted manually by measuring it with a
scale, which will later be used for verification. Table 1 shows the data from the
experiment. These results are taken directly from the oscilloscope output. This is
because, as the water height increases, the signal travels through more water than
before. Therefore, the time taken to travel the complete path also increases. The
bottom of the tank, i.e. the probe termination and air-water interface are both
considered as discontinuities. But due to the close proximity of the discontinuities
placed at close proximity to each other the reflection was smoothed into a single
discontinuity. As the water level increases, the distance between the discontinuities
Time Domain Reflectometer for Measuring Liquid … 167

Fig. 5 Experimental setup for the TDR experiment. The image on the right is the pulse generator.
The graduated cylinder allows for testing against multiple contaminated water types

Fig. 6 Output due to reflection from probe termination

also increases and therefore there are two reflections which are observed. For an
example, many points can be made out from Fig. 7. The red line represents the x-y
plot at 100 ml and blue line at 200 ml. The second peak reflects from the bottom of
168 S.R. Mamidi et al.

Table 1 Readings of TDR experiment

No. Height (cms) Time difference (ns) Voltage difference (mV) Volume (ml)
1 3.6 13.79 1360 100
2 7.1 14.4 1120 200
3 10.2 17 800 300
4 13.7 19 520 400
5 17.3 28 640 500
6 20.3 29.5 640 600
7 23.9 31 680 700
8 27.4 33 720 800
9 30.5 33.7 560 900
10 34 34 520 1000

Fig. 7 Waveforms at 100 ml (red line) and 200 ml (blue line) water

the tank. We can see that as the height of the water increases, the reflected signal
shifts toward right. Figure 8 is the waveform at 800 ml water, i.e. 27.4 cm height
and Fig. 9 is the data for the pulse edge of the 34 cm height (1000 ml).
Table 2 shows the data obtained during the measurement of the water height and
Fig. 10 shows a plot of the actual water column height versus the calculated height.
For many application this amount of accuracy is sufficient. Many wastewater
storage tank systems for the transportation industry only need to know when the
tank is full or when the tank is empty. The wave-guides used in this experiment
were covered in a thin Teflon® tubing. This tubing allowed the wave-guides to be
placed in both acidic and basic solutions with no change in the signal.
Time Domain Reflectometer for Measuring Liquid … 169

Fig. 8 x-y plot at 800 ml water (27.4 cms)

Fig. 9 x-y plot at 1000 ml water (34 cms)

Table 2 Error between empirical and actual heights

S.No. Time Empirical height, Actual height, ha Error (hc-ha) Normalized
difference (ns) he (cms) (cms) (cms) error
1 13.79 3.97 3.6 0.37 10.27
2 14.4 5.09 7.1 −2.01 −28.3
3 17 9.9 10.2 −0.3 −2.94
4 19 13.7 13.7 0 0
5 28 30.5 17.3 13.2 76.3
6 29.5 33.5 20.3 13.2 65.0
7 31 36.17 23.4 12.8 54.7
8 33 39.92 27.4 12.5 45.6
9 33.7 41.4 30.5 10.9 35.73
10 34 41.8 34 7.8 22.94
170 S.R. Mamidi et al.

Fig. 10 a Empirical height versus time difference, b actual height versus time difference

5 Alternative Sensing Method—Low Cost Doppler Radar

An alternative measurement scheme was considered which employed Doppler

sensing. The Doppler method was first considered to be the primary sensing
methodology but was subsequently chosen to be secondary to corroborate the TDR
measurements or to also serve as a backup in the event of TDR was not as sensitive
as necessary [17–20]. Water level measurements are mostly used by water man-
agers and hydrographers to compute water flow and volumes. Here we are dealing
with measurement of water level in a septic tank. A radar sensor can measure the
level of water by propagating electromagnetic waves with the help of an antenna.
The reason is, radar energy (being an electromagnetic wave) is reflected and
scattered similar to that of light. Objects in the path of propagation reflect the
microwave energy back to an antenna. The time it took for the energy to return to
the radar is determined and the resulting time of flight is used to determine the
distance of the object from the emission of energy (due to a predictable speed of
light). The advantages of radar as a level estimation procedure are clear. Radar is a
non-contact sensor that is essentially unaffected by changes in target temperature,
pressure of the gas and the vapor structure inside of a vessel. The estimation
precision is also unaffected by changes in density, conductivity and dielectric
constant of the target being measured or any turbulence in the air. Doppler systems
are primarily employed as speed and range sensing where the time-domain mea-
surements correspond to propagation of a reflected signal from a moving object.
Both the velocity and position can be determined when the reflected pulses are
compared to the initial transmitted signal pulse. This difference is commonly known
as phase delay. In this application, the liquid waste would only contain lateral
motion, typically the sloshing, or waves and vibration when the tank is in a
Time Domain Reflectometer for Measuring Liquid … 171

non-resting position relative to the ground. Figure 11 shows an concept of how a

Doppler system would be deployed in a large tank. Hence, only a reflected signal
whose amplitude would decrease following the inverse-square law should be used
to determine the relative height of the liquid waste column. A change in liquid level
could be determined, however, if additional liquid were added rapidly to the
column.
To enhance the signal a pyramidal horn antenna was needed for the measure-
ment. Early experiments with out the antenna confirmed this need. The Doppler
equation for a pulsed electromagnetic wave is:

2 ⋅ Vr ⋅ ftx
FD = ð6Þ
c0

where FD is the Doppler frequency, vr is the radial velocity of the target, ftx is the
transmitter frequency and c0 is the propagation velocity of the signal. For most
instances, c0 is given as 2.99 × 108 m/s.
Rearranging the equation to determine the radial velocity of the target

F p ⋅ c0
vr = . ð7Þ
2 ⋅ ftx

The module used in this experiment is the MACOM MA 7801-M

Mono-Doppler transceiver which has a minimum operating frequency of
24.1 GHz (Fig. 12). It contains three pins input, output and ground. It is a pulse
radar transmitter and transmits pulses inside term of nano-seconds and performs
gathering operation too in the meantime. The signal received by the mono-Doppler
transceiver is measured using an oscilloscope.

Fig. 11 Schematic of a
Doppler radar measurement
technique for a liquid
Horn
measurement system
Antenna

Waste Water
172 S.R. Mamidi et al.

Fig. 12 MACOM MA 7801-M Mono-Doppler transceiver used in this experiment. Operating

frequency is 24.1 GHz

5.1 Antenna Design

To improve the gain and directivity during signal transmission and reception, an
antenna needed to be designed to match the transceiver. To keep the cost down, the
materials used for the horn antenna had to be readily available. The material for the
horn antenna consists of circuit board sheet and copper sheet. The design of the
horn antenna was performed using Antenna Magus software. The results of the
simulation of the horn antenna is shown in Fig. 12. The antenna had a gain of
12 dB in the design and a center frequency of 23 GHz. This missed the target by a
GHz but was sufficient for this experiment. The S11 (or reflection coefficient) at
24 GHz was still −22 dB.
An antenna not only helps with gain but more important it improves directivity.
Directivity is the ability to radiate maximum possible amount of microwave energy
into a particular direction i.e., to the direction where we are measuring the solid or
liquid level. It is almost impossible to design an ideal antenna because no matter
how well the antenna may be designed a considerable amount of energy will still be
radiated into all directions. The goal is to design an efficient antenna. The output of
the modeling software is shown in Figs. 13 and 14 demonstrating the resulting gain
and directionality along with the reflection coefficient. Figure 15 shows the final
antenna construction. The antenna was machined in segments and assembled by
Time Domain Reflectometer for Measuring Liquid … 173

Fig. 13 Output of the Antenna Magus software for the horn antenna used in the test. This design
has good directionality

Fig. 14 Gain and radiation pattern for the Horn Antenna

soldering the segments together using copper strips. A copper flange was also
machined and then the horn was soldered to the flange.
The observed signal in an oscilloscope was below the resolution of the oscil-
loscope. This required an operational amplifier circuit LM 741 to increase the
output voltage range of the Doppler unit to allow for better matching to the
oscilloscope.

5.2 Test and Measurement

To get the distance to the top of the septic wastewater it will be necessary to
manipulate the Doppler equations to get the range i.e. the distance to the top of the
liquid to the opening of the horn antenna. The equations can be further manipulated
to provide this distance or range to the target
174 S.R. Mamidi et al.

Fig. 15 Pyramidal horn antenna used to improve signal to noise ratio. This is a fairly large
antenna

c0 ⋅ t r
r= , ð8Þ
2

where tr is the phase delay of the returning pulse and is typically calculated and
displayed using microcontroller technology. This measurement assumes, however,
that the signals emanating from the Doppler transceiver are transmitted and
received perpendicular to the target. Otherwise, an angular correction must be
employed to account for increased distance and increased phase delay. The Doppler
system consisted of a Ma/Com MACS-007801 transceiver. A +18 dBi horn
antenna was fabricated using copper shim stock to focus the signal toward the liquid
column. The horn antenna and mounting over the water tank used in these initial
tests is shown along with the instrumentation. Subsequent Doppler signal amplitude
measurements were made, as shown in Fig. 13 and it was determined that for the
given range of liquid column heights the change in intensity was negligible and
would not be included in the instrument package.
This measurement assumes, however, that the signals emanating from the
Doppler transceiver are transmitted and received perpendicular to the target.
Otherwise, an angular correction must be employed to account for increased dis-
tance and increased phase delay. The Doppler system consisted of a Ma/Com
MACS-007801 transceiver. A +18 dBi horn antenna was fabricated using copper
shim stock to focus the signal toward the liquid column. The horn antenna used in
these initial tests is shown in Figs. 11 and 12 shows that antenna in the test fixture.
Subsequent Doppler signal amplitude measurements were made, as shown in
Fig. 13 and it was determined that for the given range of liquid column heights the
change in intensity was negligible and would not be included in the instrument
package (Figs. 16, 17).
Time Domain Reflectometer for Measuring Liquid … 175

Fig. 16 Measurement setup for radar system. Horn antenna is over the ¼ full water tank

12

11
f(x) = 0.09x + 8.49
Amplitude in Volts

10

9
Amplitude(V)
8
Linear (Amplitude(V))

6
0 5 10 15 20 25 30
Distance (cm)

Fig. 17 Results of the Doppler experiments showing the amplified signal versus the distance.
This signal was usable but have some issues with large outliers

6 Conclusions

The TDR technique has been developed for calibration of liquid level in the tank. It
important to remember that the material in a septic system is non-ideal. The TDR
probe used in this thesis is a bi-axial cable which is designed using two brass rods
encased in a Teflon® sheath. They were assembled in such a way that the char-
acteristic impedance was close enough to 50 Ω, which matches with the source
impedance. The transmission of the wave through the probe and its parameters were
studied. The TDR circuit was built with 74AC14 IC for signal generation. The
generated signal was transmitted through the bi-axial probe, where part of the
incident signal was reflected back to the source when the signal was incident to a
discontinuity. This TDR technique was tested in the laboratory, in a plastic grad-
uated cylinder from which a few conclusions were drawn. The TDR technique is
176 S.R. Mamidi et al.

simple and accurate for measurement of liquid level, and it is a technique that can
be used in situations that regular float-type or pressure based systems cannot. To
verify whether or not this was the most effective type of radar system, the results
were compared with a Doppler based radar. This comparison shows that the TDR
has significantly higher sensitivity than the Doppler. The installation and the use of
a TDR twin-axial probe also is much simpler than the antenna since it conceptually
could use a port on the side of the tank. Other types of probes could be constructed
an implemented allowing for a probe that had a lower chance of catching solids.
This probe was a first pass design and with some problems with impedance
matching though the entire system were observed. Future work will be on opti-
mizing the concept. Additional work will be on designing a measurement technique
that will reduce the need to use an oscilloscope to measure the time-based signal.
Modern high speed oscilloscope on a chip devices could also be used but most of
the devices that can be used to collect information like this are still quite expensive.

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Waterlog
Nanowire (S3) Device for the Quality
Control of Drinking Water

Estefanía Núñez Carmona, Matteo Soprani and Veronica Sberveglieri

Abstract The control and sanitation of water it’s a worldwide concerning problem.
In particular is in developing countries where the need is more evident due to the
lack of sources and appropriate structures to cope with the outbreaks of waterborne
diseases. In most of cases, the cause of these significant epidemiological events
have microbial origin. Despite of it the situation of water supplies and sanitation has
improve all over the world in the last decades. Nanowire technology has already
shown their ability to perform very effective and fast monitoring microbiological
spoilage and quality control. The aim of this study was to test the ability of a novel
S3 (Small Sensor System) nanowire device for the detection of complex mixtures of
bacteria in potable water in order to approach into a real condition, in cooperation
with GC-MS- SPME technique. The achieved results notably advocate the use of
EN as a very easy to use, fast and accurate tool in water quality control.

1 Introduction

Water is one of the most basic chemical compounds, on Earth, it occupies the 71 %
of the total surface area. Even though it provides no calories or organic nutrients is
essential to humans and any kind of life. The amount of fresh water on earth is
limited and its quality is under constant threat. Preserving the quality of fresh water
is important for the drinking-water supply and food production (Table 1).
Nowadays in the developed continents such as Europe and North America
access to drinking water is easy, directly from aquifers, and at a low cost. This leads
to a great waste of this resource, to which there is no longer the proper social and

E. Núñez Carmona (✉)

University of Brescia, Brescia, Italy
e-mail: [email protected]
E. Núñez Carmona ⋅ V. Sberveglieri
CNR-INO Sensor Lab, Brescia, Italy
M. Soprani
University of Modena and Reggio Emilia, Reggio Emilia, Italy

© Springer International Publishing AG 2017 179

S. Mukhopadhyay et al. (eds.), Sensors for Everyday Life, Smart Sensors,
Measurement and Instrumentation 23, DOI 10.1007/978-3-319-47322-2_9
180 E. Núñez Carmona et al.

Table 1 The world’s water resources

Water source Water volume (km3) % Fresh water % Total water
Oceans, seas, and bays 1,338,000,000 – 96.54
Ice caps, glaciers, and permanent 24,064,000 68.7 1.74
snow
Groundwater 23,400,000 – 1.69
Fresh 10,530,000 30.1 0.76
Saline 12,870,000 – 0.93
Soil moisture 16,5 0.05 0.001
Ground ice and permafrost 300 0.86 0.022
Lakes 176,4 – 0.013
Fresh 91 0.26 0.007
Saline 85,4 – 0.006
Atmosphere 12,9 0.04 0.001
Swamp water 11,47 0.03 0.0008
Rivers 2,12 0.006 0.0002
Biological water 1,12 0.003 0.0001

environmental value. In particular, in a developed country as Italy were this

research has being carried out, the 60 % of the piped drinking water is loosed in
leaks every year.
Conversely in the world’s poorest areas the drinking water is rare, expensive and
inadequate compared to the necessary requirements. The major part of the popu-
lation in these regions is compelled to use natural sources of water such as: river,
ponds and rivulets to meet their drinking water needs. These resources are generally
polluted because of the human activities. When consumed, this water leads to
malnutrition and poor hygiene of the population living in these areas.
The data published by UNIDO (United Nations Industrial Development Orga-
nization) (2013) recall that: 1.4 million children die from water-borne diseases
caused by the lack of adequate sanitation every year, in average one child each 20 s.
The World Health Organisation’s (WHO) report “Progress on Drinking Water
and Sanitation” upgraded to 2014 [1] recalls that access to safe drinking water is
essential to human health, food production and urban development. The United
Nations General Assembly (UN) recognized the human right to water and sanitation
on 28 July 2010, through Resolution 64/292.
The biggest differences in the availability of drinking water and sanitation are
between urban and rural areas, the rich and the poor and marginalized. The vast
majority of those without sanitation are poorer people living in rural areas.
The drinking water availability is strictly linked with the sanitation conditions in
which people live. Since 1990, 2 billion people gained access to improved source of
drinking water and other 2 billion people gained access to improved sanitation.
Currently almost 4 billion people, enjoy the highest level of water access: a piped
water connection at their homes.
Nanowire (S3) Device for the Quality Control of Drinking Water 181

Fig. 1 Global drinking water

coverage 2014

Fig. 2 Global sanitation

coverage 2014

Conversely 700 million people still lack a ready access to improved sources of
drinking water and some 2.5 billion people do not use an improved sanitation
facility (Figs. 1 and 2).

2 Increasing the Amount of Drinking Water in the World

About 2.6 billion people—half the developing world—lack even a simple ‘im-
proved’ latrine and 1.1 billion people has no access to any type of improved
drinking source of water. As a direct consequence [2]:
182 E. Núñez Carmona et al.

• 1.6 million people die every year from diarrhoeal diseases (including cholera)
attributable to lack of access to safe drinking water and basic sanitation and
90 % of these are children under 5, mostly in developing countries;
• 160 million people are infected with schistosomiasis causing tens of thousands
of deaths yearly; 500 million people are at risk of trachoma from which 146
million are threatened by blindness and 6 million are visually impaired;
• intestinal helminths (ascariasis, trichuriasis and hookworm infection) are
plaguing the developing world due to inadequate drinking water, sanitation and
hygiene with 133 million suffering from high intensity intestinal helminths
infections; there are around 1.5 million cases of clinical hepatitis every year.
Between 1990 and 2014 the drinking water coverage is growing up from 76 to
89 % (Figs. 3 and 4).
Regarding all continents’ situation for the drinking water coverage is possible to
remark in particular:
• Europe. In Europe the drinking water coverage is optimal; the range is from 91
to 100 %;
• North America, South America, Asia and Oceania. The North America, South
America, Asia and Oceania situation is similar to the Europe one; the range is
from 91 to 100 %;
• Sub-Saharan Africa. In a further 35 countries, 26 of which are in sub-Saharan
Africa, coverage of improved drinking water supply was between 50 and 75 %.
Access to drinking water from an improved source is significantly higher in
urban than in rural areas. In rural areas, in virtually the entire developing world,
drinking water coverage from an improved source remains unacceptably low.

Fig. 3 World population with and without access to an improved drinking water source in 1990,
2004 and 2015
Nanowire (S3) Device for the Quality Control of Drinking Water 183

Fig. 4 World population with and without access to improved sanitation in 1990, 2004 and 2015

Urban drinking water coverage remained the same from 1990 to 2004 at 95 %,
whereas in rural areas coverage increased to 73 % in 2004 from 64 % in 1990. In 27
developing countries, less than 50 % of the rural population have access to
improved drinking water.

3 Sensors Background

One of the types of sensors most frequently used is the metal oxide (MOX or
MOS). The working principle of this technology is that in the presence of a vari-
ation in gas concentration ΔCgas produce a change of electrical conductivity Δσ,
and, therefore, a change of resistance ΔR, for which the measured parameter in this
case is the sensor resistance, R. In other words the principle on which is based the
MOS consists in a variation of the conductivity of the metal oxide in the presence of
volatile compounds compared to the value assumed by the same conductivity in
reference conditions.
The characteristics that should possess an ideal sensor are the following:
• High sensitivity to chemicals;
• High selectivity (low noise) and stability;
• Low sensitivity to humidity and temperature;
• High reproducibility and reliability;
• Reaction time and return short;
• Strength, durability, ease of calibration;
• Small size.
184 E. Núñez Carmona et al.

Conductometric gas sensors based on semiconducting metal oxides are among

the most promising solid state gas sensors thanks to their high sensitivity to a broad
range of chemicals, reduced size and weight, low power consumption, compatibility
with silicon technology, possibility to produce these devices by means of cheap
techniques compatible with industrial scaling up such as sputtering or evaporation
and condensation methods.
Conductometric gas sensors, also named chemiresistors, transduce the presence
in the atmosphere of a given chemical compound through a variation of their
electrical resistance. They are based on semiconducting metal oxides, whose
electrical properties are modulated by red-ox interactions with adsorbing gaseous
molecules.
In particular, active species, such as O–, O2–, O2–, OH–, have been identified as
the active centers responsible for the above red-ox reactions [3]. Such species cover
the oxide surface with their relative population depending on the oxide temperature
and atmospheric composition [4]. In the typical temperature range of metal oxide
chemiresistors (200–500 °C), O2– ions are the most abundant at low temperature
(below 300–350 °C), while a higher temperature favors the dissociation of
molecular oxygen leading to atomic oxygen ions O–. From an electrical point of
view, when a semiconducting oxide is exposed to air, the adsorption of water and/or
oxygen from the atmosphere modifies the band structure of the material at the
surface with respect to the bulk. Chemisorption, involving the transfer of electrons
between the conduction of the semiconductor and the adsorbed atom/molecule, is
that particular form of adsorption responsible for building up the population of
active ions at the oxide surface and the consequent band bending [5].
The further interaction of gaseous molecules with the aforementioned active ions
modulates their population over the semiconductor surface and thus the electrical
properties of the material. According to this mechanism, reducing gases, such as
CO and hydrocarbons, get oxidized reacting with oxygen ions and their population
over the oxide surface decreases, thus increasing the material conductance (for
n-type semiconductors). Oxidizing gases, such as NO2 and O3, are reduced by the
interaction with the oxide surface and, as a consequence, the population of oxygen
ions increases as does the material resistance (for n-type semiconductors).
Through the data acquisition system signals are collected from the n sensors
installed in the measurement chamber of the electronic nose, converted into analog
signals, then acquire, and process through a computer.
During the processing stage, the digital signal of the sensor is managed by
software and is subdivided into a pre-treatment, where they are extracted the
so-called main features of the responses, and in a final treatment for the classifi-
cation and recognition of the smell.
Each element in the sensors array produces an electrical signal in response to the
gaseous mixture. This signal is dependent on a multitude of factors such as:
Nanowire (S3) Device for the Quality Control of Drinking Water 185

• The exposure technique and the type of carrier gas used;

• The chemical nature and the concentration of the odorant;
• The kinetics of diffusion and reaction between the smell and the active material;
• The physical and chemical properties of the materials constituting the sensor;
• The environmental conditions such as temperature and relative humidity.

4 Nanowire Sensors

Metal oxides in the form of nanowires are interesting for their peculiar morphology
and their exceptional crystalline features, the first assuring a high surface to volume
ratio necessary to maximize surface related properties such as the ones governing
chemical sensing transduction principles, while the latter guarantees stable crys-
tallinity and therefore electrical properties over long-term operation, i.e., a required
quality for an industrial application of any kind of sensor in real environments.
Different experimental techniques that may lead to the formation of these quasi
one-dimensional structures. First of all there are two main groups that can be
distinguished: top down and bottom up technologies. The first starts from bulk
structures, reducing them to nanometric dimensions usually with lithographic
techniques, while the latter involve a direct assembly in the desired morphology that
can be obtained from vapor or liquid phase.
At the beginning the research was focused on the vapour phase methods that
were producing, with cheap instrumentation, high quality nanostructures in terms of
crystallinity and stoichiometry. We have thoroughly studied the deposition using
evaporation and condensation from powder in controlled environments using a
different experimental set up.
Tin oxide was preferred over other oxides thanks to its well known chemical
sensing properties and the easy preparation conditions, but indium and zinc oxide
were also studied [6–11].
The experimental procedure consists in the evaporation of the powder (metal or
metal oxide) at high temperatures in a controlled atmosphere at pressures lower than
hundreds of millibar and the following mass transport of the vapour towards the
substrates kept at lower temperatures with respect to the source evaporation region.
Argon, an inert gas, is used for the mass transport in order to avoid unwanted
reactions with the oxide vapour. Critical variables are the distance between the
source and the substrates and the temperature gradient that are controlling
the supersaturation conditions in the vapour phase causing the condensation in the
desired morphology (Fig. 5).
186 E. Núñez Carmona et al.

Fig. 5 Scheme of a Nanowire sensor, from the top to the bottom: Pt electrodes (grey colour), TiW
Pads (brown colour), ZnO Nanowires, Alumina substrate (white colour), Pt heating element (grey
colour)

5 Device Design

The S3 (Gas Sensor System srl—Spin-Off University of Brescia, Italy) used during
the experimental analysis is constituted of: Auto-sampler headspace system
HT280T (HTA srl, Brescia, Italy). The auto-sampler supports a 40 loading sites
carousel and a shaking oven, to provide the equilibrium of the samples head space.
The sensor’s chamber is a thermally controlled chamber with 9 loading sensors
places (Fig. 6).
The sensor array installed in the used instrument is described in Table 2. The
study has been carried out using an hybrid array composed by 3 Nanowires and 3
RGTO.
The advantage of having an hybrids array enhance the performance of the
instrument, that possess the capacity to detect a widest range of volatile chemical
compounds.
Nanowire (S3) Device for the Quality Control of Drinking Water 187

Fig. 6 Sensors’ chamber inside the S3

Table 2 Sensor array details

Sensor Operating Composition Description
temperature (°C)
1 245 SnO2–MoO2 RGTO sensor made of a blend of Tin and
Molybdenum oxides
2 280 ZnO Nanowire sensor made of Zinc oxide
3 375 SnO2 Nanowire sensor made of Tin oxide
4 400 SnO2//Ag RGTO sensor made of Tin oxide catalyzed
with silver
5 500 ZnO Nanowire sensor made of Zinc oxide
6 500 SnO2–WO3 RGTO sensor made of a blend of Tin and
Tungsten oxides

6 Aim

The study and introduction of innovative technologies, that make possible the
access to drinking water and sanitation, are fundamental for the poor countries’
growth and for the welfare maintenance in the developed countries. The wastewater
purification process in the developing countries is the only possible way to make
contaminated water drinkable and, at the same time, it allows to save water in the
aquifers and to increase the availability of drinking water and also to improve the
sanitation conditions.
The improvement of the water quality control systems in both developing and
developed countries is one of the better approaches to reach this objective. This
improvement will not have just an impact in the enhancement of the water sources
for agriculture and industry (incomes and outcomes), but the most important will
have a big impact on the final consumer.
188 E. Núñez Carmona et al.

Currently used methods require high tech lab equipment, high level trained lab
staff, a big investment of money and which is more important requires time. The
aim of this work was to establish a new, rapid and economic fouling, based on the
cooperation between the use of the new S3 device, nanowire tech, and chemical
analytical techniques to detect the presence of complex microbial contaminant sets
in water.
This is possible by using the innovative e-sensing device: Small Sensors System
(S3. S3 device equipped with nanowire tech is based in the analysis of the head
space. The Nanowires are gas sensors based on semiconducting metal oxide are a
promising technology thanks to their high sensitivity to a broad range of chemicals,
reduces size, weight, and low power consumption. These entire characteristic
makes S3 device equipped with nanowire sensor an optimum portable device for
the attainment of on field test. The optimization of the beginning wastewater
purification process and the management of potable water is obtained through the
identification of volatile metabolites (VMs) and volatile organic compounds
(VOCs) released from the microorganisms’ metabolism, that typically contaminate
water [12–21].

7 Materials and Methods

Samples of tap water were sterilized and inoculated with varying rates of the
reference microorganisms, to verify the threshold of the instrument to detect the
presence of bacteria in an environment as close as possible to the real one. The
samples were subjected to conventional microbiological methods aimed at assess-
ing the magnitude of microbial growth, such as measurement of pH, turbidity and
seeding on selective media. The results obtained were then compared with those
resulting from the analysis conducted by means of electronic nose. This comparison
enabled to investigate the ability of the instrument to perceive precociously the
presence of volatile organic compounds resulting from the development of the
bacterial load of the substrate to different microbial loads of departure. These tests
were conducted at first individually considering the different bacteria under study;
later were analyzed bacterial mixtures simulating a real case of multiple contami-
nations. Finally, the samples associated with better outcomes have been subjected
to analysis by GC-MS-SPME technique in order to determine the chemical nature
of the organic compounds most frequently detected from the microbial mixtures
examined.
Nanowire (S3) Device for the Quality Control of Drinking Water 189

7.1 Single Microorganisms Water Tests

7.1.1 Sample Preparation

E. coli, S. Typhymurium, L. monocytogenes and P. fluorescens cultures were

develop in 7 ml Brain Heart Infusion (BHI) (OXOID) liquid media tubes [22].
Once inoculated the tubes were incubated at 30 °C during 48 h. Once the cultures
were grow, were centrifuged at 3000 rpm during 10 min. The supernatant was
discarded and the cells were re-suspended in 1.5 ml of sterilized tap water.
A total volume of 400 ml of sterilized tap water was inoculated with the sus-
pension of cells prepared before until it reaches the same turbidity as the third
standard of the McFarland series. These standards are used as a reference to adjust
the turbidity of bacterial suspensions in order to have a number of bacteria within a
given range. Number 3 of McFarland standard corresponds with a bacterial con-
centration of 9 × 108 CFU/ml. It were prepared as well other 2 dilutions, 400 ml
of sterilized tap water inoculated with 9 × 105 CFU/ml and 400 ml of sterilized tap
water inoculated with 9 × 102 CFU/ml.
A volume of 2 ml was placed separately for every dilution in a sterilized
chromatographic vials (20 ml). Once inoculated all the vials were cover with an
aluminum crimp, a coated PTFE/silicon septum and crimped. This operation was
repeated during the 5 days of analysis (from T0 to T4).

7.1.2 Electronic Nose

The vials were placed in a randomized mode into the HT280T carousel. Each vial
was incubated at 40 °C for 10 min into the HT280T oven, by shaking it during all
the incubation in order to reach the equilibrium of the headspace. The sample
headspace (2 ml) was then extracted from the vial in static headspace path and
injected into the carrier flow (speed 4 ml/min) through a properly modified gas
chromatography injector (kept at 40 °C to prevent any condensation). Using syn-
thetic chromatographic air with a continuous flow rate of 10 ml/min performed the
sensor baseline and the recovery time was 28 min [23]. The sensor baseline was
performed by using synthetic chromatographic air with a continuous flow rate of
10 ml/min and the recovery time was 28 min. In every carousel 4 of the 40 loading
positions were dedicated to vials containing 500 µl of butanol. This compound act
as the internal standard of the instrument.

7.1.3 pH

A control of the pH was done for all the three dilutions. The pH was measured each
hour during the first 24 h of analysis. Whereas During their grow the E. coli pro-
duce organic acids that will acidify the pH of the water.
190 E. Núñez Carmona et al.

7.1.4 Photometer

To survey the development of the microorganisms in water it was measured the

Optical Density (OD) at 600 nm for all three dilutions. The OD data were taken
each hour during the first 24 h of analysis.

7.2 Microbial Blends Water Tests

7.2.1 Samples Preparation

The used microorganisms in this work are Escherichia coli, Salmonella Typhy-
murium, Listeria monocytogenes. Cultures were developed in 7 ml of Brain Heart
Infusion (BHI) (OXOID) liquid media [22]. The cultures were incubated at 30 °C
during 48 h. Subsequently the cultures were centrifuged at 3000 rpm during 5 min,
the supernatant was discarded and the cells were re-suspended in 3 ml of physio-
logical solution. A second step of centrifugation at the same conditions was per-
formed in order to clean any trace of media from the suspension. At the end of the
process the supernatant was discarded and the pellet was suspended in 4 ml of
sterilized tap water. The sterilization process was carried out at 121 °C during
15 min at one over pressure atmosphere in order to eliminate all the microorgan-
isms present in the tape water.
Once culture had been cleaned, the turbidity has been adjusted adding sterilized
tape water until it reached the same turbidity as the third standard of the McFarland
series. These standards are used as a reference to adjust the turbidity of bacterial
suspensions in order to have a number of bacteria within a given range. Number 3
of McFarland standard corresponds with a bacterial concentration of 9 × 108
CFU/ml. These microbial solutions were subsequently used to prepare the bacterial
combinations as it’s indicated in Table 3 to inoculate the samples with a total
concentration of 9 × 102 CFU/ml.
A total volume of 400 ml of sterilized tap water for each mix of bacteria was
inoculated with the suspension of cells prepared before until it reaches 9 × 102
CFU/ml. Once prepared all three dilutions were incubated in the dark at 30 °C
during the 4 days of analysis (T0, T2, T3 and T7).

Table 3 Microbial species CODE Microorganisms

combination for each kind of
prepared sample EC + LM E. coli, L. monocytogenes
EC + ST E. coli, S. Typhymurium
LM + ST L. monocytogenes, S. Typhymurium,
EC + LM + ST E. coli, S. Typhymurium, L.
monocytogenes
Nanowire (S3) Device for the Quality Control of Drinking Water 191

A control sample was also performed using sterilized tap water. In addition, in
this case the parameters of incubation were the same followed by the inoculated
samples.

7.2.2 Electronic Nose

The same procedure as the epigraph 7.1.2 was used for the analysis of samples and
data.

7.2.3 GC-MS-SPME Analysis

GC-MS analysis was performed using a Shimadzu Gas Chromatograph

GC2010 PLUS (Kyoto, KYT, Japan) equipped with a Shimadzu single quadrupole
Mass Spectrometer MS-QP2010 (Kyoto, KYT, Japan) ultra and a HT280T auto
sampler (HTA srl, Brescia, Italy) that allowed SPME analysis.
The vials were incubated in an oven thermostatically regulated at 50 °C for
15 min due to create the headspace equilibrium. In order to extract the volatile
compounds of the samples was used a DVB/carboxen/PDMS stable flex
(50/30 μm) (Supelco Co. Bellefonte, PA, USA) SPME fiber. To provide the
adsorption of volatile compounds the SPME fiber was exposed to the headspace of
the vials for 15 min at 50 °C. For desorption of the compounds the fiber was placed
in the injector of the heated GC for 6 min at 200 °C.
Volatile organic compounds were separated using and analytical capillary col-
umn (DB-WAX capillary column, 30 m × 0.25 mm × 0.25 µm, Agilent Tech-
nologies, Santa Clara, CA, USA) and the carrier gas was ultrapure helium
(99.99 %) at a constant flow rate of 1.3 mL/min. The temperature program for the
GC was performed in the following way: from 50 °C follow of a linear gradient
10 °C/min to 150 °C and held for 5 min, followed by a rise from 150 to 250 °C at
5 °C/min, temperature held 2 min.

8 Results and Discussion

8.1 Single Microorganisms Water Tests

8.1.1 pH and OD

Regarding the OD obtained results, it is possible to observe a typical microbial

curve of growth in all the three dilutions. The Lag phase goes from 0 to 8 h, then
the inoculated cells start to divide and the OD increase until it reach the stationary
phase at 20 h. A proportional but inverse response came out observing the pH data.
192 E. Núñez Carmona et al.

Fig. 7 Linear correlation and 7.70

R2 value for the pH and OD 7.60
data of the 9 × 103 CFU/ml 7.50
of E. coli 7.40 y = -8.1711x + 12.446
R² = 0.9824
7.30
7.20

pH
Series1
7.10
7.00 Linear (Series1)
6.90
6.80
6.70
0.550 0.600 0.650 0.700
O. D. (600 nm)

As the microorganisms develop inside the water, the OD increases because the
turbidity increases as well. The metabolic activities carried out by the microor-
ganisms during their grow causes the production of a big amount of organic acids
that subsequently decrease the pH values. These two variables are inversely related
so a test of correlation between pH and OD was performed for the 3 dilutions. In the
three cases, the negative correlation between the 2 variables were confirmed
obtaining a R2 > 0.98 (Fig. 7).

8.1.2 Electronic Nose

In the two following score plot (Figs. 8 and 9) the control samples are compared,
separately, with samples contaminated with E. coli and P. fluorescens in the days
T0 and T3. All the concentrations studied were considered in the statistical analysis.
For both PCA is possible to observe three clusters of dots clearly separated from
each other, the first of which (at the top left—black) regarding the samples inoc-
ulated with the microbial species of reference, the second covering not contami-
nated samples (blue) and the third (right, upper extremity—green) relative to the
internal standard (pure butanol, 500 μL).
In particular in the second chart (Fig. 9) can be observed a progressive trend line
of the statistical objects included in the cluster of E. coli against the cluster of
analytical blank. This result is in agreement with the nature of the samples subject
to analysis, which are referable to all microbial concentrations studied. In fact the
tail observed is due to samples with a lower microbial load, which will be asso-
ciated with a lower odorous intensity, arranging itself in proximity of the
non-inoculated samples. The experimental investigations were prolonged in order
to determine whether the olfactory system was able to distinguish different
microbial agents of contamination, different microbial loads and/or the different
days of experimentation. In general the instrument has proved to be able to carry
out, at fixed concentration, a proper distinction of individual species concerned over
the several days of analysis, remarkable results were obtained for E. coli at very low
concentrations (Fig. 10).
Nanowire (S3) Device for the Quality Control of Drinking Water 193

Fig. 8 Score plot PCA samples of water contaminated with P. fluorescens (all concentrations, T0)
compared with samples not contaminated and those of BuOH (internal standard)

Fig. 9 Score plot PCA samples of water contaminated with E. coli (all concentrations, T3)
compared with samples not contaminated and those of BuOH (internal standard)

From the chart above (Fig. 10) its possible to observe three homogeneous
groups of statistical objects, among them adequately separated along the first
principal component (PC1), associated with E. coli at a concentration of 9 × 102
CFU/ml. The PCA demonstrates the ability of the instrument to properly dis-
criminate the microbial presence in water for the days of experimentation T0, T1
and T3. The change in the flavor profile detected in the course of time by the
electronic nose could be due to a gradual accumulation of volatile secondary
metabolites. It is possible to relate that response to a release in the surrounding
medium of odorous compounds, which in turn can be associated with phenomena
194 E. Núñez Carmona et al.

Fig. 10 PCA Score plot: comparison of water samples contaminated with E. coli set up at the
time T0, T1 and T3

of cell lysis, frequently observed in advanced stages rather than in the more pre-
cocious. In the following graph (Fig. 11) are compared the results obtained E. coli
and S. Typhymurium (T0 and T4).
The concentration considered is 9 × 108 CFU/ml. The graph shows some
distinction of the cluster relative to E. coli from those of S. Typhymurium most
central with respect to the first, which on the contrary undergo a clear separation
along the first principal component as a function of the different days of experi-
mentation, T0 and T4. The identification of four separate groups demonstrates the
potential of the instrument to discriminate between different microorganisms and

Fig. 11 PCA Score plot of comparison of water samples contaminated with E. coli and samples
contaminated with S. Typhymurium. Days considered: T0 and T4; concentration: 9 × 108 CFU/ml
Nanowire (S3) Device for the Quality Control of Drinking Water 195

Fig. 12 PCA Score plot of a comparison of water samples contaminated with E. coli and samples
contaminated with L. monocytogenes. Concentrations considered: 9 × 102 CFU/ml and 9 × 105
CFU/ml; day: T1

for the same microorganism, among the different days of analysis considered. The
greater separation of the clusters may indicate a greater metabolic reactivity of
E. coli than S. Typhymurium as well as a greater ability to adapt and proliferation
within the medium water, generally poor in nutrients. In the next figure is showed
(Fig. 12) the scores for the water samples inoculated with E. coli and L. monocy-
togenes at the time T1 compared with the different concentrations 102 CFU/ml and
105 CFU/ml.
Although in the figure is not possible to make a proper distinction between the
different microbial loads is still evident discrimination of the various species con-
sidered in two clusters clearly separated along the first principal component (PC1).
In general the lower concentrations have proved to be those associated to the
best instrumental performance in terms of the distinction of the microbial kind than
the different days of analysis. This could be due to the by saturating effect of the
sensor with the higher microbial loads, in absolute terms, greater emissions of
volatile compounds could lead to a reduction in the resolving power of the
instrument exceeding a certain concentration threshold value.

8.1.3 Electronic Nose

In the case of the mixed microorganisms contamination, was demonstrated the

ability of the S3 device to detect the different between contaminated and uncon-
taminated samples.
Below is shown the evidence of the above relating to the mix EC + LM + ST,
well explained previously in the Table 3 (Fig. 13).
196 E. Núñez Carmona et al.

Fig. 13 PCA score plot of water samples contaminated with E. coli, L. monocytogenes e
S. Typhymurium—EC + LM + ST (T3/T7) compared with control samples and BuOH

It is possible to identify three distinct clusters, one of which, relative to the

internal standard, distinctly detached along the PC1 respect to the other two cluster.
The remaining clusters correspond, respectively, to samples not contaminated and
bacterial mixtures with two or three components. The experimental determinations
carried out on bacterial mixtures allowed to test the electronic nose in relation to a
more complex environment, simulating a real case of multiple contaminations. It
was possible to confirm their ability to correctly discriminate, for a given mix, the

Fig. 14 PCA score plot, comparison of water samples on 3 different microbial mixtures:
EC + LM + ST, EC + LM, EC + ST. Day: T2
Nanowire (S3) Device for the Quality Control of Drinking Water 197

Fig. 15 PCA score plot showing T0, T2, T3, T7 for the microbial mix EC + ST

samples obtained on different days (T0, T2, T3, T7). The best results were obtained
for the mixture of E. coli and S. Typhymurium (EC + ST) (Fig. 14).
In the chart below (Fig. 15) is shown the distribution of clusters for the microbial
mixture EC + ST within the information space identified by the principal com-
ponents PC1, PC2 and PC3 for everyday trials of analysis considered.
From the graph con be observed the correct distinction of the samples prepared
in the days of analysis as demonstrated by the identification of four separate
clusters.

Fig. 16 PCA score plot comparison between the samples of T0, T2, T3 for the microbial mix
EC + LM + ST
198 E. Núñez Carmona et al.

Fig. 17 Score plot of PCA: Comparison between the samples during the analysis time of T0, T2,
T3, T7 for the microbial mix EC + LM

Parallel results to that just described above have also been obtained for mixtures
microbial.
EC + LM + ST of which are reported the relative score plot (Figs. 16 and 17).

8.1.4 GC-MS-SPME Analysis

The experimental determinations carried out by GC-MS had as a purpose, the

identification of the main volatile organic compounds synthesized by the bacteria
under investigation, when combined in mixture. Thank to the analysis of the results
it was possible to select the odorous substances associated with higher rates of
detection. In the next table (Table 4) are shown, for each mixture, the volatile
compounds of greater importance identified in the course of several days of
experimentation.
Among the VOCs isolated from the mixtures it is possible to observe a preva-
lence of alcohols with a carbon chain of variable length from a minimum of 4 to a
maximum of 15 carbon atoms, especially in the mix EC + LM and EC + LM +
ST. The alcohols with a number of C atoms greater than 10 (dodecenol, dodecanol,
tetradecanol and pentadecanol) are synthesized and secreted by-products typical of
the degradation of fatty acids. It can be synthetized by several different bacterial
species (including E. coli) mainly in aerobic growth conditions [23]. The bio-
chemical pathways of this catabolic metabolism are highly conserved in a wide
range of different microorganisms.
A second major class of compounds isolated from the bacterial mixtures sub-
jected to analysis is aldehydes. Among these, the most frequently reported are
benzaldehyde, heptanal, nonanal and decanal.
Nanowire (S3) Device for the Quality Control of Drinking Water 199

Table 4 Main VOCs detected by each microbial mixture by GC-MS; Days: T0, T2, T3, T4
Microbial VOCs
blends
EC + LM + ST Indole, 1-pentanolo, 1-nonantiol, Nonanal, 1-dodecen-3-ol, 1-dodecanol,
3-metilbutanol, n-pentadecanol
EC + ST Indole, Benzaldeide, 3-metilbutanol, Nonanal, Decanal, Benzoic acid,
Butirric acid, 2-etilesanol, n-amilisovalerate, Acetilmetilcarbinol,
1-pentanol, 1-dodecanol, 1-tetradecanol
EC + LM Indole, Benzaldeide, Butanoic acid, Decanal, 1-pentanol, 1-ottantiol,
Nonanale, 3-metilbutanol
LM + ST Benzaldeide, Eptanal, 1-tridecen, n-tridecanol, 3-metilbutanol,
3-metilbutilformiate

The compound ever more frequently isolated from mixtures containing E. coli is
indole. Indole is a heterocyclic compound of empirical formula C8H7N. At room
temperature is presented as a white solid colorless with characteristic aroma. It is in
fact one of the compounds that give the typical smell of the fecal matter along with
several other indole-derivatives such as skatole. It can be found in low percentages
in combination with other substances such as aromatic component of many foods
such as Camembert, Swiss cheese, coconut, black and green tea, rum and toasted
hazelnuts [24]. Various microorganisms (over 85 different species among
Gram-positive and Gram-negative) secrete the indole as a by-product of protein
degradation. It constitutes one of the characteristic metabolites of E. coli, as such
frequently used as a marker for the identification/detection of the bacterium in
different culture media (indole test).
In the following histogram (Fig. 18) is shown the trend of indole emission for
each one of the mixtures studied. The maximum abundance of indole is recorded,
for all mixtures, at T0 and then gradually fell down. This phenomenon is

EC+LM+ST EC+LM EC+ST LM+ST

70000
ABUNDANCE

60000
50000
40000
30000
20000
10000
0
T0 T1 T3 T7
EC+LM+ST 49892 9785 1200 0
EC+LM 60120 45201 21954 0
EC+ST 49852 32154 22182 0
LM+ST 20198 613 400 0

TIME

Fig. 18 Yield of indole emission for each of the microbial mixtures studied throughout the week
of testing
200 E. Núñez Carmona et al.

80000
Indole 3-Methylbutanole Decanale Benzaldeyde
70000
60000
ABUNDANCE

50000
40000
30000
20000
10000
0
T0 T1 T3 T7
Indole 45892 20785 12000 0
3-Methylbutanole 0 60120 50954 0
Decanale 0 76154 19182 0
Benzaldeyde 0 0 TIME 14000 40198

Fig. 19 Yield of the emission of indole, 3-methyl butanol, decanal and benzaldehyde throughout
the week of testing. Mixtures of microbial reference: EC + ST (indole and 3-metilbutanol),
EC + LM (decanal) and LM + ST (benzaldehyde)

attributable to the microbial transfer from a rich culture media (BHI) to the water a
poorer growth medium (water) and therefore less able to support the cell metabo-
lism. It is conceivable that the biosynthetic capacity of the bacteria decreases as a
function of permanence within the system in response to a gradual decreasing of
nutrients with the consequent increase of the cell mortality. The data collected from
the mix EC + ST and EC + LM are examples of the above explanation.
The following graph (Fig. 19) shows the abundance trend versus time of indole
and three other selected VOCs, 3-metilbutanol, decanal and benzaldehyde, con-
sidered of major importance for the various mixtures considered.
In Fig. 19 can be observed 3-metilbutanol and decanal with a similar trend to
indole with a progressive reduction in the synthesis up to complete absence in last
day of analysis.
Whatever distinguishes these compounds from indole is the absence of pro-
duction in the first day of experimentation that might suggest a late synthesis in the
course of bacterial growth. It is possibly facilitated by phenomena of synergy or
competition among different microbial species once these are arranged in the same
medium of growth. An opposite trend with respect to that described above is
recorded for the benzaldehyde whose synthesis is until the time T2 to increase and
become maximum at the time T7.
Nanowire (S3) Device for the Quality Control of Drinking Water 201

9 Conclusions

During this investigation was possible to confirm the potential application of the S3
device to perform earliest and on-situ analysis of the water microbiological quality.
The results achieved demonstrate a capacity to discriminate reliably between
contaminated samples with samples of sterile water, so much as regards the indi-
vidual microorganisms as for mixtures microbial.
The most significant performance was obtained distinguishing different days of
testing (associated at different stages of microbial growth). The artificial olfactory
system (S3) has shown a remarkable versatility in finely distinguish the samples of
lower bacterial concentrations (102 CFU/ml) from samples of sterile water.
In general, the most promising responses were observed in the analysis of the
microbial samples with a concentration of 102 CFU/ml. This is due to a possible
saturation effect exerted on the sensors from bacterial higher concentrations, such as
those associated with a higher emission of volatile compounds.
Predictably mixing the bacteria under study was accompanied by a general
reduction in the ability of the device to distinguish easily the samples that share the
same microorganism. However, it was possible to correctly discriminate and
reconfirm for a given mixture, the different stages of the culture development.
It is necessary to pursue a process of continuous technological improvement
through the design and implementation of sensors, more sensitive and possibly
specific to selected VOCs they appropriate for use as a marker of contamination.
Extending the investigations for the identification and quantification of the
organic substances of microbial origin in contexts gradually more and more com-
plex would allow increasing the knowledge regarding any synergy/antagonism
between microorganisms colonizing the same ecological niche.
The future perspective will be to realize a device, possibly portable, that will be
able to provide, with high degree of sensitivity, a reliable answer in real time about
the hygienic status of drinking water by the simple analysis of odor. The artificial
olfactory system may be used as a screening tool for the distinction of water
samples subject to risk contamination and then proceed accordingly to microbio-
logical investigation.
This kind of approach will offer a considerable savings in terms of time and
money. It will allow sustained control of water sources indicating in situations of
real risk when will be important to perform traditional microbiology and chemical
investigation (longer and more expensive) [24, 25].

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Dec 2015
Milk Quality Monitoring Using
Electromagnetic Wave Sensors

Keyur H. Joshi, Alex Mason, Olga Korostynska

and Ahmed Al-Shamma’a

Abstract This chapter presents a novel approach to monitor the quality of milk
products, based on electromagnetic wave spectroscopy. A comparative analysis is
made to demonstrate the effectiveness of using microwave sensors over the other
types, existing in the wide field of sensing technology. Three broadly used com-
mercial varieties of milk, namely skimmed, semi-skimmed, and whole milk types
are considered for the test measurements. The overall quality parameters of these
products obtained from the market are comparatively measured in terms of their
composition and spoilage with reference to ageing. The experiments carried out
have illustrated that the sensor was able to distinguish one milk type from another.
Moreover, it was also able to differentiate between fresh and aged milk samples of a
given milk type as the number of days passes. The methodology used here employs
Vector Network Analyser to capture spectral signatures in the form of scattering
parameters from electromagnetic wave sensors. These data are then analysed to
evaluate quality monitoring process achieved by these sensors. This work offers a
potential platform for an economical, less complicated, and real-time milk quality
control mechanism that can be employed outside of the laboratories at medium or
large scale retailers in milk supply chain hierarchy.

1 Introduction

Milk, along with other dairy products, is consumed by over 6 billion people around
the world [1]. This shows the importance of milk and milk products, as an integral
part in daily life, especially for those who follow a vegetarian diet, inevitably due to
their nutritional values. Milk supplies nutrients like good quality proteins, fat, car-
bohydrates, vitamins and minerals in significant amount than any other single food
[2]. Dairy industries, that procure milk from dairy farms to process the raw milk in

K.H. Joshi (✉) ⋅ A. Mason ⋅ O. Korostynska ⋅ A. Al-Shamma’a

BEST Research Institute, Faculty of Engineering and Technology,
Liverpool John Moores University, Liverpool, UK
e-mail: [email protected]

© Springer International Publishing AG 2017 205

S. Mukhopadhyay et al. (eds.), Sensors for Everyday Life, Smart Sensors,
Measurement and Instrumentation 23, DOI 10.1007/978-3-319-47322-2_10
206 K.H. Joshi et al.

order to produce pasteurised milk, cheese, butter, ice-cream etc., also play a very
significant part in overall economy of many developing as well as developed
countries. The interest in milk products is continuously growing around the globe
over the years because of several factors like changing dietary habits, improving
nutritional awareness, rising population and overall development in the economy [3].
This growth can be observed from the fact that the milk production, worldwide, has
increased by over 50 %, from 482 million tons as in 1982 to 754 million tons as in
2012, in 30 years, which is projected to increase by 175 million tons (23 %) by 2024
with comparison to that of the base years (2012–2014) [4, 5]. Milk processing at
industrial level, following milk production at dairy farms, is next important stage in
the supply chain of all dairy products [6]. Milk, because of being highly nutritious
food, offers a very good environment for the microorganisms called bacterial
pathogens to develop, breed and grow, eventually causing spoilage of milk. This
phenomenon leads to short shelf-life of milk itself as well as other dairy products
made by processing the milk. Besides shortening the overall edible life span, bacteria
adulteration of any milk products can also cause consumers to contract various food
borne diseases when such affected products are consumed. This can be eliminated to
an extent by milk processing which enables its preservation over longer time-period
and also helps to avoid the problems pertaining to health deterioration because of the
lack in its quality or due to spoilage. Processing of raw milk ensures that its original
nutritional value is maintained which also allows its preservation. Milk with
improved overall natural quality is more preferred over the milk products that have
artificially added nutritious values by processing. The increasing intake of dairy
products provides vital health benefits to a large population of the globe especially
that of the developing countries, in spite of the fact that millions of people in these
nations still cannot afford better quality diets which are expensive [7]. These high
costs of production are not only because of the high value raw milk but its subsequent
stage of milk processing also adds to overall retail value of the end product.
Various milk quality testing techniques are available in industries and are being
developed within research laboratories. The tests focusing on adulteration of milk
are predominant in the industries, besides certain general tests applied to check
overall quality of milk; like phosphatase test used on pasteurised milk and the
acidity development test done on Ultra High Temperature (U.H.T.) processed milk
[3]. There is also growing interest in techniques that are specifically aimed at
determining the contamination within milk, such as Detergent Residue Testing [8].
Microwave sensors are used for a wide variety of applications including mea-
surement of distance, movement, shape, and particle size, but the largest group of
applications is concerned with the measurement of material properties [9]. Novel
applications for these types of sensor have been introduced in food and water
quality monitoring—for meat products [10], vegetable oils [11], and analysis of
water contaminants [12] in the past. The other domain of application for these
sensors is health monitoring where various applications have been introduced
which includes the real-time indication of neurological impairments during surg-
eries [13, 14], and in detection of specific biomarkers in human cerebrospinal fluid
[15]. The fundamental principle of EM wave sensors that operate at microwave and
Milk Quality Monitoring Using Electromagnetic Wave Sensors 207

radio frequencies (RF) is based on the interaction of these signals with the material
under the test. The object under test changes the actual velocity of the electro-
magnetic wave signal, by either attenuating or reflecting it. The advantage of
microwave sensors is that they can be implemented cheaply for a wide range of
applications in a non-destructive yet effective manner and are capable of measuring
without physical contact over a short distance, with the help of penetrating waves
without creating any health hazards [16].
This chapter reports on a novel measuring technique that assesses overall quality
of the milk by employing EM wave spectroscopy approach. Bespoke EM sensors
that operate at microwave frequencies were developed and tested. The quality
assessment is done in terms of classification of the milk type and detection of
spoilage or bacterial adulteration developing over the days within the milk samples.
The three categories of milk majorly sold in the market; namely whole milk,
semi-skimmed milk and skimmed milk were tested. The sensor developed for this
purpose was a resonator cavity designed to radiate within microwave range of
frequencies between few hundred MHz to few GHz. The full laboratory setup
makes the use of Vector Network Analyser (VNA) connected with the EM wave
cavity to record the spectral signatures. The results of these test experiments, as
explained in the following sections, are quite promising for further design and
development of an all-in-one system. This innovative system for quality monitoring
of milk products using EM wave spectroscopy is real-time, with less complexity
and bearable costs, in comparison with many other existing methods currently in
practise. This does not only classify one type of milk from another but also dis-
tinguishes between fresh and aged milk samples under test conditions.

2 Milk Production Stages and Need for New Quality

Control Techniques

Milk is a perishable product, hence, spoils very quickly. Its nature of having lower
acidity and higher nutrients make it the perfect breeding platform for bacterial
micro-organisms, including those which are responsible for food poisoning, known
as pathogens. Bacteria contaminate the milk, and their destruction is the main
reason for milk processing which enables milk preservation. This can be achieved
by fermentation, heating, cooling, and removal of water or concentration or sepa-
ration of various components from milk, to produce foods like butter and cheese
[17]. Table 1 lists the nutritional content of milk types used for making test
samples.
Milk quality control is the use of approved test methods to ensure standards
concerning the milk and milk products are regulated to accepted levels. This takes
the account of composition and purity as well as the level of different
micro-organisms within milk. It includes testing milk and milk products for quality
and monitoring that milk products, processors and marketing agencies adhere to
208 K.H. Joshi et al.

Table 1 Nutritional content value of the three categories of milk

Typical values (per 100 ml) Milk type
Whole milk Semi-skimmed milk Skimmed milk
Energy (kJ) 268 (64 kcal) 209 (50 kcal) 147 (35 kcal)
Fat (g) 3.6 1.8 0.1
Saturates (g) 2.3 1.1 <0.1
Carbohydrate (g) 4.7 4.8 5.0
Sugars (g) 4.7 4.8 5.0
Fibre (g) 0.0 0.0 0.0
Protein (g) 3.2 3.6 3.4
Calcium (mg) 120.0 124.0 124.0

accepted codes of practices [3]. The milk producer expects a fair price in accor-
dance with the quality of milk that they produce. The milk processor pays the
producer and assures that the milk received for processing is of normal composition
and is suitable for processing into various dairy products. The consumer expects to
pay a fair price for milk and various other milk products of acceptable to excellent
quality.
To design a methodology and for developing a system that can test the overall
quality of milk products, it is required to understand the basics of the milk cate-
gories under consideration. Here, the three commercially predominant categories of
milk in consumer market—whole milk, skimmed milk and semi-skimmed milk are
explained along with their spoilage patterns. The Dairy Council, UK, classifies the
three types based on the fat content that they carry. Skimmed milk should not have
fat in excess of 0.3 g per 100 ml whereas whole milk is expected to have a min-
imum of 3.5 g per 100 ml, while, the fat value in semi-skimmed milk ranges
between 1.5 and 1.8 g of the 100 ml of product [18]. Several parameters for the
spoilage of milk were studied and discussed including bacterial growth for both the
milk types, and the observations showed that the bacterial growth patterns in the
skimmed milk did not significantly vary from those in the whole milk. In addition
to that, it was also confirmed that the milk spoilage bacteria grow at similar rates, in
both, skimmed and whole milk types but have different metabolic behaviours
within the two of them [19]. This also supports the results achieved in this work and
the results of other researchers who observed similar rates of growth in skimmed
and whole types [20–22]. These findings lead us to a common conclusion that the
different shelf-lives of skimmed and whole milk types are not characterized by
different bacterial growth rates within them.
In the past two decades, the evolvement in high-speed instrumental testing
techniques to measure milk and dairy product composition provided the required
platform for improvement in overall effectiveness and accuracy of classical
chemical analysis methods [23]. For example, the development of Gas Chro-
matography Olfactrometry (GCO), in combination with mass spectrometry is the
development of analytical tools that can be correlated with aroma/odour perception
of foods. GCO basically detects aroma compounds developed due to degradation of
Milk Quality Monitoring Using Electromagnetic Wave Sensors 209

proteins and amino acids. In improving the milk preservation techniques, spoilage
detection plays a vital role.
Milk spoilage can be defined in many ways and its measure could be different each
time depending upon the context it is discussed in. For example, the simplest defi-
nition of quality product, for a common buyer it would be, a product that tastes good
and smells good [24]. Many times we may find that the milk which is expired as per
its ‘Use By’ date, labelled on its packaging, is not actually outdated and sometimes it
is the opposite way around. This vagueness troubles both, the consumers as well as
the manufacturers. Buyers are mostly reluctant to purchase products close to their
dates of expiry. This ultimately imposes a negative financial impact on dairy industry
[25]. Therefore, there’s a developing need for an accurate milk spoilage detection
method as much as there’s a growing demand in preventing the wastage of milk and
the illnesses occurring due to deteriorated milk consumption.

2.1 Issues Involved in Milk Supply Chain

Shown in the Fig. 1, is the basic block diagram of milk supply chain. To understand
where the crucial challenges and problems lie in the system, it is necessary to study
this hierarchy including the inherent difficulties involved in it. This ranges from the
procurement level of milk taking place in dairy-farms, to the transport and handling
of milk, and stretches to the end consumer level. Primary quality concerns rise at
various stages of this chain, including the retailers that sell the packaged and
processed milk products received from the dairies. For example milk is tested at
both, procurement and packaging levels, by the industries for required amount of
quality and its assurance, but after each phase of transportation it is most likely that
the quality of milk product is altered, especially when the distance is longer and the
quantity is large.
Fragmented Milk Production, where milk production takes place in an unorga-
nized sector, is a big challenge and raises concerns when it comes to milk quality

Farms Transport Industrial Units

(Processing /
(Procurement) (Handling)
Packaging)

Consumer Retailers Transport

(End Use) (Storage) (Handling)

Fig. 1 Basic block diagram of milk supply chain hierarchy

210 K.H. Joshi et al.

and milk procurement over many economies like India—which is the largest pro-
ducer as well as consumer of milk, having the largest livestock worldwide [26]. The
research report by the team also adds that milk supply chains face difficulties in
transporting milk, especially in large quantity, under desired conditions over longer
distances (>200 km) while ensuring the quality of milk products.
This research work is motivated by the need to eliminate the above mentioned
adversities faced by the dairy industry, milk supply chain and the consumers with
regards to the contamination, spoilage and overall quality of milk in terms of
constituents present, including milk adulteration. The issues concerning suitable
levels of fat, added sugar and flavouring in milk also needs to be addressed [7],
where no economical, effective yet easy-to-use method currently exists to achieve
these goals [25]. In the past two decades, the evolvement in high-speed instrumental
testing techniques to measure milk and dairy product composition provided the
required platform for improvement in overall effectiveness and accuracy of classical
chemical analysis methods [23].
In October 2015, raw milk produced by a dairy in state of California, USA, was
ordered to be immediately recalled and quarantined, by a state veterinarian,
whereas consumers were asked to dispose of any products from the given batch of
code date Oct 24 [27]. The order was enforced after confirmed detection of
Campylobacter type bacteria were found in raw whole milk, by the inspectors at
routine sample test. Infection caused by these bacteria could show no symptoms at
all or it could harm the immune system and be life threatening too. Mainly it
includes symptoms like diarrhoea, cramps in stomach, or fever after 2–5 days of
being exposed to the bacteria and remains around a week. Less likely yet possible
symptoms could be joint pain or swelling. Also, a rare illness known as
Guillain-Barré syndrome which brings weakness and paralysis can also occur some
weeks after the initial sickness.
This is one of many stories, which surface regularly from around the world,
related to milk, its contamination, spoilage or adulteration. Food Safety and Stan-
dards Authority of India (FSSAI) defines adulteration in food as, ‘An act of
intentionally debasing the quality of food offered for sale either by admixture or
substitution of inferior substances or by the removal of some valuable ingredient’
[28].
Adulteration can be in either form:
• Deliberate, which is done to gain commercial benefits, like addition of water or
• Accidental, that occurs incidentally due to several reasons like inappropriate
handling.
Around 68 % of milk in India, which is the largest producer of milk worldwide
with 16 % share of global milk production [4], doesn’t meet the quality standards as
recommended [29].
Milk Quality Monitoring Using Electromagnetic Wave Sensors 211

2.2 Application and Need for Novel Methods of Milk

Quality Monitoring

This work seeks to address the issues faced at consumer end of the milk production
supply chain hierarchy as at the milk procurement level dairy industries already
have the robust quality assessment techniques suitable just within the industries as
explained in following Sect. 3 of this chapter.
With this novel sensor application at retailers’ end, the sellers can implement
random checks for the packaged products from a given batch of packaged milk
without having to check every single pack of the same batch. Therefore, it is
broadly applied at the link just before the very end consumer filling in the gap that
the dairy industry has after long transport phase where milk is most likely to
get altered in its quality over longer distances as explained earlier. This can also
eliminate the need to send the test samples to laboratories and awaiting their quality
test results for a day or two, offering a real-time solution to the problem.

3 Current State of the Art

3.1 Spoilage Detection Techniques

Following is brief review of the current advancements being experimented for

spoilage detection in milk.
• pH indicators, is one simple yet widely used sensing scheme. It normally sense
the pH level, and on the basis of detected pH value they aim to determine the
deterioration which leads to inaccurate results. For example, the pH value for
milk which is hygienic enough to be consumed is around 6.7, and this is the pH
level suitable for many types of bacterial micro-organisms to develop [30]. At
lower pH values between 4.0 and 5.0, lactic acid bacteria can grow and produce
lactic acid, which is the phenomenon being used for fermentation of milk for
making various other dairy products at dairy industries and processing units.
• Disposable wireless sensors, are another approach applied for spoilage detec-
tion by the means of detecting bacteria. Remote-query sensor, used to measure
the bacterial count of Staphylococcus aureus ssp. anaerobius (S. aureus) in
milk, is normally a magneto-elastic sensing layer made of ribbon-like thick-film
linked with some chemical. It’s a stand-alone unit. S. aureus are the bacteria that
are residing in milk and breed in multiple as milk spoils; S. aureus infection can
cause human illnesses like toxic shock syndrome, septicaemia or endocarditis
[31]. The disposable sensors are generally made up of a magnetoelastic sensor
composed by a magnetic strip. This sensor is normally a low-cost design but
with magnetoelastic sensors, bacteria detection becomes complex following the
reason that speed becomes a problem with the ATP (Adenosine Tri-Phosphate)
212 K.H. Joshi et al.

bioluminescence method and the PCR (Polymerase Chain Reaction) [25].

Hence, this approach is not so favourable for real-time and rapid testing systems.
The sensor reacts in terms of shifts in its resonance frequency depending upon
the viscosity changes pertaining to Staphylococcus aureus (S. aureus) growth.
Thereby, it undertakes sensing of the spoiled milk. The sensitivity of the sensor
is achieved better in milk than in the culture medium as milk is having higher
viscosity than the culture medium. The passive sensors, particularly, don’t
require internal battery as they receive the power from the query-field. These
sensors get deformed mechanically when they are exposed to magnetic field,
which launches elastic waves that have the highest value at mechanical reso-
nance frequency, within the sensor [32]. Eventually, the mechanical deformation
of the sensor generates specific amount of magnetic flux which is detected
remotely by a pickup coil, without any physical connection between sensor and
remaining apparatus.
• Gas sensor arrays, specifically aim to detect the strains due to the strong
volatile compounds, and they require a very bulky and costly setup. These
arrays normally involve solid state devices, i.e. Metal Oxide Semiconductor
(MOS) and MOS Field Effect Transistor (MOSFET) supported by IR based CO2
gas-sensor arrays [33]. The growth of three various spoilage bacteria, Serratia
marcescens, Serratia proteamaculans and Pseudomonas putida, in milk was
investigated by applying a commercial, solid state system of gas-sensor array. It
was shown that the gas-sensor signals can be used as early indicators for the
beginning of bacterial growth. Start detection for volatile bacterial metabolites
was achieved around 7 h after inoculation corresponding to bacterial number of
104 (cfu/ml). In summary, the gas-sensor detects bacterial metabolites which are
volatile by predicting the strain cultures that a certain compound produces. This
operational behaviour of gas-sensors imposes a limitation to the whole mech-
anism, as for each independent volatile compound produced by different bac-
teria—it is required to establish a dedicated gas sensor to detect resulting strains.
In addition to that, in case of bacteria that generate compounds which are less
volatile, the sensitivity of the sensor has to be made significantly high in order to
be able to sense the low amount of strains.
• Infra-Red (IR) spectroscopy is less famous in industrial platform than the
other methods and also requires a costlier laboratory setup. The biochemical
changes occurring in milk following pH level reduction occurred due to bac-
terial growth can be detected by visible and Short Wavelength Near Infra-Red
(SW-NIR) diffuse spectroscopy (600–1,100 nm). This distinguishes between
good-quality and spoiled milk samples without having to take account of every
individual bacterium by monitoring quality loss in pasteurised skimmed milk
[34]. The main disadvantage of this method is its high installation cost for
experimental setups as the frequency of operation here is in terms of few
hundred GHz to few hundred THz.
Milk Quality Monitoring Using Electromagnetic Wave Sensors 213

• Electrical methods are traditional and use the changes in current through an
amperometric sensor as a measure of determining spoilage. This technique
employs a potentiostat and two electrodes which are immersed in milk samples
having different concentrations of bacterial inoculums and containing methylene
blue [35]. In these types of method spoilage is detected when growing meta-
bolism due to multiplying bacteria leaves a coloured solution into colourless
[25]. The microbial metabolism causes the reduction in methylene blue, which
eventually results into change of current through the electrodes. The Detection
Time (DT) required to sense the detectable change of current gives the measure
of present microorganisms at a given time. This is simpler method as compared
to the orthodox bacteria plating techniques with the only drawback that it
requires continuous supervision.
• Optical test methods, which are conventional, are costly approach to determine
milk spoilage because of the reason that fresh milk micelles have sizes that require
scattering setups to include sources and detectors that operate at wavelengths
λ < 300 nm, which are on the deep Ultraviolet (UV) range, covering the visible
(VIS) range [36]. An approach, with low-cost optical capillaries, to test the quality
of milk involves an optical sensor configuration along with the fibre optical setup
used a simple photonic system with optical capillaries to determine the milk
quality by observing under certain heating conditions [37]. It proved that the
optical capillary is a suitable medium to analyse liquids that show high scattering
of light, e.g. milk. The overall setup used there is still more complex than the
proposed technique based on EM wave sensor in this chapter. Also, such instru-
mentation is relatively costlier, compared to the proposed work here, as that is
made up of a light source, fibre optical link, sensing head, and two photo-detection
units which are controlled by an intelligent detection-and-control system. It, pri-
marily, focused on the variation in quality resulting from predefined storage
conditions. This process requires the heating of milk, as the test takes into account
the influence of temperature on the structure of milk, and hence local heating to the
capillary is introduced [38], which results in quite a large instrument setup.
• Protein count or fat count is also one approach to determine the spoilage in
milk as by measuring the protein or fat counts [39]. Pseudomonas aeruginosa
(P. aeruginosa) have been correlated to proteolytic activities in all food systems
by many other studies as well. It produces a large amount of proteinases and
lipases as well as plays an important role in producing by-products by taking
part in lipid and protein breakdown along with temperature effects and storage
time conditions [40]. So a good amount of technical ability and knowledge is
required, which makes this method less favourite amongst end users. The
industrial approach for determination of protein levels is known as Dumas
method, which is more preferred as it is enhanced version of the standard
214 K.H. Joshi et al.

Kjeldahl method [41]. Both the methods first need to convert measured nitrogen
concentration to a protein concentration, as they don’t directly measure the
protein, which leads to inaccuracies.

3.2 Composition Analysis Methods

As one report from Food and Agriculture Organization of the United Nations
suggests that even after the efforts over past half-century, there still exists the need
for an internationally accepted methods with supporting data [42]. In fact, as it
further describes, the development of new methods for analysing specific compo-
sition elements that yields energy (like protein, fat or carbohydrates) has further
increased the complexity and made this need greater than ever before.
Milk sensing technologies, currently being used, still lacks the intelligent
approaches in practice [43]. As after the determination of good or poor quality of
milk, most of the systems don’t offer the automated diversion of poor quality of
milk so as to maintain the high standards of their products at manufacturers end.
From the above discussion, it is clear that there is scope and also need of
improvement in milk quality testing methods. When it is hard to overcome all the
limitations in all the characteristics as shown in Table 1, there is still a way to
minimize the overall shortcomings of existing approaches.
The use of EM wave sensor can offer good balance among the overall aspects
including performance, costs, reliability and less complexity, in comparison with
the currently used standards. In this chapter, as described in following section, the
attempt is to address these limitations by the design and development of a sensory
system that is able to distinguish among given types of milk based on:
• Fat composition (five different samples ranging from 3.6 to 0.1 g per 100 ml)
and
• Spoilage detection between fresh and old milk samples
Table 2 summarises these current advancements, as discussed above, for
detecting milk quality using various measures, along with the main parameter that
they detect to enable the test, its main limitation and primary advantages as further
explained in [25]. The techniques are categorised based on whether they are
spoilage detection methods or composition tests. This list can be more extensive
with increasing amount of interest in the field of food quality assessment, especially
with the help of various sensing technologies. This work is an attempt to address the
shortcomings that the current technologies have while giving optimum results for
determining the milk quality.
Milk Quality Monitoring Using Electromagnetic Wave Sensors 215

Table 2 Summary of current advancements in milk quality testing technique

Type Techniques Detection parameter Advantage Limitation
Spoilage pH Indicators pH levels due to Instantaneous Inaccuracy;
detection presence of lactic response pH level
methods acid bacteria fluctuates
(Lactobacillus,
Lactococcus,
Leuconostoc)
Disposable Viscosity changes Low-cost raw Speed
remote-query due to S. aureus material; No deficiencies
sensors growth external
power
required
Gas-sensor Volatile compounds Rapid and Less sensitive
arrays (produced due to S. accurate towards
marcescens, S. determination bacteria
proteamacufans, Ps. of shelf-life producing less
putida) volatile
compounds
IR/NIR Metabolic High High
spectroscopy byproducts efficiency costliness
(developed due to
proteolysis and
lipolysis)
Electrical Changes in current No Time
method flowing through an supervision redundant
amperometric sensor required
(due to microbial
organisms)
Optical Scattered light Suitable for Milk samples
sensors through fresh and analysis of in optical
old milk samples in liquids giving capillaries
optical capillaries high light require
scattering heating
Protein/fat Changes in milk Fast methods Extensive
count lipids/proteins due to sample
varying preparation;
P. aeruginosa levels Requires
acquired skill
Composition Fat analysis Milk fat released Low-cost Not
analysis (Gerber using centrifugation methods automatic;
methods method; in butyrometer with Requires high
Babcock sulfuric acid and concentration
method) Isoamyl alcohol sulfuric acid
Protein Measures nitrogen Automated High initial
analysis levels to convert into and costs
(Kjeldahl protein value quick-time
method;
Dumas
method)
216 K.H. Joshi et al.

4 Electromagnetic Wave Sensing Technology

4.1 Fundamentals of Microwave Sensors

The antennas used for wireless and mobile communication operate on the EM wave
transmission and reception. The EM wave based sensors, as used in this work, are
the similar devices customized for different type of applications of sensing and
detection. Wide range of variety exists within this group of sensors based on the
way they are made, type of operation or range of frequency they work upon. EM
wave or microwave sensors are mainly categorized into two groups, based on their
applications. One group is of the radiometer, topographic and radar sensors for
applications related to distance, movement and shape measurement [44]. The sec-
ond group, which is related to this research work, is of the sensors like resonance
cavity, waveguide sensors and transmission or reflection sensors, which are used for
measuring material property, especially those of liquids and gases flowing or held
through within them [9].
EM wave sensing or microwave sensors operate based upon the fact that the
material under test condition, e.g. milk sample in this case, when placed into
proximity or in direct contact with a microwave sensor, interacts with the EM
waves that can be specifically correlated with the properties of the given material
(milk). Particularly, the sensing is based on the interaction of propagating or res-
onating modes with the liquid under test. Due to this interaction, the permittivity of
the material changes and it reflects itself as a frequency change, attenuation of the
signal or a phase shift [45].
The material to be tested with this methodology is exposed to the electromag-
netic field generated by the sensor fed through a source. For example, the 2-port
microwave resonator cavity is designed to hold the test-tube containing milk sample
to carry out the quality sensing, as depicted in Fig. 2. The changes captured in the
sensor’s spectral responses, through a network analyser, then become indication of
the differences among samples under consideration [46]. These differences could be
based on the composition, i.e. milk types, or could be changes between the
adulterated (spoiled) and fresh samples of the same milk product.

Fig. 2 An EM wave
resonator cavity sensor
Milk Quality Monitoring Using Electromagnetic Wave Sensors 217

These types of sensor have following primary advantages over the types that
have been discussed in earlier sections:
• Less complexity in installation of experimental/lab setups
• Universal applications (i.e. not specific to each bacteria/lipid/protein type)
• Wide range of variety according to needs of the application
• Better accuracy and less costs

4.2 Dielectric Properties of Milk

For development of a new technology that can evaluate milk quality, it can be
important to possess the understanding of dielectric properties of milk. The
dielectric constants for both, the raw milk (with 100 % concentration of milk) and
the diluted milk (with 70 % milk concentration to deionized water) decreases with
increasing frequency, more so at the lower frequency range of 10–4500 MHz, but
dielectric constants for raw milk decreased more rapidly than in case of the diluted
one, at room temperature of 22 °C [47]. For raw milk it was 97.7, 68.1, and 65.9,
whereas 93.3, 70.9 and 69.1 for 70 % milk solution, at 10 MHz, 915 MHz, and
2450 MHz, respectively. The dielectric loss factor can be another potential indi-
cator for prediction of milk concentration as well as freshness. Since, the adulter-
ation of milk with water dilutes the ionic concentration within milk, the loss factor
decreases with the increase in water content, which is decrease in the milk
concentration.
Another work, concludes, that both, the dielectric constant as well as the loss
factor, for cow milk, are affected by the protein content and also the temperature of
milk. The frequency of electric field influences these two values, too. The dielectric
constant decreased with increase in the frequency within range 10–4500 MHz [48].
The dielectric loss factor increased with increasing temperature below around fre-
quency values of 600 MHz and decreased above frequencies of 1000 MHz. Poor
correlation was seen between the dielectric constant and the protein content in the
region of 100–600 MHz frequency values which means that this frequency range is
insufficient for being used to develop milk protein detector on the basis of dielectric
constant values.

5 Methodology and Measurements

This work takes into account the literature studied and uses resonator cavity as an
EM wave sensor operating at microwave frequencies to evaluate milk quality. The
procedures adopted to carry out the milk sensing and quality tests using this sensor,
are explained below.
218 K.H. Joshi et al.

5.1 Sample Preparation and Measurement Conditions

Three milk types, namely skimmed, semi-skimmed and whole milk were bought
from a local chain of stores for the tests. Five samples were made from each of this
categories and labelled as shown in Fig. 3. To ensure that we have more accurate
results and more no. of points for Fat versus Frequency graphs, another two cat-
egories were made by mixing two types of milk respectively. That is 50 % whole
milk was mixed with 50 % semi-skimmed milk and 50 % of skimmed milk to the
another 50 % of semi-skimmed milk which ultimately gives us 2 more varieties (5
in total) in terms of fat content. Each sample was of 15 ml in size, held in a
polypropylene plastic test-tube.
The samples were made at room temperature and the storage conditions were
governed in a temperature controlled climate with minimum fluctuations. For the better
accuracy of captured spectral data, 5 repetitions were made for each of the 5 samples for
all 5 categories of milk giving eventually 125 iterations to be mathematically analysed.
The test-tubes as shown in Fig. 3, were labelled as W-1, W-2, …, W-5 for whole milk,
SS-1, SS-2, …, SS-5 for semi-skimmed milk and S-1, S-2, …, S-5 for skimmed milk as
abbreviated, respectively. Similarly semi-skimmed + skimmed milk solution and
semi-skimmed + whole milk solutions were labelled SSS-1, SSS-2, …, SSS-5 and
SSW-1, SSW-2, …, SSW-5, respectively. Table 3 lists the test measurement specifi-
cations with sample storage condition.
For the measurements with EM wave cavity resonator sensor a slot that can be
inserted with the milk samples in 15 ml test-tubes, was used as shown in Fig. 4.
The 2-port cavity was calibrated with the VNA, prior to measurement to enable
accurate measurements of S11 (reflected back signal to input port-1) and S21
(transmitted signal from input port-1 to output port-2). The captured raw data of
spectral signatures consisted of 60,000 point values each for different frequency
within the range given, i.e. 10 MHz–15 GHz. Laser beam thermometer along with
the digital probe thermometer were used to ensure stable temperature conditions
before, during and after the measurements as can be seen from the illustration.
For the measurements a 2-port EM wave cavity was used as shown in Fig. 4
along with a VNA. Wide frequency sweep (10 MHz–15 GHz) allows more spectral

Fig. 3 Sample preparation for milk quality testing using EM wave spectroscopy
Milk Quality Monitoring Using Electromagnetic Wave Sensors 219

Table 3 Measurement specifications and sample storage conditions

No. of measurements 5 Samples × 5 Repetitions × 5 Categories = 125 Iterations
EM wave resonator cavity Φ = 130 mm (distance between ports)
h = 20 mm (height of cavity)
Size of samples 15 ml (polypropylene test tubes)
Period of supervision 1 week
Temperature 21 ºC ± 1 ºC
Frequency sweep 10 MHz–15 GHz
Channel base power 0 dBm

Fig. 4 EM wave cavity testing milk sample using VNA in temperature controlled climate

data to be captured before sending to further analysis ensuring comparison of more

spectral signatures for better results. The distinguishing frequencies were identified
for all 3 types of milk to enable their classification. Same goes for the detection of
spoilage for a given type of milk and its comparison with previous day measure-
ments to the following days in 1 week period. S11 and S21 parameters plots were
captured with the use of VNA, in one minute, for each sample test.

5.2 HFSS Design and Simulations of the Sensor

The EM wave cavity sensor was modeled and simulated with the help of High
Frequency Structure Simulator (HFSS), as shown in Fig. 5, before the development
of its fabricated hardware. The resonance frequencies for TE mode and TM mode
equations for microwave cavity are given by Eq. (1) and Eq. (2), respectively [49]:
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
 ′ 2  
1 Xmn pπ 2
fmnp = pffiffiffiffiffi + ð1Þ
2π μϵ R L
220 K.H. Joshi et al.

Fig. 5 HFSS model of the resonator cavity

Fig. 6 3-D Polar plot of EM wave cavity for the frequency sweep 10 MHz–15 GHz
Milk Quality Monitoring Using Electromagnetic Wave Sensors 221
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
 
1 Xmn 2 pπ 2
fmnp = pffiffiffiffiffi + ð2Þ
2π μϵ R L

where, R and L are radius and length for a cylindrical cavity, respectively. Xmn
represents nth zero of mth Bessel function and X′mn represents nth zero of derivative
of mth Bessel function. µ and ϵ are permeability and permittivity of the medium,
respectively. Here, p is the no. of half waves in the axial direction.
Figure 6 illustrates the field polar plot in 3-dimensions showing how the radiated
EM wave energy spreads through the cavity. The primary difference between the
microwave sensors and communication antennas is their far-field patterns. As we
can see from the plot, in the case of a sensor, radiation is mainly near-field whereas
it is opposite in case of an antenna. The reason behind that is, an antenna is
supposed to radiate over a distance to enable wireless communication between two
points while a sensor is ideally meant to sense the material in its nearest proximity
with or without physical connection with the material being sensed.

6 Results Discussion

As shown in Fig. 7 for whole milk, there is a clearly visible distinction between the
curves for S21 plot of Day-1 and Day-7. Five repetitions for each sample were
made. Similarly, Figs. 8 and 9 show the graphs for semi-skimmed and skimmed
milk, respectively. These plots are identical with minor shifts for all 3 given types

Fig. 7 S21 variations between Day-1 (Blue) and Day-7 (Grey) for whole milk
222 K.H. Joshi et al.

Fig. 8 S21 variations between Day-1 (Green) and Day-7 (Grey) for semi-skimmed milk

Fig. 9 S21 Variations between Day-1 (Red) & Day-7 (Grey) for skimmed Milk

of milk and shows effective results to distinguish between the aged and fresh milk
samples.
Figure 10, on the other hand, distinguishes among the 5 various samples made
from 3 categories, based on their fat content, of milk and labelled as S, SSS, SS,
SSW and W as explained earlier. The figure shows spectral graph of S21 against the
fat content of milk. The biggest advantage of this novel technique is, it does not
Milk Quality Monitoring Using Electromagnetic Wave Sensors 223

Fig. 10 S21 variations with respect to fat contents of 5 types of milk samples (Day-1)

Fig. 11 S21 variations with respect to protein contents of 5 types of milk samples (Day-1)

only detect ageing but also distinguishes quite well among the types of milk as can
be seen below. These 5 samples are achieved by 3 different milk types; skimmed,
semi-skimmed and whole, and another two by adding 50 % of each, Skimmed milk
with Semi-skimmed milk, and 50 % of each Semi-skimmed milk with the Whole
milk, in order of fat content values.
We see the linear regression with correlation value, R2 = 98 %, at the frequency
value of 5.4598 GHz. This technique is less complex, and therefore, quick-time
result oriented method than other methodologies previously explained in this arti-
cle. The results achieved in this preliminary work of the whole project give accurate
detection and efficient outcomes.
Figure 11 shows the S21 plot versus the protein content graph of the five types of
milk. Here, unlike in case of fat content variations, the linear regression gives
224 K.H. Joshi et al.

R2 = 94.99 % at 4.989 GHz, which is due to relatively less variations in protein

content. These results, in a way, compliment the previous findings by others as
discussed in the dielectric properties of milk section of this chapter.

7 Future Work

The future extension of this work contains:

• Design and development of a single EM wave patch (resonator) sensor, instead
of a cavity, that can accommodate the following three quality check and control
parameters:
(i) Spoilage/Adulteration
(ii) Composition and
(iii) Contamination
Optimization and customization of the final design that integrates all these
objectives into a single sensor can further help for real-time, stand-alone operation.
With a patch resonator, which is of few centimetres by centimetres sizes, the milk
sample can actually pass between the wings of resonating patch sensor using a
fluidic pipe system for determination of quality.
Also, it should be noticed that the same category of consumer milk may still
have differences in its compositional values, the ultimate design with certain cus-
tomisation can be targeted to achieve grading among various samples given. To
enable real-time operation, and grading of samples, the support of tools like
MATLAB or LAB View can be incorporated.

8 Conclusion

The electromagnetic wave cavity is acting as a microwave sensor to detect adul-

teration and the type of milk. A wideband source applied to the cavity helps locate
the values of frequency thereby allowing customization of the design that gives
optimum results. Once having located the responding frequency values, dedicated
EM wave sensors including microwave patch sensors, like Interdigitated Electrodes
(IDE) or hairpin resonator, can be designed to operate on the same corresponding
resonant frequencies for an optimized milk quality testing system.
This technique indeed shows a promising future for design and development of a
milk quality testing and control system, of milk products, as it has several
advantages over the other already existing standard practices. These advantages
include less complexity, higher accuracy, time and cost-effectiveness and universal
approach to milk types and quality detection. This work presents a very good
prototype model for a novel, online EM wave based quality testing system that can
Milk Quality Monitoring Using Electromagnetic Wave Sensors 225

be made standalone and applied to large or medium scale retailers’ level of milk
supply chain hierarchy to avoid ambiguities and wastage of large quantity of milk
as well as prevent any food-borne illness occurring due to spoilage or adulteration
of milk.
This, with further optimasation, can help the large-scale or medium-scale
retailers, who receive the milk from dairies for selling in packaged form after long
stages of transport, to help allow the quality assurance and also to ensure that the
customers are getting what they are paying for. This work not only will establish a
strong base for the laboratory based research but also must aid towards the problem
solving that the dairy industries and end consumers face due to either complexity or
costliness of existing standard practices for milk quality control.

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Grated Parmigiano Reggiano Cheese:
Authenticity Determination
and Characterization by a Novel Nanowire
Device (S3) and GC-MS

Veronica Sberveglieri, Manohar P. Bhandari, Andrea Pulvirenti

and Estefania Núñez Carmona

Abstract Parmigiano Reggiano (PR) cheese is produced from the bovine milk in a
limited geographic area in northern Italy. It is one of the oldest traditional cheeses
manufactured in Europe (XII century) and is still one of the most esteemed Pro-
tected Designation of Origin (PDO) cheeses of Italy. The Parmigiano Reggiano
Cheese Consortium (CFPR) is the institutional system that covers all the cheese
dairy factories and controls the cheese production in terms of cow feeding, cheese
manufacture and ripening processes. The aim of this study was to establish a new,
rapid, portable, easy-to-use, economic and non-destructive fouling based on
nanowire technology device (S3) to control the presence of false grated PR. All the
analyzed samples were collected from the Consortium that picked the samples
produced in different European countries (three samples from Germany, one from
Ireland, one from Latvia and one from Lithuania). The achieved samples were
analyzed with the cooperation of multidisciplinary technologies like Colorimeter,
pH Meter, GC-MS with SPME and the new nanowire gas sensor device (S3). The
applied techniques were able to create a specific database for the S3 device, capable
to give results in a few minutes. The use of a Small Sensor System (S3) device to
determine the specific volatile organic compounds (VOCs) of the grated PR is a
promising approach offering, at the same time, a simpler, faster and easier to handle
(no specialized technicians are required) solution with respect to the analytical
techniques (GC-MS, HPLC). However, from the commercial point-of-view, low
cost and reduced power consumption are the fundamental features that should entail
a sensor device. In this study, S3 device was applied and found to be efficient in the
discrimination of the different grated PR cheese samples. In particular, the dis-
crimination was checked quali-quantitatively thanks to the analysis performed with
the GC-MS-SPME technique. In fact, the achieved results demonstrated the

V. Sberveglieri (✉) ⋅ M.P. Bhandari ⋅ E.N. Carmona

Sensor Lab, CNR-INO, Brescia, Italy
e-mail: [email protected]
M.P. Bhandari ⋅ E.N. Carmona
Department of Information Engineering, University of Brescia, Brescia, Italy
A. Pulvirenti
Department of Life Sciences, University of Modena and Reggio Emilia, Reggio Emilia, Italy

© Springer International Publishing AG 2017 229

S. Mukhopadhyay et al. (eds.), Sensors for Everyday Life, Smart Sensors,
Measurement and Instrumentation 23, DOI 10.1007/978-3-319-47322-2_11
230 V. Sberveglieri et al.

quali-quantitative differences of the VOCs emitted by the samples. S3 device is a

promising tool for the quality discrimination of the PR cheese and other foodstuffs.
In our future works, specific database of the grated PR will be amplified for the
direct use of S3 in the cheese-chain productions.

1 Introduction

Parmigiano Reggiano is a hard cheese, slowly matured, made from the raw
semi-skimmed milk from cows whose diet consists mainly of fodder from the
original area (Reggio Emilia, Parma, Modena, Bologna and Mantova). The milk
may not be subjected to a chemical treatment and is not allowed for the use of
additives [1–4].
Through this characteristics a form of cheese is produced called as Parmigiano
Reggiano, a Protected Designation of Origin (PDO) product, according to the
European EEC Reg. 2081/92 and the recognition of Reg. (EC) No 1107/96 by its
disciplinary and as evidenced by the Consortium.
This organization, therefore, has the task to protect the Parmigiano Reggiano
from its imitations and many frauds that are being reported around the world. In
fact, the designation of origin of the cheese ‘Parmigiano Reggiano’ extends to the
grated type cheese.
In addition, the cheese must have some special characteristics: fat content in dry
matter must not be less than 32 %; aging not less than 12 months and within the
limits fixed by the production standard.
It must not contain additives; organoleptic characteristics must be consistent
with the definitions laid down by the production standard; humidity not less than
25 % and not more than 35 %; aspect: not crumbly, homogeneous, particles of
diameter less than 0.5 mm not exceeding 25 %; rind quantity not greater than 18 %;
amino acid composition: specific of ‘Parmigiano Reggiano’ [4, 5].
All these characteristics will be treated deeply in the next epigraphs of the
current chapter.

1.1 Production Area and Spinneret

The link between Parmigiano Reggiano and its area of origin is essential. Parmi-
giano Reggiano comes from the territory and the tradition of man. It is produced
today just as nine centuries ago: the same ingredients (milk, salt, rennet), the same
care and passion, the same area of origin.
The area of production of Parmigiano Reggiano (Fig. 1) is located in the pro-
vinces of Parma, Reggio Emilia, Modena, Bologna to the left of the Reno River and
Mantova to the right of the River Po.
Grated Parmigiano Reggiano Cheese: Authenticity … 231

Fig. 1 The area of production of Parmigiano Reggiano

This area must be involved either in the milk production or its transformation
into the cheese.

1.2 Production Technique

The milk for the production of Parmigiano Reggiano comes from the cattle fed with
natural fodder and the production process starts from the raw milk. The actual
process is carried out using the same ancient technique but in modern settlements
with new machinery.
The raw material is the evening milk, which is allowed to stand in large stainless
steel tanks, as shown in the Fig. 2, to bring out the cream, and the whole milk from
the morning milking. In the morning, it proceeds with mixing the semi-skimmed
milk and the whole milk in copper vats shaped like an inverted bells.
The whey and the calf rennet are added after the milk has been heated to a
temperature of 33 °C. After the mongrel coagulation, which takes place in 15 min,
and thanks to the spino (Fig. 2), the curd is broken into small fragments having the
size of a grain of rice and is cooked up to 55 °C [1].
After these operations, the mass is left to rest for 30 min, then extracted with a
linen canvas of 1 m2 and is placed in the molds, where it undergoes a pressing step.
After a few hours, the wet cloth is changed with a new one and then is removed
to insert a matrix for stamping the identification data of the form on the crust: month
and year of manufacture, the serial number of the dairy and the dots-label for
Parmigiano Reggiano. Salting is carried out by bathing in brine for 25–30 days.
Maturation takes place in appropriate constant temperature and humidity
warehouses, where the forms are constantly brushed and turned; to perform a
homogenous seasoning and to prevent the overgrowth of surface mold.
Only after a minimum period of 12 months, the forms that will be found correct
by the examination of the Consortium Body Control become full Parmigiano
Reggiano.
232 V. Sberveglieri et al.

Fig. 2 a The addition of rennet, b the dowelling, c collection in the linen bands, d the molding,
e salting and f the curing in a controlled environment

Therefore, it becomes important to find a method to determine the origins of the

grated PR cheese based not only on the classical expensive and slow chemical and
physical techniques. The possibility of detecting the addition of cheese (with a big
range of different seasoned cheeses from different country of origin) to the grated
PR cheese has been always studied by means of destructive chemical methods.
Aroma (fingerprint) is one of the most significant parameters of foods from the
sensory point of view, and it may offer information about the safety and quality of
the food, acting sometimes as an indicator of processing mistakes as well.
Grated Parmigiano Reggiano Cheese: Authenticity … 233

The use of a Small Sensor System (S3) device, to determine the specific VOCs
of grated PR is a promising approach offering, at the same time, a simpler, faster
and easy to handle (no specialized technicians are required) solution with respect to
the analytical techniques (GC-MS, HPLC).
However, from the commercial point-of-view, low cost and reduced power
consumption devices are the fundamental features.
Gas chemical sensor arrays or Electronic Noses (EN) have been identified in the
past few years as the valuable candidates for different applications including food
quality control.

1.3 Aim

The aim of this study was to establish a new, rapid, portable, easy-to-use, economic
and non-destructive fouling based on the nanowire technology device S3 to control
the presence of false grated PR. All the grated cheeses were prepared using the same
grinding machine using a predefined mesh dimension (ASTM series, mesh n°35).
The possibility of detecting the addition of cheese (with a big range of different
seasoned cheeses from different country of origin) to the grated PR cheese has been
always studied by means of the destructive chemical methods.
Thus the application of a novel nanowire device S3 can serve as an effective
means to determine the authenticity of a PR cheese and also to characterize its
quality parameters at the same time. Six different foreign cheese samples originated
from Latvia, Lithuania, Ireland and Germany (Hartkase, Hartkase 1, Hartkase 11)
were analyzed.

2 Materials and Methods

2.1 Sample Preparation

The preparation of the samples (Table 1) was carried out as follows: 2 g of grated
cheese was placed in a 20 ml chromatographic vial. Subsequently all the vials were
covered with the Silicon-PTFE septum and crimped with an aluminium crimp. At

Table 1 Foreign cheese ple List Aw

samples and their Aw values
Latvia (CMP1) 0.821
Lithuania (CMP6) 0.824
Ireland (CMP4) 0.836
Harkcase1 (CMP2) 0.833
Hartkase11 (CMP3) 0.832
Hartkase (CMP5) 0.823
234 V. Sberveglieri et al.

the same time, the water activity was measured in order to control and assure that
this parameter will not influence the sensor response.

2.2 S3 Device Analysis

At SENSOR laboratory, the studies on chemical sensors started in 1988 with the
improvement of thin films and then of a new technique for the planning of thin films
with an extremely porous structure.
In 2002, quasi-one-dimensional metal oxide nanostructures were achieved with
several advantages compared to their thin and thick film counterparts such as large
surface-to-volume ratio, lateral dimensions comparable to the surface charge region,
and superior stability when in the single crystal structure.
The novel nanowire device S3 is a production of the SENSOR laboratory.
The Small Sensor System (S3) device (Fig. 3) is equipped with a thermally
controlled sensor chamber of 20 ml internal volume where there are placed 6 MOX
gas sensors.
Three of these sensors were prepared with the RGTO thin film technology [6],
and the other three constructed with the nanowire technology [7]. In fact, two of the
three nanowires in the array are zinc oxide sensors but with different operating
temperatures and the third one is a tin oxide sensor [8].

Fig. 3 Small Sensor System

(S3) device
Grated Parmigiano Reggiano Cheese: Authenticity … 235

The vials containing different samples were placed in a randomized mode into
the HT280T carousel. Each vial was incubated at 40 °C for 10 min into the
HT280T oven, by shaking it throughout the incubation.
The sample headspace (4 ml) was then extracted from the vial in the static
headspace path and injected into the carried flow (speed 4 ml/min) through a
properly modified gas chromatography injector (kept at 40 °C to prevent any
condensation).
Using synthetic chromatographic air with a continuous flow rate of 10 ml/min,
the sensor baseline was performed and the recovery time was 28 min. The data
analysis was run by means of Principal Component Analysis (PCA), operated with
the Nose Pattern Editor software (SACMI Imola scarl, Imola, Italy).
The scheme of the sensor device based on an alumina transducers 2 × 2 mm2
with the heater on the backside is shown in Fig. 4 together with the SEM images of
nanowires. Tin and Zinc oxide nanowires exhibit a remarkable crystalline quality
and a very high length-to-width ratio, resulting in an enhanced sensing
performance.
The nanowire sensors thus manifesting a very high length-to-width ratio create a
3 dimensional network (Fig. 4). In this way, the adsorption surface is increased in a
huge amount enhancing the response of the instrument and decreasing the
threshold.
They exhibit a remarkable crystalline quality as well. These characteristics result
in an enhanced performance and a long-term stability for the sustained operations.
The data analysis was run by means of Principal Component Analysis (PCA).
Data were processed by EDA software, a home written software developed in
MATLAB® at SENSOR laboratory [9].

Fig. 4 Left Schematic sketch of the conductometric device. Alumina substrate is white colored in
the middle, platinum heater and contacts are in metallic gray. SEM images of Tin (center) and Zinc
(right) oxide nanowires
236 V. Sberveglieri et al.

Feature extraction is usually unsupported, the most common example being the
Principal Component Analysis. PCA can, by itself, transfer a good visual idea of the
interclass split-up; in fact, this is how it is usually applied.
The goal was to obtain a good visual separation of the clusters, not just to have
high estimate accuracy. To this end, PCA was systematically used to judge the
clusters separation [10, 11].

2.3 GC-MS Analysis

GC-MS analysis was performed using a Shimadzu Gas Chromatograph

GC2010 PLUS (Kyoto, KYT, Japan) equipped with a Shimadzu single quadrupole
Mass Spectrometer MS-QP2010 (Kyoto, KYT, Japan) ultra and a HT280T
autosampler (HTA srl, Brescia, Italy) that allowed SPME analysis.
The vials were incubated in an oven thermostatically regulated at 50 °C for
15 min in order to create the headspace equilibrium. In order to extract the volatile
compounds of the samples, a DVB/carboxen/PDMS stable flex (50/30 μm)
(Supelco Co. Bellefonte, PA, USA) SPME fiber was used.
To provide the adsorption of the volatile compounds, the SPME fiber was
exposed to the headspace of the vials for 15 min at 50 °C. For desorption of the
compounds, the fiber was placed in the injector of the heated GC for 6 min at
200 °C.
Volatile organic compounds were separated using an analytical capillary column
(DB-WAX capillary column, 30 m × 0.25 mm × 0.25 μm, Agilent Technolo-
gies, Santa Clara, CA, USA) and the carrier gas used was ultrapure helium
(99.99 %) at a constant flow rate of 1.3 ml/min. The temperature program for the
GC was performed in the following way: 40 °C held for 8 min, linear gradient
4 °C/min up to 190 °C and held for 5 min, followed by a rise from 190 to 210 °C at
5 °C/min.

3 Results and Discussion

3.1 S3 Device

The data were processed by the software ‘Nose Pattern Editor’. In Fig. 5, PCA
score plot can be observed showing the comparison of all the samples for the
foreign cheeses. The instrument was able to well differentiate the groups of the
samples, here represented by different colors.
The two PC components alone covered over 60 % of the total information. This
difference is then explained by the analysis first conducted with the GC-MS in
Grated Parmigiano Reggiano Cheese: Authenticity … 237

Fig. 5 PCA score plot from the foreign cheeses esters

which several compounds are observed between the different samples and also
different amounts of the same compounds (Fig. 5).
The next step was then to compare these foreign samples with the pulp and crust
composition of the real Parmigiano again using the PCA analysis. From the
obtained PCA (Fig. 6), the clusters of the samples were observed to be quite
compact.
From the figure, it is seen that the foreign samples are not confused with the real
Parmigiano Reggiano cheese samples, but some similarities in the foreign cheese
samples with the crust or the pulp are found. In fact, in the left side the black dots

Fig. 6 PCA score of foreign cheeses in comparison with 100 % pulp and 100 % crust of
Parmigiano Reggiano
238 V. Sberveglieri et al.

are the detached samples of the crust and near these are all Hartkase1 and Hart-
kase11 samples.
These samples are more similar to Parmigiano Reggiano crust compared to the
pulp or to other foreign samples, confirming the fact that probably these samples
have very high percentages of the crust that characterize them.
On the other hand, the PCA score plot includes the pulp cluster of the real
Parmigiano close to the clusters of Ireland, Hartkase and Lithuania. Probably these
samples show the most similarities to the pulp of Parmigiano Reggiano over the
crust.

3.2 Gc-Ms with Spme Analysis

The figures below report the frequency histograms of the compounds present in
different samples divided into two parts to allow an easier viewing of the graphs
(Figs. 7 and 8).
The samples analyzed are very different from the true Parmigiano: even with a
fast sensory analysis many atypical features are observed later confirmed by the gas
chromatography, which included the analysis of different true Parmigiano Reggiano
cheese samples.
In particular, there are very significant compounds present such as butanoic acid
derivatives that characterize especially the Ireland grated sample.
The most abundant compounds in this sample are propanoic acid, butanoic acid
and derivatives, tridecyl-3-butyric acid ester, acetic acid phenylmethyl ester.
These compounds are typical for Cheddar cheese, therefore the Irish sample
could possess a small percentage of real Parmigiano (in fact possesses some sim-
ilarities: 1-butanol-2methyl, 2-nonanone, octanoic acid ethyl ester and propanedioic

Fig. 7 Frequency histogram of foreign cheeses compounds from 1 to 24.1 min

Grated Parmigiano Reggiano Cheese: Authenticity … 239

Fig. 8 Frequency histogram of foreign cheeses compounds from 24.1 to 59.5 min

acid) but for the major part it seems to have been mixed with the Cheddar cheese. It
is also very different from the other foreign samples.
The German samples have similarities between them and even consist of dif-
ferent compounds. They are very different from the true Parmigiano, small analo-
gies may be found with the crust as confirmed by the PCA provided by the
Electronic Nose and could probably contain Emmental or Camembert as confirmed
by the comparison with the bibliography.
The Latvian sample is the only one to get closer to the true profile of Parmigiano
Reggiano (see for example: 2-heptanone) which presents the typical compounds of
Parmigiano both from the pulp and the crust.
However, the analogy is greater for the crust (see the presence of 2-pentanol,
2-heptadecanone, 2-octanone, 2-nonanone, octanoic acid ethyl ester, 2-nonanol,
2-undecanone, heptanoic acid, octanoic acid).
Significant is the presence of dodecanoic acid which denotes a typical aroma of
the cheese crust and the presence of 5-methyl-2-hexanol, wood aroma denoted by
the real Parmigiano crust during ripening in which the forms remain for months on
the wooden planks.
The only foreign presence of phenylmethyl acetic acid ester and anethole in the
samples makes us suspect that the foreign samples and imitations are mixed with
the small percentages of Parmigiano indicating the commercial fraud.
Here the compounds found in the chromatograms have been classified selecting
only those compounds that characterize the different origins of the foreign cheese
samples defining the aroma.
• Latvia: The compounds that characterize the aroma of the cheese from Latvia
were:
240 V. Sberveglieri et al.

– N-tert-Butyl ethylamine: Mainly present in Latvia sample and even small

part in the pulp of real Parmigiano. From the published papers, it is found to
have a smell of ammonia [12, 13].
– 2-pentanol: Compound present in Latvia in the pulp samples and real
Parmigiano crust. More abundant in the crust than the pulp, while it has
intermediate values for Latvia sample. Found in many foods: fruit, cheese,
drinks and gives fresh aroma [13].
– 2-Decanone: Aroma trace of the crust of Parmigiano Reggiano and present in
a lesser amount in the sample of Latvia but absent in all other samples. From
bibliography, it is an aroma from various plants [13].
– 2-Nonanol: Compound behaving exactly like the previous one. It is present
in oranges, ginger and some wines and cheeses [13].
– Butanoic acid phenylmethyl ester: Aroma trace in Ireland and Latvia samples
(more in the latter than the former). It is present in purple, papaya, black tea,
vanilla, sweet smell of apricot and pear [13].
– Benzyl alcohol: Constituent of Jasmine scent from bibliography, present in
orange juice, tangerine peel oil, pineapple, cinnamon, cloves, mustard, basil
and sage [13].
– Heptanoic acid: Found in Latvia sample and the pulp samples of Parmigiano
in similar quantities. Absent in other samples. It is found in strawberries,
ginger, apples, black tea and grains. It has a rancid odour of fatty acids [13,
14].
– 9-Decenoic acid: This aroma is found in traces in the pulp of Parmigiano, in
Latvia and in most of the Parmigiano Reggiano crust samples. It is typical of
Parmigiano Reggiano [12].
• Ireland: The compounds that characterize the aroma of the cheese from Ireland
were:
– 3-Pentanol: From bibliography, it is a characteristic odor from olive and is
also present in cranberry [13].
– 2-Hydroxy-3-pentanone: It is a part of lavender, ginger, peppermint [13].
– Tetramethyl-pyrazine: It is present in french fries, bread, sausages, tea,
cocoa, coffee, beer, dairy products and soy products [13, 14].
– Propanoic acid: Aroma present in all the samples in a trace amount but
abundant in the Ireland sample. It gives a pungent odor and is a preservative
often used in agriculture. It gives a pungent fruity aroma in Cheddar cheese
[13, 14].
– 2-Tridecanone: In literature, it is shown to be isolated from the vegetable oils
such as palm oil and coconut, blueberry, raspberry, grapefruit, onion, ginger
and cheese [13].
– 2-methyl-butanoic acid: Abundant in the Irish sample. It is present in
bananas, apples, butter, bread, papaya, black cherry and cheese [13].
– Heptadecane: Compound ubiquitous in all the samples analyzed. Slightly
more abundant in Ireland sample. It is present in vegetables such as beans
and sunflower [13].
Grated Parmigiano Reggiano Cheese: Authenticity … 241

– Tridecyl-3-butyric acid ester: It is found in apples, bananas, papaya, bread,

cheese, butter and coffee [13].
• Hartkase: The compounds that characterize the aroma of the cheese from
Germany were:
– Methylene heptane: Present only in Hartkase1 in low quantity. From bibli-
ography, it is a component of some flowers [13].
– 3-methyl-4-oxo-pentanoic acid: Compound present only in Hartkase1 in a
small quantity. It has an aroma of cocoa, Fontina cheese, cooked asparagus,
beer and pumpkin [13].
– Ethanol: Present only in Hartkase1 and Hartkase11 in a small quantity. It has
a fermentative aroma [13].
– 3,7-dimethyl-decane: Present in Hartkase in a very small quantity. It has a
fruity and floral aroma [13].
– 2,2-dimethyl-1-octanol: Compound in trace amount only in Hartkase1. In
bibliography, it is described to have a penetrating aroma of different essential
oils [13].
– 4-methyl-undecane: Present only in Hartkase1 in a trace amount. It is an
aroma component of chickpeas [13].
– Styrene: Aromatic compound found in trace amount in Hartkase. It is present
in blueberries, grapes, vinegar, parsley, milk and dairy products, coffee,
cocoa, roasted hazelnuts and peanuts [13].
– Acetic acid: Present in Hartkase, provides pungent odor in vinegar.

4 Conclusion

The fight against counterfeiting has been a priority for the protection of PDO
products. The globalization of markets not only provides several opportunities but
also many risks: the ability to package the product in the world makes the making
of documentary controls increasingly difficult.
In this sense, the Parmigiano Reggiano Cheese Consortium is working to change
the rules of the production of Parmigiano Reggiano, to make the packaging com-
pulsory in the area and to develop the sophisticated solutions for the traceability of
the product.
In parallel, however, the target is to find the technical and organizational solu-
tions that increase the chances of the cheese downstream control that enters into the
commercial circulation, in terms of compliance with the same standards imposed by
the regulations and the way it is included in the agreements signed between the
Consortium and the packers.
In addition to this, several foreign samples and imitation of Parmigiano Reg-
giano are widely available in the market. The grated suspects were examined and
found to be mixed with the PR. Using the SPME-GC-MS and Electronic Nose
242 V. Sberveglieri et al.

techniques, the most significant compounds of the different samples were identified,
observing many differences in the chromatogram and in the PCA score plots
obtained from the Electronic Nose. In particular, the butanoic acid compounds and
derivatives were found to characterize especially the Ireland grated sample.
This sample presented different levels of those compounds in comparison to the
other samples. It is more abundant in propanoic acid, butanoic acid and derivatives,
tridecyl-3-butyric acid ester and acetic acid phenylmethyl ester.
These compounds are typical for the Cheddar cheese, therefore the Irish sample
could have possessed a small percentage of real Parmigiano but for the most part, it
seems to have been mixed with the Cheddar. The German samples are very different
from the true Parmigiano; little analogies may be found with the crust as confirmed
by the PCA provided by the Electronic Nose [15].
They could probably contain Emmental or Camembert cheese as confirmed by
the comparison with the published literature. The Latvian sample is the only one to
get closer to the true profile. It, in fact, presents the typical compounds of Parmi-
giano both from the pulp and the crust.
S3 device is a promising tool for the quality discrimination of different cheeses
and other foodstuffs. This ability to distinguish cheese quality by an easy-to-use,
rapid, economic, portable, non-destructive and low power consumption S3 device is
crucial as it can be utilized to validate if a given sample is according to the law and
standards in order to assess the fraudulent or imitative production.
The nanowire based S3 Electronic Nose represents a simple, fast, economic and
portable tool for the quality control and authenticity evaluation of grated PR cheese.
In our future works, we propose to illustrate an amplified database of the grated
PR for the direct application of S3 in the cheese-chain productions and also to
perform a data fusion by integrating different results for a deeper analysis.

References

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Lard Detection in Edible Oil Using
Dielectric Spectroscopy

Masyitah Amat Sairin, Samsuzana Abd Aziz,

Nina Naquiah Ahmad Nizar, Nurul Adilah Abdul Latiff,
Alyani Ismail, Dzulkifly Mat Hashim and Fakhrul Zaman Rokhani

Abstract Food adulteration is the process of adding or mixing of substance(s) that

should not be into food products for financial gain or other motives. Food adul-
teration is a serious problem worldwide not just because it is a fraud to consumer,
but it can also harm the health and causes serious consequences to the well being of
people. Among the food products, edible oil has been identified as the top ingre-
dient involved in food fraud. Studies show that adulteration in fats and oils are
mainly economically motivated and in some cases intended to enhance food flavor.
In general, adulteration of edible oil causes two great concerns to the consumer.
First, it concerns consumers that practice vegetarian diet or followers of religions
that prohibit from consuming pig, pork or any of its products. Second, it may cause
serious health related issues particularly those who have allergies to certain types of
substances or consumers who suffer coronary disease. Several conventional tech-
niques have been utilized in order to study food adulteration particularly on fats and
oil, such as polymerase chain reaction, differential scanning calorimetry, electronic
nose and chromatography. Until recently, dielectric spectroscopy technique that
have been widely used to analyze food products, attain research community’s
attention in the study of adulteration on fats and oil. In this chapter, a review on
conventional techniques and dielectric spectroscopy approach for analyzing food
products are presented. In particular, a review on dielectric spectroscopy to study
adulteration in fats and oils and recent work on lard detection at both low and high
frequency range are discussed. Results show that dielectric sensing can be a great
technology to detect lard adulterated edible oil and applying data analysis technique
can further enhance the detection ability.

M.A. Sairin (✉) ⋅ N.N.A. Nizar ⋅ A. Ismail ⋅ D.M. Hashim ⋅ F.Z. Rokhani (✉)
Halal Product Research Institute, Universiti Putra Malaysia, Seri Kembangan, Malaysia
e-mail: [email protected]
F.Z. Rokhani
e-mail: [email protected]
M.A. Sairin ⋅ S.A. Aziz ⋅ N.A.A. Latiff ⋅ A. Ismail ⋅ F.Z. Rokhani
Faculty of Engineering, Universiti Putra Malaysia, Seri Kembangan, Malaysia

© Springer International Publishing AG 2017 245

S. Mukhopadhyay et al. (eds.), Sensors for Everyday Life, Smart Sensors,
Measurement and Instrumentation 23, DOI 10.1007/978-3-319-47322-2_12
246 M.A. Sairin et al.

1 Introduction

Food fraud is a collective term to explain the intentional substitution, addition,

tampering or misrepresentation of food, food ingredients, or food packaging [1].
Food fraud can be in the form of adulteration, tampering, over-run, theft, diversion,
simulation and counterfeiting. Among the food-related risk, food fraud is highly
economically motivated and can cause public fear and possibly lowering the price
of product industry-wide [2]. Adulteration is the process of adding or mixing of
substances which should not be contained within other substances for legal or other
reasons [3]. It can be further breakdown into several types which includes substi-
tution or dilution, unapproved additive, counterfeit, mislabeling, transshipment or
origin masking and intentional distribution of potential hazardous materials [2].
Oil is a food product that has been consumed widely throughout the years for
baking, frying and in other food preparations like in salad dressing, condiments,
flavorings and confectioneries [4, 5]. Edible oil can come from both plant and
animal sources. Examples of plant-based edible oils mostly comes from coconut,
palm kernel, palm, soya bean, groundnut, cottonseed, linseed, sunflower, rapeseed,
olive and sesame [6] while animal-based fats or oils can come from livestock (such
as cattle, mutton, pigs), poultry (such as chicken, duck and goose) and fish [7].
Food industries that produce food products like spreads, butter, ghee, margarine,
baking fats and shortenings, frying oils and fats, salad oils, mayonnaise, salad
cream, salad dressing, chocolate and confectionery, ice cream and dairy products
are the major industries that used fat and oil in their food preparation [8]. Examples
of the major industries include fast food chains and bakeries that use tons of oil for
frying chicken and fast food products and infused oil or fats into shortenings and
moistening agents, respectively.
Among food products categories, edible oil has been identified as the top
ingredient involved in food fraud adulterated for economic motivated reason as
shown in Fig. 1 [2]. Report indicates oils, among other food categories, are the
most reported type of food fraud.
In the food industry, technically, food manufacturers adulterate oil with other
substances for the purpose of increasing the apparent value of the product or
lowering the cost of its production [2, 9, 10]. In [11, 12], some refineries spike olive
oil with cheaper oil while other refineries mix vegetable oils with natural food
coloring (i.e. beta-carotene and chlorophyll) to give the look of green-gold color of
olive oil and misbranded them as a fake olive oil. In 1993, the Food and Drug
Administration (FDA) ordered a recall of Rubino U.S.A. Inc., (Cincinnati, Ohio)
olive oils which were from pure canola oil [13]. In 2013, Greek police made several
arrests on suspects that are accused of trying to sell soybean oil mixed with col-
orants as extra virgin olive oil [14]. In 2014, Wei Chuan Foods Corp. in Taiwan
was accused of blending oil made from unsold pork scraps with an illegal substance
—‘gutter oil’, and sold them as cooking oil [15]. Other than economically moti-
vated purpose, oil adulteration can serve the purpose of inducing more desirable
flavors and texture in food [16].
Lard Detection in Edible Oil Using Dielectric Spectroscopy 247

Fig. 1 Breakdown of food fraud being reported based on food ingredient category [2]

Figure 2, shows the breakdown of the world consumption for major fats and oils
in 2015 as reported by IHS Inc [17]. It can be observed that animal-based fats and
oils such butter, lard, tallow and grease ranked fourth most consumed fats and oil
globally [17]. According to [16], animal fats were used immensely for domestic
frying due to the desirable flavors they impart on some foods. For example, tallow
and lard was added to french-fried potatoes and pie-crusts respectively, to enhance
the flavor. In addition, animal fats are used as ingredient in the formulation of food
products such as breads and cakes due to exhibiting good stability and economical
[16, 18]. While both genuine and industrially-modified randomized lard are com-
mercially available [19], they are also used to blend with vegetable oils to produce
cost-effective margarines, shortenings and other oil-based foods [20].

Fig. 2 Breakdown of world

consumption of major fats and
oil in 2015 [17]
248 M.A. Sairin et al.

In general, adulteration of edible oil causes two great concerns to the consumer.
First, animal-based fats and oils adulteration in edible oil present great concern to
followers of vegetarian diet such as Hindus or Buddhist [21]. In particular, lard
adulteration prompt concern to followers of Islamic and Judaism religions as both
religions prohibit the consumption of lard and pork [22, 23]. Several reported cases
include shortening, butter, margarine and other specialty food oils made of veg-
etable oils blended with lard or tallow [24, 25], goat and pig body fat detected in
vegetable ghee and cow/buffalo ghee respectively [26, 27] and recently, sunflower
oil contaminated with chicken fat [28].
Second, health issues concern, which can be very vital to people who have
allergies to a certain types of food as well as the relationship of dietary cholesterol
and saturated fatty acid to coronary heart disease [29]. In 1997, European Com-
mission reported that around 103,400 tonnes of olive oil adulterated with estimated
20,680 tonnes of hazelnut oil were to be placed on the market [30]. The presence of
nut oils could cause complication for people with food allergies to nuts [2]. In [31],
non-optimal intakes of polyunsaturated fat, trans fat and saturated fat each con-
tribute to significant coronary heart disease.
It is clear that there is high dependency of consumers throughout the world to
oils and fats. With the vast consumption of oils and fats, greedy manufacturers
attempted to reap profits by illicitly adulterating original oils with alternative
substances leading to numbers of food fraud cases. While in certain cases oil
adulteration is intended to enhance food flavor or give stability as ingredient, these
may cause serious health related issues or unable to be consumed by certain group
of people. Thus, concern in adulteration in oils and fat should not be taken lightly or
ignored. It is crucial to develop a verification system that can distinguish adulterated
edible oils to combat food fraud. This thus can induce a healthier and safer eating
lifestyle among the citizen of all ages, races and religions.

1.1 Conventional Techniques in Lard Detection

In the recent past, a number of verification techniques in differentiating and

detecting lard in food products have been introduced. These methods can be cat-
egorized into two groups, which are labeling-based technology and spectral-based
technology. Labeling-based technology includes polymerase chain reaction
(PCR) techniques while spectral-based technology includes differential scanning
calorimetry (DSC), electronic nose (E-Nose), gas chromatography, liquid chro-
matography and spectroscopy. Note that in the following examples, we also dis-
cussed the application of techniques used on pork as a derivative from pig aside
from lard.
Labeling-based technology is a technique in lard detection that labels the sample
with the observation of DNAs presence in them. PCR method has been used to
analyze raw meats and fats of pigs and the identification of pork derivatives in food
products like sausages, bread and biscuits [32, 33].
Lard Detection in Edible Oil Using Dielectric Spectroscopy 249

Spectral-based technology is the study of the interaction of electromagnetic

radiation (EMR) with atoms and molecules to provide qualitative and quantitative
chemical and physical information that is contained within the wavelength or fre-
quency spectrum of energy that is either absorbed or emitted [34, 35].
Spectral-based technology in lard detection can be broken down into three cate-
gories namely DSC, chromatography and spectroscopy.
DSC is a thermoanalytical technique where the measurement of the change of
the difference in temperature between the sample and the reference sample while
they are subjected to a controlled temperature program [36]. DSC have been used in
the study to detect lard and randomized lard as adulterant in palm oil in [37], to
detect animal the presence of adulterated animal fat, i.e., chicken fat, in butter [38]
and in the detection of lard in beef tallow and chicken fat [39].
Chromatography is a study of formation, change and movement of analyte
chemical compounds of a studied sample in a flow of mobile phase with respect to
solid or liquid stationary phases or particles [40]. Chromatography techniques can
be further classified into gas chromatography and liquid chromatography. One
example of gas chromatography is E-Nose. E-Nose has been used to analyze the
aroma of food products such as cooked chicken meat, stored oysters, processed
cheese and evaporated milk, stored vegetable oils, chocolates, edible oils, milk,
honey, fruit, wheat, tea, corn and coffee [41]. While in the study of detection of lard
adulteration in RBD palm olein, a detection limit of 1 % of lard in refined, bleached,
deodorized (RBD) palm olein was achieved [42]. Another example of gas chro-
matography is gas chromatography mass spectrometry (GCMS). An investigation
used GCMS coupled with elemental analyzer-isotope ratio mass spectrometry
(EA-IRMS) to differentiate lard from chicken fat, beef fat and mutton fat [43].
Another study used different types of gas chromatography, a gas
chromatography-flame ionization detector (GC-FID) to differentiate lard from other
edible fats which are chicken and beef [44]. In [45], a gas chromatography
hyphenated with time-of-flight (GC-ToF) mass spectrometry is used to detect lard
by comparing the fatty acids profile with other animal fats like chicken, cattle and
goat [45]. The study identified three fatty acid biomarker belonging specifically
only to lard namely methyl trans-9, 12, 15-octadecatrienoate (C18:3 n3t), methyl
11, 14, 17-eicosatrienoate (C20:3 n3t) and methyl 11, 14-eicosadienoate (C20:2
n6). These fatty acid methyl ester (FAME) profiles could be used as a basis or
biomarker to discriminate lard from other animal fats in food authentication pro-
cess. An example of liquid chromatography is high-performance liquid chro-
matography (HPLC) that has been used to distinguish lard from other animal fats in
admixtures of some vegetable oils [46].
Lastly, spectroscopy techniques utilize the electromagnetic radiation in obtaining
electrical properties of the materials. Fourier transform infrared (FTIR) spec-
troscopy is one of the earliest lard detection technologies and it measures the
electromagnetic absorption or emission of the material in an infrared spectrum.
A number of investigations on lard detection using FTIR spectroscopy have been
recorded, which analyze the potential of lard adulteration in chocolate and
chocolate products [10], pork adulteration in beef meatball [47], lard adulteration in
250 M.A. Sairin et al.

Table 1 Summary of conventional techniques used in lard detection on several types of samples
with different detection limit, and spectrum measured
Category Techniques Detection Spectrum Sample
limit measured
Labeling-based PCR – – Raw meats and fats [32]
– – Pork derivatives in sausages
and the casings, bread and
biscuits [33]
Spectral-based Electronic Nose 1.0 % Volatile RBD palm olein adulterated
compounds with lard [42]
spectrum
DSC 0.5 % Thermal Beef fat and chicken fat
spectrum adulterated with lard [37]
GCMS & – Mass Lard, chicken fat, beef fat and
EA-IRMS spectrum mutton fat [43]
GCFID 0.5 % Ion intensity Beef fat and chicken fat
spectrum adulterated with lard [44]
GC-TOF-MS – Mass Chicken fat, lard, goat fat and
spectrum cattle fat [45]
Liquid 2.0 % Mass Palm oil, palm kernel oil and
chromatography spectrum canola oil adulterated with
lard, beef tallow and chicken
fat [46]
FTIR 4.0 %a Absorbance Lard adulteration in chocolate
spectrum and chocolate products [10]
1.0 %a Pork adulteration in beef
meatball [47]
1.0 %a Cod-liver oil adulterated with
lard [48]
a
17.0 % Lard adulteration in cake
formulation [49]
1.0 % Lard blended with mutton and
cow body fats [50]
10.0 % Lard mixed with body fats of
chicken, lamb and cow [51]
– Lard, beef, chicken and
mutton fats, cod liver oil and
other vegetable oil [20]
a
assumed based on the lowest lard adulteration concentration investigated

cod-liver oil [48], lard adulteration in cake formulation [49], lard in mixture of body
fats of mutton, cow and chicken [50, 51] and to differentiate lard from other edible
oil [20]. Generally, these studies utilize the frequency region of 4000 cm−1 until
650 cm−1 which lies in the infrared spectrum of frequency. Table 1 summarizes all
of the techniques that have been discussed with their respective samples.
Lard Detection in Edible Oil Using Dielectric Spectroscopy 251

1.2 Data Analysis in Lard Detection Approach

Aside from the data collected from measurements techniques discussed in previous
topic, data analysis is important to enhance the detection ability. The main goal of
this data analysis is to represent sample’s data in a way that the differentiation
between samples is significantly distinct.
Several examples of data analysis techniques that have been used in previous
studies are partial least squares (PLS), discriminant analysis, principal component
analysis (PCA), cluster analysis (CA), stepwise multiple linear regression (SMLR),
least significant differences (LSD), analysis of variance (ANOVA), linear regres-
sion analysis, and Pearson’s correlation analysis. Other statistical analysis tech-
niques include mean difference (MD), standard deviation (SD), standard error
(SE) and t-test. Some studies used one analysis technique while others used mul-
tiple analysis techniques at different stages during the data analysis process. Table 2
summarizes the different types of data analysis techniques and their respective
functions.
As an example, a study to analyze the adulteration of lard in cod-liver oil utilized
the PLS technique to develop a calibration model for quantitative measurement of

Table 2 Summary Of Data Analysis Techniques Used In Lard Detection

Category Examples of data Concept
analysis techniques
Hypothesis Analysis of variance Analyze variability in data in order to infer the
testing (ANOVA) inequality among population means [52]
Pearson’s Measure the relation strength of two linear variable
correlation analysis [53]
T-test Comparison two population means [54]
Clustering Discriminant Determine which continuous variables discriminate
analysis between two or more naturally occurring groups [55]
Principal component Identify patterns in data, and expressing the data in
analysis (PCA) such a way as to highlight their similarities and
difference [56]
Cluster analysis Divides data into groups (clusters) that are
(CA) meaningful, useful or both [57]
Modeling Linear regression Predict scores on one variable from the scores of
regression analysis another variable [58]
Partial least squares Constructing predictive models when the factors are
regression (PLS) many and highly collinear [59]
Stepwise regression Regressing multiple variables while simultaneously
removing those that aren’t important [60]
Validation Mean difference Measure variability [58]
(MD)
Standard deviation
(SD)
Standard error (SE)
252 M.A. Sairin et al.

Fig. 3 a FTIR spectra of cod-liver oil adulterated with lard at different concentrations and
b Coomans plot of pure cod-liver oil (squares) and cod-liver oil spiked with different proportion of
lard (triangles) [48]

the adulterant, together with discriminant analysis method to classify cod-liver oil
samples from other animal fats, beef, chicken, mutton and lard. Figure 3 shows the
Coomans plot obtained from the discriminant analysis for the classification of pure
cod-liver oil and the ones spiked with lard. From the plot, it is observed that there is
clear group separation between pure cod-liver oil (squares) and the one that is
spiked with lard (triangles). Other than that, the values of root mean standard error
of cross validation (RMSECV) and coefficient of determination (R2) were used as
the validity criteria for the calibration model. The validation was further investi-
gated using the MD and standard deviation of difference (SDD) for accuracy and
reproducibility.
In this case, PLS is successfully used to detect the level of adulterant and
discriminant analysis allows one to make a classification of cod-liver oil and
potential adulterants of animal oils.
Figure 3a shows the data of FTIR spectra for different samples before data
analysis was applied. Through naked eye, it is challenging to analyze, let alone to
be able to detect the lard adulterated samples. A Coomans plot after discriminant
analysis is applied in Fig. 3b showing the clear separation of lard adulterated with
the original samples, thus enhance the detection ability. Multiple data analysis will
not only enhance detection by developing a regression model but can also provide
different information about the data collected from measurements like the accuracy,
repeatability, significance difference among the samples by hypothesis testing and
many more [61].

2 Dielectric Spectroscopy

A dielectric material is materials that are neither conductors nor insulators that can
be polarized by an applied electric field [62]. A dielectric material does not have
loosely bound electrons like a conductor material. When a dielectric material is
Lard Detection in Edible Oil Using Dielectric Spectroscopy 253

Fig. 4 The conditions of the

molecule inside dielectric
material when unpolarized
and polarized by an applied
electric field [67]

placed in an electric field, electric charges in the material slightly shift from their
average equilibrium position. This cause a phenomenon called polarization, in
which the positive charges was displaced towards the electric field, while negative
charges shift on the opposite direction as illustrated in Fig. 4 [63]. The polarization
creates internal electric field that reduces the overall field within and increases the
capacitance. Dielectric spectroscopy or spectral permittivity is the measure of the
ability of the material to resist (resistance) or store (capacitance) the electric field
created [64]. Dielectric constant also known as relative permittivity is the permit-
tivity of the material in relative to that of free space [65, 66].
According to [68], the dielectric parameter (Ɛ) can be calculated from the fol-
lowing equation
 
Cp 1
εr = −j ð1Þ
C0 ωC0 Rp

where, Ɛr is the complex permittivity, Cp is the capacitance of the material, C0 is the

capacitance of free space, Rp is the equivalent parallel resistance, ω is the angular
frequency; ω = 2πf and f is the frequency.
Ɛr of a dielectric material consists of two parts, a real part and an imaginary part
as shown in Eq. (2). The real part, called dielectric constant, Ɛ′r, relates to the
ability of the material to store electromagnetic energy (capacitance) and the
imaginary part, called loss factor, Ɛ′′r, relates to the ability of the material to resist
the electric field, thus dissipates heat [62]:

εr = ε′r − ε′′r ð2Þ

where, Ɛ′r is the relative dielectric constant and Ɛ′′r is the dielectric loss.
254 M.A. Sairin et al.

Thus, dielectric constant can be defined as the ratio between the capacitance of
the dielectric material, Cp, with the capacitance of that in free space or vacuum, C0,
as shown in Eq. (3) below:

Cp
εr = ð3Þ
C0

2.1 Measurement Principles

There are a number of methods available for dielectric measurement. According to

[69], the methods relevant for any desired application depend on the nature of the
dielectric material to be measured, both physically and electrically. This means a
few variables should be taken into consideration to use a suitable method such as,
the state of the material (i.e. solid, liquid or semisolid), the melting or boiling point
of the material, the frequency of interest and the degree of accuracy required.
A specific sample holder or probe design also plays an important part to justify with
the nature of the material. The methods for dielectric property measurement include
waveguide and coaxial transmission line methods [70, 71], short-circuited line
technique [72, 73], open-ended probe technique [74, 75], time domain reflectometry
(TDR) method [76], free-space transmission technique [77], microstrip transmission
line [78], six-port reflectometer using an open-ended coaxial probe [79], colloid
dielectric probe [80], test cell with Boonton RX-meter [81] and cavity perturbation
technique [82]. Dielectric property measurement techniques is used in wide
applications and materials includes; food and agriculture [83–85], biological tissues
[86], wood and fibrous materials [87], resin and plastics [70, 88], ceramics [70, 89]
and also soils and minerals [90].

2.2 Factors Influencing Dielectric Spectroscopy

Measurement

Being a spectroscopy method, which relate the interaction of electromagnetic

radiation with atoms or molecules [34, 35], dielectric spectroscopy depended on the
nature of the atoms or molecule itself. This includes the characteristics of the
material itself, i.e. dipole and ionic characteristics, and the behavior it possess upon
external influences. The behavior of material’s molecule is influenced by the fre-
quency of the electric field introduced, temperature and moisture of the material.
These factors affecting the measurement of dielectric spectroscopy will be discussed
in this section below.
Lard Detection in Edible Oil Using Dielectric Spectroscopy 255

2.2.1 Frequency Dependence

Frequency dependence of dielectric properties of food relates the polarization of the

molecules with the electromagnetic field. According to [69], the frequency
dependence of the dielectric properties comes from the frequency dependence of
dipolar and ionic food materials.
At low frequency, dipoles are able to follow the variations of the applied field,
while at a very high frequency; the dipoles are unable to follow the rapid field
reversal leading to higher and lower dielectric constant, respectively. Thus, in most
of the dielectric measurements on dipolar food materials showed gradual decrease
with frequency. Dipolar food materials can be in the form of polar or non-polar in
which the molecules in the former have permanent dipole moment and the latter do
not. For example, pure water, a very polar compound has a very high value of
dielectric of 80.2, while that of oil, a non-polar compound, has a lower dielectric
value of within 0–3 [69].
In ionic food materials, typical ionic compound like salt (i.e. NaCl) reduces the
dielectric constant and increased the dielectric loss factor when compared to dipolar
food material [91]. The reduction of Ɛ’r and increase in Ɛ’’r is due to the binding of
free water molecules by counter-ions and the addition of conductive charge carriers
of dissolved salts, respectively.

2.2.2 Temperature Dependence

Temperature dependence also relates with the polarization of the molecules with the
electromagnetic field in terms of viscosity and water phases of the food material. At
low temperature, high viscosity leads to longer relaxation time and little dipole
rotation and thus results in low dielectric constant [69, 92]. More on this will be
discussed in the next section.
While in food materials with high water content, the dielectric constant highly
dependent on the phase of the water in the food. Figure 5 illustrate the temperature
dependence of dielectric value for various food materials from freezing to melting
state [93]. The dielectric value of all the food materials experience abrupt change
from very low to very high at around the melting point temperature of –5 to 0 °C,
suggesting that no free water molecule is present during freezing and otherwise
during melting. As temperature increases, the dielectric constant reduces following
dielectric profile of water.

2.2.3 Moisture Dependence

Moisture content is one of the major influences in dielectric properties of food

materials due to water is a polar compound and can easily absorb energy [69].
256 M.A. Sairin et al.

Fig. 5 Temperature
dependence of dielectric value
for various food substance at
2.8 GHz [93]

Fig. 6 Effect of moisture

content on dielectric constant
and loss factor in freeze-dried
potato at 3 GHz [94]

Increase in moisture content increases the polarization, result in increase in

dielectric constant and loss factor [69]. Figure 6 showed the effects of increase
moisture content on the increase of both dielectric constant and loss factor of
freeze-dried potato [94].
Lard Detection in Edible Oil Using Dielectric Spectroscopy 257

2.3 Dielectric Spectroscopy on Food Products

Dielectric spectroscopy has been applied to variety of agriculture and food prod-
ucts. The understanding of dielectric properties of food products becomes
increasingly important for consistent and predictable product, process and equip-
ment development [69]. Dielectric spectroscopy has been used to analyze and
characterize fruits and vegetables, meat and seafood, milk and dairy products, oil
and many more.
In [84], a study on the frequency dependence of the dielectric constant and loss
factor of fresh fruits using a network analyzer in the range from 200 MHz to
20 GHz was conducted. The study also explored the possibility of sensing the
maturity of fresh peaches. Investigation in [85] suggests that higher moisture
content in fruit results in slightly higher dielectric constant, and decreased in
dielectric constant with the increased of temperature or frequencies, for most fruits.
In [95], the permittivity and conductivity of various beef and chicken were
measured within the frequency range of 1 Hz–1 MHz. The work observes the
differences in fresh raw meat of commercially purchased with that after being
cooked in microwave. Raw meat showed higher dielectric constant measurements
than cooked meat, potentially due to high moisture content in raw meat.
A study on milk and dairy product in [96], investigated the dielectric properties
of UHT skim, low fat and homogenized whole milk. The study concludes that the
dielectric constant for all types of milk are close together in the high frequency
region of 1–10 GHz, and display larger differences at lower frequency range.
Figure 7 illustrate the dielectric constant of whole milk, low fat milk, skim milk and
water at frequency range from 1–10 GHz. It can be observed that water gives the

Fig. 7 Dielectric constant profile for whole milk, low fat milk, skim milk and comparison with
water [96]
258 M.A. Sairin et al.

highest dielectric constant due to highest water content as compared to milk

products. In addition, skim milk has higher water content than low fat and whole
milk based on the dielectric constant profile.

2.4 Dielectric Spectroscopy on Oil and Fats

Several works have been reported on the usage of dielectric spectroscopy to study
the dielectric properties of oils and fats. A research group from Japan investigated
on discriminating olive oil adulterated with vegetable oil in the frequency range of
101 Hz–1 MHz [97]. The olive oil is spiked with other vegetable oils, soy, corn,
canola, sesame and perilla oils with different concentration from 0 to 100 %.
Figure 8 shows a PCA score plot for soy oil and perilla oil adulterated in olive oil,
respectively. Leveraging on data analysis technique, the adulterated oil can be
easily detected from the original oil as can be observed in Fig. 8.
A study edible oils and fatty acids as a function of frequency, temperature,
moisture and composition has been reported in [92]. In this study, 10 edible oils and
6 fatty acids were used and the dielectric properties were measured over the fre-
quency range 100 Hz–1 MHz. The effects of temperature (20–45 °C), moisture
content (0.02–0.31 %), and fatty acid component on dielectric properties of oils
were investigated. From the investigation, it can be concluded that the dielectric
constant of oils affected by their fatty acid composition significantly, the dielectric
constant of the oils increased with increasing moisture content, this effect dimin-
ished as frequency increases, and both dielectric constant and loss factor of edible
oils demonstrated a gradual decrease with increasing temperature, as well as the
dielectric constant of fatty acids.

Fig. 8 PCA score plot for different concentration of soy oil in olive oil (left) and PCA score plot
for different concentration of perilla oil in olive oil [97]
Lard Detection in Edible Oil Using Dielectric Spectroscopy 259

Fig. 9 Dielectric constant of

the seven types of oil [99]

Another investigation on studying the dielectric properties of different varieties

of rapeseed-mustard oil at different temperature [98]. The study suggests that the
dielectric properties of rapeseed-mustard oil show dependence on different per-
centage of erucic acid content.
In [99], dielectric spectroscopy is used to study quality control of vegetable oil.
This study observe a specific frequency ranges in which the permittivity of the
different vegetable oils; olive, peanut, sunflower, corn, soybean and various seeds,
can be discriminated. Figure 9 shows the dielectric constant of the seven different
types of vegetable oil in the frequency range of 0.2–100 MHz. Table 3 summarizes
previous dielectric spectroscopy studies and the frequency range used in the
investigation.

2.4.1 Frequency Dependence in Oils and Fats

In most oil and fats, different frequencies result in little changes in the dielectric
constant. Figure 10 shows the dielectric values dependency on frequencies for
different fatty acids (i.e. caprylic, linolenic, linoleic, oleic, palmitic and stearic) and
also of a few vegetable oils (i.e., sesame, soy, corn, canola, olive, safflower and

Table 3 Summary of previous studies on dielectric spectroscopy for oils and fats
Study Sample Frequency
Bansal (2001) Rapeseed-mustard oil 100 kHz–8.93 GHz
Inoue (2002) Soybean oil 1 kHz–100 kHz,
50 kHz–30 MHz
Lizhi (2008) Vegetable oil & fatty acids 100 Hz–1 MHz
Cataldo (2009) Vegetable oil 100 kHz–1 GHz
Lizhi (2010) Olive oil adulterated with other vegetable oil 100 Hz–1 MHz
260 M.A. Sairin et al.

Fig. 10 Spectra of dielectric constant of saturated and unsaturated fatty acids at 75 °C (left) and of
various oils at 25 °C (right) [92]

sunflower) [92]. It is explained that the dielectric spectra indicated general plateau
and maximum value in frequency range between 100 Hz and 500 kHz suggesting
that there exist equilibrium among the orientation of oil molecule and the electric
field at low frequencies. At higher frequency, the dielectric spectrum is observed to
decrease gradually. This is explained in [69] that at higher frequency, the dipoles
are not reacting to the electric field as they are unable to follow the rapid field
reversal.

2.4.2 Temperature Dependence in Oils and Fats

In [92], effects of temperature range between 20–45 °C were investigated.

Figure 11 illustrate the effect of temperature on dielectric constant and loss factor of
soybean oil. It can be observe from Fig. 11 that both dielectric constant and loss
factor demonstrated a gradual decrease with increasing temperature.

Fig. 11 Effect of temperature on dielectric constant (left) and loss factor (right) of soybean oil
[92]
Lard Detection in Edible Oil Using Dielectric Spectroscopy 261

According to [90], at low temperature, high internal viscosity leads to longer

relaxation time and little dipole orientation, thus result in low values of dielectric
constant. As the temperature increased, the viscosity decrease causing the decrease
of relaxation time and increase in dipole moment, thus decreasing the dielectric
constant. This pattern can be observed for most of study on dielectric properties on
food materials.

2.4.3 Moisture Dependence in Oils and Fats

Work in [92] also studied the effect of moisture on dielectric constant. The oil
moisture content ranges from 0.02 to 0.31 % (w/w), was determined in accordance
with Air Oven Method 1.4.1-2013 [100]. Figure 12 shows the effect of moisture
content on dielectric constant of corn oil. As discussed earlier, water is a polar
molecule with higher dielectric constant than water, thus lead to increase of
dielectric constant with increasing moisture content [69].

3 Dielectric Spectroscopy for Lard Detection

The major animal fats, also termed meat fats, traded world-wide are produced from
pigs (Sus scrofa), termed as lard or rendered pork fat, from cattle (Bos Taurus) or
sheep (Ovis aries) termed tallow, and from poultry, primarily chickens (Gallus
gallus) termed as poultry fat. Tallow from domestic cattle is known as beef tallow,
whereas that from sheep is termed mutton tallow. “Acylglycerol” is the primary
component of animal lipids, which may exist as either fat or oils. At room tem-
perature, 24 °C, the former are primarily solid and the latter are liquid [16].
Lard is the fat rendered from fresh, uncontaminated, healthy fatty tissues from
the meat of sound swine (Sus scrofa) at the time of slaughter, and hence, fit for

Fig. 12 Effect of moisture

content on dielectric constant
of corn oil at different
frequencies [92]
262 M.A. Sairin et al.

human consumption. It is also imperative that the fat is pure and without the
presence of bones, isolated skin, blood or any other viscera. Edible tallow (drip-
ping), on the other hand, is the product obtained by rendering the clean, sound fatty
tissues, including trimming and cutting fat, attendant muscles and bones of bovine
and/or sheep in good health at the time of slaughter and fit for human consumption
[101].
In our recent study, sample of animal fats which are lard, beef tallow, mutton
tallow and chicken fat were extracted by rendering of adipose tissue of animals
collected from local slaughter houses and market according to the method proposed
by [37]. The rendering was done at 90–100 °C for two hours in the oven. The
extracted fats was filtered through double-folded muslin cloth and dried over
anhydrous sodium sulphate (Na2SO4) to remove residual moisture through filter
paper. The filtered samples were stored in a freezer at –20 °C before further
analysis. Before being used for analysis, all animal fats were thawed at 60 °C until
they melted. As some of the animal fats are in solid form at room temperature, a
solvent is needed for uniform sampling. Hexane is used as a standard oil-based
solvent. Polar solvent dissolve polar compound, while non-polar solvents dissolve
non-polar compounds [102]. As oil and fats are non-polar compounds, non-polar
solvents are needed [103]. Common extraction solvents include hexane, methylene
chloride, methy isobuthyl ketone (MIBK) and xylene [102]. Thus, the concentra-
tions mentioned in the discussion of dielectric spectroscopy would indicate the
concentration of each fat and oil in hexane.
Two works has been done for the lard detection in animal fats using dielectric
spectroscopy. The first work utilizes the higher frequency region, 200 MHz–
20 GHz [104], while the second study utilizes lower region frequency, 100 Hz–
100 kHz [105].

3.1 High Frequency Dielectric Spectroscopy for Lard

Detection

The investigation on high frequency range for dielectric spectroscopy on animal

fats and plant oil was conducted at room temperature. The samples used in this
study are beef tallow, chicken fat, lard, palm oil and soybean oil. Lard was spiked to
beef tallow and palm oil respectively and dielectric profile are observed across the
range of frequencies. 85070B dielectric probe kit and N5230A PNA-L Network
Analyzer was used for dielectric data acquisition. Distilled water was used as the
calibration fluid. 200 points of frequency was set from 200 MHz to 20 GHz.
Figure 13 shows the dielectric constant of individual fats; i.e., beef tallow,
chicken fat, lard, palm oil and soybean oil. Based on Fig. 13, it is observed that the
dielectric constant of the samples decreased as the frequency is increased from
200 MHz up until 15 GHz. As explained on the effect of frequency on oil and fat in
the previous section, higher frequency results in the decrease of dielectric constant.
Lard Detection in Edible Oil Using Dielectric Spectroscopy 263

Fig. 13 Dielectric constant of individual fats; a beef tallow, b chicken fat, c lard, d palm oil and
e soy bean oil [104]

Figure 14 shows the comparison on the dielectric constant and loss factor between
beef tallow sample, lard sample and beef adulterated with lard sample. It can be
observed that frequency between 8.2–14.2 GHz shows most clear separation of the
dielectric constant between beef tallow and samples that contain lard, pure lard and
beef adulterated with lard. While the loss factor shows separation in different fre-
quency range, which is between 10.2–2.2 GHz.
It is concluded that the dielectric constant of all individual fats samples
decreased as the frequency increased for all concentration. Lard adulterated sample
can be distinguished from non-adulterated samples by its dielectric constant and
loss factor spectral pattern at certain frequency range.
264 M.A. Sairin et al.

Fig. 14 Comparison of a dielectric constant and b loss factor between beef tallow sample, lard
sample and beef adulterated with lard sample [104]

3.2 Low Frequency Dielectric Spectroscopy for Lard

Detection

The study of the animal fats at low frequency was conducted at room temperature as
well. Animal fats used in this study were beef tallow, chicken fat, mutton tallow and
lard. An Agilent 16452A liquid dielectric test fixture was used as the probe and

Fig. 15 RSD values for dielectric measurements at frequency range of 10 Hz–100 kHz for
different animal fats: a chicken, b lard, c beef and d mutton [105]
Lard Detection in Edible Oil Using Dielectric Spectroscopy 265

Table 4 Anova results Frequency (Hz) P-value

shows that the p-value at
every frequency studied are 100 2.47e−8
less than 0.05 120 1.93e−8
1k 1.68e−8
10 k 1.76e−8
20 k 3.44e−9
100 k 3.76e−9

connected to an Agilent 4263B LCR meter. The dielectric values were measured at
six discreet frequencies; 100 Hz, 120 Hz, 1 kHz, 10 kHz, 20 kHz and 100 kHz.
This study utilizes data analysis of Relative Standard Deviation (RSD),
ANOVA, and PCA. Figure 15 illustrate the RSD values obtained from all of the
animal fats.
It can observed that the RSD values of all samples are well below 1.8 %, which
is very good for precision, as the minimum RSD required for normal analysis is
around 10 % [106]. Table 4 shows the result from ANOVA analysis, which shows
that at every frequency, the p-value is less than 0.05 indicating that different animal
fat samples have significant difference at these frequencies. Figure 16 shows a PCA
score plot for four different types of animal fats; i.e., beef tallow, mutton tallow,
lard and chicken fat. From the observation on the PCA score plot, it is clearly
depicted a well separation between different types of animal.
From this study, it is concluded that the dielectrics value is not a function of
frequencies but a function of sample’s concentration levels. Using ANOVA, it is
statistically concluded that there is significant difference between different groups of

Fig. 16 PCA score plot for different types of animal fats in which B (beef tallow), M (mutton
tallow), L (lard) and C (chicken fat) can be observe was well separated between each other [105]
266 M.A. Sairin et al.

sample, i.e., animal fats. PCA technique positively show clear group separation
among different animal fats, thus highlight the ability of dielectric spectroscopy in
lard detection.

4 Conclusion

This chapter has reviewed the motivation of detecting lard in lard adulterated food
product such as edible oil, several conventional techniques that have been used in
lard detection and a number of data analysis that have been applied on lard
detection study. The factors influencing dielectric spectroscopy technique and use
of dielectric spectroscopy on food products have been discussed. In addition to the
applications presented on food products, the dielectric spectroscopy measurements
on oil and fats was also discussed in detail with the factors influencing the dielectric
constant and loss factor. Work has also been performed to distinguish lard from
other animal fats by using the dielectric spectroscopy method with data analysis to
help enhance lard detection ability.

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Optical-Based Interference Cancellation
in Wireless Sensor Networks

Matthew P. Chang, Jingyi (Jenny) Sun, Monica Lu,

Eric Blow and Paul R. Prucnal

Abstract One of the biggest challenges facing the widespread implementation of

wireless sensor networks is wireless interference and radio-frequency (RF) spec-
trum crowding. Even today, wireless networks are already straining under society’s
relentless demand for higher data rates and constant connectivity. For wireless sensor
networks to become a reality, research on increasing network capacity and allocat-
ing spectral resources must necessarily involve new techniques for handling wireless
interference scalably and efficiently. This chapter focuses on analog interference can-
cellation using optical signal processing as a path towards operating in the presence
of wireless interference. Canceling interference before it enters a receiver allows
wireless sensor networks to conserve scarce spectral resources and relax system
requirements, resulting in robust operation, increased battery life, and reduced size
and cost. Through its unique physics, optics enables new RF functionalities that are
extremely valuable to canceling interference in the RF front-end, chief among them
being wide processing bandwidth. The wideband nature of optics is key to antici-
pating the rise in data rates, bandwidths, and channel counts of future networks, and
endows optics with the potential to realize true multiband radio transceivers. Our
goal in this chapter is to present an overview of optical-based RF interference can-
cellation and discuss the key characteristics that make optics an outstanding technol-
ogy platform for the job. We then show several system architectures and a sample of
their experimental performance. We leave the readers with a discussion on the future
prospects for this technology, focusing specifically on photonic integrated circuits.

1 Introduction

Wireless sensor networks can provide valuable insight into the patterns and processes
of our surroundings that we were formerly unaware of. Yet, connecting thousands or
millions of wireless devices in a seamless network brings a unique set of challenges

M.P. Chang ⋅ J. (Jenny) Sun ⋅ M. Lu ⋅ E. Blow ⋅ P.R. Prucnal (✉)

Lightwave Communications Research Laboratory, Electrical Engineering Department,
Princeton University, Princeton, NJ 08540, USA
e-mail: [email protected]

© Springer International Publishing AG 2017 273

S. Mukhopadhyay et al. (eds.), Sensors for Everyday Life, Smart Sensors,
Measurement and Instrumentation 23, DOI 10.1007/978-3-319-47322-2_13
274 M.P. Chang et al.

that must first be overcome before this promise can be fulfilled. Chief among them
are the problems of wireless interference and RF spectrum crowding.
Wireless interference is the greatest problem in wireless communications because
of the very nature of our shared transmission medium. Interference mitigation tech-
niques involve sharing other radio resources such as time (time-division duplexing,
TDD), codes (code-division duplexing, CDD), and frequency (frequency-division
duplexing, FDD). These techniques have successfully permitted multiple users to
communicate without interfering with each other, but they come at a cost: RF spec-
trum, the universal currency of wireless communications. As data rates and the num-
ber of connected devices continue to rise exponentially [1], the limited RF spectrum
has grown extremely crowded, and the price for bandwidth worldwide has soared
into the billions of U.S. dollars for 10s of MHz of spectrum. Similarly, the number
of communication bands and the market for RF front-end components, particularly
filters, the gateways to different bands, has followed suite (see Fig. 1).
Adding more bands and filters may seem like a solution, but this trend is not sus-
tainable. Most RF components, like filters, operate in a single, fixed frequency band,
meaning each band requires a dedicated chain of RF components. As a result, RF
front-ends, like those in Fig. 2, have grown complex, bulky, and expensive. Mean-
while, limited circuit board real estate (and profit margins) in size-sensitive plat-
forms like handsets mean that hardware designers have to sacrifice functionality for
the expanding RF front-end. Finally, no amount of additional filters actually creates
capacity, it only divides it up further.
New methods of operating in the presence of interference will be required in
widescale wireless sensor networks, as well as in the larger scope of 5G. These
methods will need to work in tandem with the traditional TDD, FDD, and CDD
techniques. Furthermore, any new hardware must be tunable and wideband, lest they
be vulnerable to the same scaling limitations of existing front-ends and risk facing
irrelevance in 5G.

Fig. 1 a The projected growth of revenue for RF front-end components, dominated by filters.
Taken from [2]. b The rise in the number of different band filters. Source Triquint
Optical-Based Interference Cancellation in Wireless Sensor Networks 275

Fig. 2 RF front-end architecture for the 700–900 MHz bands, showing the front-end complexity

In this chapter, we discuss the importance of interference cancellation in future

wireless communication systems. In particular, we present our vision for using opti-
cal signal processing techniques, instead of traditional RF approaches, to cancel
interference. Optics possesses the key property that it can operate over extremely
wide bandwidths and frequencies, which is necessary to not only cancel interference
over wide bandwidth channels, but also to enable a true multiband transceiver and
future-proof them to newly defined bands and frequencies. This latter point is espe-
cially important to stem the expansion of RF front ends. The chapter is organized as
follows: we first give an overview of interference cancellation and determine the key
characteristics of an interference canceller. We then turn our attention to optical inter-
ference cancellation, particularly as it pertains to self-interference cancellation. We
discuss how optical cancelers meet the key characteristics and then present various
system architectures with their experimental results. Last, but not least, we discuss
the feasibility for optical technology in commercial markets via photonic integrated
circuits.
276 M.P. Chang et al.

2 Interference Cancellation in Wireless Sensor Networks

Interference cancellation refers to the process of actively nulling interference by sub-

tracting the interference signal from the corrupted signal. This is in contrast to other
interference mitigation techniques, which use some form of temporal, spectral, spa-
tial, or code-based isolation to protect the desired signal from interference; some
examples are provided in Fig. 3. The need for interference cancellation arises because
these methods are not perfect and in some cases not applicable. For example, in in-
band full-duplex communications, or simultaneous transmit and receive on the same
frequency, filters are no longer applicable and circulators, which typically provide
20 dB of isolation, are insufficient to protect the receiver.
Interference cancellation is often confused for spectral filtering, but the two
techniques are different and should be used together, rather than as substitutes, to
address different components of interference. The key differences between cancel-
lation and filtering are summarized in Table 1. The main advantages of interference
cancellation are (1) its ability to address in-band interference and (2) its frequency-
independence. With regard to the first advantage, interference cancellation nulls
interference without harming the desired signal regardless of the spectral charac-
teristics of either signal. In contrast, filters indiscriminately reject (pass) signals out-
side (inside) of its passband, regardless of whether it is the desired signal or the
interference. With regard to the second advantage, cancellation can occur at any fre-
quency, assuming that the hardware performing the cancellation can operate at that
frequency. On the other hand, the majority of RF filters operate only over a fixed fre-
quency range at any given time. However, the advantages of cancellation can only be
leveraged if the system has prior knowledge of the interferer, and this often translates
into increased system complexity and processing power.

Fig. 3 Different forms of interference mitigation techniques: (left) cancellation, (middle) spatial
isolation, (right) spectral isolation or filtering
Optical-Based Interference Cancellation in Wireless Sensor Networks 277

Table 1 Interference cancellation versus filtering

Characteristic Cancellation Filtering
Interference spectrum In-band and out-of-band Out-of-band only
Operational bandwidth Wideband (practically limited) Narrowband (fundamentally
limited)
Interference knowledge Required Not required

2.1 Interference Cancellation Model

The ability of a system to cancel interference depends strongly upon the source of the
interference, the coupling channel between the interference source and the receiver,
herein called the interference channel, and any apriori knowledge about the inter-
ference and the desired signal. In a general interference cancellation scenario, the
received signal consists of a signal of interest, s(t), corrupted by an unknown interfer-
ence signal, n(t), which is assumed to be strong enough to block the receiver (Eq. 1).
The purpose of the interference cancellation system is to extract the interference from
the aggregate signal and subsequently subtract the extracted interference, np (t), from
the aggregate signal, recovering the signal of interest. The output is given by Eq. 2,
where the term in brackets represents the residual interference.

r(t) = s(t) + n(t) (1)

y(t) = s(t) + {n(t) − np (t)} (2)

Apriori knowledge can consist of anything from the waveform of the interference to
its statistical nature and will in general dictate the signal processing that is required
to extract the interference from the aggregate signal.
Interference can be divided into two categories: known and unknown. When
the interference signal is unknown, statistical methods must be used to distinguish
the interference from the desired signal. This is known as blind source separation.
Assuming that the signal of interest and the interference are statistically independent,
techniques such as principal component analysis (PCA) and independent component
analysis (ICA) are often employed. These techniques aim to separate the aggregate
signal into two or more components, demarcated by their statistical properties. An
interference canceller would then eliminate the components related to the interfer-
ence. Much research has been devoted to the topic of blind source separation, and
we refer the readers to these sources [3–5]. Herein, we focus on the situation where
the interference signal is either known or has been successfully extracted.
278 M.P. Chang et al.

2.2 Self-interference

A specific type of known interference is self-interference. Self-interference is unin-

tentionally generated by one’s own system, and therefore, a reference of the interfer-
ence is locally available. Examples of self-interference are shown in Fig. 4. As adja-
cent bands move closer together and communication platforms are required to sup-
port more and more transceivers, the growth of self-interference is hindering efforts
to increasing capacity. As a specific example, in in-band full-duplex communica-
tions, a transmitter and a receiver purposefully operate on the same frequency band
at the same time and can theoretically halve spectrum usage [6]. The self-interference
generated by a full-duplex system is enormous because the receiver has no protec-
tion against the strong transmitter operating in close proximity. Receiving a desired
signal at −90 or −100 dBm when the transmitter is outputting at +30 or +40 dBm
would require >130 dB of self-interference cancellation!
A model for self-interference is shown in Fig. 5. In self-interference cancellation,
because a reference of the interferer is available, the purpose of the interference can-
cellation system’s signal processing is to estimate the interference channel that the
transmitted signal propagates through prior to combining with the received signal.
To first order, the interference channel will attenuate and delay the transmitted sig-

(a) (b) (c)

(d) (e)

Fig. 4 Examples of self-interference: a Transmitter leakage, b Co-located antenna systems, c Adja-

cent channel interference, d Self-Interference from full-duplex communications, e Cognitive radio
and dynamic spectrum access [7]
Optical-Based Interference Cancellation in Wireless Sensor Networks 279

Fig. 5 A general model for self-interference cancellation

nal, but more complex channel effects, such as multipath, reflections within the RF
circuitry, amplifier noise, and nonlinear distortion are also present [8, 9]. The self-
interference at the receiver can be given by
∞
∑
n(t) = (𝛼n n0 (t − 𝜏n )) + w(t) + nnl (t) (3)
n=1

where n0 (t) represents the original interferer at the transmitter, 𝛼n and 𝜏n are the
channel attenuation and delay for the nth multipath component, w(t) represents wide-
band amplifier noise, and nnl (t) represents all nonlinear byproducts. The ability of
the system to estimate and mimic these effects determines the maximum amount of
interference cancellation achievable.

2.3 Key Characteristics of an Interference Canceller

An interference canceller must emulate the interference channel as closely as possi-

ble to maximize interference cancellation. To quantify how closely one must match
the interference channel to achieve a certain level of cancellation, consider the can-
cellation of a sinusoidal interferer by subtracting from it another sinusoid with
slightly different phase and amplitude. The phase and amplitude mismatch between
the two signals represent the error of the interference canceller and its signal process-
ing. Cancellation, or the relative reduction in the interferer power from its original
power, is shown in Fig. 6. We will call these curves mismatch curves.
280 M.P. Chang et al.

Fig. 6 Mismatch curve: the

maximum interference
cancellation of a sinusoid 20 dB
that can be achieved given a 25 dB
certain amplitude and phase 30 dB
mismatch
35 dB
40 dB
45 dB
50 dB
55 dB

Figure 6 shows that achieving levels of interference cancellation above 40 dB

requires less than 0.4◦ of phase mismatch and 0.04 dB of amplitude mismatch
between the two sinusoids. This level of precision is a formidable task, and grows
even more demanding for higher cancellation depths. Hence, the first key character-
istic of an interference canceller, perhaps intuitively, is extremely precise control of
the amplitude and phase. The mismatch curves provides insight into the precision
requirement.
Although the mismatch curves are useful, they only indicate the cancellation
achievable at a single frequency. Actual cancellation will depend upon the band-
width of the interfering signal, as well as the frequency responses of the interference
canceller and the interference channel. Even if the cancellation conditions are met
perfectly at a single frequency, it is unlikely that these same conditions will be met
at other frequencies. This creates an important tradeoff between average cancella-
tion depth and bandwidth of cancellation. The second key characteristic is therefore
wideband operation of the canceller and the RF front end. The flatter the frequency
responses of the canceller, RF front-end, and interference channel, the wider the
achievable cancellation bandwidth for a fixed cancellation depth.
The third key characteristic of an interference canceller is low latency tunability.
Practical RF environments are dynamic, even ones that are physically fixed. Wind
effects on antennas, temperature drifts, and objects moving around the antennas all
affect the RF environment and the interference channel. Any practical canceller must
be able to adapt to changes, and sufficiently quickly, to minimize system down-time.
Finally, the fourth key characteristic of an interference canceller is extremely wide
dynamic range. An interference canceller must not only be able to accept high powers
from an interferer, but simultaneously be able to resolve weak signals of interest.
Interference cancellers which cannot process high powers will generate unacceptable
harmonics and intermodulation products, which will also mask the desired signal.
Conversely, interference cancellers which cannot resolve low power signals will lose
the desired signal under the noise floor.
Optical-Based Interference Cancellation in Wireless Sensor Networks 281

3 Interference Cancellation Using Optical Signal

Processing

In this section, we give a brief introduction to analog optical signal processing and
make a case for using optics to perform interference cancellation based on its ability
to satisfy the four key characteristics of an interference canceller:

∙ Wideband operation
∙ Precise amplitude and delay (phase) control
∙ Low latency tunability
∙ High dynamic range

3.1 Analog Optical Signal Processing and Microwave

Photonics

Despite the omnipresence of digital electronics in our world, there has recently been a
strong resurgence of interest in RF analog signal processing. This is because convert-
ing an analog RF signal into a digital signal with high fidelity is extremely demand-
ing. It requires a large number of bits to achieve high dynamic range and a large
sampling rate to represent high bandwidths. These tall technical requirements make
it cost prohibitive, if not impossible, to implement a truly software-defined radio
(SDR) today.
Following the development of the laser and the optical fiber in the late 1960s,
researchers began investigating the potential of optics to perform high-fidelity trans-
mission, distribution, and processing of analog RF signals [10]. In this process, the
RF signal is first modulated onto an optical carrier (historically 1310 and 1550 nm
because of propagation characteristics in optical fiber), which was generated by a
laser or an LED. The modulated optical carrier is transmitted through an extremely
low-loss optical fiber over long distances to a destination, where it is converted back
into an RF signal by a photodetector. The goal was to capture the natural advantages
of optical fiber, namely very low propagation loss and RF frequency-independent
propagation (i.e. wide bandwidths). Today, optical fiber exhibits losses as low as
0.5 dB/km and carries aggregate data rates over 1 Tbps; in contrast, RF cables have
losses of 360 dB/km at 2 GHz [11] and gets even lossier at higher frequencies. Mil-
itary and other weight sensitive platforms also sought lightweight optical fibers to
replace heavy RF cables (1.7 kg/km vs. 80–600 kg/km) [12].
Soon after data transmission using fiber-optics had proven successful, researchers
turned towards using optics to perform actual RF signal processing functions (see.
Fig. 7). In 1991, the term microwave photonics was coined [13] to describe the
general field of analog RF signal processing, distribution, and generation using
optics and photonics, and has since continued to captivate the research community.
Microwave photonics seeks to leverage the physics of optics to achieve functional-
282 M.P. Chang et al.

Fig. 7 A general analog optical link, showing RF input and output, and optical signal processing
and distribution in the middle

ity and performance that is impossible to obtain using RF components. These key
performance advantages include high dynamic range, low loss fiber, low suscepti-
bility to electromagnetic interference, ease of reconfigurability, and perhaps most
importantly wide bandwidth [11, 14–16].
The performance of a microwave photonic link, generically shown in Fig. 7, is
determined by three main parts: the electrical-optical (EO) conversion, the interme-
diate optical signal processing, and the optical-electrical (OE) conversion. To speak
a common language with RF engineers, microwave photonic links are often char-
acterized using traditional RF figures of merit: link loss, noise figure, and dynamic
range. Because the EO and OE conversions determine the fidelity of the signal as it
transitions between the electrical and optical domains, the modulators and detector
devices that perform this conversion have a dominant effect on the link loss (or gain),
noise figure, and dynamic range. Over the years, microwave photonic links have
shown consistent improvement in all three figures of merit and commercial products
are now on the market [17–19]. The intermediate optical signal processing archi-
tecture determines the actual photonic circuit function. Microwave photonic imple-
mentations of FIR (or matched) filters [20–22], beamformers [22–25], wideband
phase shifters [21, 26, 27], true-time delays [16, 21, 28], and interference cancellers
[7, 29–33] have all been demonstrated.

3.2 Wide Bandwidth Operation

The wide bandwidth of optics is one of the primary reasons why optics is the de facto
carrier of the Internet, and these benefits apply to wideband interference cancella-
tion as well. Optics is able to process extremely wide bandwidth signals because
Optical-Based Interference Cancellation in Wireless Sensor Networks 283

Fig. 8 A standard RF signal is essentially narrowband when modulated onto an optical carrier

of the tiny fractional bandwidth of an RF signal on an optical carrier. Whereas a

single 20 MHz LTE channel may represent a significant bandwidth when modu-
lated onto a 700 MHz RF carrier, it is virtually narrowband when modulated onto a
193 THz (1550 nm) optical carrier (Fig. 8). Modern optical devices can easily process
RF signals from DC to 20 GHz, offering unprecedented flexibility to process wide-
band channels and tune freely between bands throughout the entire cellular spectrum
and beyond. Innovations such as traveling wave electrodes [34] and uni-traveling car-
rier photodiodes have pushed the limit of RF frequencies that can be processed by
optics well into the millimeter-wave regime [25, 35–37]. In contrast, RF front-end
components are typically designed for a single frequency band and a relatively small
instantaneous bandwidth (e.g. 20 MHz). Generally, RF is narrowband and fixed,
whereas optical circuits is wideband and tunable. The wideband and tunable advan-
tages of optics can enable enormous cost-savings by consolidating the RF front-end
and create a path toward a true multiband radio.

3.3 Precise Amplitude and Delay Control

The precision of amplitude and delay control achievable by an interference canceller

determines the maximum amount of cancellation that can be realized, per Fig. 6. The
physics of optics enables relatively simple control of these two parameters so that
continuous tunability and high precision can be obtained.
284 M.P. Chang et al.

To effect amplitude control, mirror and semiconductor based devices with tun-
able gain or insertion loss are commonly used. Commercial mirror-based variable
optical attenuators (VOAs) can achieve an RF attenuation resolution better than
0.01 dB/mV over a range of 30 dB, which is sufficient to obtain 50 dB of cancel-
lation given sufficient phase matching. Semiconductor optical amplifiers (SOA) and
electroabsorbers use a bias current or voltage to change a semiconductor’s optical
gain or absorption coefficient, respectively. SOAs can achieve similar gain resolu-
tion as a mirror-based VOA, but it is typically not a linear function of the SOA bias
current and is also dependent on the input optical power. Additionally, memory and
cross-gain saturation effects within the SOA can induce crosstalk between RF signals
modulated onto different wavelength-division multiplexed optical carriers.
Tunable optical delay lines have been researched intensively for their important
role in applications such as wideband true-time delays, FIR filters, beamforming,
and optical buffers [16, 38–41]. They have been implemented through a variety of
mechanisms such as mechanical positioning of mirrors, thermally-tuned refractive
index spiral waveguides, microring resonators, Bragg gratings, and switching delays.
Sub-picosecond delay resolution can be readily achieved by multiple delay technolo-
gies. At 10 GHz RF frequency, this corresponds to a phase shift of 0.01◦ , which is
sufficient to meet high cancellation depths.

3.4 Low Latency Tunability

The minimum acceptable latency of an interference canceller is determined by the

coherence time of the interfering channel, or how long it takes for the channel’s
response to change significantly. This depends strongly on the RF environment; as
an example, a typical indoor office environment has a coherence time of about 100
ms [9]. Therefore, the chosen amplitude and delay tuning technologies must exhibit
millisecond or shorter latencies to reduce system overhead. This rules out mechan-
ical and thermal methods, which typically require at least 10s of milliseconds to
settle down. The preferred tuning methods are therefore current/voltage controlled
or switch-based. For amplitude control, current and voltage control mechanisms are
either based on stimulated emission and absorption for III-V compounds or the free-
carrier plasma dispersion effect in silicon [42, 43]. These effects are currently used
in high-speed III-V and silicon modulators to achieve data rates of well over 10 Gbps.
Therefore, they can easily satisfy the low latency requirements to track an interfer-
ence channel as it dynamically evolves. For tunable delay and phase control, switch-
ing delays typically exhibit 10s of microseconds of latency, whereas tunable delays
based on tuning resonances and wavelengths will depend on the semiconductor car-
rier and photon cavity lifetimes. Both of these are in the domain of nanoseconds and
less.
Optical-Based Interference Cancellation in Wireless Sensor Networks 285

3.5 High Dynamic Range

Lastly, an interference canceller must be able to both resolve weak signals of inter-
est and deal with strong interferers simultaneously. Many microwave photonic links
have demonstrated experimental dynamic ranges surpassing 120 dB/Hz2∕3 [19] (here
we use third-order intermodulation spurious-free dynamic range or SFDR as the
representative metric), which meets the stringent requirements of many analog RF
applications.
In a microwave photonic link, the ceiling on the dynamic range is often set by the
optical modulator, because of its nonlinear transfer function. With direct modulation
(modulating the laser bias current using the RF signal), dynamic range is maximized
by using a laser with as linear a light-current relationship as possible, maximizing
gain, and minimizing relative intensity noise (RIN) [19, 44]. In direct modulation,
the dynamic range is also a strong function of frequency, declining sharply as the
operating frequency approaches the laser relaxation oscillation frequency [19, 45].
External modulators have the benefit of operating a continuous-wave laser and
therefore, do not have the dynamic range degradation with respect to frequency
that directly modulated links exhibit. However, both Mach-Zehnder modulators
(MZM) and electro-absorption modulators (EAM) exhibit nonlinear transfer func-
tions, which limit the link’s dynamic range at high powers. Because an MZM’s
transfer function is predictable, it can be linearized by pre-distorting the input RF
signal to eliminate the third-order intermodulation product [46]. Such linearized
links have demonstrated SFDRs larger than 130 dB/Hz4∕5 [19], albeit at limited fre-
quencies. Other techniques, such as low-biasing the MZM to lower noise and using
dual-parallel MZMs to cancel third-order intermodulation products, have also been
used to increase SFDR [13, 47, 48]. Overall, microwave photonic links can exhibit
extremely large dynamic ranges. However, careful consideration of the link appli-
cation requirements must be taken in account, as there is almost always a tradeoff
between dynamic range, gain, noise figure, and bandwidth.

4 Optical Interference Cancellation System Architectures

An optical interference canceller can achieve unprecedented performance in terms of

wide instantaneous bandwidth, tunable operating frequency range, and cancellation
depth. The canceller architecture and components determine the canceller’s capa-
bilities and the tradeoffs between key parameters. We now present several system
architectures that have been experimentally demonstrated, and analyze their perfor-
mance. This section culminates in the demonstration, for the first time, of a mono-
lithic photonic integrated circuit for interference cancellation, which has the poten-
tial to catapult the benefits of optical interference cancellation into cost-sensitive and
commercial markets.
286 M.P. Chang et al.

4.1 Two-Tap Manual Canceller with Balanced Photodetector

A two-tap discrete optical interference canceller architecture is shown in Fig. 9 [29].

The canceller propagates the corrupted received signal, r(t) = s(t) + n(t), on one
fiber path of the system, while the interference reference, n0 (t), is processed and
propagates on a second fiber path, which we call the cancellation path. With a sin-
gle cancellation path, this canceller is designed to remove the dominant source of
self-interference, which is usually either the line-of-sight signal in the case of a two-
antenna communication system or the strongest leakage signal (e.g. circulator leak-
age or antenna return loss) in a duplexed single-antenna system. The optical mod-
ulation devices are two electro-absorption modulators (EAMs), which each receive
a +10 dBm optical carrier from the same C-band (i.e. 1550 nm) laser source. The
optical-to-electrical converter is a balanced photodetector, which also performs the
subtraction. The overall system has a bandwidth of 10 GHz, limited by the EAMs.
To match the interference channel, a MEMS variable optical attenuator (VOA)
and two manual tunable delay lines (TDL) based on free-space mirrors are used in
the cancellation path. The MEMS VOA has attenuation resolution of 0.01 dB/mV
with a range of 30 dB, while the combined TDL has sub-picosecond resolution with
a full range of 375 ps. To subtract the processed interference reference from the cor-
rupted received signal, a balanced photodetector is used, which outputs an electrical
current proportional to the difference between the optical intensities incident on two
separate photodiodes. To characterize the system, a wideband interference signal was
combined with a much weaker, single-tone signal of interest. Interference cancella-
tion was optimized by observing the output of the system on a spectrum analyzer
and manually tuning the VOA and TDL until interference power was minimized.
Experimental results (Fig. 10) show that the system can cancel interference in
both the 900 MHz and 2.4 GHz ISM (industrial, scientific, and medical) bands. All of
these results were obtained by the same optical canceller by simply tuning the VOA

Fig. 9 Architecture of a two-tap canceller. s(t) = signal of interest, n(t) = self-interference,

n0 (t) = tap of original transmitter signal
Optical-Based Interference Cancellation in Wireless Sensor Networks 287

(a) 10 kHz

65 dB
SOI

(b) 10 kHz

65 dB
SOI

(c)

40 dB
SOI

50 MHz

(d)

30 dB
SOI

40 MHz

Fig. 10 Experimental results of interference cancellation in the (top) 900 MHz band and (bottom)
2.4 GHz band for broadband (left) and narrowband (right) interfering signals. SOI = signal of
interest. Taken from [29]
288 M.P. Chang et al.

Simulation

Experiment

Simulation

Experiment

Fig. 11 Interference cancellation measured over 400 MHz in both the (top) 900 MHz band and
(bottom) 2.4 GHz band. Taken from [29]

and TDL to account for the interference channel’s frequency response, illustrating the
wide tunability of the optical canceller. In fact, any system operating frequency from
DC to 10 GHz can be selected by the VOA and TDL. The system achieves greater
than 65 dB of cancellation of a narrowband interferer, demonstrating the high ampli-
tude and delay precision of the optical components. For broadband cancellation, the
system achieves better than 40 and 30 dB of cancellation for a 50 MHz and 40 MHz
signal in the 900 MHz and 2.4 GHz bands, respectively. In all cases, the signal of
interest is recovered, despite the in-band interference, which is a key advantage of
interference cancellation over filtering. Because the cancellation system operates on
the RF-level of the communication system, the results are completely independent
of either signal of interest or interference signal modulation format.
The tradeoff between cancellation depth and bandwidth (see Sect. 2.3) can be
studied by observing cancellation for a fixed system state across a wide bandwidth,
as shown in Fig. 11. Cancellation degrades with bandwidth because of the inability
of a two-tap system to model the interference channel’s response at every frequency.
Nonetheless, the optical system has clearly demonstrated the ability to operate over
an extremely wide bandwidth.

4.2 Adaptive Canceller Using a Semiconductor Optical

Amplifier

A limitation of the previous system was that the optical delay line was tuned mechan-
ically, and therefore could not adapt to rapidly changing RF environments. The archi-
tecture featured in Fig. 12 utilizes similar principles to the interference canceller
in the previous section; however, unlike the previous architecture, a semiconduc-
tor optical amplifier (SOA) is inserted into the cancellation path to provide a fast
and fully electronic control interface. The SOA performs three key signal-processing
Optical-Based Interference Cancellation in Wireless Sensor Networks 289

Fig. 12 Architecture of an adaptive canceller using a semiconductor optical amplifier based tun-
able delay line and variable optical weight. BPF = Bandpass Filter, EDFA = Erbium-Doped Fiber
Amplifier, Mod = Modulator, PC = Polarization Controller

functions related to interference cancellation: amplitude control, delay control, and

signal inversion. The SOA achieves a tunable optical delay by controlling the group
velocity of the propagating signal through both the SOA bias current and input
optical power. Controlling the group velocity of optical semiconductors has been
coined slow and fast light, and has been investigated thoroughly for its applications
in microwave photonic filters, beamformers, and optical buffers. [26, 40, 49, 50].
In addition to setting a time delay, the SOA bias current and input optical power
also affect the SOA gain; therefore, the SOA can also be used to control the RF
signal amplitude. Simultaneous and independent control of the signal amplitude and
delay is realizable because two independent control variables (SOA bias current and
input optical power) are used to drive the SOA. The relationships between SOA bias
current, input optical power, RF gain, and RF time delay are shown in Fig. 13. The
SOA can be operated in constant-gain mode, constant-delay mode, or variable gain
and delay mode [38].
Finally, the SOA is also used to invert the RF signal by counter-propagating a
second, continuous-wave optical signal of different wavelength through the SOA
and subjecting it to cross-gain modulation in the SOA. The second optical signal
exits the SOA with the RF signal imprinted onto it, except inverted. The subtraction
occurs in a 50/50 optical coupler, which combines the received signal path with the
processed and inverted cancellation path. The output is detected by a photodetector.
The SOA-based architecture achieves similar performance to the previous archi-
tecture: 40 dB cancellation over 60 MHz at 900 MHz band and 56 dB narrowband
cancellation [30]. The narrowband cancellation is reduced by 9 dB compared to the
previous architecture because the noise floor rises with the addition of the SOA. The
290 M.P. Chang et al.

Fig. 13 Relationship (a)

between SOA bias current
(ISOA ) and input optical
power (Ppump ) on a RF gain,
and b RF delay. Curves
correspond to constant-gain
lines and constant-delay
lines. Taken from [38]

(b)
3

2
1
2
1

9 dB rise in noise floor is in agreement with estimated SOA noise figure, and is one
tradeoff of using the SOA.
The SOA’s fully electronic control variables are used to implement a computer-
controlled optimization algorithm to adaptively cancel interference. An example
experimental run of the algorithm is shown in Fig. 14a. A map of the output residual
interference power as a function of the SOA control variables is retroactively super-
imposed. Figure 14b demonstrates that the algorithm converges to the global min-
imum solution over a delay mismatch range of 83 ps (the maximum SOA-induced
delay range was 120 ps). We note that 120 ps is not a sufficient delay range to account
for delay variations in most RF environments, particularly if antennas are subject to
movement. Indeed, additional coarse delays (either optical or RF) will be required
to account for large delay variations. With regards to speed, the settling time of the
SOA corresponds to the inverse of the modulation bandwidth of the SOA, which is
about 1 µs for these devices. This can be improved by selecting SOAs designed for
high modulation bandwidths. The SOA-based tunable delay is thus well-suited to
react to rapid but small changes in delay, such as antenna vibrations.
As a bit of foreshadowing, the SOA-based interference canceller sheds light on a
possible path to achieving a fully-integrated interference canceller, by designing the
signal-processing functions of amplitude control, delay control, and signal inversion
into a semiconductor.
Optical-Based Interference Cancellation in Wireless Sensor Networks 291

(a) (b)

Fig. 14 a The SOA-based interference canceller adaptively canceling interference using the SOA
bias current and input optical power as control knobs. b The system converges to the global mini-
mum over a range of 83 ps. Insets show the output spectra as the algorithm progresses. Taken from
[30]

4.3 Adaptation to Wireless Environments

In practical wireless environments, multipath propagation introduces multiple copies

of self-interference, each with a different set of attenuation and delay (see Eq. 3).
Therefore, any practical implementation of an interference cancellation system will
need to consider multipath components as additional interference sources.
Here, we examine the architecture of an optical self-interference canceler for a co-
located transmitter-receiver in an outdoor environment [51]. This architecture boasts
a scalable method of canceling multiple copies of self-interference. Figure 15 shows
the architecture of the optical canceler and how it interfaces with the RF front end
of a communication system, complementing the following system description.
The system takes two inputs: (1) the reference interference signal from a tap of
the transmitter output, xTX (t) = n0 (t), and (2) the corrupted received signal, xRX (t) =
∑
s(t) + Ni=1 ni (t), where s(t) is the signal of interest (SOI) and ni (t) is the ith multipath
component of xTX (t). For example, n1 (t) is the line-of-sight self-interference and
n2 (t) is the strongest multipath component etc. The reference interference is tapped
from the transmitter using a balun, which provides an inverted copy of the reference
interference for the optical canceler (see Fig. 15)
The RF input signals are then each separately modulated onto two optical carriers
at 1552.56 and 1550.55 nm using electroabsorption modulated lasers. The modulated
self-interference reference signal is split into N cancellation paths using a 1:N optical
splitter, one for the line-of-sight and the rest for multipath components. Here, we use
N = 2 cancellation paths.
The receive antenna picks up a sum of distorted multipath components of the
∑
transmit interference signal, Ni=1 ni (t), which underwent channel effects of atten-
uation, delay, other front end components, and noise. Because of these effects, the
N interference reference copies in the cancellation paths, n0copy(i) (t), do not exactly
match the interference signals in the receiver, ni (t), and must be adjusted in ampli-
292 M.P. Chang et al.

Fig. 15 Simplified diagram

of the scalable optical
cancellation system
connected to two directional
antennas [51]. EML =
Electroabsorption Modulated
Laser, VOA = Variable
Optical Attenuator, SM-MM
= SingleMode to
MultiMode, and MM-PD =
MultiMode Photodetector.
Fiber delay lines are
represented by blue loops

tude and phase to match. The goal of the optical canceller is to delay and attenuate
each interference reference copy n0copy(i) (t), with unique parameters 𝜙i and 𝛼i , respec-
tively, such that it resembles each ni (t) as closely as possible, thereby achieving the
maximum cancellation. To perform these adjustments, each cancellation path under-
goes delay matching using fixed optical fiber lengths and tunable optical delay lines,
and amplitude matching using variable optical attenuators, yielding 𝛼i n0copy(i) (t − 𝜙i ).
After tuning adjustments, both the cancellation and received signals are fed into
separate inputs of a custom-built 8 × 1 singlemode to multimode combiner (SM-
MM) combiner. The SM-MM combiner maps each singlemode input onto orthog-
onal spatial modes of a multimode fiber [52]. Since each optical signal resides in
an orthogonal spatial mode, all optical carriers can share wavelengths without suf-
fering coherent beat noise. This eliminates the need for a separate optical source
for each multipath component as well as the associated multiplexers/demultiplexers/
modulators that would be necessary otherwise. Specifically, without the SM-MM
combiner, this system, with N = 2 taps, would require three distinct optical sources
and modulators. Although this allows each laser and modulator to be tailored to opti-
mize different trade-offs, its scalability is limited.
Finally, the combined optical signal is detected by a multimode photodetector.
Because each optical signal resides in a different spatial mode of the multimode fiber,
Optical-Based Interference Cancellation in Wireless Sensor Networks 293

the photodetector incoherently sums each optical signal in the output RF photocur-
rent. This operation results in the subtraction of the self-interference copies from the
received signal, since the self-interference copies were initially inverted by a balun.
The system output can be represented as:

∑
N
y(t) = xRX (t) − 𝛼i n0copy(i) (t − 𝜙i )
i=1
{ }
∑
N
∑
N
= s(t) + ni (t) − 𝛼i n0copy(i) (t − 𝜙i )
i=1 i=1

where our goal is to reduce the term in brackets to 0 such that y(t) → s(t).
Figure 16 shows the results of the optical canceller used in an outdoor environ-
ment to uncover a weak signal of interest [51]. The canceller, wielding two can-
cellation paths, canceled the line-of-sight component of self-interference and the
strongest multipath component of the same self-interference. The system achieved
34 dB of narrowband cancellation and >29 dB of cancellation across 20 MHz of
instantaneous bandwidth. Multipath cancellation contributed more than 10 dB of
additional cancellation. This additional cancellation enabled the system to uncover
a weak sigal of interest received at 5 dB above the noise floor [51].

4.4 A Monolithically Integrated Optical Canceller

Although discrete optical cancellers achieve impressive performance, they are imprac-
tical for cost-sensitive commercial applications due to their large size, high cost, and
power hungry nature. Miniaturizing the optical canceller into a monolithic photonic
integrated circuit (PIC) can offer a panacea to these issues and pave avenues to new
applications. A PIC is compact and mobile, since it is a single semiconductor chip;
scalable and low cost, since it can leverage the economies of scale of the semicon-
ductor industry; and robust to thermal and vibrational shock, since it is purely solid-
state. With these advantages, the PIC canceller creates a win-win situation for both
performance and cost. Here, we introduce the design and demonstration, for the first
time, of a monolithically integrated PIC canceller.

4.4.1 Integrated Circuit Architecture and Design

The PIC canceller is designed to mimic the functionality of the discrete optical can-
celer while eliminating its weaknesses. First, the PIC canceller is optically self-
contained, meaning that it has monolithically integrated lasers and photodetectors
so that the electrical-optical and optical-electrical conversions are all performed on-
chip. This eliminates the expensive and tedious fiber-coupling process that drives
294 M.P. Chang et al.

Fig. 16 A weak signal of interest received at 5 dB above the noise floor is uncovered with the help
of the multi-tap optical canceller. The spectrum analyzer plots show the output of the canceller (top)
without cancellation, (middle) with cancellation using only the line-of-sight cancellation path, and
(bottom) with cancellation using both the line-of-sight and the multipath cancellation paths. Only
the last configuration is able to uncover the weak SOI
Optical-Based Interference Cancellation in Wireless Sensor Networks 295

packaging costs in optical components and other PICs. Instead, the PIC can be
packaged using standard IC packaging technology. Second, instead of optical fiber,
semiconductor optical waveguides carry the optical signal from one optical device
to the next (Fig. 17), greatly reducing the loss caused by cascaded fiber-couplings
between discrete optical components. This loss can be 1–2 dB per fiber-coupling,
which results in 2–4 dB of RF loss due to the square law relationship between opti-
cal and RF power. Link designers now have more margin in the loss budget and can
make tradeoffs to improve dynamic range, noise figure, or bandwidth.
As with the discrete optical canceller, the optical modulators are critical to the per-
formance of the PIC canceller. The PIC canceller erforms electrical-optical conver-
sion via direct modulation of etched facet Fabry-Perot lasers as the optical modulator
(see Fig. 18). Although, distributed feedback (DFB) lasers are usually the mono-
lithic laser source in PICs, the etched-facet laser design eliminates the requirement
for complicated electron-beam or stepper lithography, as well as one regrowth step,
which adds cost and reduces yield. The etched facet is created by dry-etching a trench
to produce a vertical sidewall that is sufficiently smooth to act as a reflective laser

Fig. 17 Mode-matched
ridge

Fig. 18 Etched facet laser

296 M.P. Chang et al.

(a) (b)
Dry-Etched
Trench
InP P-Contact

MQW Active Region MQW

SiO2
Ti/Pt/Au
N-Contact

Laser VOA SOA Photodetector

Fig. 19 a Schematic of the chip layout and composition. b Scanning Electron Microscope image
of a fabricated PIC

facet. The 5 µm wide trench is etched 3 µm deep into the existing ridge waveguide,
which connects the laser to the remainder of the photonic circuit. The lack of an
external modulator also reduces insertion loss and the need for an additional device;
however, further research on alternative laser and modulator devices is ongoing.
Architecturally speaking, each PIC canceller is composed of two paths: one for
the propagation of the reference interference signal (the cancellation path) and one
for the propagation of the corrupted received signal (see Fig. 19a). Both paths have
tunable amplitude and phase devices to maximize tunability range. All elements on
the PIC canceller are connected by integrated waveguides, which carry the opti-
cal/RF signal from one element to the next with minimum loss. Both paths consists
of a monolithic laser, tunable delay line, semiconductor optical amplifier (SOA), and
photodetector. As with the architecture presented in Sect. 4.2, the SOA plays a criti-
cal role in the functionality of the canceller. It overcomes the speed bottleneck that is
present in the discrete optical canceller while also implementing amplitude match-
ing of the RF signal via current injection. A waveguide photodetector converts the
processed optical signal back into an RF signal. Gold wirebonds are used to transfer
the RF signals to and from the PIC. Finally, the subtraction mechanism is performed
by using a differential transimpedance amplifier following the photodetectors.
The PIC is fabricated on a 1550 nm multiple quantum well laser-diode epitaxial
wafer. The active region of the wafer consists of 5 InGaAlAs quantum wells grown on
a semi-conducting InP substrate; the photoluminescence spectral peak of the wafer
is 1542 nm. The fabrication of the PIC requires five mask layers: ridge definition,
electrical isolation, trench etch, contact window opening, and p-contact deposition.
Following fabrication, the PICs are lapped, cleaved, and mounted to a silicon sub-
mount, which facilitates electrical contact and testing. Each cleaved die, which also
includes test structures and other elements, is 2.5 mm × 2 mm. A scanning electron
microscope image of a single PIC die is shown in Fig. 19b.
PICs were characterized for both DC optical performance and interference cancel-
lation. Self-interference cancellation tests were conducted by generating an interfer-
Optical-Based Interference Cancellation in Wireless Sensor Networks 297

(a) (b) 0
-5

Cancellation (dB)
125 mV
-10
No Cancellation
Vatt = 1.35 V -15
Transmitter Laser Off
-20
-25
-30
-35
Vatt = 1.37 V Vatt = 1.42 V -40
10 15 20 25 30 35 40
Frequency (MHz)

Fig. 20 a Oscilloscope plots of the PIC dynamically reducing AM self-interference. b Cancellation

versus bandwidth

ence signal using a signal generator and modulating it onto both paths of the PIC. The
system was then tuned to optimize cancellation of the self-interference by adjusting
the laser and photodetector bias voltages to amplitude match the reference interfer-
ence with the interference in the corrupted received signal.
Preliminary results of the experiment are shown in Fig. 20a and demonstrate the
convergence of the PIC from zero cancellation to maximum cancellation. In these
experiments, the delay is matched ahead of time, and the amplitude is tuned from
completely unmatched (i.e. cancellation path is off) to optimum matching. As the PIC
improves the amplitude matching between the interference reference and the actual
interference signal, the residual interference at the PIC output is slowly reduced
until it hits the noise floor. The cancellation versus bandwidth tradeoff for the PIC
is shown in Fig. 20b, indicating that optimum cancellation is achieved over about
5 MHz instantaneous bandwidth and degrades sharply outside that bandwidth. The
degradation is a result of deviations between the frequency responses of the two dif-
ferent paths of the PIC. We believe that the deviation results from significant differ-
ences in parasitics, such as wirebond lengths and the traces on the silicon submount.
Fabrication adjustments to improve the chip bandwidth are currently underway.

5 Integrated Microwave Photonics and Future Prospects

For the past few decades, research on microwave photonics has primarily focused
on discrete fiber-optic systems. These systems were built to address niche appli-
cations, such as military and defense, where performance is the top priority over
cost. However, the recent years have witnessed a flurry of interest in high data rate
(Gbps) telecommunications, such as wireless sensor networks, broadband public
access points, and small cell and picocell backhaul. These applications are much
more cost-sensitive and are not appropriate for discrete fiber systems. The emerg-
ing field of integrated microwave photonics is poised to address these high data rate
298 M.P. Chang et al.

applications, while also meeting their price-point. The high volume demand of these
applications can also serve as the catalyst to generate the capital needed to propel
the integrated microwave photonic infrastructure to commercial readiness.
Integrated microwave photonics seeks to package the advantages of optics, such
as wide bandwidth and frequency-agnostic performance, into an integrated circuit,
where it can leverage the economies of scale of the semiconductor industry. The pri-
mary barriers to the commercial viability of such systems are the economics (yield)
and the fabrication of materials and devices, which must satisfy stringent applica-
tion requirements. As opposed to electronic ICs, where the transistor is the dominant
device, multiple optical devices are needed per photonic integrated circuit (PIC),
leading to a more difficult fabrication process. Unlike discrete microwave photonics,
where each device can be optimized on separate materials, integrated microwave
photonics compromises this degree of freedom for manufacturing simplicity. Yet,
great strides have been made in recent years to increase the number of devices inte-
grated on one PIC and reduce the killer defect density to increase yield (see Fig. 21).
Infinera, the first widely successful PIC company, has led the charge by fabricating a
PIC with over 400 devices, capable of aggregate data rates of 500 Gbps [53]. Indeed,
a Moore’s Law of Photonics has already been declared.
Photonic integrated circuits (PICs) are primarily being built in three core material
platforms: InP and GaAs (III-V), silicon-on-insulator, and silicon nitride. Each plat-
form has its unique advantages and disadvantages and should be selected based on
the application requirements; a review for each platform is provided in [55]. Multi-
Project Wafer (MPW) consortia for standardized PIC development, such as IMEC
and JeppiX in Europe, have made PIC research much more accessible to researchers
and developers worldwide. These initiatives consolidate resources and know-how to
make it affordable for industry and academic researchers to experiment with PICs.
A standard software ecosytem (layout, verification, extraction) and simulation plat-
form is also needed to unite the PIC community in a similar fashion to what was
achieved in silicon. Companies such as PhoeniX and PhotonDesign have begun this
effort.
It is an exciting time to be involved in integrated microwave photonics research
because manufacturing technology maturity, device performance, and market demand

Fig. 21 a Device count per PIC. Taken from [54]. b Killer defect density. Taken from [53]
Optical-Based Interference Cancellation in Wireless Sensor Networks 299

for high-performance RF analog signal processing have arrived at a common inter-

section. Wireless sensor networks and interference cancellation will certainly benefit
from the progress being made in these fields, and we expect that they will be but one
of many.

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Traffic Adaptive Channel Access
Scheme for IEEE802.15.4 Cluster-Based
WSNs Under Spatial Non-uniform Traffic
Condition

Akiyuki Yamauchi, Kazuo Mori and Hideo Kobayashi

Abstract Difference in transmission performance arises between cluster heads

(CHs) involved in inter-cluster communication on IEEE 802.15.4 cluster-based
wireless sensor networks (WSNs) under spatial non-uniform traffic condition where
the CHs have various amount of traffic. In this chapter, we first
quantitatively-clarify appearance of the performance difference between different
traffic loaded CHs under such traffic condition, and then proposes traffic adaptive
channel access scheme to mitigate this performance difference. In the proposed
scheme, introducing autonomous traffic adaptive priority access control, the CHs
adjust their backoff exponent BE, which is one of key control parameters in IEEE
802.15.4 MAC, based on their estimated traffic status relative to other CHs.
Through performance evaluation by computer simulation, this chapter shows that
the proposed scheme can reduce the performance difference between CHs with
different traffic loads in inter-cluster communication under spatial non-uniform
traffic conditions.

1 Introduction

Due to limited network resources such as battery capacity and processing capa-
bility, wireless sensor networks (WSNs) absolutely require lower energy con-
sumption and simpler processing mechanism to achieve long network lifetime
under limited network resource condition [1, 2]. To satisfy these requirements, duty
cycle mechanism, under which sensor nodes (SNs) periodically put their commu-
nication functions in inactive state, and cluster-based network topology, under
which neighbouring SNs form a cluster and each SN transmits its measured data to
its cluster head (CH) and then the CH sends the aggregated data to a sink node (or a
parent CH), are deeply investigated in recent years [3, 4].

A. Yamauchi ⋅ K. Mori (✉) ⋅ H. Kobayashi

Mie University, Tsu, Japan
e-mail: [email protected]

© Springer International Publishing AG 2017 303

S. Mukhopadhyay et al. (eds.), Sensors for Everyday Life, Smart Sensors,
Measurement and Instrumentation 23, DOI 10.1007/978-3-319-47322-2_14
304 A. Yamauchi et al.

As a practical example of medium access control (MAC) mechanisms for WSNs,

IEEE802.15.4 MAC [5] specifies beacon enabled mode, and this mode provides
energy saving operation based on the duty cycle mechanism. The beacon enabled
mode adopts superframe structure in time axis on communication channels and
achieves active/inactive alternative operation at SNs based on the superframe,
leading to lower energy consumption in WSNs. On the other hand, the cluster based
topology also contributes to reduction of energy consumption in WSNs due to
reduced transmission power at SNs and traffic load dispersion. Hence, previous
studies have investigated clustering mechanisms to achieve low energy WSNs [6–8].
In cluster-based WSNs, the data communication consists of two parts;
intra-cluster and inter-cluster communications. CHs collect measured data from
their subordinate SNs in the intra-cluster communication, whereas in the
inter-cluster communication, child CHs (CCHs), which are lower level CHs in a
network and generally located near the periphery of the network, send the data
received from their SNs to their parent CH (PCH) which is a higher level CH and
located near the center of the network. We focus on the inter-cluster communication
and investigate its transmission performance in this chapter.
For network characteristic, on the other hand, the WSNs indicate different
characteristics from other wireless networks, such as cellular and wireless local area
networks (WLANs). These characteristics include spatial (geographical)
non-uniform traffic, where the traffic volume generating in a given area differs from
that in other geographical areas. For example, for the event-driven WSNs, event
generation might concentrate in a particular area, and such event generation leads to
spatial non-uniform traffic. Under this traffic condition, introducing cluster topology
into the WSN, the traffic volume generated within a cluster is different between
clusters. As a result, in the inter-cluster communication where some CCHs transmit
their data to the same PCH with a shared communication channel, the difference in
the transmission performance, such as packet dropping probability and transmission
delay, might arise among CCHs with different cluster traffic. For several applica-
tions including environmental monitoring, it is undesirable to have non-uniformity
in quality of data collected from clusters (or regions), such as the difference in
accuracy and instantaneity. Hence, WSNs need to mitigate such non-uniformity in
data quality between clusters by suppressing the different transmission performance
between CCHs with different cluster traffic.
For this issue, a priority channel access is one of promising solutions which can
suppress the different transmission performance between CCHs. As an example of
the priority channel access schemes, WLAN systems adopt the MAC scheme
specified in IEEE 802.11e [9] to provide quality of service (QoS) support [10]. In
this scheme, the priority control based on enhanced distributed channel access
(EDCA) is performed to offer required QoS to multi-medium services, such as
speech, video streaming, and so on. The EDCA is an extended form of distributed
coordination function (DCF) specified in IEEE 802.11, and achieves QoS provision
by means of classification of transmitting information into several access categories
(ACs). For the QoS provision in WSNs, the recent studies have investigated its
application to WSNs in order to handle their multimedia traffic [11–13].
Traffic Adaptive Channel Access Scheme for IEEE802.15.4 … 305

From above background, focusing on the inter-cluster communication in

cluster-based WSNs employing IEEE 802.15.4 beacon enabled mode under spatial
non-uniform traffic, the objectives in this work are to (1) clarify non-uniformity in
transmission performance between CCHs with different cluster traffic in a quanti-
tative way, and then (2) provide mitigation scheme against this performance
non-uniformity between CCHs in order to achieve better uniformity in data col-
lected from the WSN under such traffic condition. To achieve latter objective, this
chapter proposes a traffic adaptive channel access scheme in which each CCH
autonomously controls channel access priority based on its current cluster traffic.
The proposed scheme achieves traffic adaptive priority access by adjusting a control
parameter, backoff exponent BE, for backoff operation in slotted carrier sense
multiple access/collision avoidance (CSMA/CA), specified in IEEE 802.15.4 MAC.
The performance for the proposed scheme is evaluated through computer simula-
tion and its effectiveness is demonstrated.
This chapter is organized as follows. Section 2 briefly describes previous work
related to this chapter. In Sects. 3 and 4, the system model under our consideration
and the problem to be solved in this chapter are discussed, respectively. Section 5
proposes an autonomous traffic adaptive channel access scheme to mitigate
non-uniformity in transmission performance between CCHs. In Sect. 6, the simu-
lation condition used in our evaluation is described, and then, Sect. 7 shows various
simulation results and demonstrates the effectiveness of the proposed scheme.
Finally Sect. 8 concludes the chapter.

2 Related Work

Shared communication channel access in cluster-based WSNs is focused on in this

chapter and the objective is to provide priority channel access scheme for shared
channels according to current traffic load in each cluster. The typical work related to
shared channel access in WSNs and priority channel access in wireless networks are
as follows.

2.1 IEEE 802.15.4 MAC

IEEE 802.15.4 [5] specifies physical (PHY) and MAC protocols for low-rate
wireless personal area networks (LR-WPANs) and is often employed to lower layer
protocol in WSNs, such as ZigBee [14, 15], due to its lower energy consumption.
The beacon enabled mode specified by IEEE 802.15.4 MAC provides power saving
operation based on duty cycle mechanism by using superframe structure. The
superframe is divided into active and inactive periods, and its active period is also
divided into two periods: contention access period (CAP) and contention free
306 A. Yamauchi et al.

period (CFP). This chapter focuses on shared channel access with slotted
CSMA/CA in the CAP, and dedicated channel access in the CFP is out of scope.
The slotted CSMA/CA channel access normally adopts backoff operation to
prevent signal collisions on shared communication channel. Before transmitting
data, each sender randomly selects access delay interval from a backoff window
(BW) defined by a range of [0, 2BE-1]. The backoff exponent BE is initially set to
BEmin and is increased up to BEmax when clear channel assessment (CCA) detects
busy channel after a timeout of selected access delay interval. The transmitting data
is discarded after the number of the backoffs exceeds a predefined value
(‘macMaxCSMABackoffs’ in IEEE 802.15.4).
Equal transmission opportunity is generally given to all the nodes willing to
transmit their data in the slotted CSMA/CA access with normal backoff operation.
This is because the above control parameters such as BEmin, BEmax, and
macMaxCSMABackoffs commonly take the same values for all nodes. However,
this parameter setting and thus equal transmission opportunity for all nodes, is
undesirable to the cluster based WSNs with spatial non-uniform traffic.

2.2 IEEE 802.11e EDCA

IEEE 802.11e EDCA [9] is a typical well-known priority access scheme for shared
communication channels in WLANs, and can offer QoS provision to multi-medium
communication services in WLANs by utilizing backoff operation in CSMA/CA
mechanism.
The EDCA defines multiple access categories (ACs) depending on required
QoSs, such as transmission delay and so on. Transmission data is categorized into
one of these ACs based on its required QoS and is stored separately in the trans-
mission queue corresponding to each AC. The EDCA selects the transmission data
from one of the AC queues based on their priority order and then transmit wireless
frame containing selected data.
To offer priority channel access depending on the required QoS, the control
parameters, arbitration inter-frame space (AIFS) and contention window (CW) are
set to an adequate value for each AC according to its priority order. Specifically, the
AIFS and CW take smaller values for the AC with higher priority, and larger ones
for lower priority AC. Thus, the EDCA provides priority operation by adjusting
access delay interval before data transmission, and enables the QoS provision
required by each communication service.
Traffic Adaptive Channel Access Scheme for IEEE802.15.4 … 307

3 System Model

Let us consider a cluster-based WSN with one PCH and Ncch CCHs subordinating
some SNs, as illustrated in Fig. 1. All nodes in the WSN operate with duty cycle
mechanism in accordance with IEEE 802.15.4 beacon enabled mode, and the dif-
ferent time period in the IEEE 802.15.4 superframe is assigned as an active period
for intra-cluster communication to different cluster in order to avoid interference
between any intra-cluster communications. The active period for inter-cluster
communication is also assigned different time period from those for any
intra-cluster communications, as shown in Fig. 2. Therefore, this active period

Parent cluster head (PCH)

Inter-cluster
communication
Ncch child
cluster heads (CCHs)
CCH1 CCH2 . . . CCH Ncch
cluster1 cluster Ncch
cluster2
...

Sensor nodes (SNs)

Fig. 1 Topology model

IEEE 802.15.4 superframe

Inter-cluster
Beacon CCHs PCH
PCH (inactive) CAP (inactive)
Intra-cluster
SNs CCH1
CCH1 CAP (inactive) CAP (inactive)
Intra-cluster
SNs CCH2

CCH2 (inactive) CAP (inactive) CAP (inactive)

...

Intra-cluster
SNs CCH Ncch
CCH Ncch (inactive) CAP CAP (inactive)

Time

Fig. 2 Frame structure model

308 A. Yamauchi et al.

assignment causes no interference between inter-cluster and any intra-cluster

communications.
Every CCH receives data from its SNs during the CAP in its active period
assigned to intra-cluster communication, and then transmits the data to its PCH
during the CAP in the active period assigned to inter-cluster communication.
Hence, the CAP for the inter-cluster communication can be considered as a shared
communication channel, where Ncch CCHs compete to transmit their data. IEEE
802.15.4 beacon enabled mode employs the slotted CSMA/CA with backoff
operation as a channel access scheme for the shared communication channel. In this
channel access, every CCH normally employs the same parameter setting for its
control parameters as others.
Considering spatial non-uniform traffic conditions, each cluster has different
traffic load from others, for example having different number of subordinate SNs as
illustrated in Fig. 1.

4 Motivation

Normal slotted CSMA/CA fundamentally provides fair channel access among

CCHs regardless of their traffic load. This characteristic results from control
parameter settings common to all CCHs for the backoff operation, such as BEmin,
BEmax, and macMaxCSMABackoffs. This common setting is preferable for the
channel access where the CCHs having the same traffic load compete with each
other for the shared channel.
Under the spatial non-uniform traffic condition, however, common parameter
setting causes negative effect to the system performance, that is non-uniform
transmission performance between CCHs with different traffic, because each CCH
has different traffic load. For example, frequent buffer overflow occurs at high traffic
CCHs due to insufficient transmission opportunity for their traffic load. This leads to
high packet dropping probability and long transmission delay. In contrast, low
traffic ones can obtain too much opportunity for their traffic, and therefore, enjoy
quite low packet dropping probability and also short delay.
This performance difference might cause non-uniform quality in the data col-
lected at a sink node (center node). The non-uniform quality in collected data might
bring negative impact on application services offered by the sink node utilizing the
collected data. Hence, each CCH should retain uniform transmission performance
to provide higher quality application services. Then priority channel access scheme
should be required for the inter-cluster communication involving the CCHs with
various traffic loads, such as under spatial non-uniform traffic conditions.
Traffic Adaptive Channel Access Scheme for IEEE802.15.4 … 309

5 Autonomous Traffic Adaptive Backoff Control Scheme

This section proposes a countermeasure technique to the above-mentioned problem

appearing on the inter-cluster communication in cluster-based WSNs with spatial
non-uniform traffic. The proposed scheme aims to supress the performance
non-uniformity among CCHs with various traffic loads on the inter-cluster
communication.

5.1 Requirements for Proposed Mechanism

Contemplating the causes raising the above problem, the proposed scheme requires
two basic functions: traffic adaptive channel access control and autonomous dis-
tributed control.
For the traffic adaptive channel access, the CCHs with high/low traffic should
operate with high/low priority for shared channel access to supress the performance
difference between CCHs with different traffic. In addition, this priority control
should be achieved by using autonomous distributed control mechanism since
WSNs should avoid additional control signal exchange due to their limited network
resources, such as communication capacity, computational and battery power.

5.2 Pruority Channel Access Based on Cluster Traffic Status

In the traditional priority access mechanism in WLAN systems, IEEE 802.11e, each
mobile terminal (MT) decides the channel access priority by selecting the size of
AIFS and CW in backoff operation for CSMA/CA channel access, as mentioned
before in Sect. 2.2. IEEE 802.15.4 MAC employs the same kind of backoff oper-
ation as IEEE 802.11 WLAN systems, and the BW for IEEE 802.15.4 MAC
corresponds to the CW for IEEE 802.11e. The size of both BW and CW is given by
the same control parameter of backoff exponent BE. Therefore, the proposed
scheme also controls the access priority by adjusting the BE.
The proposed scheme sets different access priority to the CCHs according to the
traffic conditions in their clusters. The priority control can be achieved by setting
different value to this BE at each CCH with different traffic load. Figure 3 illustrates
a conceptual diagram of the proposed autonomous traffic adaptive backoff control
scheme.
In the proposed priority control, as a basic framework, the high traffic loaded
CCHs obtain high priority state, being able to get more transmission opportunity,
by setting a smaller value to their BE. The smaller BE brings a shorter waiting
interval before channel accesses, leading to high priority in the shared channel
access. The low traffic loaded CCHs, on the other hand, take a larger value to their
310 A. Yamauchi et al.

Start High More tx.

priority oppotunity
High traffic CS
Short waiting
Small BE Data tx.
CCH 1

Short backoff window

PCH
...

Long waiting Suppress

tx.
Low Less tx.
Large BE priority oppotunity
CCH n
Low traffic

Long backoff window

Fig. 3 Priority control based on backoff operation

BE in order to increase the BW size and this parameter setting forces them to wait
for a larger interval, leading to low priority state, being hard to get more trans-
mission opportunity. From these BE setting, the CCHs with higher traffic can obtain
more transmission opportunity than the CCHs with lower traffic, as illustrated in
Fig. 3. As a result, each CCH can transmit the data received from its SNs in
proportion to its own traffic load, and then, WSNs can suppress the non-uniform
transmission performance between CCHs, resulting in system performance
improvement.
IEEE 802.15.4 MAC defines two control parameters for the BE; BEmin and
BEmax. The BEmin adjustment could impact the access priority at the earlier stage of
backoff operation. BEmax adjustment, however, cannot influence at the earlier stage,
do only at the final stage. Therefore, in this work, we employ the BEmin to control
the priority levels for CCHs.

5.3 Traffic Status Estimation

To achieve the above-mentioned priority access, each CCH needs to know its
current traffic status relative to other CCHs competing the same CAP. Therefore, as
an indicator of the relative traffic status, the proposed scheme introduces the length
LCAPend
queue (packets) of transmission queue at the end point of the CAP assigned to the
communication from the CCHs to their PCH.
At the end point of a given CAP, the data stored in the transmission queue shows
the data which the CCH cannot complete to transmit during that CAP. Monitoring
the amount of the non-completed data allows each CCH to recognize its trans-
mission status, good or poor status, reflecting the competition for the CAP with
Traffic Adaptive Channel Access Scheme for IEEE802.15.4 … 311

Channel access at CCH1

CS High traffic
Backoff CS BEmin
Data decrease Data

Short backoff CCH 1

Tx. queue
Long
Superframe Traffic
ON estimation ON

...
(monitoring) PCH
Tx. queue
Short
Long backoff CCH n
Backoff CS BEmin CS
Data increase Data Low traffic
Channel access at CCHn

Fig. 4 Backoff exponent BE adjustment based on traffic status estimation

other CCHs. Hence, each CCH can estimate its traffic status relative to other CCHs
by observing the transmission queue length LendCAP
queue .
Figure 4 partly illustrates an example for the proposed traffic status estimation,
where the CCH1 (upper one) with many SNs detects a long LCAPendqueue at the end of the
current CAP. Then, the CCH1 can estimate its traffic status at high traffic condition,
where it obtain insufficient transmission opportunity compared with its current load.
Conversely, the CCHn (lower one) with a small number of SNs has a short LCAPendqueue
which shows it can get sufficient transmission opportunity during that
CAP. Therefore the CCHn can cognize that it is in low traffic status. From these
considerations, the transmission queue length LCAPendqueue at the end of the CAP is
useful for estimating traffic status relatively to other CCHs.

5.4 Control Procedure

In the proposed scheme, the backoff exponent BEmin is adjusted by a following

procedure, as illustrated in Fig. 4.
In every superframe, the CCHs observe the transmission queue length LCAPendqueue at
the end of the CAP used for data transmission to their PCH, and then estimate their
traffic status based on the observed LCAPend
queue . After the traffic estimation, they adjusts
their BEmin value which will be applied in the next superframe (CAP).
As criteria for traffic status estimation, the proposed scheme introduces a pre-
defined constant threshold THqueue for evaluating the observed LCAPendqueue . The CCHs
312 A. Yamauchi et al.

estimate high traffic status relative to others when detecting the observed LCAPend
queue is
greater than the threshold THqueue. In contrast, they estimate their low traffic status
queue ≤ THqueue .
after detecting Nup consecutive LCAPend
For the specific procedure for controlling the BEmin, the CCHs under the high
traffic status decrease the value of BEmin by a decrement step ΔBEdown in order to
increase their access priority, whereas CCHs with the low traffic status increase the
BEmin by an increment step ΔBEup to lower their access priority. These adjustment
steps ΔBEdown and ΔBEup are predefined and constant control parameters. The
detailed controlling procedure for the BEmin and its adjustment range is given by:
8 before
< BEmin + ΔBEdown
> ; LCAPend
queue > THqueue
after before
BEmin = BEmin + ΔBEup queue ≤ THqueue in consecutive Nup
; LCAPend
>
: before ð1Þ
BEmin ; otherwise,
upperr
lower
subject to BEmin ≤ BEmin ≤ BEmin ,

lower upper
where BEmin and BEmin are a minimum and maximum value for BEmin. The
optimal settings for Nup, ΔBEdown and ΔBEup will be discussed in Sect. 7.2.

6 Performance Evaluations

The performance for the proposed autonomous traffic adaptive backoff control is
evaluated through computer simulation with following assumptions. The statistics
are collected from the inter-cluster communication involving one PCH and its Ncch
subordinate CCHs, as illustrated in Fig. 1.

6.1 Wireless Channel Model

The radio channels are assumed to be ideal without any consideration of propa-
gation loss, shadowing and fading fluctuation in this evaluation. Packet transmis-
sion error occurs only due to packet collision caused from simultaneous
transmission from multiple CCHs. The CCA at each CCH is perfect without impact
of hidden terminal problem.

6.2 Traffic Model

The packets are continuously generated at each CCH following Poisson distribution
with an average cluster traffic load of Gx (packets/Lpkt), which corresponds to
Traffic Adaptive Channel Access Scheme for IEEE802.15.4 … 313

cluster traffic load. The Lpkt is a packet length and is same for all generated packets.
After the packet generation, the packet is stored in transmission buffer with a length
of Lbuffer (packets) at each CCH. The packet is discarded due to buffer overflow
when the buffer is full. At the buffer overflow the oldest packet is discarded.
Three different cluster traffic loads, Gx (x = ‘low’, ‘mid’, or ‘high’) are defined
to simulate spatial non-uniform traffic condition. Ncch CCHs are equally separated
into three CCH groups, and each CCH group has one of Gx without duplication
each other. Defining the ratio (Rlow : Rmid : Rhigh) for traffic loads (low : mid : high),
the traffic load Gx for the cluster in group x is given by using average network traffic
load G (packets/Lpkt):

Rx
Gx = ⋅ G ̸ NCCH ð2Þ
∑ Rx
x = low, mid, high

For transmission failure, the packets are retransmitted following IEEE 802.15.4
MAC specification.

6.3 Evaluation Metric

We evaluate the packet dropping probability Pdrop and transmission delay Dtx as
transmission performance, where Pdrop and Dtx are given by a ratio of the number of
dropping packets due to transmission failure or buffer overflow at CCHs to that of
generated packets, and a time duration elapsed from packet generation at CCHs to
successful reception at the PCH, respectively. We also evaluate standard deviations
(SDs) σ drop and σ delay for the packet dropping probability Pdrops and the trans-
mission delay Dtxs observed at all the CCHs as an indicator showing uniformity in
the transmission performance among CCHs with different cluster traffic.
In the performance evaluation, we compare the above each performance for the
proposed scheme with that for the system employing fixed BEmin setting of 5, which
is called ‘standard system’ in this evaluation.

7 Evaluation Results

Using the parameter settings listed in Table 1, we evaluated the system perfor-
mance for the proposed scheme, comparing with the standard system. Note that
MAC parameter settings except shown in Table 1 employ their default values
specified in the IEEE standard.
314 A. Yamauchi et al.

Table 1 Simulation Parameter Settings

Symbol Value
Transmission rate Rrate 250 (kbps)
aUnitBackoffPeriod UBP 0.32 (ms)
Duration of aUnitBackoffPeriod TUBP 48 (UBPs)
Beacon order BO 8
Superframe order SO 3
Beacon interval BI 12288 (UBPs)
CAP length LCAP 384 (UBPs)
Beacon frame length Lbcon 5 (UBPs)
Data packet length Lpkt 8 (UBPs)
ACK frame length Lack 2 (UBPs)
macMaxCSMABackoffs 5
Initial BE BEmin, BEmax 5, 8
lower upperr
Range of BEmin BEmin , BEmin 2, 5
Threshold for BEmin adjustment THqueue 0
Tx. buffer length Lbuffer 10 (packets)

7.1 Non-uniform Performance Between CCHs

with Different Traffic Loads

This section clarifies the non-uniformity in transmission performance between

CCHs with different cluster traffic loads for inter-cluster communication under
non-uniform traffic condition with the number of CCHs Ncch = 6 (thus, every CCH
group has 2 CCHs) and the traffic ratio of (Rlow : Rmid : Rhigh) = (1.0 : 1.5 : 2.0).
Figure 5 shows the packet dropping probability Pdrop for each CCH group with
low, middle, or high cluster traffic load. Each CCH group shows quite different Pdrop
performance in the network traffic G of over around 0.01, and the Pdrop for high traffic
CCHs clearly degrades compared with that for lower traffic ones. This result clarifies
that the transmission performance has clear non-uniformity between CCHs with
different traffic loads for such spatial non-uniform traffic. Hence, this non-uniformity
caused from different cluster traffic should be mitigated even under spatial
non-uniform traffic condition in order to improve overall system performance.

7.2 Optimal Parameter Settings for Nup, ΔBEup,

and ΔBEdown

Before evaluating the performance of the proposed scheme by comparing with the
standard system, optimal parameter settings for Nup, ΔBEup, and ΔBEdown should
be obtained to achieve better system performance for the proposed scheme.
Traffic Adaptive Channel Access Scheme for IEEE802.15.4 … 315

Fig. 5 Performance
non-uniformity between
CCHs with different cluster
traffic loads

Therefore, their optimal values are derived through computer simulation. Here, we
employ, as an evaluation metric, an average packet dropping probability Pave drop over
all CCHs in the network traffic region of 0.002 ≤ G ≤ 0.03, and its standard
deviation σ ave
drop for Ncch CCHs.
Firstly we determine an optimum value for the number of detection times Nup
required for estimating low traffic status. Figure 6 shows the Pave drop and σ drop per-
ave

formances for various Nup under the same conditions as Fig. 5. The packet dropping
probability Pave
drop in Fig. 6 is slightly better for smaller Nup. However, the standard
deviation σ ave
drop degrades at Nup of 1 and is better for Nup ≥ 2. In addition it is
almost the same for Nup ≥ 2, and thus, Nup of 2 is concluded to be optimum value
from these observations.
Next, Fig. 7 shows the Pave drop and σ drop performances for varying the increment
ave

step ΔBEup, to discuss its optimal value. The σ ave drop performance degrades with
increasing ΔBEup, while the Pave drop is almost equal for all ΔBEups. Therefore, these
results show the ΔBEup should be set to 1 as its optimum value.
Then, for optimization of the decrement step ΔBEdown, Fig. 8 shows the Pave drop
and σ ave
drop performances for various ΔBE down setting. Roughly speaking, both the
Pdrop and σ drop indicate almost the same performance regardless of ΔBEdown value,
ave ave

Fig. 6 Packet dropping

probability for varying Nup
316 A. Yamauchi et al.

Fig. 7 Packet dropping

probability for varying ΔBEup

Fig. 8 Packet dropping

probability for varying
ΔBEdown

however, the larger ΔBEdown gives slight better σ avedrop performances. From these
results, therefore, we conclude ΔBEdown of 3 as its optimal setting.
Setting the optimum values derived above to Nup, ΔBEup, and ΔBEdown, Fig. 9
shows the BEmin behaviour for varying network traffic load G, under the same
conditions as Fig. 5. From Fig. 9, each CCH can adjust the BEmin to a smaller value
with higher traffic load and a larger value with lower traffic load in middle and high
network traffic load regions. This BEmin behaviour proves the proposed scheme
works well according to the traffic load estimated at each cluster.

7.3 Transmission Performance Comparison

The transmission performances Pdrop and Dtx are shown in Figs. 10 and 11 for the
proposed scheme (referred as ‘Traffic adaptive BE’ in Figs.) and the standard
system under the same conditions as Fig. 5. The performance for each traffic group,
Traffic Adaptive Channel Access Scheme for IEEE802.15.4 … 317

Fig. 9 BEmin behaviour for

each CCH group (low, mid,
and high)

Fig. 10 Packet dropping

probability Pdrop performance

Fig. 11 Transmission delay

Dtx performance

low, middle or high traffic, is separately shown when varying the network traffic
load G in these figures.
In Fig. 10, the packet dropping probability Pdrop is nearly equal between dif-
ferent traffic groups of CCHs for the proposed scheme, despite the standard system
with different Pdrop performance, and thus, the proposed scheme can suppress
318 A. Yamauchi et al.

Fig. 12 Standard deviation

of packet dropping probability
Pdrop

non-uniformity in Pdrop across CH groups with different cluster traffic. For the
transmission delay Dtx, almost the same behaviour can be found in Fig. 11 as the
Pdrop. Hence, the non-uniformity in the transmission performances can be reduced
for all network traffic load regions, applying the proposed scheme.
To provides quantitative analysis of the uniformity in transmission performance
between CCH groups with different cluster traffic, Figs. 12 and 13 show the
standard deviations σ drop and σ delay of Pdrops and Dtxs observed at all the Ncch
CCHs. In Comparison with the standard system, both the standard deviations σ drop
and σ delay are largely reduced for high network traffic load regions by applying the
proposedscheme, and we can find in Figs. 12 and 13 significant reduction against
the transmission performance non-uniformity, provided by the proposed scheme.
This performance improvement is given by proper BEmin control based on current
cluster traffic offered to each CCH, which is a new mechanism provided by the
proposed scheme and is a main contribution of this work.
From the above results and their considerations, applying the proposed scheme
can provide quite effective mitigation against the non-uniformity in the transmission
performance between different traffic loaded CCHs on the inter-cluster communi-
cation in cluster-based WSNs under spatial non-uniform traffic.

7.4 Performance for Various Network Conditions

In the previous section the effectiveness of the proposed scheme is basically pre-
sented for the typical network condition. Since the network has various operating
condition, this section examines the performance for the proposed scheme under for
various network operating conditions.
First, we examine the performance under various spatial non-uniform traffic
conditions, and then the packet dropping probability Pdrop is evaluated for the
conditions with spatial non-uniform traffic of (Rlow : Rmid : Rhigh) = (1.0: 1.0: 1.0),
(1.0: 1.25: 1.5), (1.0: 1.5: 2.0), (1.0: 2.0: 3.0), (1.0: 2.5: 4.0), and (1.0: 3.0: 4.0). The
Traffic Adaptive Channel Access Scheme for IEEE802.15.4 … 319

Fig. 13 Standard deviation

of transmission delay Dtx

standard deviation σtraffic in offered cluster traffic loads under these traffic conditions
is 0.0, 0.2, 0.41, 0.82, 1.2, and 1.6, respectively, which indicates degree in
non-uniformity of the offered cluster traffic. Figure 14 shows the standard deviation
σ ave ave
drop of the Pdrop s at the CCHs, which is the same evaluation metric as shown in
Fig. 6, for varying the standard deviation σ traffic of offered traffic. We can see from
Fig. 14 that the proposed scheme provides superior σ ave drop performance to the
standard system for any σ traffic (spatial non-uniform traffic conditions). Moreover,
the performance improvement obtained by the proposed scheme increases with the
σ traffic. This result concludes that the proposed scheme can provide the effectiveness
under various spatial non-uniform traffic conditions, and the effectiveness gets
larger for the larger spatial non-uniform traffic conditions.
Next, we examine the transmission performance for various network scale,
which includes the number of CCHs Ncch competing the CAP in the inter-cluster
communication. The proposed scheme adjusts the BEmin according to the traffic
load offered to each CCH, and higher traffic CCHs tend to use smaller BEmin to
achieve higher priority in the channel access. However, the smaller BEmin likely
increases the possibility of channel access collision between competing CCHs, and
thus, the impact of smaller BEmin setting to the performance should be clarified for

Fig. 14 Packet dropping

probability for various spatial
non-uniform traffic conditions
320 A. Yamauchi et al.

Fig. 15 Standard deviation

of packet dropping probability
for varying the number of
competing CCHs

Fig. 16 Packet dropping

probability performance for
varying the number of
competing CCHs

the proposed scheme. Figures 15 and 16 show the packet dropping probability
performance for various number of competing CCHs. From the standard deviation
σ ave
drop shown in Fig. 15, the proposed scheme show better performance and can
achieve a reduction in the performance non-uniformity compared with the standard
system for any values of the Ncch. Therefore, an effectiveness of reducing the
performance non-uniformity can be obtained even under the conditions with larger
Ncch. However, the improvement is getting smaller with increasing Ncch, and thus,
the effectiveness gradually disappears with increasing Ncch. Additionally, the packet
dropping probability Pave
drop for the proposed scheme is slightly getting worse with
increasing Ncch, compared with the standard system, and therefore, the network
scale, such as the Ncch, gives no small impact to the transmission performance for
the proposed scheme. Hence, the proposed scheme has to pay some cost to achieve
uniformity in the transmission performance and requires countermeasure against
this drawback, which is left as our future work.
Traffic Adaptive Channel Access Scheme for IEEE802.15.4 … 321

8 Conclusion

This chapter has discussed non-uniformity in transmission performance between

CCHs with various cluster traffic loads on inter-cluster communication in
cluster-based WSNs employing IEEE 802.15.4 MAC. This chapter has firstly
quantitatively-clarified appearance of the performance non-uniformity among dif-
ferent traffic loaded CCHs under spatial non-uniform traffic condition, and then has
proposed the countermeasure technique, the autonomous traffic adaptive channel
access, which controls the backoff exponent BEmin in backoff operation based on
the current traffic status estimated at each CCH, in order to mitigate such perfor-
mance non-uniformity.
The transmission performances, packet dropping probability, transmission delay
and their standard deviations as an indicator showing performance uniformity, have
been evaluated for the proposed scheme through computer simulation under various
network conditions. These simulation results prove that the proposed scheme can
significantly reduce the performance non-uniformity between different traffic
CCHs, and thus, can achieve fairer transmission performance under spatial
non-uniform traffic conditions.
Consequently, the proposed autonomous traffic adaptive channel access scheme
is quite effective for cluster-based WSNs under spatial non-uniform traffic
conditions.

Acknowledgments This work is partly supported by Japan Society for the Promotion of Science
(JSPS), Grant-in-Aid for Scientific Research (c) 25420366, 2013–2015.

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Author Index

A K
Akiyuki Yamauchi, 303 Kassim, Mohamed Rawidean Mohd, 137
Alahi, Md Eshrat E, 109 Kazuo Mori, 303
Al-Shamma’a, Ahmed, 205 Kocanda, Martin, 157
Arregui, Francisco J., 55 Korostynska, Olga, 205
Ascorbe, J., 55
Axmann, H., 1 L
Aziz, Samsuzana Abd, 245 Latiff, Nurul Adilah Abdul, 245

B M
Bergmann, A., 1 Mamidi, Shreya Reddy, 157
Bhandari, Manohar P., 229 Mason, Alex, 205
Blow, Eric, 273 Matthew P. Chang, 273
Bukka, Kaushik, 157 Matias, Ignacio R., 55
Burkitt, L., 109 Monica Lu, 273
Mukhopadhyay, Subhas, 109
C Mukhopadhyay, Subhas Chandra, 55
Carmona, Estefania Núñez, 229
Corres, J.M., 55 N
Nizar, Nina Naquiah Ahmad, 245
E Núñez Carmona, Estefanía, 179
Eichberger, B., 1
P
H Prucnal, Paul R., 273
Haji-Sheikh, Michael, 157 Pulvirenti, Andrea, 229
Harun, Ahmad Nizar, 137
Hashim, Dzulkifly Mat, 245 R
Hideo Kobayashi, 303 Rokhani, Fakhrul Zaman, 245

I S
Ikezawa, Satoshi, 21 Sairin, Masyitah Amat, 245
Ismail, Alyani, 245 Sberveglieri, Veronica, 179, 229
Shuk, P., 81
J Soprani, Matteo, 179
Jiaming Li, 39
Jingyi (Jenny) Sun, 273 T
Joshi, Keyur H., 205 Taherinezahdi, Mansour, 157
Jun Yamamoto, 21 Toshitsugu Ueda, 21

© Springer International Publishing AG 2017 323

S. Mukhopadhyay et al. (eds.), Sensors for Everyday Life, Smart Sensors,
Measurement and Instrumentation 23, DOI 10.1007/978-3-319-47322-2
324 Author Index

W Y
Wall, Josh, 39 Ying Guo, 39
West, Sam, 39
Z
X Zinger, Donald, 157
Xie Li, 109