Mastersizer 3000 user manual

www.malvern.com
3000

User manual

Malvern Instruments Limited

Enigma Business Park
Grovewood Road, Malvern
Worcs, WR14 1XZ, U.K.
Tel: +44 (0) 1684 892456
MAN0474
Fax: +44 (0) 1684 892789 MRK1738-01
Mastersizer 3000
User Manual
MAN0474 Issue 1.0 October 2011
Copyright 2011 Malvern Instruments Ltd.

Malvern Instruments pursues a policy of continual improvement due to technical development. We

therefore reserve the right to deviate from information, descriptions, and specifications in this
publication without notice. Malvern Instruments shall not be liable for errors contained herein or
for incidental or consequential damages in connection with the furnishing, performance or use of
this material. No reproduction or transmission of any part of this publication is allowed without the
express written permission of Malvern Instruments Ltd.

Head office:

Malvern Instruments Ltd.

Enigma Business Park,
Grovewood Road,
Malvern,
Worcestershire WR14 1XZ
United Kingdom.

Tel + [44] (0)1684-892456

Fax + [44] (0)1684-892789

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countries, and are owned by Malvern Instruments Ltd.

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 Table of Contents

Table of contents
Part 1 - Operators Guide

Introduction to this manual

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1
About this manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1
Access to the instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-2
Assumed information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
Where to get help . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-4

Introducing the Mastersizer 3000

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
About the Mastersizer 3000 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-2
Typical systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Optical unit components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-7
End panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-9
Cell components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-10

Software overview
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
Powering on and starting the software . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2
Software user interface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-3
Customising the software interface . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-11
Maintenance utilities . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-15

Making measurements
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1
Measurement types and process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-2
Measurement prerequisites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-2
Making SOP measurements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-4
Making manual measurements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-14
Measurement settings reference . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-23

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Table of Contents

Viewing measurement results

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1
Working with measurement files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-2
Analysis report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-9
Fundamental concepts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-12
Optical models . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-19

Part 2 - Supervisors Guide

Sample preparation guidance

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-1
Sample preparation flow chart . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-2
Representative sampling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-3
Considerations for dry samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-4
Considerations for wet samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-5
Symptoms of poor sample preparation . . . . . . . . . . . . . . . . . . . . . . . . . 6-10

Reporting
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-1
About reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-2
Viewing and using reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-2
Creating and editing reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-8

System security
About security . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-1
Activating security . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-1
Software licensing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-2
Audit history . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-4

Advanced features
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-1
Doing more with SOPs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-2
Editing results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-6
Exporting data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-7

Page 2 Mastersizer 3000

 Table of Contents

Part 3 - Appendices

Setup reference
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-1
Installing the software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-1
Making connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-2

Specifications
Optical unit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-1
Chemical compatibility . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-2
Regulatory Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-3

Mastersizer 3000 Page 3

Table of Contents

Page 4 Mastersizer 3000

Part 1 -
Operators Guide
 1

Introduction
to this manual
Introduction
This manual covers the operation of the Mastersizer 3000 particle characterisation
system. The instrument measures the size of particles contained within a sample,
presenting data according to the users needs.
This user manual is a companion to the Mastersizer 3000 Basic Guide, which
gives Health and Safety, maintenance, troubleshooting and other vital information
which all users must read.

About this manual

The manual is divided into the following three sections.

Part 1 Operators guide

The Operators guide contains all the information required by an operator:
An overview of the Mastersizer 3000 hardware and software.
A guide to making measurements and how to read the results.

Part 2 Supervisors guide

The Supervisors guide concentrates on administration and extension of the sys-
tems functionality. Topics covered are:
Sample preparation guidance.
Reporting - creating and editing reports.
System security.
Advanced features.
The supervisor should also read the Operators guide.

Mastersizer 3000 Page 1-1

1 Chapter 1 Introduction to this manual

Part 3 Appendices
Appendix A gives setup reference material and Appendix B details specification
and regulatory information.

Warning!
The instrument and the samples to be measured may be hazardous if mis-
used. Users must read the Health and Safety information in the Basic
Guide before operating the system.

Access to the instrument

This manual refers to the various people who will have access to the instrument, as
follows.

Malvern Instruments personnel

Malvern Instruments personnel (service engineers, representatives etc.) have full
access to the instrument and are the only people authorised to perform all service
procedures that may require the removal of the covers.

Warning!
Removal of the covers by unauthorised personnel will invalidate the war-
ranty of the instrument. Unless advised within the content of this manual,
only Malvern Instruments trained personnel are permitted to remove the
main cover of any part.

Supervisor
The supervisor is the person responsible for the management and safety of the
instrument and its operation. The supervisor is responsible for the training of the
operators. The supervisor can perform all user maintenance routines identified in
the Basic Guide and within this manual.

Warning!
Under no circumstances should the supervisor or an operator remove the
main cover of the instrument.

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Introduction to this manual Chapter 1

Operator
An operator is a person trained in the use of the system. The operator can perform
all user maintenance routines identified in the Basic Guide.

Warning!
Failure to follow these guidelines could result in the emission of laser radi-
ation. Laser radiation can be harmful to the body and cause permanent eye
damage.

Assumed information
To make full use of this manual, the user should understand the following points.

Naming convention
Within this manual:
The Mastersizer 3000 is referred to as the optical unit or the instrument.
The sample dispersion units are referred to as the Hydro MV or the Aero
S, or as the dispersion unit. Wet dispersion units refers to the Hydro LV,
MV and EV. Dry dispersion units refers to the Aero S.
The combination of the optical unit, one or more dispersion units and the
computer is referred to as the system.

Ribbon commands
The control ribbon in the Mastersizer software is divided into tabs:

The first button on this tab bar is referred to as the Application button and has a
similar function to the File menu on older systems.
Ribbon commands are referred to in this manual in the form: ribbon tab selection,
followed by option. For example, Home-Manual Measurement describes click-
ing the option shown below which is found on the Home tab:

Whenever a ribbon option also has a sub-item this is shown as Home-Print-Print

Report. Ribbon commands are always shown in bold text.

Mastersizer 3000 Page 1-3

Chapter 1 Introduction to this manual

Where to get help

This section describes the available sources of information on the system. The pri-
mary sources of information on the system are instrument and accessory manuals
and the softwares help system. The manuals give an overview of the system as a
whole, while the online help system gives more detailed information on the Mas-
tersizer software. Some features are described in both the manuals and Help sys-
tem.

Manuals
The following manuals are available for the Mastersizer 3000:
Basic Guide
A concise yet essential guide that provides an introduction to the system and its
usage covering Site requirements, Health and Safety and an instrument and
accessory overview. Finally a brief guide to making a measurement and view-
ing the results is included.
User Guide
The primary source of information about the Mastersizer 3000 hardware and its
use. See About this manual earlier in the chapter.
Dispersion unit guides
Separate guides are supplied with both the Hydro and Aero dispersion units. These
provide essential information on the connection, operation and maintenance of the
dispersion units.

Help System
Each key software window has a Help button giving information specific to it.
Additional Info Tips are also available whenever is shown - simply move the
mouse pointer over this icon to see a relevant tip.

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Introduction to this manual Chapter 1

Technical support
Malvern Instruments offers several methods of technical support, which are
described in this section.

Email support

Note
This is the primary support method only use the other methods if this is
not available at your location.

Customers with internet access should use the Contact Malvern

feature in the softwares Maintenance window. This is described
fully in Chapter 3. This feature ensures that our support team have
all the relevant information about your system.
If you do not have internet access, contact your local Malvern Instruments repre-
sentative - details of all local telephone numbers are available at www.malvern.com.
Always quote the following information:
Model and serial number of the instrument. The serial number is shown
on the Mastersizer software status bar.
The software and firmware version. To find this select Tools-Mainte-
nance in the software and then examine the System information section -
alternatively, move the mouse over the instrument status bar icon. The Appli-
cation Version is the main firmware version number to note.

Additional support
Contact the International Malvern Helpdesk if the local Malvern Instruments
representative is not available:

Telephone: +44 (0)1684 891800 or email: [email protected].

Note
This help line is primarily English speaking.

Remote support
Malvern Instruments offers a remote support service, delivered by an internet con-
nection. Benefits include fast and efficient fault diagnosis, as well as reducing
downtime and costs.

Mastersizer 3000 Page 1-5

Chapter 1 Introduction to this manual

Malvern website - www.malvern.com

The Malvern Instruments website offers a comprehensive range of particle charac-
terisation resources for use by customers 24 hours a day, seven days a week.

Page 1-6 MAN 0474

 2

Introducing the
Mastersizer 3000
Introduction
This chapter provides information about the Mastersizer 3000 hardware and iden-
tifies all major features of the system.
The following topics are covered:
A description of the purpose of the instrument and its accessories.
A hardware overview of a typical wet and dry system.
Detailed reference on the physical parts of the optical unit.
Information about the parts of the cell, including how to insert and remove it.

Note
Hardware maintenance for details on how to maintain the hardware,
please refer to the Basic Guide and the separate dispersion unit guides.

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2 Chapter 2 Introducing the Mastersizer 3000

About the Mastersizer 3000

The Mastersizer 3000 is comprised of the main optical unit, one or more dispersion
units and a measurement cell. Commonly, a dispersant such as de-ionised water is
also connected directly to the dispersion unit.

Optical unit
The main optical unit, sometimes referred to as the optical bench or just the instru-
ment, is the core of the Mastersizer 3000 system. In its simplest terms, its purpose
is to transmit red laser light and blue light through a sample and then use its detec-
tors to generate data about the light scattering pattern caused by the particles in the
sample, which can be interpreted by the Mastersizer software to provide accurate
particle size information.

Dispersion units overview

There are two types of dispersion unit: wet and dry. Wet units (Hydro MV/LV/
EV) control the dispersion of a sample suspended within a liquid dispersant. The
function of the dry unit (Aero S) is to ensure that a dry sample is dispersed and
evenly fed to the measurement cell within a continuous stream of air.

Measurement cell
The cell is the interface between the dispersion unit and the optical unit. The sam-
ple is routed between measurement windows in the cell so that the laser can pass
through it in order to make a measurement.

Computer (Mastersizer software)

At the heart of the system lies the Mastersizer software, which runs on a computer.
This application controls the optical unit and dispersion unit hardware, and also
processes the raw data gathered by the system, providing flexible data analysis and
reporting features.

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Introducing the Mastersizer 3000 Chapter 2

Typical systems
Wet dispersion
A wet system consists of the optical unit and either the Hydro LV/MV or EV dis-
persion unit. These dispersion units are designed to circulate a liquid sample
through the Mastersizer 3000's measurement cell. Many materials need to be meas-
ured as wet dispersions. Typically these are materials that are used or produced wet
in the manufacturing process or need to be dispersed in a liquid in order to achieve
reproducible dispersion.

Hydro LV/MV
The Hydro MV and LV units are designed to create a suspension of particles in
water or other liquid media. The Hydro LV can handle a liquid volume of 600ml,
whereas the Hydro MV unit has a volume of 120ml. Both can be configured to
automatically deliver liquid dispersants and also dispose of the sample following a
measurement. This enables the cleaning and filling of the units as part of an SOP.
The large capacity of the Hydro LV makes it ideally suited to the measurement of
samples which have very broad size distributions or contain large particles. In some
cases, sample materials are not plentiful and the MV's smaller volume sample dis-
persion unit is a sensible choice to minimize sample and dispersant consumption
while retaining the benefits of totally automated sample dispersion and measure-
ment.

Hydro EV
In the mineral, chemical, metal powder refining and cement industries, measure-
ments of larger sample volumes are often most appropriate for QC of the manufac-
turing process and finished product. The large capacity of this unit makes it ideally
suited to the measurement of such samples as well as larger materials having broad
size distributions.
The Hydro EV is a wet dispersion unit designed to circulate a liquid sample held
within a standard laboratory beaker through the Mastersizer 3000's measurement
cell. As such the filling and emptying of this unit is a manual process.

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Chapter 2 Introducing the Mastersizer 3000

The following illustration shows a typical wet dispersion unit installation:

3 1 2 4

ill 8620
This shows:
Optical unit (as described in the next section) measures the sample using
red and blue light wavelengths.
Dispersion unit (in this case the Hydro LV) circulates the sample through
the cell
Wet cell sample flows through the air cell so that it passes through the
instruments laser path.
Computer running the Mastersizer software this controls both the opti-
cal unit and the attached dispersion unit, as well as processing and presenting
the measured data.
Other wet dispersion units include the Hydro MV and Hydro EV.

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Introducing the Mastersizer 3000 Chapter 2

Dry dispersion
A dry system comprises of the main optical unit plus the Aero S dispersion unit.
The Aero S is designed for providing an even circulation of dry powder throughout
Mastersizer 3000 measurement cell.
Direct software control over the feed rate and air pressure is provided, which ena-
bles flexible control of both the sample throughput and dispersion. The unit can be
controlled either independently of measurement or from within a manual/SOP
measurement. The following illustration shows a typical dry dispersion unit instal-
lation:

4 5 2 3 1

ill 8652
This shows:
Optical unit (as described in the next section) - measures the sample using
laser and blue light detection.
Dry dispersion unit (in this case the Aero S) - circulates the sample through
the cell.
Dry cell - sample flows through the air cell so that it passes through the instru-
ments laser path.

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Chapter 2 Introducing the Mastersizer 3000

Vacuum unit removes the sample from the cell exhaust once it has been
measured.

Ancillary switching unit an external control accessory that is used to

switch on the vacuum unit required for the sample extraction during each
measurement.

Computer running the Mastersizer software (Not shown) this controls

both the optical unit and the attached dispersion unit, as well as processing and
presenting the measured data.

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Introducing the Mastersizer 3000 Chapter 2

Optical unit components

This diagram shows the optical unit, the main component of the Mastersizer 3000
system. The unit directs red and blue light through the sample and then collects the
light scattered by the particles within the sample using a set of light-sensitive detec-
tors. This data enables the system to calculate particle size:

3 6 4 1

5 7 8 9 2
ill 8622
The optical unit comprises:
Optical unit
Cell (in this example, the wet cell). The following types of cell are available:
wet - for Hydro units and dry (sometimes known as the air cell) - for use with
the Aero S unit.

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Chapter 2 Introducing the Mastersizer 3000

Instrument status LED the status is indicated as follows: Standby (i.e.

powered on, but not making a measurement): pulsating dim; Active (i.e. mak-
ing a measurement) - constant bright; Error - flashing bright.
Cell bay holds the cell securely in the instrument so that sample passing
between the cell windows can be analysed by the optical units laser beam.

End panel provides the communication connectors for the optical unit as
well as the power connection and switch. See Appendix A for further connec-
tion reference.

Protection window stops dust/dirt entering the system. Clean this window
periodically. See Appendix B for more information on cleaning the protection
window.

Adjustable feet it is important to ensure that the instrument is levelled on

the bench - adjust the feet individually in order to accomplish this.
Drain allows any spillages in the cell area to exit onto the laboratory bench.

Tube/cable routing neatly routes all connection pipes and cables under-
neath the instrument.

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Introducing the Mastersizer 3000 Chapter 2

End panel
The end panel of the instrument provides the communications and power connec-
tions.

1
2

ill 8623

Power switch press once to power on the unit, press again to power off.
USB provides data communication with the PC. For best performance con-
nect to a high speed USB port on the PC:
CAN 1-3 supplies power and data communication to the dispersion unit.
Power input input for 24V power supply unit.

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Chapter 2 Introducing the Mastersizer 3000

Cell components
The following illustration shows the key parts of a wet cell for a more detailed
description of both the wet and dry cells, refer to the Hydro or Aero Dispersion
Unit Guides respectively:

1 2

6
3

ill 8625
Cell eject button ejects the cell from the cell bay locking mechanism so that
it can be withdrawn from the cell bay.
Cell handle only lift the cell by this handle.
Sample output (blue) connected to the sample in (blue) on the dispersion
unit.

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Introducing the Mastersizer 3000 Chapter 2

Temperature regulator throughput provides throughput connections to

a water jacket within the cell. This allows an (optional) heater/chiller to regu-
late the sample temperature to help minimise the effect of ultrasound heating.
Sample input (yellow) connected to the sample out (yellow) on the disper-
sion unit.
Cell windows sample passes through the window and is measured by the
system. Cell windows should always be kept clean to ensure accurate measure-
ments - see the Hydro Wet Dispersion Units Guide.

Inserting and removing the cell

Always follow this process when inserting or removing the cell from the instru-
ment. This section assumes that all relevant tubing connections between the dis-
persion unit and cell have already been made. Refer to the dispersion unit manuals
for verification of these connections.

Inserting the cell

1. Lift the cell by its handle .
2. Insert cell into the instrument as shown in the illustration on p. 2-7.
3. Do not force the cell into the instrument - only slide it into the cell holder until
it stops.
4. The cell now automatically locks into place within the cell bay.

Removing the cell

1. Press the cell eject button to eject the cell from the cell bay.

Caution!
Do not try to remove the cell from the cell bay without first pressing the
cell eject button as this could damage the locking mechanism.

2. Withdraw the cell from the instrument using its handle in the direction
shown in the illustration on p.2-7.

Note
If the cell is raised and lowered too many times in a short period, the firm-
ware will lock the cell in place for a period of time before it can be ejected
again; this is to prevent damage to the locking mechanism.

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Chapter 2 Introducing the Mastersizer 3000

Page 2-12 MAN 0474

 3

Software overview
Introduction
The Mastersizer software serves several key functions: it controls both the optical
unit and the dispersion unit; it allows users to create and edit measurement files; it
enables users to run manual or SOP measurements on both wet and dry samples,
and finally it provides access to powerful reporting and data analysis features.
This chapter gives details on the following:
Powering on and starting the software.
Description of the software user interface.
Customising the software interface.
Maintenance utilities.

Note
This section provides a description of the key elements of the software
only. For information on how to run a measurement, see Chapter 4.
Some advanced features of the software are also detailed in the Supervisors
section of this guide and reference information for all features is provided
in the Help system.

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3 Chapter 3 Software overview

Powering on and starting the software

1. Ensure that the optical unit, dispersion unit and computer are connected (con-
nection reference is given in Appendix A).
2. Power up the computer and printer (if available) by following the instructions
in the manuals supplied.
3. Connect the optical units power supply to the mains power supply.
4. Press the on/off switch on the instruments side panel once to power on.
The blue indicator on the top of the instrument illuminates, together with the
blue indicator on the front of the dispersion unit, which pulsates to indicate
that standby mode is active.
5. Log in to the computer that is connected to the instrument and start the Mas-
tersizer software by double clicking on the Mastersizer 3000 desktop icon.

6. The main Mastersizer 3000 software window is now displayed.

A correct connection to the instrument shows both the instrument and
accessory name in the status bar:

If the instrument is not connected correctly, the status bar indicates:

If this is the case, check the instruments connection to the USB port on the
PC and the power connections to the instrument.

If the dispersion unit is not detected, the following is shown:

If this is the case, check the connection from the instrument to the dispersion
unit. Also, a blue pulsating power light on the dispersion unit indicates that it is
connected correctly to the instrument.

Note:
Before using the instrument to measure a sample, wait for 30 minutes for
the laser to stabilise.

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Software overview Chapter 3

Software user interface

The main software window, with a measurement file loaded, is shown as follows:

5
6

Ribbon selector tabs provide quick access to the different control ribbons.
The Application button (leftmost) gives quick access to file, print and soft-
ware options (including security) as well as software version information.
Control ribbon single-click access to key software functions.

Record View panel lists all measurements within the active measurement
file. Multiple measurement files can be opened simultaneously, which are then
accessible by different tabs within the Record View.
Reports tabs provides access to reports on the currently selected record. The
reports shown are a function of the currently selected workspace - this is dis-
cussed later in this chapter.
Data Quality tab provides guidance on the measurement quality and dis-
plays a simple pass/fail data report based on selected models, together with tips
on how to improve the measurement. Described further later in this chapter.
All files tab view all records from all open measurement files in a single tab.

Status bar shows the instrument mode, connected user, 21 CFR status,
notifications (see later in this chapter), connected accessory type and the instru-
ment connection status (as well as its serial number when connected).

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Control ribbons
Control ribbons provide quick access to key software functions.
To select an option, click on the appropriate direct-access button, for example
Extract SOP.

If you contract the software window horizontally, the individual ribbon options are
grouped under a single icons instead. The ribbon then operates in a similar manner
to menus in that the group must be selected initially to reveal the sub-items, for
example Result-Extract SOP.

To select a different control ribbon, click the selector tabs above the ribbon
(Home, View Tools or Audit).

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Record View tab

The Record View allows you to view and edit the records contained in Master-
sizer 3000 measurement files. It is also possible to open files that were created by
Mastersizer 2000 instruments, but not edit them. Mastersizer measurement files
consist of a number of individual measurement records.

Each open measurement file is given a tab in the Record View: click one of
these tabs to show all of the records contained in that measurement file.

Note
You can open as many measurement files as required, and also combine
results, using All Files, to view all records within a single tab, making
graphical data overlay possible. See Merging records in Chapter 5 for
more information.

Each measurement record consists of a set of parameters, one of which is shown in

each column. (It is possible to edit the selection of parameters that are displayed if
required.) Many parameters contain numerical data measured by the system, but
some contain other information, such as Scattering Model, Accessory Name
and so on. Some parameters also answer simple yes/no questions, such as Has
Background Alarm Triggered? Items like this are checked if affirmative.

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Tip
To copy the data shown in the record view to the clipboard, select records
from the record view and then choose Clipboard-Copy on the Home
ribbon. This data can then be pasted into any other compatible Windows
application, for example, Word or Excel.

Powerful analysis features also allow records to be sorted, grouped and filtered so
that users can focus on only those records that are of relevance to their application.
See Chapter 5 for more information on grouping and filtering.

Editing which parameters are displayed

To choose different columns of data to display in the Record View:
1. Right click on a column header and choose Column Configuration.
2. Then, from the Parameter Selection window, select items in the Available
column and add them to the Selected column. Use the Search feature in this
window to quickly find a parameter.
3. Click OK to complete the process.

Sorting on a parameter column

Click the column header. Click the header again to reverse-sort based on that selec-
tion - sorting is either alphabetical, numeric or boolean, depending on the parame-
ter selected.

Locked measurement files

Any tab indicated with a padlock icon is a read only file that cannot be edited.
This is the default status for any Mastersizer 2000 files that are opened with the
Mastersizer 3000 software.

Selected Records Information

At the bottom of the Records view a summary is provided that details the number
of records currently selected within each measurement file.

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Reports tab
Reports are displayed automatically whenever you select a record, or number of
records, from the Record view (assuming that the selected view is showing the
Reports tab).

Note:
For detailed information on the process of viewing, editing or creating new
reports, see Chapter 7 Reporting.

Data Quality tab

The Data Quality tab presents a custom analysis of any records selected in the cur-
rent measurement file.
1. Select the records for which you wish to view a data quality report.
2. Click the Data Quality tab (next to the Reports tab) and then choose the
analysis type from the drop down menu:

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The display is updated to show a quality review of each record selected. Click
to toggle whether items that have passed or failed are displayed.

Items that have passed the quality check are shown .

Items that have failed the quality check are shown .

If the Record View is selected again, and different records are then selected, the
information shown on the Data Quality tab remains the same unless the option to
Refresh the data quality results is selected from within the Data Quality tab.

Workspace Viewer
This section describes the purpose of workspaces and the Workspace Viewer.

Note
See the Help system for information on the Macros tab.

Workspaces are a collection of settings that define the information presented in the
Reports and Record View, as well as which folders the system uses for accessing
SOPs, measurement data and export data.
Each user can access both a Private or Shared workspace, both of which are config-
urable. This makes it easy for an individual to optimise the software for their own
use, with the Private workspace, or to collaborate better across an organisation
using a Shared workspace. The latter is particularly useful within quality con-
trolled environments.
The following settings and data are associated with the workspace:
SOPs and SOP Templates presented to users (i.e. their file locations).
Record parameters shown in the Record View.
Reports listed in the Reports view (see also Chapter 7).
Measurement data file location.
Exported data and Export Templates file locations.

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Note
Any of these items that are created when the Shared workspace is active
will be available to all users of that system (providing their security privi-
leges allow them access to these functions). If the Private workspace is
selected, these items are only available to the current user.

Selecting the workspace

Reveal the Workspace Viewer panel by clicking its vertical tab on the right of the
window. (Keep the Workspace Viewer visible by clicking the pin icon at the top of
the panel .) To select the workspace click the button at the top of the Work-
space Viewer panel:

Any work subsequently performed on the system will now use the selected work-
space both to save data and to access settings.

Recent measurement files

This is a simple list of the last five measurement files that have been accessed
within the selected workspace.

Record and reports views

The Record parameters shown in the Record View and the Reports listed in the
Reports view are controlled using the Record and reports views section of the
Workspace Viewer.
You can add as many different views as required these are stored within either of
the currently selected workspaces.
To add a new view:
1. Click Add new view from the Workspace Viewer panel.
2. Enter a View name in the Result View Properties window.
3. Click Configure record view columns to show the parameter selection win-
dow. Select the required parameters and then click OK.
4. Click Configure report selection to display the Report Selection window,
select the required reports and tab order, and then click OK.

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5. Once you have added new views, make them the active view by clicking on
them - an arrow is shown next to the selected view name.


The reports and the Record View are updated immediately.
6. To edit or delete a view, first select it and then move the mouse pointer over
the view name again to reveal the Edit and Remove icons.

Shortcuts
The shortcuts listed are links to Mastersizer system folders and provide quick
access to all of your SOPs, measurement files and exported data.
The folder that is linked to from this panel is specific to the selected workspace.
Clicking on a shortcut to a folder will open that folder within Windows Explorer.
If the Private workspace is selected, the folders all stem from:
C:\Users\YOURNAME\Documents\Malvern Instruments\Mastersizer
3000\Workspace\

If the Shared workspace is selected the folders stem from:

C:\ProgramData\Malvern Instruments\Mastersizer 3000\Workspace\

Creating shortcuts
Shortcuts are an easy mechanism for users to set-up a set up links to folders, e.g. on
a network, that can be shared between all users on that PC.
To create a shortcut: Create new shortcuts to files/folders by dragging them into
the Shortcuts panel from Windows Explorer. Shortcuts to web sites can be added
by dragging a bookmark from Internet Explorer into the Shortcuts panel.

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Customising the software interface

In addition to the options available as part of the Workspace specification, several
further features provide control over how the software is presented to the user.

Options
Choose Options from the Application button menu to display the Mas-
tersizer 3000 Options window. Then click the required link on the left to view its
corresponding settings.

General Preferences
Click General from the Options window to choose the following settings:
Show settings when running manual measurements this automatically
displays the measurement settings window whenever a manual measurement is
initiated. This can be useful during method development where the user needs
to switch back into the record view after making each measurement and then
make slight alterations to the measurement settings for the subsequent meas-
urement. If this option is de-selected, the settings are still available to the user
by clicking on the Manual Measurement window.
Show edited records at the same level as original records in the record
view - rather than stagger edited records as sub-items of the records from
which they originate, they are displayed at the same level in the tree. This gives
the software the same layout/behaviour as the original Mastersizer 2000 soft-
ware.

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Themes
Several themes are available which modify the colour settings of the user interface.
Click Theme from the Options window and then select a scheme that suits your
preference by clicking Use this theme.

Graphs
Choose Graphs from the Options menu to access further options that relate to
the presentation of graphs:
Line weight specify the line weights (Normal, Light or Heavy) to be used in
all graphs.
Colour scheme choose from one of several colour schemes. The Master-
sizer 2000 theme emulates the appearance of the Mastersizer 2000 graph col-
our scheme, Greyscale is optimised for printing on a monochrome printer,
High Contrast provides better on-screen visibility.

Save/Restore My Layout
Save My Layout is a simple feature that allows you to store the exact position of all
elements of the Mastersizer 3000 interface. This could be useful in situations
where you have optimised the interface for your current analysis process.

Positioning elements within the user interface

To reposition items - drag any of the following panels to another position within
the main window: Record View, Data Quality, Reports and Workspace Viewer.
The following tool is shown on the screen when dragging:

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This indicates that pre-set positioning options are available for the element. Whilst
still holding down the mouse button, move the mouse pointer over one of the
direction arrows in this tool - a shaded box is shown indicating how the element
will be placed. Release the mouse button to place the element.

Saving or restoring the window layout

To save commonly used panel and window arrangements for future use:
1. Position any of the panels of the software as desired, for example, the Work-
space Viewer, Record View etc.
2. Click Save My Layout on the View ribbon.
3. The New Layout File window is displayed enter a name for the layout (all
layouts have the .mlay file extension) and click Save.
4. To access a previously saved layout, click Restore My Layout and then locate
the relevant .mlay file.

Note:
By default the system initially returns to the window layout that was pre-
sent when the software was last closed.

Predefined Window Layouts

The Predefined window layouts allow to you quickly select from a number of
optimised panel arrangements within the Mastersizer user interface.
From the Predefined window layouts group in the View ribbon, select the
required layout.

Quick Access Toolbar

The Quick Access Toolbar provides an alternative method for accessing com-
monly-used functions.
1. To add any ribbon function button to the Quick Access Toolbar, right-click it
and choose Add to Quick Access Toolbar. The button is now additionally
displayed (in reduced form) in the title bar of the software:

In this example, the Manual measurement, Save and 2-pane tabbed buttons
have been added to the Quick Access Toolbar.
2. To remove the button, right-click it and choose Remove from Quick Access
Toolbar.

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Maintenance utilities
The Maintenance window gives access to various background information about
the system that can be useful as part of an ongoing maintenance schedule or in the
process of contact with the Malvern Instruments Help Desk.
Choose Tools-Maintenance from the ribbon to display the Maintenance
window:

The window is broken down into the following sections:

Notifications
Notifications are brief notes that indicate any errors, problems or necessary reme-
dial/investigative action that may be required in order to keep the system function-
ing correctly. Follow the advice given in any notifications and then remove them by
clicking Clear All.
The Status bar also provides a visual reminder that notifications are available:

Click the Notifications icon on the status bar to view the Maintenance window.

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System information
The main purpose of the system information area is to display details about the
software, operating system and hardware connected. This information must be
passed to the Malvern Instruments Helpdesk whenever you log a support call. To
send this information to Malvern Instruments:
If you have email software on the Mastersizer computer:
Click Contact Malvern, complete the form and then click OK. Your default
email software then starts and an email is generated containing the relevant.
If you do not have email software on the Mastersizer computer:
Click Save text report to save a text file containing this information. Then
copy this information onto a data stick and transfer it to a computer that has an
email connection in order to attach the file to send to Malvern Instruments.
Print the information using the Print option and then refer to this information
if you wish to contact the Helpdesk via telephone.

System usage
The system usage section provides details on the total Running Time of the instru-
ment and any connected accessory. Additionally details are provided on the run-
ning time of the accessory stirrer running time and ultrasound if applicable.

System health checks

The system health checks section gives a list of any maintenance issues with either
the optical unit or accessory that may require user intervention.

Logs
The Logs section contains links to all the logs generated in the previous 24 hour
period. After 24 hours, if no further log files have been generated, only the last log
file generated is retained. Log files contain no data that is of direct use to users, but
may be requested by the Malvern Helpdesk when trying to resolve any issue. Either
click the links to open the file, enabling the text to be copied into an email, or
choose Open folder and then locate the log file you wish to send.

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 4

Making
measurements
Introduction
The Mastersizer 3000 is capable of measuring samples dispersed in a wet or dry
medium, either manually as a one-off (or for developing an SOP method) or by
utilising predefined settings stored within an SOP file.
This chapter is the main reference for the measurement making process and
includes sections on:
Measurement types a brief background on the overall process of making a
Mastersizer measurement.
Measurement file basics how to create and open measurement files.
Making an SOP measurement includes how to create SOPs as well as the
steps involved in running an SOP.
Making a manual measurement the basic steps involved in manual meas-
urement with a wet dispersion unit.
Measurement settings reference detailed reference on all measurement
settings available to both SOP and manual measurements.

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4 Chapter 4 Making measurements

Measurement types and process

The Mastersizer 3000 is capable of making two types of measurement:
Manual measurements all of the measurement settings are specified before
the measurement and some further user input is required during the running
of the measurement. The measurement process is also split into key stages,
which are paused after the completion of each stage.
Manual measurements tend to be used for one-off measurements or as part of
method development (i.e. establishing the optimal settings for measuring the
sample and then saving into an SOP file).
Standard Operating Procedure (SOP) measurements most of the
measurement settings are stored within an SOP file which has been previously
created by the user. Once an SOP has been initiated, the measurement
sequence requires less user intervention than a manual measurement.

As SOPs lock-down most of the measurement settings they improve consist-
ency and provide greater repeatability; features that are important in quality-
controlled environments.
The process of both measurement types is broadly as follows:
1. Power on the system and create a measurement file.
2. Specify the measurement settings for a manual measurement or SOP.
3. Run the measurement.
4. Check the results, looking for any problems.
5. Clean the system.

Measurement prerequisites
Note
The instrument and accessory must have been connected and set up in
accordance with the guidance in the Mastersizer Basic Guide and the dry
or wet dispersion unit guide. This section assumes all appropriate connec-
tions have been made.

Before a measurement can be made, the instrument must be powered up and a

measurement file must be created. Measurement files contain all data acquired by
the Mastersizer during a measurement. Each measurement file can contain a num-
ber of individual records.

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1. Switch on the optical unit. The pulsating blue light on the top of the instru-
ment indicates that it is on. Check also that the blue light on the dispersion unit
is pulsating - power to the dispersion unit is drawn from the instrument.

Note
Leave the instrument powered on for 30 minutes before making a
measurement to allow the laser to stabilise.

2. When 30 minutes has elapsed, switch on the computer, log in to Windows on

the PC and start the software by double-clicking on the Mastersizer 3000 icon
on the desktop:

Note
If, after successfully starting the Mastersizer software, any of the functions
described in the rest of this section are unavailable to you, this will be due
to your login credentials contact your system Supervisor for assistance.

3. Ensure that the status bar indicates that the instrument is connected correctly:

4. If the instrument is not connected correctly (i.e. if anything else is shown in the
status bar), refer to Chapter 3 for more information on how to fix this.
5. Create a new measurement file by selecting New-Measurement File from
Home section of the control ribbon:

Alternatively new measurements can be added to an existing measurement file.

6. Choose Save and then name the measurement file, for example Starter sam-
ple.mmes.

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Making SOP measurements

SOPs are predefined measurement sequences that can be used to both automate
and standardise Mastersizer measurements. Widely used in the pharmaceutical
industry to provide traceability, SOPs also provide non-pharmaceutical users with a
reliable means of automating measurements, ensuring that a wide selection of per-
sonnel can obtain consistent results regardless of familiarity with the instrument.
SOPs can control the configuration of the optical unit and the sample dispersion
unit, including the measurement parameters, timings, analysis models and other
specific set-up information. They can also be configured to prompt the operator to
perform specific tasks such as sample preparation steps.
The quality and value of an SOP depends on the quality of the method develop-
ment work on which it is based. A series of manual measurements is required to
establish the ideal parameters for use in an SOP. A number of standard SOP tem-
plates have been prepared in advance for typical measurements, which may be used
unchanged or as the basis for a new SOP.
The Mastersizer software's powerful SOP editing facility enables users to review
and refine SOPs as part of their ongoing quality control process.

Creating or editing an SOP

SOPs need to be created and saved before they can be used. To create a new SOP:
1. Select New-SOP from the Home ribbon. (To edit an existing SOP, choose
Open-SOP instead.)

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2. Select an SOP template from the list in the New SOP window or click the
From an existing SOP... button to locate an SOP in the file system that fulfils
(or is close to) your required criteria.
3. The SOP Editor window is now displayed as illustrated (the Material set-
tings are shown in this example):

4. Step through the SOP Editor by clicking the section titles on the left (Sample-
Identification, Sample-Material etc.) or clicking the Forward / Back arrows on
its toolbar.

Note
Complete each of the sections detailed in the Measurement Settings
Reference section in later in this Chapter.

5. When all the required settings have been specified, save the SOP by choosing
Documents-Save on the ribbon (or Save from the Application button menu)
and then giving the SOP a logical name.

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Running an SOP (Hydro units)

If you are using a wet dispersion unit (the Hydro LV/MV/EV) work through the
steps in the order given here. No manual control of the dispersion units is required
after loading the sample; the software controls all settings.
1. Select Run SOP from the Measurements section of the ribbon.
2. The SOP Selector window is shown, which initially presents all SOPs filtered
for the connected accessory (Accessory filtered).
Alternatively, click the All SOPs button to show those that are not specific to
the connected accessory.

Click on an SOP to display its properties in the bottom panel of this window.
3. After selecting an appropriate SOP, click OK.
4. The Measurement Display window is shown.

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The progress status bar at the top of the window reports both the current status
and what to do next.

5. Click the Start button to Initialise the instrument. If specified in the

SOP settings, the system prompts the user to enter/confirm sample documen-
tation details. Following this stage. the system automatically moves to the
Measure Background stage and measures both the red and blue light values
of the background.

Note
To stop both the SOP and the accessory during a measurement, click the
Abort button . This all stop command should only be used when
a problem is suspected - this is because the sample will stop circulating,
which could affect further measurements if the sample is not then refilled.

6. When the Measure Background stage is complete, the SOP pauses. The sys-
tem now requests that you add sample - do this until the Obscuration bar
indicates about 10-20% for a wet dispersion unit. (This is a rough guide only
as this setting is highly sample-dependent - refer to the Help system for more
guidance.)
7. Click Start again. The measurement now commences, measuring first the red
and then the blue light values. The SOP may make a number of measurements
before completion, depending on the Number of measurements specified in

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the SOP settings. When complete, the Trend view is updated with the new
measurement figures:

8. Complete the measurement by closing the SOP Measurement window.

9. The results are now presented in the Record View.

More about the Trend view

The Trend view is a powerful analytical tool that shows record data in a graphical
format as soon as it has been measured by the system.
The main purpose of the default view is to indicate that sample measurements are
stable. For example, if the sample was slowly dissolving then the apparent sizes may
appear to be reducing. In many industries, measurement repeatability is quantified
by specifying a maximum Relative Standard Deviation (RSD) over a number of
measurements. The Trend view allows you to highlight a number of measure-
ments and display the RSD, and other statistics in real time. Any other parameter
can be added to the Trend view, for example to see how Ultrasound Power settings
are affecting the measurement.
By default, each measurements Dv10, Dv50 and Dv90 figure is shown, so it is very
simple to make a quick assessment of the result. The Dv50 category shows the
median particle size. Further statistics and measurement parameters can also be
viewed on the Trend view.
Once a number of measurements have been performed, it is possible to select mul-
tiple records in order to view combined figures for the range. It is also possible to
modify the data displayed on the graph, and add entirely new graphs with a differ-
ent focus of interest if required.

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This is an example of the trend view after four measurements have been made. The
currently selected range in this example includes just two records: Record Number
2 and 3 - the figures displayed in the coloured boxes relate only to those two
records.

Statistics shown in the live trend view

The live trend view identifies each line with a key, which shows statistical informa-
tion about the measurement:

The data shown relates either to the individual measurement or range of measure-
ments selected by the user. The default view shows particle size statistics. Trend
plots can be configured to show any parameter the statistics shown on a plot line
relates to a single parameter only.
Main figure the actual size measurement (m) for the single base record
that is currently selected (Dv10 - blue, Dv50 - green, Dv90 - red).
Av the average particle size (m) for the selected range.
RSD Relative Standard Deviation (%) for the selected range.
Min the minimum particle size (m) for the selected range.
Max the maximum particle size (m) for the selected range.
To modify which figures are shown in the Trend view:
1. Right-click anywhere on the trend graph and choose Statistics.
2. Select or de-select the items required.

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Tip
Click anywhere on the graph line to display data points - click again on the
line to remove them. Move the mouse pointer over a data point to display
its record number and size figure, for example 4, 891.09 indicates that
Record 4 has a measured size of 891.09m.

Selecting a range of records in the trend view

After running several measurements, just one record is selected. Initially this is the
last measurement made. This record is shown by a vertical hairline bar with the
record number indicated at the bottom - for example, . The vertical hairline bar
always shows the currently selected record.
To expand the range to incorporate more records, click the left or right
selection arrow buttons at the top of this bar. The bar expands to cover the
records selected:
Click and drag this header bar to the left or right to reposition the selection
within the range of records. Alternatively, right-click the trend graph and
choose: Statistics range and then select the number of records.
To contract the range, click and drag the left hairline bar that denotes the
initial record in the selected range. Alternatively, right-click on the trend graph
and choose: Statistics range and then select the number of records to include
in the selected range. If you have manually dragged the bar to cover a number
of records not listed in the Statistics range menu, Custom and the number
of records currently selected is displayed.
All numerical data then provided is the arithmetic mean of the currently selected
records, with the exception of the initial particle size figure, which is still the figure
for the single record.

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Adding further trend graphs

Add additional plots using the following method (note that the new plot needs to
be configured prior to making the measurement in order to display data):
1. Right-click on the trend graph and select Add above or Add below to add a
new plot.
2. Then choose parameters from the Parameter Selection window and click
OK.

(To remove the new plot, right-click it and choose Delete.)

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Running an SOP (Aero units)

The software controls most of the dispersion unit settings except the hopper
height, which is a manual adjustment. Work through the steps in the order given
here.
1. Open the Aero S sample area lid and set the hopper flow rate to an appropri-
ate gap level using the dial (marked from 0-4mm - refer to the Aero Series Dry
Dispersion Units Guide for more information):

D
A

ill 8655
2. Empty the sample into the hopper .
The mesh basket and ball bearings may be used on coarser samples to smooth
the flow of sample, breaking up any loose agglomerates before they fall into the
hopper.
3. Close the lid of the Aero.
4. Select Run SOP from the Measurements section of the ribbon.
The SOP Selector window lists all available SOPs.
5. Choose an appropriate SOP for the Aero dispersion unit (ensure also that the
SOP is optimised for the venturi type that is fitted to your Aero unit - either
stainless steel or ceramic venturi) and then click OK.

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The Measurement Display window shown below is displayed:

6. Click Start the SOP automatically aligns the optical system and then
measures the background using red and blue light.
7. After this, the sample tray starts vibrating and the SOP-specified air pressure is
applied. The overall rate at which the sample is fed into the cell is a function of
the combination of air pressure, vibration rate and hopper flow-rate setting.

Note
To stop both the SOP and the accessory during a measurement, click the
Abort button .

8. The SOP selected should be optimised for the dry dispersion unit and will only
make a measurement once the obscuration is within the specified range (1-10%
obscuration is the rough guide for a dry dispersion unit).
9. The results are shown immediately in the Trend view as they are gathered.
When all of the measurements have been made, the system pauses - optionally,
click Clean System on the top progress bar to initiate a cleaning cycle.
10. Complete the measurement by closing the SOP Measurement window.
11. The results are now presented in the Record View.

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Making manual measurements

In addition to SOP measurements, users can also make manual measurements.
This may be useful, for instance, when investigating the most appropriate method
for sample dispersion prior to setting up an SOP. This section provides details on
how to run a basic manual measurement.

Note
This process description assumes that a wet dispersion unit is connected to
the instrument.

The basic procedure is similar to that outlined in the SOP measurement section,
but requires the user to set up the measurement settings initially, and then manu-
ally initiate more stages during the live measurement process:
1. From the Home ribbon click Manual measurement from the Measure-
ments group. The Manual Measurement window is displayed, together
with the Manual Measurement Settings window:

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Making measurements Chapter 4

Note
This section now provides information on how to enter only some of the
key measurement settings - for complete details on all settings, see Meas-
urement settings reference later in this chapter.

2. Choose the Sample-Identification settings to record both the Sample

Name details and define any further information fields (for example, Notes)
that will help users to repeat the measurement at a later date.
3. Use the Sample-Material section to define the optical properties (the
Refractive index and Absorption index) of the new material. The material
may already be stored in the systems Materials database. Check this first by
clicking Browse database - select the material if it is present to automatically
add the RI and Absorption values to the measurement.
4. Use the Measurement-Duration section, shown below, to set up measure-
ment times for the red and blue measurements.

5. In the Measurement-Obscuration section define the lower and upper

obscuration limits - as a very rough guide, about 10-20% for a wet dispersion
unit and 1-10% for a dry dispersion unit.
6. Click OK to close the Manual measurement settings window.

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7. From the Initialise Instrument drop down menu, select Auto Alignment.

8. Click the Start button to initialise the instrument - when complete, the
system progresses to the Measure Background stage.
9. Filling and starting the dispersion unit:

Depending on the accessory that is currently connected, the control options
(shown in the panel on the right) will vary. For a wet dispersion, a steady circu-
lation of dispersant needs to be in place before adding the sample. To do this,
ensure the accessory is filled with dispersant - if using an LV/MV, click Fill in
the Dispersant section of the Accessory panel.

Note
See Controlling dispersion units (manual mode) later in this chapter
for more information.

10. When the accessory is full, set the Stirrer speed and start the accessory:
11. Click Start on the measurement progress bar at the top of the window. Both
the red and blue light values for the background are measured.
12. The system now requests the user to Add Sample - add small quantities of
sample to the dispersion unit until the obscuration is within range (10-20% in
the case of a wet dispersion). Refer to the Help system for more guidance. With
a dry dispersion, the system will skip this step.

Note
With dry dispersions, the whole sample is loaded into the hopper in the
Aero before the measurement process is started.

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13. Click Start again twice to begin the measurement. First the red and then the
blue light values are measured. When this is complete, the Trend view is
updated with the new measurement figures (see Running an SOP in this
chapter for more detailed information on the Trend view). The particle Size
Distribution graph is shown in the upper right panel. In the example shown
here, just a single measurement was specified in the manual measurement set-
tings.

14. Continue this final Measure Sample process as many times as required by
clicking Start again. To complete the measurement, just close the Manual
Measurement window. The new records are now added to the Record View.

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Controlling dispersion units (manual mode)

Use the Accessory controls panel from the manual measurement mode to con-
figure the currently attached accessory.

Normally, an SOP or Manual measurement controls the accessory's operation

within the context of a measurement. Alternatively, the Accessory controls panel
allows you initiate the current accessory before the measurement is actually made.
This is essential when observing the effects of variation to the accessory's settings
on the live Laser and Light Scattering panels, in order to optimise the sample's
concentration and circulation prior to making a measurement. This option could
also be used as part of a manual cleaning process.
To access the Accessory control panel: the instrument must be in Manual
Measurement mode, then click the Accessory controls tab on the right of the
Manual Measurement window.

Tip
The same controls are also available, when not making a measurement,
from the Active accessory control feature (choose Tools-Accessories
from the main control ribbon). This option could be useful, for example, if
you wanted to keep a sample in circulation whilst undertaking a report
analysis.

The options available on this panel depend on the connected accessory as follows:

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Hydro LV/MV
The accessory controls panel for the Hydro LV/MV is shown as follows (in this
example the dispersant has been filled):

Option Description
Stirrer Use the slider bar to set the RPM of the stirrer. In Manual
Measurement mode it is necessary to start the stirrer
manually before making the measurement. To initiate the
stirrer once the speed has been set, click the Start but-
ton. To stop the stirrer click the Stop button.
The green bar represents the user-requested speed. The
thin grey bar beneath this is the actual stirrer speed. There
will be a small lag as the actual speed adjusts to match
the requested speed.

The optimal stirrer speed is normally a choice between

stirring fast enough to ensure that all the sample is sus-
pended, but not so fast that bubbles occur. You can also
type directly over the RPM indicator to set a precise
value.
Ultrasound Choose an appropriate level of ultrasound for the sample
by moving the slider bar.

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Option Description
Enable pulsed In this mode, sonication is applied in pulses (with fixed
sonication duration on and off pulses). This option can be used in
combination with both continuous or timed sonication
mode. Specify the duration of on and off pulses by enter-
ing the required values (seconds) into the corresponding
boxes. This can prevent overheating of the sample, and is
also useful on fragile samples that could otherwise be
broken up by more aggressive ultrasonication.
Manual Select this option if you wish to start and stop the stirrer
manually for a period of time.
Timed Select this option to perform a precisely timed period of
ultrasound application. When Timed is selected, the timer
controls become available - click +/- to increase/decrease
the time period for which ultrasound will be applied.
Fill Fill the Hydro unit with dispersant. This function opens the
(dispersant) dispersant valve and then pumps dispersant into the unit
until the correct level is reached (detected by a sensor)
and then closes the dispersant valve. The tank indicator
next to this button shows full and empty respectively:

Empty Empty all dispersant (and sample) from the Hydro unit.
(dispersant) This function opens the drain valve and initiates a pump-
ing sequence - the process stops when the unit is empty
and then closes the drain valve.
Drain valve Opens/closes the drain valve. This will allow any disper-
(dispersant) sant and sample in the system to drain naturally. No pump
is applied, so this process will not completely void the
system to the same extent as the Empty function. This
could be useful if, for example, the system had been man-
ually overfilled and needed some adjustment of the level.
Dispersant Opens/closes the dispersant input valve. It is necessary to
valve open the valve before manually adding dispersant. This
might be necessary if, for example, the system had been
partially drained (using the Drain valve option) and then
needed to be manually topped up.

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Hydro EV
The accessory controls panel for the Hydro EV is shown as follows:

Option Description
Stirrer Use the slider bar to set the RPM of the stirrer. In Manual
Measurement mode it is necessary to start the stirrer
manually before making the measurement. To initiate the
stirrer once the speed has been set, click the Start but-
ton.
Ultrasound Choose an appropriate level of ultrasound for the sample
by moving the slider bar.
Enable pulsed In this mode, sonication is applied in pulses (with fixed
sonication duration on and off pulses). This option can be used in
combination with both continuous or timed sonication
mode. Specify the duration of on and off pulses by enter-
ing the required values (seconds) into the corresponding
boxes. This can prevent overheating of the sample, and is
also useful on fragile samples that could otherwise be
broken up by more aggressive ultrasonication.
Manual Select this option if you wish to start and stop the stirrer
manually for a period of time.
Timed Select this option to perform a precisely timed period of
ultrasound application. When Timed is selected, the timer
controls become available - click +/- to increase/decrease
the time period for which ultrasound will be applied.

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Aero S
The accessory controls panel for the Aero S is shown as follows (in this example the
Air pressure/Feed rate have been set and the accessory started):

The following options are available:

Option Description
Standby By default the Aero is in standby mode when the acces-
sory is connected and powered up, but not active. In this
mode the front LED is pulsating.
Air flow This enables the vacuum cleaner and also the com-
pressed air supply used for sample dispersion.
Feed Start the vibrating feed tray. Selecting this option also
automatically turns on the Air Flow.
Stop Stop all operations and close all valves. The accessory is
returned to the Standby status.
Air pressure Use this slider bar to set the air pressure at which the
sample is circulated (from 0-4 bar, in 0.1 bar increments).
Lower air pressures tend to be better for fine or fragile
particles, higher air pressures for agglomerates or metallic
particle samples.
Feed rate Use the slider bar to set the rate at which the sample is
fed into the system - effectively this controls the vibration
speed of the feed tray. The correct feed rate is one at
which the sample is circulated steadily through the sys-
tem and gives the required obscuration - this rate is best
established as part of a method development process.

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Measurement settings reference

Note
SOPs and Manual Measurements involve specifying a number of settings
before the measurement can be run. This section relates equally to both.

The Measurement settings window is displayed whenever you create a new SOP or
manual measurement. This window groups settings into logical sections in which
various parameters for the measurement are defined as follows:
Sample identify the sample and provide more information to users of the
SOP. Define the physical characteristics of the sample and dispersant.
Measurement set both the red and blue light measurement durations, the
number of, and delay duration between, measurements. Specify the obscura-
tion levels for the measurement.
Sample Dispersion control the behaviour of the currently connected acces-
sory.
Data Processing specify the scattering model, latex analysis options and
modify the light detectors used in a measurement. Define any Analysis
Smoothing, Size Range/Resolution options and set size banding for all meas-
urement histograms and tables.

Note
When progressing through the settings, any icon next to a field indicates
that the user must specify a value for the field before continuing to the next
section.

The rest of this section goes through each of the measurement settings in more
detail.

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Sample - Identification
The Sample Identification settings section allows you to enter details that will both
identify the sample and provide more information to users. When the measure-
ment is run, the user is prompted to confirm or alter the fields specified here.

Complete the fields identified below:

Field Description
Sample Name A descriptive name for the sample, such as "Batch 1A" or
(mandatory) "Series 3, Sample 1". This is the only default sample iden-
tification field.

To add further fields for example, Notes, Batch, Lot, Group etc., click the
Add button. The new field is added to the list. Enter a name for the field in the
drop down menu to the left of the field. Check Required field if this is man-
datory for the operator to enter.
To re-order the list of fields, drag the item up or down by clicking and drag-
ging the icon next to the item.

To remove unwanted identification fields, click the icon adjacent to

the field.

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Sample - Particle Type

The Particle Type settings allow you to specify the shape of particles under analy-
sis in order for the software to apply the optimal analysis model.

Particle Type Description

Non-Spherical This analysis mode is applicable for particles which are
irregular in shape, or have a rough surface structure. For
example, it should be selected for milled or crushed mate-
rials. This mode uses Mie Theory, and therefore requires
input of the optical properties of your sample in order to
calculate a particle size distribution. The advantage of this
is that it provides the possibility of obtaining accurate size
distributions for all particle sizes.
Spherical This analysis mode is applicable for particles which are
perfectly spherical in shape. For example, it should be
selected for polymer latex samples or for emulsions. This
mode uses Mie Theory, and therefore requires input of the
optical properties of your sample in order to calculate a
particle size distribution. The advantage of this is that it
provides the possibility of obtaining accurate size distri-
butions for all particle sizes.
Opaque Parti- The Fraunhofer Approximation can be used to calculate
cle (Fraunhofer particle size distributions in cases where the particle size
Approximation) is large and where the particles can be assumed to be
completely opaque. It is the easiest mode to use, as you
do not have to provide any optical properties in order to
calculate a size distribution. However, its use may lead to
inaccurate results, particularly for small particles below 50
microns in size or for those which are transparent.

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Sample - Material
Use the Material properties section to enter physical characteristics of the mate-
rial being measured.

To select a previously added material, click Browse database, then select an item
from the database and click Use these values. See the Help system for more on
the Materials and Dispersants databases.
Alternatively, manually complete the fields detailed below.

Field Description
Material name Descriptive name for the material.
Refractive Value of between 0 and 5. This value relates to the speed
index of light within the material, which in turn allows the degree
of refraction (light bending) to be predicted when light
passes from one medium to another.
Absorption Value between 0 and 10, which is a measure of the quan-
index tity of light absorbed by the particles. Generally, transpar-
ent samples will have a low or zero absorption while
coloured or black samples will have a higher value.
Density Value of between 0.001 and 25g/cm.

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Field Description
Different blue- If required, add the Refractive index (blue-light) and
light properties Absorption index (blue-light). See Help System for more
information.
References and Any further comments that help to describe the material.
notes

Sample - Dispersant
Use the Sample Dispersant section settings to specify the properties of the dis-
persant used in the measurement.

It is possible to specify the dispersant details manually or to choose from the Dis-
persants Database. To select a previously added material from the Dispersants
Database, click Browse database, then select an item from the database and click
Use these values.
Alternatively, manually complete the fields detailed below.

Field Description
Dispersant Descriptive name for the dispersants, for example, Etha-
name nol.

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Chapter 4 Making measurements

Field Description
Refractive Value of between 0 and 5. This value relates to the speed
index of light within the material, which in turn allows the degree
of refraction (light bending) to be predicted when light
passes from one medium to another.
References and Enter any further comments that help to describe the dis-
notes persant.

If the newly added dispersant will be used in the future, add it to the Dispersants
Database by clicking Add to database.

Sample - Instructions
Use the Sample Instructions settings to specify pre-measurement and post-
measurement instructions that need to be drawn to the attention of the user.

These are then shown in the Sample Documentation panel/window before and fol-
lowing the measurement respectively. In this example pre-measurement instruc-
tions have been specified and are displayed above the Sample Name field in the
Sample Documentation window.

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Measurement - Duration
The Measurement Duration settings can be used to separately specify both the red
and blue light measurement durations.

Complete the following Red Measurement Duration options:

Field Description
Background This facility will make a measurement using only clean
measurement dispersant this is then subtracted from the sample
duration measurement by the system in order to clean the data.
(seconds) This is often set to the same duration as the sample
measurement.
Sample meas- The optimum measurement time depends on the size of
urement dura- the sample, its particle size distribution and the dispersion
tion (seconds) accessory used. If a material is monomodal, its essential
particle size characteristics can be captured in less time
than a material with a broad particle size distribution,
which will need to be measured longer to ensure that the
coarser particles have been properly represented.

Similarly, complete the Blue Measurement Duration options.

Blue light measurement is more effective when measuring particles under
approximately 1m in size. There is a gradual reduction in the effectiveness (and
hence significance to the overall measurement result) of the use of blue light on
samples containing particles above this size.

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Some red and yellow samples (such as pigments) can absorb light in the blue spec-
trum. This may lead to problems with the validity of the data acquired during the
blue light part of the measurement. If you have such a sample, the blue light meas-
urement can be disabled, so limiting the measurement to the main red laser.
If no blue light measurement is required, select Don't perform blue light meas-
urement. This will speed up the measurement time.

Measurement - Sequence
The Measurement Sequence settings window allows you to specify the number of
measurements and the duration of any delay between measurements.

Select either Automatic to have the system measure until stability is reached, or
Use the number I specify and then enter the Number of measurements (up to
999) and Delay between measurements (up to 9999 seconds). Specifying several
measurements, e.g. 5, allows repeatability to be assessed.
If the material is difficult to disperse, requiring ultrasonication, surfactant or both
to achieve a stable dispersion, several measurements of the same sample may be
required in order to determine the ideal dispersion time. In general, repeat meas-
urements are performed until the last measurement obtained agrees closely with
the previous one.

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Measurement - Obscuration
The Measurement Obscuration settings enable you to specify the obscuration lev-
els between which the measurement will be conducted. This is critical for ensuring
the correct amount of sample is added to the measurement system.

The optimal obscuration settings for a measurement are both sample and disper-
sion unit dependent. As a rough guide, use a range of 10-20% for a wet dispersion
unit and 1-10% for a dry dispersion unit.

Note
For more advice on obscuration settings see the Help.

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Chapter 4 Making measurements

In the Measurement obscuration limits section, set the following parame-

ters:

Field Description
Obscuration Enter a percentage value from 0.1 to 50 above which the
lower limit (%) measurement should be run.
Obscuration Enter a percentage value from 0.1 to 50 below which the
higher limit (%) measurement should be run.

This information is subsequently indicated on the Laser pane of the measure-

ment sequence. For example, a lower limit of 10% and an upper limit of 30%
has been set here:

In the Enable measurement to auto-start section, if required, select Auto

start measurement when obscuration is in range. If selected, it is also nec-
essary to set a Stabilisation time delay in seconds - this will then add a delay
before the measurement initiates after the obscuration level is first detected
within the specified band.
Select the Enable filtering option in the Measurement obscuration filter-
ing section to optionally set the software to only record data where the obscu-
ration was within the specified range. The Time out option forces the
measurement to stop if no such data are recorded within the specified number
of seconds.

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Sample Dispersion - Accessory

The Accessory control settings allows you to set up the behaviour of the currently
connected accessory. Depending on the accessory that is connected the settings
presented differ accordingly.

Accessory control settings: Aero S

This section describes the Aero S accessory control settings.

Field Description
Air pressure Use this slider to set the air pressure at which the sample
is circulated (from 0-4 bar, in 0.1 bar increments). Lower
air pressures tend to be better for fine or fragile particles,
higher air pressures for agglomerates or metallic particle
samples.
Feed rate Use the slider bar to set the rate at which the sample is
fed into the system effectively this controls the vibration
speed of the feed tray. The correct feed rate is one at
which the sample is circulated steadily through the sys-
tem and gives the required obscuration - this rate is best
established as part of a method development process.

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Chapter 4 Making measurements

Field Description
Venturi type Select the currently attached venturi type. If you do not
know this, select Unknown Venturi.
Tray type Select the currently attached tray type. If you do not know
this, select Unknown Hopper.
Hopper gap Enter the gap as currently set on the hopper hardware.
(mm)

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Accessory control settings: Hydro LV/MV/EV

This section describes the Hydro LV/MV accessory control settings.

Field Description
Stirrer speed This accessory type has an independent stirrer allowing
flexible control of sample flow and agitation. The stirrer
speed may be controlled manually using the Wet Acces-
sory dialogue or by a predefined SOP for automatic oper-
ation.
Manual control would typically be used to determine the
optimum measurement setting prior to using an SOP pro-
cedure or when doing one-off manual measurements.

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Field Description
Stirrer speed To control the stirrer from an SOP, determine the opti-
(continued) mum stirrer speeds initially using manual control, ensuring
that the lowest setting to give satisfactory dispersion is
obtained. Make a note of the settings and enter these into
the SOP Accessory control settings. Click and drag the
slider bar to set the speed.
It is also possible to control the accessory manually by
using the Accessory Controls panel (from the manual
measurement window) or the from the Tools-Accessories
option at any other time.
Tank fill The tank can be filled with dispersant manually or auto-
behaviour matically. When set to Automatic the dispersant is
plumbed into the dispersant inlet port at the rear of the
(Hydro MV/LV accessory and a solenoid valve controls the flow of dis-
only) persant into the tank.
However, if a solvent is to be used as a dispersant, it is
unlikely that the solvent will be plumbed into the acces-
sory. In these situations the filling of the tank can be set to
Manual. Under manual filling the solenoid valve is
switched off (this will mean that the dispersant inlet does
not have to be disconnected during a manual fill) and the
tank can be filled by hand. The software will tell the opera-
tor when to fill the tank during an SOP measurement.
Ultrasonics This sample dispersion unit has an ultrasonic probe which
can assist the dispersion of cohesive samples. The level
and duration of ultrasound may be set manually using the
Wet Accessory dialogue or may be set by a predefined
SOP for automatic operation.
To determine the correct ultrasonic level for an SOP, ini-
tially determine the optimum ultrasound level and duration
using manual control, ensuring that the lowest setting giv-
ing satisfactory dispersion is obtained. Record the set-
tings and transfer these to the SOP in the Sampler
Settings page using the slider controls. Click and drag the
slider bar to set the power level.

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Field Description
Ultrasonics Set the Ultrasound Mode to one of the following:
(continued...) Manual - this is typically be used to determine the opti-
mum measurement setting prior to using an SOP proce-
dures or when performing one-off manual measurements.
Pre-Measurement - ultrasound is activated for a set time
prior to measurement. For pre-measurement mode, enter
the required duration in seconds in the Duration box.
Continuous (from Sample Addition) - ultrasound is acti-
vated after sample is added and will run continuously.
Continuous (from Measurement Start) - ultrasound is
active throughout the measurement. Ultrasound will start
after the electrical background is complete. The stabilis-
ing period will add a delay between the electrical back-
ground and the optical alignment - during this delay
ultrasound is active, allowing bubbles to be driven from
the dispersant.
To manually control the ultrasonic level from the Wet
Accessory dialogue, either select and drag the Ultrasound
slider bar to set the level, or select the bar and use the
keyboard control up/down/left/right arrows; this will step
the ultrasonic level up or down in 10% divisions.
Alternatively, for an exact setting, double click on the dis-
played ultrasonic value and type in the required level.
Pulsed Enable pulsed ultrasonication - in this mode, ultrasoni-
Ultrasonics cation is applied in pulses (with fixed duration on and off
pulses). This option can be used in combination with both
continuous or timed ultrasonication mode. Specify the
duration of on and off pulses by entering the required val-
ues (seconds) into the corresponding boxes. This can pre-
vent overheating of the sample, and is also useful on
fragile samples that could otherwise be broken up by
more aggressive ultrasonication.

Note
The Ultrasonics will switch off automatically after 20 minutes continuous
use.

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Sample Dispersion - Cleaning

The Cleaning options allow you to specify both a clean sequence and whether to
use ultrasound as part of the sequence. This ensures that all traces of the sample
just measured are removed so that no contamination of the next sample occurs.
Cleaning following a measurement is essential to ensure that background noise,
consisting of particles agglomerating within the system and forming accumula-
tions, is minimized.

Field Description
Clean Each Clean type specifies a set number of cycles (noth-
Sequence ing further is changed in the cleaning method). Select a
Clean type of either Quick, Normal, Extensive or Cus-
tom. If Custom is selected the user must also manually
specify the number of Clean cycles. If measuring the
same sample type in succession a Quick clean may be
sufficient. If making the last measurement of the session,
it is prudent to perform an Extensive clean to ensure that
the system is as free as possible from contamination in
readiness for the next measurement session.
Ultrasonication Ultrasound can reduce agglomeration, which may help
further with cleaning. Select whether to Use ultrasound
during the clean sequence or No ultrasound during
clean.

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Data Processing - Analysis

The Analysis settings allow you to specify the scattering model, latex analysis
options and modify the light detectors used in a measurement.

Tip:
If you are unsure which analysis settings are best suited to your application,
try reapplying different analysis settings to the measurement records. To
do this, use the Edit Result feature after the first set of measurements has
been made see Chapter 5 for more information.

Field Description
Analysis Model General Purpose this model is appropriate for most
samples, including naturally occurring and milled materi-
als. You should select this model unless you know that
your sample meets more specific requirements stated for
the other analysis modes provided for the system.

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Chapter 4 Making measurements

Field Description
Analysis Model Narrow Modes this model is appropriate for sample
(continued...) consisting of one or more narrow modes, where each
mode spans much less than a decade in size. It is not
intended for use with broad distributions which exhibit
more than one peak.
Verification Latex this model is designed to enable the
analysis of one or more very narrow Latex size standards,
such as those used during verification of the optical unit
performance.
For all of the analysis models use the Keep a single
result mode option in the Advanced settings to force the
analysis to only report the most significant mode present
within the sample.
Fine Powder This option should be enabled for samples containing a
Mode significant proportion of material below 10 microns in size.
(Aero units only) It can help improve the result reproducibility, and can be
used with any of the Mastersizer 3000 analysis modes.

Click the Advanced button to reveal the following additional options:

Field Description
Advanced: Use Keep a single result mode if you know your sample
Analysis Modes has a single mode size distribution. This option eliminates
any small modes produced by noise on the measurement.
Advanced: Set the number of low scatter-angle detectors to be
Disable Detec- ignored by the analysis. Thermal fluctuations in the dis-
tors persant can cause signals in the inner channels to be
interpreted as large particles. Set the number of detectors
to remove the effect of these fluctuations, at the expense
of reducing the sensitivity to the presence of genuinely
large particles.
Advanced: Remove Blue Light from Analysis allows a measure-
Red Light Only ment made with red and blue light to be analysed as if the
blue light was not used.

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Data Processing - User Sizes

The Data Processing: User Sizes settings allow size banding for the measure-
ment to be defined for all histograms and tables used in reports.

A practical use of size bands is when using sieves that conform to specific standard
sizes - size bands could be set to corresponding ranges.
The system can either automatically set size bands for histograms and charts, or
these can be user-specified.
To automatically select appropriate high and low sizes based on the measure-
ment result, click Use default sizes.
To manually define size bandings, click Use the sizes that I specify. The
User sizes (m) and Generate user sizes panels become active.
Creating size bands:
1. From the Generate user sizes panel, enter the required Lower size and
Upper size limits (in m).
2. Then enter the Number of bands into which the table or histogram should
be divided.
3. Select a Distribution type:
Linear: Divides the bands into equal sizes.
Logarithmic: Bands are represented by multiples of a constant factor that
accounts for the size range specified.

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Chapter 4 Making measurements

4. Click Generate sizes to populate the set of figures in the User sizes panel.
5. To add more size bands, enter a figure into the Size (m) field and then click
the button. The new figure is added to the list in the correct numerical posi-
tion.
6. To delete one of the size bands, select the figure you wish to remove and then
click .
7. To save size band information that you wish to re-use within other SOPs, click
to save the current sizes. To use previously saved sizes, click and then
locate the relevant .siz file.

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 5

Viewing
measurement results
Introduction
The Mastersizer 3000 delivers powerful features for manipulating and presenting
the data gathered in measurement files.
This chapter provides the following information:
An overview on working with measurement files.
Features of the Analysis report.
Fundamental concepts to help understand measurement data.

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5 Chapter 5 Viewing measurement results

Working with measurement files

To make a measurement it is necessary first to open, or create, a measurement file.
Measurement files can be thought of as containers for the individual records cre-
ated by each measurement.
A measurement file can contain any number of individual records. Often these will
have been made at a similar time, but equally they could have been generated on
different dates. Similarly, a measurement file could contain records that are either
the result of measurements from one or more dispersion unit types.
Multiple measurement files can be opened at the same time, each of which is dis-
played in its own tab (see also Chapter 3). When working with multiple measure-
ment files, it can also be useful to compare data by merging all of the files into a
single list; the All files tab offers this feature. Additionally, if required, individual
measurement records can be copied between files or copied into an empty meas-
urement file.

Opening existing measurement files

This topic provides information on how to open and close existing Mastersizer
3000 (.mmes files) and Mastersizer 2000 (.mea files).

Note
Although Mastersizer 2000 files can be opened for analysis, they cannot be
edited. They are shown with a differently coloured icon and also a lock,
which indicates their read-only status (like the Examples file shown here):

To open a Mastersizer 3000 measurement file: from the Home ribbons

Documents section, choose Open-Measurement File. Mastersizer 2000
measurement files can be opened by selecting Open-Mastersizer 2000 Meas-
urement File.
To close a measurement file: click in the right corner of the tab of the
measurement file you wish to close.

Tip
To view more information about an open measurement file, move the
mouse pointer over its tab - information about the file type, access mode
and location are provided.

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Creating and saving measurement files

1. Select New-Measurement file from the Home ribbon.
2. From the Home ribbon choose Save As and then enter a new file name.
Alternatively, choose Save from the Home ribbon if the file has already been
saved and you wish to just overwrite the last saved instance.
If multiple measurement files are simultaneously open, select Save All to save
the changes of all modified files.

Filtering the Record View

This section provides information on how to set up parameter filters within the
Record View.
To simplify the analysis of large numbers of records (perhaps when using the All
files feature or a large measurement file), it is possible to set up parameter filters.
These are used to hide or make visible entire groups of records as required. It is
possible to filter on any parameter, e.g. operator name, measurement date, sample
name or a value range of a particular measurement parameter, like Dv50 >
50m.
1. From the Record view, move the mouse pointer over one of the column
headings until a down arrow is displayed next to the title of the column, for
example:

2. Click the down arrow to display a list of available parameter values upon which
to filter (these are the values shown in the record).
3. Select any of the values to show only those records with values matching the
checked filters. When a filter has been set, the column header shows the fol-
lowing icon: . As many filters as required can be set up in this way.

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Chapter 5 Viewing measurement results

4. It is also possible to extend the functionality of this grid by manually typing text
into the sorting header area - filtering criteria can include numerical informa-
tion, date ranges and strings. Click on the column header and then enter text -
the display updates immediately to show only those items that are within the
scope of the filter - see Parameter filtering logic in the Help system.

In the example shown here a filter of >50 has been applied (meaning, show
only those items whose Dv50(m) value is greater than 50).

To remove a filter that has been selected from the predefined list, either de-select
the individual check box from the filter menu or choose the Clear filter option -
this removes all filters for that column. For any filter text that has been manually
entered, either delete the text or click the X button which is shown next to the text
(in the adjacent column).

Note
Check box filters: having all filters either selected or deselected has the
same effect, namely that all of the records are shown.

Grouping records
Read this section for details on how to group records by parameter type.
The Record view allows records with the same parameter values to be grouped
into collapsible sections. Any parameter can be selected on which to group. It is
then possible to add further sub groups. Examples of the use of groups include,
grouping by Operator Name, Measurement Date, Accessory Type etc.
1. To group items by a parameter, drag the required column header into the area
above the columns, titled Drag a column header here... The records are
now presented in collapsible groups based on groupings of the chosen parame-
ter of the same value. For example if Scattering Model was used as the group-

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Viewing measurement results Chapter 5

ing parameter, items would be grouped either in the Fraunhofer, Fraunhofer

Extended or Mie groups.
2. To collapse the groups, click next to the group section's title. To expand a
group that has been collapsed, click next to the title.
3. Add further groupings in the same way - these are then indicated in the area
above the records in the order in which the grouping was applied. The parame-
ter that is leftmost is applied first.

The image below shows several groupings applied; the up arrow in Has Align
Alarm Triggered indicates that sorting is applied on that field:

The grouping hierarchy can be edited by dragging and dropping the group
parameter headers left or right as appropriate.
4. To remove groupings, drag the group parameter header back into the records
area.

Merging records
This section provides information on how to use the All files feature of the
Record View.
When working with multiple Mastersizer measurement files, it can be useful to
compare data by merging all of the files into a single (virtual) measurement file so
that Mastersizer's powerful sorting, grouping and reporting features can be
exploited.
1. Open more than one measurement file.
2. Click the All files tab (rightmost):

The records contained in all of the open measurement files are shown combined
into a single file. It is now possible to sort, group, filter and report on the records
displayed in this view. If graphically analysing multiple records in reports, each
record's data is overlaid using a different colour.

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Chapter 5 Viewing measurement results

Creating an averaged record

The Create Averaged Record feature allows you to create a new record that con-
tains the average values of all selected records.
1. From the Record View, select the records from which to create an average and
choose Create average from the ribbon. Alternatively, right-click a selection
of records and choose Create Averaged Record.

Note:
This feature is not available from the All files view.

The Create Averaged Result window is displayed:

2. Enter a Sample name and a Reason for creating the new result.
3. Then click the Create Average button.
A new record is created within the current measurement file. To retain the
newly created record, save the measurement file.

Editing records
Each Mastersizer record is the result of the processing of raw measurement data.
By editing a record it is possible to re-apply new values to some of the parameters
used in the original measurement settings in order to generate a completely new
record.
This can be used to explore the effect of using different settings from those chosen
when the measurement was made. Typically adjustments are made to improve the
fit of the calculated result to the data. Use the SOP summary report (see Chap-
ter 9) to show which parameters have been altered.

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Viewing measurement results Chapter 5

To edit a record:
1. From the Record View, right click on a record, or group of records, and
choose Edit Result.

The Result Editor window is displayed. This contains all of the information
set up in the original measurement. Some of the options are unavailable
because they relate only to the physical set up of the original measurement, for
example, all of the Measurement Duration options.
2. Edit any available sections of the Result Editor as required. Any edited infor-
mation is clearly highlighted by a different background colour.
3. Click OK when all settings have been altered to your specification. The newly-
set values are now re-applied to the existing raw measurement data. A brief
message is displayed whilst this happens. When the result has been edited, the
edited result is then displayed as the first item in a tree structure.
4. Expand the edited record to show the "contained" original result by clicking the
icon. Note: It is not possible to edit a record without also retaining its origi-
nal settings. Further edits to the record result in more items contained within -
the most recently edited record, which is always shown as the container record
(in this example, edit 3 was the final edit made):

Note:
If you save the measurement file, the new settings will overwrite the origi-
nal file settings. To create a result-edited version of a file and still retain the
original file settings, just save the file with a different name before editing.

Selecting records to display in a report

Mastersizer reports display data from all measurement records that are currently
selected in the Record view. It is possible to select either single or multiple records
for report analysis. Records can also be sourced from different measurement files
and still compared in the same report see Merging records for more informa-
tion.
1. To view a report of the data contained in a single record, click on it within the
list of records. The display is updated immediately to reflect the selection
(assuming that you are using a view that shows a report and records simultane-
ously - see Chapter 3).

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Chapter 5 Viewing measurement results

2. To select multiple records to display in a report, use the standard Windows

selection methods; either hold SHIFT and click to select multiple contig-
uous records or hold CTRL and click to select non-contiguous records.
When more than one record is selected, and a graph is displayed in the cur-
rently shown report, the graph indicates the data taken from individual records
by using a different colour for each. A key to the colours used is presented
beneath the graph.

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Viewing measurement results Chapter 5

Analysis report
The Analysis report provides a useful breakdown of the
measurement data.
To display this report, select the record(s) to analyse in the Record View and
then click the Analysis report from within the Reports tab.

7
1

6 5
9 8
10
3 2

The following information is displayed in the report:

Weighted Residual an indication of how well the calculated data was fitted
to the measurement data. A good fit is indicated by a residual of under 1%. A
residual of over 1% may indicate use of incorrect refractive index and absorp-
tion values for the sample and dispersant.

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Chapter 5 Viewing measurement results

The statistics of the distribution are calculated from the results using the
derived diameters D[m,n] an internationally agreed method of defining the
mean and other moments of particle size. See British standard BS2955:1993 for
more details.
1
m 3 ------------
-

Vi di
D m n = ---------------------------
mn

n3
Vi di

Dv 50, Dv 10 and Dv 90 are standard percentile readings from the analysis.

Dv 50 the size in microns at which 50% of the sample is smaller and 50%
is larger. This value is also known as the Mass Median Diameter (MMD)
or the median of the volume distribution. The v in the expression Dv 50
shows that this refers to the volume distribution. This can be replaced by s
for surface, l for length or n for number distributions.
Dv 10 the size of particle below which 10% of the sample lies.
Dv 90 the size of particle below which 90% of the sample lies.
D[4,3] the Volume Weighted Mean or Mass Moment Mean Diameter,
also known as the De Broucker mean.
D[3,2] the Surface Weighted Mean, also known as the Surface Area
Moment Mean Diameter or Sauter mean.
Span is the measurement of the width of the distribution. The narrower the
distribution, the smaller the span becomes. The span is calculated as:
d x 0.9 d x 0.1
Span = ------------------------------------------------
d x 0.5
The x is replaced by any of the letters v, s, l or n that define the distribution
type.
Concentration the volume concentration. This is calculated using Beer-
Lamberts law. For full details see the following section.
Obscuration this helps the user to set the concentration of the sample when
it is added to the dispersant. It is a measure of the amount of laser light lost due
to the introduction of the sample into the analyser beam.
The obscuration term can be expressed mathematically:
L
Ob = 1 -----s
Lb

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Viewing measurement results Chapter 5

Ls is the light intensity measured in the central detector when a sample is pre-
sent in the cell, Lb is the same but with clean dispersant (i.e. with no sample).
Obscuration is usually expressed as a percentage: 100 x Ob.
An ideal range is between 3 and 20%, depending on the sample and dispersion
unit used.
Distribution shows the type of distribution the analysis has used. Options
include change from volume to surface area, length or number. Remember
that the Mastersizer measurement is fundamentally a measurement of the vol-
ume distribution - transforming the result into a surface, length or number dis-
tribution is a mathematical process that may amplify any error in the original
result, especially at the fine end of the size distribution.
Uniformity a measure of the absolute deviation from the median.

X i d x 0.5 d i
Uniformity = ------------------------------------------------
d x 0.5 X i
Here d(x,0.5) is the median size of the distribution (where x is replaced by v, s,
l or n) and di and xi are respectively the mean diameter o f, and result in, size
class i.
Specific Surface Area (SSA) the total area of the particles divided by the
total weight.
V
6 -----i
d 6
SSA = ----------------i = ---------------------
pD 3 2
p Vi

where Vi is the relative volume in class i with mean class diameter of di and p is
the particle density.
If the SSA is used, it is important that the density of the material is defined (in
the SOPs Material settings). This figure is a mathematical calculation based
on the assumption that the particles are both spherical and non-porous.

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Chapter 5 Viewing measurement results

Fundamental concepts
To understand the meaning of the results from the Mastersizer, a number of fun-
damental concepts require explanation. These are:
How the concentration is calculated.
The results are volume-based.
The result is expressed in terms of equivalent spheres.
How the distribution parameters are derived.

Calculating the Concentration (Cv)

Beer-Lambert law
The software uses the Beer-Lambert law to calculate the concentration of the sam-
ple. This may be expressed as:

---I- = e
b
I0

Where:
I is the intensity of light at a distance b in the particle field of absorbance .
I0 is the intensity of the light beam as it enters the particle field.
I / I0 is the relative transmission T of the beam (measured directly by the
instrument). I0 is the intensity of the laser beam measured at the receiver when
no sample is present and I is the intensity with sample in the beam.
Expressing the Beer-Lambert law in terms of relative transmission and re-arranging
to solve for absorbance gives:
1
= ------ Ln T (1)
b

Volume concentration
The term contains information about the concentration and size of the particles.
From scattering theory the light attenuated by a particle i may be described by:
2
a i = Q i r i n i

Where:
Qi is the efficiency of light extinction (by scattering and absorption), calculated
from Mie theory for a particle of radius ri.

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Viewing measurement results Chapter 5

The second term is the cross-sectional area of the particle and the final term ni
is the number of particles of radius ri.

4 3
In terms of the volume of particles V i = --- r i n i , the equation above becomes, for
3
an ensemble of particles:

3 Qi Vi
i = --- ----------
-
4 ri

The size of the particles is expressed by the diameter d and the volume terms can be
separated into a relative volume distribution v and a total concentration Cv (total
volume of particles in a unit volume of dispersant). The equation then becomes:

3 Qi Vi
i = --- C v ----------
-
2 di

Substituting the above into equation (1) and solving for the concentration gives:
2Ln T -
C v = -----------------------
Qi vi
3b --------- -
di

If d is measured in m and b in mm, and v is the relative concentration of the size

distribution (such that vi = 1 ) then:

2000Ln T
C v ppm = ------------------------------
Qi vi
3b --------- -
di

This equation provides the concentration in parts per million (ppm). To calculate
the value as a percentage volume concentration, the final value is divided by 10,000.
In the above equation:
The Transmission (T) is a value between 0 and 1 and is measured directly by
the instrument.
The particle size distribution vi is the relative volume in size-class i with mean
diameter di.
Qi - the mean extinction term for size-class i - is calculated from scattering the-
ory and is a function of the optical properties of the particle and dispersant
media.

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Chapter 5 Viewing measurement results

Concentration at different obscurations

This advice gives an approximate idea of the obscuration ranges to use during a
measurement.
It is possible to convert the obscuration limits into an equivalent volume concen-
tration but there is a strong size dependence that makes it difficult to use the data at
the time of measurement. The relative volume concentrations of monomodal (sin-
gle sized) particles that would give a certain obscuration is illustrated below. The
actual curves differ according to the presentation being used. It will be clear that
there is a size dependence; an obscuration of 30% means a widely varying volume
concentration dependent on size.
Concentration at different obscurations
Calculated for glass beads in water (n=1.54 +i0) in water

In the more realistic situation of a polydisperse (or multimodal) sample it is not

possible to provide simple graphical correlations of volume concentrations and
obscuration. The system calculates concentration, however, using the size distribu-
tion result and the obscuration.
For a polydisperse sample the curve of the above figure can be used if the
Surface Weighted Mean (D[3, 2]) of the material is taken as single size.

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Viewing measurement results Chapter 5

Volume-based results
The first, and probably most important, point to remember in interpreting results
is that the fundamental size distribution derived by this technique is volume-based.
This means that when a result indicates, for example, that 11% of the distribution is
in the size category 6.97-7.75 microns, this means that the volume of all particles
with diameters in this range represents 11% of the total volume of all particles.
It is useful to consider a numerical example to illustrate this point. Suppose, for
simplicity, that a sample consists of only two sizes of particle, 50% by number hav-
ing a diameter of 1 micron and 50% by number a diameter of 10 microns. Assum-
ing that the particles are spherical, the volume of each of the larger particles is 1000
times the volume of one of the smaller ones. Thus, as a volume distribution, the
larger particles represent 99.9% of the total volume.
The graph below illustrates this for a more realistic distribution:
%
30

20
1 1

10

0
0.1 1.0 10.0 100.0 1000.0 10000.0
Particle Diameter (m.)

ill 1874

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Chapter 5 Viewing measurement results

Equivalent spheres
Mie theory presumes that the particles measured are perfect spheres. In practice
they are very rarely so. This causes a problem in the definition of the term meas-
ure the particles size: if the particle is an irregular shape, which particular dimen-
sion should be measured?
As an example, imagine that I give somebody a matchbox and a ruler and ask them
to tell me the size of it. They may reply by saying that the matchbox is 50mm x
25mm x 10mm. They cannot say that the matchbox is 25mm as this is only one
aspect of its size. It is not possible to describe the three dimensional matchbox with
one unique dimension. Obviously the situation is even more complex for irregular
shaped particles such as grains of sand or the pigment particles in paint.
Most people want a single measurement to describe their sample, for example, they
wish to say that their sample is made up of 50 micron particles. What is required is
a unique number that describes the particle. There is only one shape that can be
described by one unique number and that is a sphere. If we say we have a sphere of
50 microns, this describes it exactly. We cannot do the same even for a cube as 50
microns can refer to its edge or to a diagonal.
One way to get a single unique number to describe an irregular shaped particle is to
compare some feature of the actual particle to an imaginary spherical particle.
Some typical methods of doing this are:
Equivalent surface area calculating the diameter of a theoretical sphere
that has the same surface area of the original particle.
Equivalent maximum length this is where the diameter of a theoretical
sphere is the same as the maximum dimension of the original particle.
Equivalent minimum length this is where the diameter of a theoretical
sphere is the same as the minimum dimension of the original particle.
There are many other methods available to do this. This technique is known as
equivalent spheres.
The Mastersizer uses the volume of the particle to measure its size. In the example
above, the matchbox has a volume of 50 x 25 x 10mm = 12500mm3. If the Master-
sizer was able to measure this size of particle it would take this volume and calcu-
late the diameter of an imaginary sphere that is equivalent in volume - in this case it
will be a sphere of about 30mm diameter.
Obviously the answer will be different if the surface area or maximum dimension
of the matchbox is used to calculate an equivalent sphere. All of these answers are
correct but each is measuring a different aspect of the matchbox. We can therefore
only seriously compare measurements that have been measured using the same
technique.

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Viewing measurement results Chapter 5

Consider a cylindrical particle of diameter 20 microns and length 60 microns. The

volume of the cylinder is:
2
V = 10m 60m

ill 7973
The sphere of equivalent volume would have a diameter centred on:

6V
3 ------- = 33m

with a spread from 20 to 60m.
It is interesting to compare this with other techniques. Sieving would pass the par-
ticles through a 20m aperture and classify them as 20m. Sedimentation would
give a result related to the total surface area, in this case reporting a diameter of
around 40m.

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Chapter 5 Viewing measurement results

Derived distribution parameters

The particle size distribution reported by the software is expressed in a set of size
classes which are optimised to match the detector geometry and optical configura-
tion, giving the best resolution. All parameters are derived from this fundamental
distribution.
Distribution parameters and derived diameters are calculated from the fundamen-
tal distribution using the summation of the contributions from each size band. In
performing this calculation the representative diameter for each band is taken to be
the geometric mean of the size band limits:

d i l di

This number will be slightly different to the arithmetic mean:

di l + di
-------------------
-
2
For example, the size band 404.21 - 492.47 microns has a geometric mean of 446.16
microns and an arithmetic mean of 448.34 microns. In most cases the difference is
small but the geometric mean is chosen in these calculations as more appropriate to
the logarithmic spacing of the fundamental size classes.
The same principle of calculation applies to the distribution statistics standard devi-
ation, skewness and kurtosis, as shown below:
standard deviation

2
X d d
i i 2
= ---------------------------------- = D [K + 2,K] + D [K + 1,K
X i

skewness

X d d D K + 3 K d d + 3
3
i i 3 2 2
kew = ---------------------------------- = -------------------------------------------------------------------
3
X
3
i

kurtosis

X d d
4
i i 4 3 3 2
D K + 4 K d 4D K + 3 K + 3d + 6d
rt = ---------------------------------- 3 = -------------------------------------------------------------------------------------------------------------------------
4
X
4
i

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Viewing measurement results Chapter 5

In the above formulae K and X depend on the distribution being calculated as

shown in this table:

Distribution K Xi
Volume 3 Vi
Surface 2 Vi /di
Length 1 Vi /di 2
Number 0 Vi /di 3

The various derived diameters are related by:

m
mn D m 0
D m n = ----------------------
n
-
D n 0
For mono-size distributions such as latex, the distribution mean is reported as
the geometric mean of the size class and standard deviation, skewness and kur-
tosis are reported as zero.
The procedure used for other parameters of the distribution is to create a spline fit
to the fundamental result. Intermediate values are then read from this curve allow-
ing interpolation of percentile points which do not coincide with the measurement
size band boundaries.

Optical models
This section contrasts the Fraunhofer approximation used in some instruments
with the Mie theory which underpins Mastersizer 3000 operation. Although Mie is
the preferred scattering model, users can also select Fraunhofer if required from
the Data Processing - Analysis measurement settings.

Fraunhofer approximation
Older instruments and some existing instruments rely on the Fraunhofer approxi-
mation only. This assumes that:
The particle is much larger than the wavelength of light employed. ISO 13320
defines this as being greater than 40x wavelength (25m when a He-Ne laser is
used).
All sizes of particle scatter with equal efficiencies.
The particle is opaque and transmits no light.

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Chapter 5 Viewing measurement results

These assumptions are incorrect for many materials and for small particles they can
give rise to errors approaching 30%, especially when the relative refractive index of
the material and medium is close to unity, or when the particles are transparent.
When the particle size approaches the wavelength of light the scattering efficiency
becomes a complex function with maxima and minima present.

Mie theory
The Mastersizer 3000 uses the full Mie theory which completely solves the equa-
tions for interaction of light with matter. This allows completely accurate results
over a large size range.

Requirements for using Mie

The Mie theory assumes the particle is spherical, as opposed to Fraunhofer, which
is a projected area prediction. The penalty for this complete accuracy is that the
refractive indices for the material and medium must be known and the absorption
part of the refractive index must be known or estimated. However, for the majority
of users this will present no problems as these values either will be known or can be
measured.
A standard set of materials is available for selection in the SOP (presented in the
Sample - Material section of the measurement settings). Further materials can be
defined by a user within the materials database, but the following parameters must
be specified accurately:
Refractive Index (Real) this value relates to the speed of light within the
material, which in turn allows the degree of refraction (light bending) to be
predicted when light passes from one medium to another.
Absorption Index an imaginary number that describes the amount of
absorption that takes place as the light enters the particle.

Density the density in g/cm3. This is used to calculate the Specific Surface
Area (SSA). Users who want to include the SSA as a derived parameter must
complete this field.
The residual shown in the Parameters report indicates how well the calculated
data fitted the measurement data.

Refractive index of medium

This value is needed by the software in order to provide accurate calculations and is
specified within Mie theory.

Page 5-20 MAN 0474

Part 2 -
Supervisors Guide
 6

Sample preparation
guidance
Introduction
Preparation of the sample before it is added to the system can be critical. Over half
the problems encountered when measuring a sample are caused by poor sample
preparation. If the sample is sticking together, dissolving or floating on the surface,
or if it is not a representative sample, the result will be incorrect.
There are many techniques available to ensure that the sample is prepared success-
fully. Once a suitable dispersion technique is found for the sample, standardise the
procedure (using an SOP) so that comparisons can be made between samples.
This chapter gives information on:
Sample preparation flow chart summarises the process.
Representative sampling.
Considerations for dry samples.
Considerations for wet samples.
Symptoms of poor sample preparation.

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6 Chapter 6 Sample preparation guidance

Sample preparation flow chart

This flow diagram shows the route taken to prepare an unknown sample:
SAMPLE

Take Representative Sample

(mix well or riffle if dry powder)

Yes Does it No
disperse in
water?

Ultrasound if
necessary Yes No
Does it
float?

Analyse
Try Surfactant
No Does Yes
Ultrasound
work?

Yes No Analyse
Does this
disperse it?

Ultrasound if Try Solvent

necessary
e.g. Ethanol
Propan-2-ol (IPA)
Methanol
Analyse Acetone
Butanone (Methyl Ethyl
Ketone)
Hexane
Toluene
Dimethyl Digol

Ultrasound if
necessary

Analyse
ill 7825
Using liquid-borne particle suspensions, such as latex and emulsions, is usually
straight forward. Use the suspension phase as the dispersant, mix the sample well
and add directly to the Mastersizer beaker. Ultrasound is not usually necessary and
will almost certainly affect the size of liquid particles.

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Sample preparation guidance Chapter 6

Representative sampling
When taking a sample for a measurement, it is vital to ensure that the sample used
is representative of the whole sample. This section gives guidelines.
If the sample is taken from a bottle or container, take care to ensure that it is thor-
oughly mixed. When the sample is a powder, large particles tend to rise to the top
of the container as smaller ones work their way to the bottom.
In most samples there are some large and some small particles, but the majority fall
between these extremes. If a sample is taken from the top of the container, mainly
large particles will be measured. If this is compared to a measurement with the
sample taken from the centre of the container the results will differ noticeably.
If the sample is stored in a container this should be mixed thoroughly before meas-
urement. Do not shake the container as this often increases the separation of the
particles. Instead, hold the container in both hands and gently roll the container,
continually changing its orientation for about 20 seconds. This method works bet-
ter if the container is only half full.

Spinning rifflers
If the distribution of particles within a sample is particularly broad, representative
sampling can be difficult. If problems continue, using a spinning riffler may help.
This is a vibrating hopper which vibrates the sample down a chute.
The act of vibrating the sample causes the larger particles to separate out and travel
down the chute first. At the end of the chute a set of rotating pans collects the sam-
ple evenly. When all of the sample has passed down the chute each collecting pan
will contain a representative sample.

Liquid samples
Liquid samples can also separate out if stored in containers, with larger particles
sinking to the bottom. Again, its necessary to mix the sample thoroughly to get a
representative sample. Sample splitters/rifflers are also available for liquid samples.
Beware of using a magnetic stirrer to mix a liquid sample. Large particles tend to
move to the outside of the container due to centrifugal separation, and this can lead
to sample biasing.

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Chapter 6 Sample preparation guidance

Considerations for dry samples

The first step when analysing a sample for the first time is to decide whether to ana-
lyse the sample in a wet or dry state. This is usually determined by the nature of the
end use of the sample. If the product is to be used and stored in a dry form, a dry
analysis may be preferred.
Some samples can only be measured in a dry state as they react with all wet disper-
sants, for example they may dissolve or the particles may swell when in contact
with a liquid.
Another consideration is whether the material in its dry state is free flowing. Good
pouring characteristics indicate a non-cohesive powder which will usually disperse
well in a dry powder feeder without any difficulties, whereas a highly cohesive
material tends to stick and clump together, giving biased measurements.
Sample clumping together can often be overcome by drying the sample in an oven.
Obviously care should be taken with delicate materials where drying in the oven
may damage the sample. To drive the moisture from the sample, set the oven to the
highest temperature possible, but not above its melting point!
If it is obvious that using an oven is going to damage the sample, use a desiccator.
A fresh sample that has not had time to absorb moisture from the atmosphere is
always preferable and usually gives better results. If hygroscopic samples need to be
conveyed to the system over some distances, they should be sealed into tubes as
soon as possible with a silica gel bag if this is practicable.

Note
Application Notes describing how to develop a method for dry sample
analysis are available at www.malvern.com.

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Sample preparation guidance Chapter 6

Considerations for wet samples

This section covers sample preparation considerations for wet samples. When ana-
lysing a sample in a wet medium there are even more choices to be made than for
dry samples.

Choice and preparation of the dispersant

The majority of samples will allow water to be used as the dispersant. If the parti-
cles are soluble in water or react chemically an alternative must be used. For exam-
ple, flour added to water will float on the surface but it disperses well when added
to propan-2-ol (IPA).
The first choice to consider when measuring a wet sample is the choice of suspen-
sion medium (dispersant). When analysing a sample for the first time, it is always
best to check the dispersion beforehand. Add the selected dispersant (for an initial
measurement it is usual to use water) to a little of the sample in a beaker and visu-
ally note the result. The sample may dissolve; this can usually be seen visually. If
unsure, analyse the sample and observe the obscuration figure. If the obscuration
figure decreases the sample is probably dissolving.
The dispersant may itself contain impurities or particles that could be significant.
We recommend filtering the dispersant before use either with an in-line pipe filter
or, for small quantities, a syringe based disposable type. Filtration to 1 micron is
generally adequate with 0.22 microns being commonly available and an ideal size.
If the dispersant is stored under pressure or at low temperature it may be necessary
to consider degassing before use. A pressure release or a temperature rise will
reduce the solubility of gasses, resulting in the formation of bubbles in pipes and
cells, etc. Bubbles are a problem as they are measured with the sample and are
counted as particles, biasing the results. This is particularly a problem with some
mains water supplies. The simple answer is to store sufficient dispersant at room
temperature and pressure for several hours before use to allow the degassing to
occur. Also see the section on bubbles later in this chapter.
Note that the use of cold dispersant in a warmer environment can also give rise to
condensation on the outside surfaces of the cell windows. For systems plumbed
into the mains supplies a small header tank may overcome this problem. Filter this
water prior to use. Another solution is to warm the dispersant (for water typically to
60-80 C) and then allow it to cool before use.

Warning!
Do not warm a dispersant to allow re-gassing if the dispersant is volatile.
Never allow dispersants to reach their boiling points.

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Chapter 6 Sample preparation guidance

If condensation is a problem in a water-based system, a quick remedy is the addi-

tion of warm water to the sample tank. The increase in obscuration caused by the
condensation will quickly disappear.
When analysing particles suspended in a liquid dispersant, one of the most impor-
tant decisions is which liquid to use. The dispersant can be any clear (at 633nm
wavelength), optically uniform liquid that does not interact with the sample caus-
ing it to change its size. Clearly users wish to use the safest, lowest cost liquids that
are effective. Particles that give problems, such as dissolution, in one medium may
be quite suitable in another.

Warning!
If a volatile solvent has to be used as dispersant, leave the sample area door
open during use to aid ventilation.

Whenever difficulties in dispersion are experienced, consider using another disper-

sant. This list gives commonly used dispersants with their refractive indices:

Dispersant Refractive index

Water 1.33
Ethanol 1.36
Propan-2-ol (Isopropyl-alcohol) 1.39
Dimethyl Digol 1.41
Butanone 1.38
Hexane 1.38
Acetone 1.36

The cost of some of the organic dispersants may limit their use to the Hydro MV,
which typically only uses 120ml of dispersant. The problem of the safe disposal of
the sample after measurement must also be considered. Always adopt the correct
procedures for disposing of the sample and dispersant, following any local guide-
lines. Most local regulations forbid hazardous samples and dispersants to be tipped
down the drain, allowing them to enter the water system.

Note
Application Notes describing how to develop a method for wet sample
analysis are available at www.malvern.com.

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Sample preparation guidance Chapter 6

Surfactants and admixtures

If experiencing problems such as the sample floating on the surface of the disper-
sant, addition of a surfactant or admixture may help.

Surfactants
Adding a surfactant may help in preparation of the sample it will lower the surface
tension, which promotes wetting of the particles.
Surfactants have to be added in minute quantities, typically one drop per litre of
dispersant. If too much surfactant is added the action of stirring and pumping the
sample may cause it to froth, causing bubbles to be introduced into the system.
Bubbles are seen by the system as particles which can bias the measurement. Anti-
foaming agents may be added to prevent the formation of bubbles but, owing to the
fact that these may contain particulates, they should be added to the dispersant
before the background is measured.
Try adding a drop of surfactant to a quantity of sample and dispersant mixed in a
small beaker. If the sample sinks to the bottom of the beaker in large clumps, dis-
pose of the sample and start again. This time add the sample to a dry beaker, add a
drop of surfactant and mix thoroughly to a thick paste. Add the dispersant and mix
well. This usually avoids the agglomeration caused by adding the dispersant first.
A list of recommended surfactants in order of common use is given below:

Surfactant Nature
Igepal Non-ionic
Teepol L Non-ionic
Synperonic N Non-ionic
Aerosol OT Anionic (solid)
Sodium dodecyl sulphate Anionic
Hyamine 2389 Cationic

Admixtures
Admixtures work by causing the particle surface to become charged, causing parti-
cles to repel each other (i.e. providing a zeta-potential to aid dispersion). Admix-
tures are added in larger quantities, typically 1g/l. A list of commonly used
admixtures is given below:
Sodium Hexametaphosphate (e.g. Calgon)
Sodium Pyrophosphate
Trisodium Phosphate
Ammonia

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Chapter 6 Sample preparation guidance

Sodium Oxalate
Calcium Chloride
As many of these are solid materials that are dissolved into the dispersant, the solu-
tion should be filtered after preparation to remove impurities.

Slurries
The act of mixing up a small quantity of concentrated sample, dispersant and addi-
tives before it is added to the dispersion unit tank is known as preparing a slurry.
Once the particles have been successfully dispersed into a slurry, the sample may be
added to the dispersion unit without any further additions of surfactants etc. The
problem of the sample settling out within the beaker can be solved by using a
pipette to continually stir the sample. While stirring, continually fill and empty the
pipette. Use the pipette to add the sample to the dispersion unit tank.

Use of ultrasonics
In addition to the processes described above, ultrasonics can be applied to help the
dispersion, whether or not it contains a surfactant.
When mixing the sample in the suspension medium, a visual inspection often
shows whether ultrasonics are necessary. If large agglomerates of particles sink to
the bottom of the beaker, try applying two minutes of ultrasonics by placing the
slurry and its beaker in an ultrasonic bath. It will be immediately apparent if this has
been effective. Further ultrasonics can be applied when the sample is added to the
tank, if necessary. This often prevents re-agglomeration, but is not always needed.

Note
Be wary of using ultrasonics with fragile particles; the ultrasonic action
may break up the particles themselves. If in any doubt, microscopic obser-
vation before and after the ultrasonics can establish whether it has helped.

Samples with unstable concentrations

When adding the sample to the dispersion unit tank using the softwares Add sam-
ple facility, users may experience obscurations that change during the dispersion
period. Most samples disperse very quickly so users will not notice the obscuration
value rising. With some samples the slow dispersion of the sample can be clearly
seen. Do not make a measurement until the obscuration has stabilised, indicating
that the sample has properly dispersed. When adding very fine material and relying
on the action of the ultrasonics to achieve a good dispersion, add less sample than
you would expect. The action of the ultrasonics will cause the obscuration to rise.

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The obscuration and its behaviour during the dispersion of the sample can also
warn of other potential problems.
If the obscuration decreases the size of the particles within the sample may be
increasing; either the sample is sticking together or the particles are actually swell-
ing due to the dispersant. Other causes could be the larger particles settling out due
to inadequate pumping and stirring or even the particles dissolving.
If obscuration increases rapidly, particles may be attaching themselves to the cell
windows due to surface charges. This means material is in the laser beam continu-
ously and the obscuration appears to increase. To solve this, use an admixture.

Bubbles
The Mastersizer sees bubbles as particles and measures them. Bubbles vary in size
but are typically around 100 microns in size. In many cases these bubbles can be
seen clearly as a second and separate peak when the measurement data is analysed.
Always be wary of bubbles in the system.
When the dispersant has been added to the dispersion unit and circulated, we
advise stopping the unit briefly (using the Stop all operations button in the
Active Accessory control) to allow trapped air to escape the system. Also, during
installation, ensure there are no twists or loops in the connected sample tubing.
When adjusting the pump and stirrer speed for a particular sample, ensure the
speed is not so fast that it introduces air into the system.
When a surfactant is added to the sample, excessive speed of the stirrer/pump may
cause frothing. This will force bubbles into the system.

Degassing
If dispersant is stored under pressure or at low temperature, consider de-gassing
before use. The pressure release or temperature rise reduces the solubility of gases,
resulting in bubble formation in the pipes and tank etc. This is a problem with
some mains water supplies. The best answer is to store enough dispersant at room
temperature and pressure for several hours before use to allow de-gassing to occur.
For more information see Choice and preparation of the dispersant above.
Pulses of ultrasonics can help to degas the dispersant after the tank has been cleaned
and filled with fresh dispersant. To do this, use the Active accessory control
panel (Tools-Accessories) and then select Enable pulsed sonication.

Note
Ensure that all dispersants are degassed before being added to the system.

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Chapter 6 Sample preparation guidance

Symptoms of poor sample preparation

Use this table to identify sample dispersion problems:

Problem Symptom Action

Sample dissolving Obscuration decreases. Try another dispersant.
Dispersant contains Poor background read- Filter the dispersant
impurities ings. before use.
Bubbles within the dis- Bubbles typically show Degas the system.
persant as a secondary peak at
100 microns.
Sample floating on the Sample seen on the sur- Add surfactant or
surface of the dispersant face of the dispersant in admixture.
the tank.
Sample clumps together Obscuration decreases. Add surfactant or admix-
ture, or use ultrasonic
action.
Sample sinks to the bot- Obscuration decreases Increase the pump/stir-
tom as the larger particles rer speed.
settle out.
Sample swells in disper- Obscuration decreases. Try another dispersant.
sant
Particles sticks to the Rapidly increasing Use an admixture or sur-
windows obscuration. factant.
Condensation on the cell Rapidly increasing If (and only if) the disper-
windows obscuration. sant is water, add a
quantity of hot (not boil-
ing) water to the tank. If
the obscuration falls,
condensation is the
problem.
Bubbles sticking to win- Difficulty in obtaining low Drain the sampling tank.
dows background despite The bubbles will burst.
many rinses. Fill the system carefully
with degassed disper-
sant. In a new system,
adding Decon 90 to the
tank overnight and rins-
ing 7 or 8 times will wet
out the cell surface and
reduce bubble formation.

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 7

Reporting
Introduction
Reports help to make sense of all the data that is generated in a Mastersizer meas-
urement. They enable you to graphically analyse measurement data and also isolate
areas that are of interest using tables and graphs.
This chapter provides the following information:
About reports.
Viewing and using reports.
Creating and editing reports.

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7 Chapter 7 Reporting

About reports
Mastersizer's reports consist of information sections that are displayed together in a
single report for easy on-screen analysis or printing. Reports can be configured so
that only those items that are of interest to the user are displayed. It is also possible
to alter the order in which the report elements are displayed.

Note
It is only possible to edit user-defined reports, not those supplied with the
system. It is possible however to copy the system reports and create new
reports that are based on them.

Malvern reports
In addition to the ability for users to build reports tailored to their own require-
ments, Malvern Instruments supplies a number of standard reports with the soft-
ware. These are:
Analysis a report that provides a mixture of key parameter sections and a particle
size distribution graph. See Chapter 5 for more information on this report.
Data this report mainly focuses on the raw light scattering data gathered by the
instrument during the measurement. It includes a light scattering graph.
Parameters a summary of the key parameters measured by the system.

Note
Although the Malvern Reports cannot be modified directly, it is possible to
open them for editing and then use a different Report Title to effectively
save a copy.

Viewing and using reports

This section describes how to view and manipulate reports about the records con-
tained within measurement files. It is assumed that a measurement file is open and
that it contains several records.

Displaying reports
1. Select a record or number of records from the Record View.

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Reporting Chapter 7

2. If it is not already shown in the current view, select the Reports tab. One of
the reports for the current workspace is then shown (by default this is the Anal-
ysis report).
It can be easier to work in 2-pane Vertical Split view whilst initially selecting
the records. Any selections or de-selections of records are then updated imme-
diately in the visible report.

Collapsing/expanding report sections

To collapse the individual sections within a report, click the up arrow icon to
the left of the report section title. To expand an already collapsed report section,
click the down arrow icon to the left of the report section title.

Graphs
Three types of graph are used within the reports: result, trend and data graphs.
Whenever a graph is displayed, click on the plot lines to display data points. Move
the mouse pointer over the data lines to see numerical information relating to that
data point.

Scrolling layout/paging layout

By default, reports are presented in sections that are stacked vertically. To reveal all
of the information on the report requires the use of the scroll bar; this is the
Scrolling Layout.
To present the information on the report horizontally, click the Paging Layout
button on the bottom left of the report. When Paging Layout is selected either
use the horizontal scroll bar or to click the arrows next to the page numbers at the
foot of the report in order to view all of the information.

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Chapter 7 Reporting

Zooming in and out of reports

To zoom in and out use the Zoom slider on the bottom right of the
report pane. In Paging Layout view, the number of pages in the report is adjusted
accordingly.

Selecting reports to display in a workspace

The set of reports that are displayed are associated and saved with the workspace
that is currently selected. See Workspace Viewer in Chapter 3 for more informa-
tion. This section gives information on how to choose the set of reports that are
shown in the current workspace and how to arrange the order of the report tabs
shown.
1. From the Workspace Viewer panel, select the workspace for which you wish
to select reports.
2. From the Reports section of the Home ribbon, choose Report Selector to
display the Report Selection window.

3. This window contains a list of Available Reports on the left and Selected
Reports on the right. Reports shown with are reports that were created by
Malvern Instruments.
4. Move reports from the Available Reports column to the Selected Reports
column by selecting them and then clicking the Add button. Similarly, move
Selected Reports back to the Available Reports list by selecting them and
then clicking the Remove button.

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5. To move a report up or down within the Selected list, select it and then click
the up or down arrow icons as required. The order of this list corre-
sponds to the left/right position of the Reports tabs, the leftmost tab being the
top report in the Selected Reports list.
6. Click OK when you have organised the reports as required.

Trend Graphs (in reports)

Similar to the trend plot shown in Manual Measurements, the reporting trend
chart shows a graphical plot for each record from a measurement that is currently
selected in the Record View.
By default trend graphs plot Dv10, Dv50, Dv90 data against record number. Each
parameter is given a different colour. Click on the graph line to reveal data points -
move the mouse pointer over those points to reveal numeric values.

Editing a Trend Graph

To alter the axis scaling limits:
1. Move the mouse pointer over the X or Y axis to display the scale adjustment
feature.
2. Click MANUAL and then enter the required lower and upper limits (click
anywhere outside the input box to confirm the figure).
3. To return the graph to the automatically-adjusted setting, click AUTO.

Tip
This feature is also available in the live Trend View, Light Scattering
and Size Distribution panels in the measurement window.

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Chapter 7 Reporting

To alter the information shown on the graph:

1. From the report editing mode, click the properties button next to the graph
you wish to alter. The Trend Chart Properties window is displayed.
2. Select either the X or Y Axis button on the left. The data currently plotted is
shown in the top panel of the window.

3. To remove the currently plotted data, click next to the parameter descrip-
tion.

4. To add or select a new data item against which to plot, click the button.
A new <Empty Axis> element is added into the top panel.
5. Select the new <Empty Axis> element to display its properties in the lower
panel.

6. Click the button to add a parameter from the Report Parameter

Selection window.

Note
Parameters with numeric values (such as percentiles) are editable and indi-
cated with . To edit the parameter numeric value, click the parameter
and amend the value. Any value entered that is inappropriate for the
parameter is flagged with an exclamation mark icon - amend the value
accordingly if this is the case. It is possible to enter multiple variants of the
same parameter with different values associated (for example Dv10, Dv50
and Dv90). These are then indicated on the graph with different colours.

7. Select the Position in which the axis should be labelled - left or

right.

8. Finally, choose a Scale Type of - Linear or Logarithmic.

9. Click OK when you have completed the settings.

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Printing reports
Before sending a report to the printer, it can be helpful to view a preview initially.
The print preview option shows how a report will appear when printed on paper,
enabling the effect of alterations to a report to be easily established without wasting
paper.
1. Choose Print-Report Print Preview from the ribbon. A preview of the cur-
rently selected report is displayed:

The following display options are available:

Zoom to zoom in and out of the print preview, click the icons
respectively. When zoomed in it may be necessary to use the scroll bars in
order to see all of the elements on the report.
100% shows the report at 100% zoom.

Page width stretches the page to view the width of the page within the cur-
rent window.

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Chapter 7 Reporting

Whole page zooms out to so that an entire report page can be viewed in the
window.
Two pages zooms out so that two pages of the report can be seen side by
side.

Note:
Use of these options does not have any impact on the final report printout.

2. To print the report, click the Print icon .

Creating and editing reports

In addition to the standard Malvern reports shipped with the system, the Master-
sizer 3000 provides a quick and simple way to define and modify reports to a user's
specification. This section gives information on how to define and modify reports.

To create a new report (or edit an existing report)

1. Choose New from the Reports section on the ribbon (or choose New from
the Documents section of the ribbon and then select Report). To edit an
existing report, first select the report from the Report tab and then choose
Edit from the Reports section of the ribbon.

The report is now displayed in edit mode.

Note:
Actual data from the selected measurements is still shown whilst in edit
mode. This greatly simplifies the process of visualising the final output.

2. Enter an appropriate name for the report in the top field (New Report is shown
by default). The report name is used to identify the report in the Reports tabs
and can be modified later if required.

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Reporting Chapter 7

3. To add a new item to a report, click the Insert new item

here button. If editing an existing report, this button is
placed between each section of the report.
4. The Add a Report item window is displayed, from which the following
choices are available:

Add a parameter grid - a parameter grid contains just parameter informa-

tion, it is also possible to then select the individual parameters that are required.
Add a graph - choose from either the Result, Trend or Data graph type.
Add a table - choose from either the Result, Trend, Data or Fit table.
5. Choose one of these options and then select a more specific kind of report ele-
ment from the window that follows.

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Chapter 7 Reporting

The new section is now added to the report in the main report editing window.
In this example, a parameter grid has been added:

6. To undo the last change made to the report, click the Undo button . If
required, continue to click Undo until all edits in that session have been
undone. To re-do a change that has been undone, click the Redo button .
7. Click anywhere in the report section's heading area to activate the cursor, then
edit the heading for the report section as required.

Tip:
To display a thumbnail preview of the complete report move the mouse
pointer over the icon.

8. To move items up or down in the report, click the arrow buttons on the
right of the item. Alternatively, click and hold the icon and then drag
the element up or down to the required position.

Tip:
To move items around a large report it is often easier to zoom out initially
(so that more of the report is visible) and then drag the report section to
the required area of the page. The mouse pointer must not be positioned
over any of the buttons when clicking and dragging.

9. When you have finished editing the report, click the Finish Editing button at
the top of the window.
10. The software asks whether you would like to save (changes to) the report -
click Save, Don't Save or Cancel as required.

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 8

System security
About security
By default the Mastersizer software uses Windows user security. That is, only a
user logged into the computer that is physically connected to the instrument can
access the system. For many environments this level of security is sufficient.
For quality controlled environments however, the optional Malvern Access Con-
figurator (or MAC) adds a fully-featured security system to the Mastersizer soft-
ware. The MAC not only provides control over an individual users access to the
various features of the software, but also logs an audit trail of significant system
events, who performed them and when.

Activating security
Note:
This process should only be undertaken after setting up security privileges
for Mastersizer 3000 in the MAC.

1. Choose Options from the application button menu to display the

Mastersizer 3000 Options window and then choose Security.
2. Select Enable security features to activate the security features - this option
is only available if the optional Malvern Access Configurator (MAC) is
installed.

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8 Chapter 8 System security

3. Once selected, the user is prompted to enter a user name and password:

The user who logs in must be a user with both administrative rights on the
computer and also one who has been set up with Disable/Enable Security
permission in the MAC.
4. Click the Validate credentials button.
5. Select Browse and then locate the security definitions file (permissions.xml).
This file can be located wherever required but, by default, it is located in:
C:\Program Files\Malvern Instruments\Mastersizer 3000
6. Click OK to finalise the process.
Following this, only users with valid permissions that have been set up in the MAC
will be able to access the functions of the system.

Software licensing
Without a valid licence, the Mastersizer software will not function. The software
automatically generates a licence on the computer that is connected to the instru-
ment. After first installation of the software you will be prompted to accept this
license.

Click Accept licence to accept the license file. If the software was set up by
your administrator or Malvern Instruments, you may not see this window -
this means that the software is already activated.

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System security Chapter 8

Sharing a licence file

You can share a Mastersizer software licence so that other computer can use the
software without having an instrument connected. This could be useful if you
wanted to undertake analyses on measurement files whilst away from instrument.

Note:
The licence file contains the identification of the user and the instrument
from which it was generated. Do not share the licence outside of your
authorised user group.

1. From the Application button menu, choose About.

2. Click the View licence button to display details of the active licence.
3. To export the licence, click Share this licence - the software provides details
about what is included in the licence.

4. Click Yes and then specify a file name and location in which to save the
licence. Then just send a copy of this .licence file to the Mastersizer 3000 soft-
ware user without a licence. After first attempt to run the software, the user is
prompted with the following:

5. Click Install licence and then browse to the location of the .license file.
6. The credentials of the licence file are then displayed - click Install licence.

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Chapter 8 System security

Audit history
Note:
Auditing is only available when 21CFR Part 11 mode is enabled. This
requires a special feature key, which can be purchased from Malvern
Instruments.

Enabling auditing
After you have purchased a feature key from Malvern Instruments:

1. Select Options from the application button menu.

2. Choose 21 CFR Part 11. and then enter the key you have been sent.
3. Click OK (the OK button is only available if you have entered a valid key).
4. Ensure that Enable auditing is selected.
Once enabled, the audit feature logs every system event and measurement record
amendment.

Viewing the audit history

1. To view the audit log click System from the Audit ribbon.
2. The Audit history window is displayed, which shows all non-archived system
events that have been recorded.

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3. Click on the column headers to sort the data or use the methods described for
filtering the record view (see Filtering the Record View in Chapter 5).
The log shows:
Time stamp the time in the following format:
YYYY-MM-DDTHH:MM:SS (e.g. 2011-05-05T12:55:35).
Action type a self explanatory name for the action performed, for example
RecordCreated, Record Edited, RecordDeleted, Startup etc.
User ID the unique ID of the individual user logged onto the system.
Computer ID the network name of the computer that accessed the system.

Tip
Right click a record from the Record View and choose View Record
Audit History to view a history of the selected record only.

For edited records, the following properties are shown in the expanded tree view:

Property the record property (for example, Sample Identifiers) that was
altered.
Old Value the previous value recorded for the property.
New value the new value recorded for the property.
Reason for change this is for averaged records only where a Reason was
specified by the user at the time the averaged record was created.
Modified file name the (.rmd) file name of the record that was modified.
Modified record the record number within the measurement file that was
modified.

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Chapter 8 System security

As the audit history records all significant system events, the log can grow quite
quickly, making it more difficult for a user to visually analyse the data. The
Archive schedule feature allows you to set the frequency for archiving for the
audit trail. The archived data is still available, but is stored separately to the active
archive. You can view archived data by selecting System (including archived
entries).
4. Click [Archive] Schedule from the Audit ribbon.

5. Choose a frequency of either Daily, Weekly or Monthly as required and then

click OK.

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 9

Advanced features
Introduction
Advanced users can exploit additional features of the Mastersizer software that are
not normally required as part of the basic measurement process. These features
enable a supervisor to set up options that may help operators use the system in a
more standardised way.
This chapter focuses on the following areas:
Doing more with SOPs, including how to set up SOP templates and analyse
the development history of an SOP.
Editing records that have already been made.
Exporting data and working with export templates.
Maintenance utilities.

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9 Chapter 9 Advanced features

Doing more with SOPs

Extracting an SOP from a measurement
From time to time it can be useful to extract the settings used to make a measure-
ment into an SOP, so that the same settings can be applied to further measure-
ments.
1. From the Record View, right click on the record that you wish to extract the
settings from and choose Extract SOP.
2. The SOP Editor is shown containing all of the settings used at the time the
measurement was created.
3. Save the SOP by choosing Save from the SOP Editors Windows Feature but-
ton menu.

Alternatively, save the SOP as an SOP Template by choosing Save as tem-
plate. Refer to Creating and Editing an SOP in Chapter 4 for more informa-
tion.

SOP Templates
SOP templates allow you to create SOPs based on predefined settings, improving
both the speed of creation and consistency. Effectively SOP templates are just
SOPs with additional, optional, metadata attached to them; a Name, Description,
Category and image. It is a good idea to create a template whenever the core set-
tings of an SOP are to be used repeatedly.
The process of creating an SOP template is very similar to creating a standard SOP.
You can either create an SOP from scratch and then save it as a template, or open a
previously created SOP/template, make amendments to it and then save it. SOP
templates can be edited, saved as new templates or just saved as standard SOPs.

Note:
SOP Templates are stored as .msot files in the Windows file structure. If
required, use the Workspace shortcut from the Workspace Viewer panel to
locate the SOP Template folder (the templates are organised in folders
based on any categories that users have assigned to the templates). If any
associated image is removed from the SOP Template folder, a default
image is used instead.

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Creating an SOP template

1. From the Home ribbon select New-SOP.
2. Then select the appropriate template from the list (or From existing SOP...)
and click OK.
3. Edit the SOP details as required and then choose File-Save as template.

4. In the Save SOP Template window, give the new SOP template a: Name (a
descriptive name for the SOP template), a Description and, if required, assign
a Category (previously added categories are available from the drop down
menu). Categories could be of assistance when your environment has multiple
SOP templates.
5. To save over an existing SOP template (i.e. to edit an existing template), select
Allow new template to override any existing template from the Save
SOP Template window. Also, ensure that the new template uses the same
name as the existing template.

Tip:
To view a set of pre-selected SOP templates relevant only to the currently
attached dispersion unit, choose File-New from the Manual Measure-
ment settings window.

SOP Summary Report

The SOP Summary Report feature provides a simple means of quickly observing
the SOP settings that were used for an individual or multiple records in a measure-
ment file.

Mastersizer 3000 Page 9-3

Chapter 9 Advanced features

1. In the records view, select the record(s) for which you want to review the SOP
summary and then click View SOP summary on the Home ribbon. Alterna-
tively, from the SOP Editor, choose View-Summary Report.
The SOP Summary report window is displayed. This lists all settings applied
by the SOP at the time of measurement. If more than one record is selected
from the records view, each record is shown in its own column.

2. To Save, Copy (to clipboard) or Print the information shown, click the
appropriate option from the SOP Summary Report window toolbar. The date
that the SOP summary was created is appended to all three options.
3. Select the following options from the SOP Summary Report window tool-
bar as required:
Show all - this is the default view and shows all SOP settings from all
items.
Highlight differences - shows all items (as the default view), but high-
lights using different colours, areas where different values or SOP settings
were applied.
Show only differences - shows all items, but only those SOP settings
where differences exist.

Page 9-4 MAN 0474

Advanced features Chapter 9

Compare to - becomes active when either Highlight Differences or Show

only differences is selected. This option then allows you select a 'source'
item against which to compare the others - any field in another item that
differs from the source is highlighted or isolated (as selected).
4. Select any required View options from the list as follows:
Column headers in each section - adds each record name to each sec-
tion's header.
Move source column to the left - moves the column selected in the
Compare to field to the leftmost position for easier analysis.

SOP History
Each time an SOP is edited and re-saved, its history is recorded for future audit
purposes. The SOP History feature exposes any differences between versions of
the SOP.
This feature only applies to SOPs that have been revised and re-saved. If the Save
As option is used the SOP's history is not maintained.
1. Select View SOP History from the Home ribbon and then choose the
required file. The SOP Version History window is displayed. This lists all
parameters as applied by the SOP. Each version of the SOP is shown in its own
column.
2. To Save, Copy (to clipboard) or Print the information shown, click the
appropriate option from the SOP Version History window toolbar. The date
that the SOP history summary was created is appended to all three options.
3. Select the following options from the SOP Version History window toolbar as
required:
Show all - this is the default view and shows all SOP settings from all
items.
Highlight differences - shows all items (as the default view), but high-
lights using different colours, areas where different values or SOP settings
were applied.
Show only differences - shows all items, but only those SOP settings
where differences exist.
Compare to - becomes active when either Highlight Differences or Show
only differences is selected. This option then allows you select a 'source'
item against which to compare the others - any field in another item that
differs from the source is highlighted or isolated (as selected).

Mastersizer 3000 Page 9-5

Chapter 9 Advanced features

Editing results
This section provides help on the Edit Result feature of the Records view.
Each Mastersizer record is the result of the processing of raw measurement data.
By editing a record it is possible to re-apply new values to some of the parameters
used in the original measurement settings in order to generate a completely new
record.
1. From the Record View, right click on a record, or group of records, and choose
Edit Result. The Result Editor window is displayed.
This contains all of the information set up in the original measurement. Some
of the options are unavailable because they relate only to the physical set up of
the original measurement, for example, all of the Measurement Duration
options.
2. Edit any available sections of the Result Editor as required. Any edited infor-
mation is clearly highlighted by a different background colour (in the example
shown here the lower field has been edited).

3. Click OK when all settings have been altered to your specification. The newly-
set values are now re-applied to the existing raw measurement data. A brief
message is displayed whilst this happens. When the result has been edited, the
edited result is then displayed as the first item in a tree structure.
4. Expand the edited record to show the "contained" original result by clicking the
icon. It is not possible to edit a record without also retaining its original set-
tings. Further edits to the record result in more items contained within - the
most recently edited record is always shown as the container record (in this
example, edit 3 was the final edit made):

Note:
If you save the measurement file, the new settings will overwrite the origi-
nal settings. To create a result-edited version of a file and still retain the
original settings, first copy the file (using Windows) and then edit the copy.

Page 9-6 MAN 0474

Advanced features Chapter 9

Exporting data
Data recorded by the system can be exported for analysis in other software applica-
tions, for example Microsoft Excel.
It is possible to export either selected records or all records contained in a single
measurement. Additionally, by selecting the All Files tab when multiple measure-
ment files are open, a selection of, or all records from, multiple measurement files
can be exported.
The ability to create export templates further enhances the flexibility of the system,
allowing you to select only those parameters required for your analysis, as well as
providing control over other data formatting options.

Export data settings

1. To export selected records only, select the required records and choose Export
Selected Records from the Home ribbon. To export all records from the
currently active record choose Export All Records.
The Export Data window is displayed, which shows a preview of the data to
be exported as specified by the currently selected export template.

2. Select an appropriate export template from the drop-down list - the preview
pane is updated accordingly.
3. Change the presentation of the data using the Ordering, Delimiter, Format-
ting and Header options (see Export templates for more information).
4. Click Export to file to save the data as a separate (.txt or .csv) file, or select
Export to clipboard to copy the data to the clipboard.

Tip:
Drag and drop record data from the Record View straight into Microsoft
Excel/Word. The parameter values copied are all of those currently shown
in the records view.

Mastersizer 3000 Page 9-7

Chapter 9 Advanced features

Export templates
Export templates provide a means of storing, and quickly accessing, commonly-
used sets of parameters and format settings for exporting data. You can build and
store any number of export templates.

Note
Each export template is associated only with the workspace in which it was
constructed. This means, for example, that a template defined in the Mal-
vern default workspace, will not subsequently be displayed in a custom
workspace.

Creating or modifying an export template

1. To create a new export template: from the Home ribbon select New-
Export template (or click Add from the Export Data window).
To modify an existing template: select it from the drop down in the
Export Data window and click Modify.
The Export Template Settings window is shown:

2. Enter a Name and then a short Description that explains the purpose of the
template. For example, Name: "Quick size results", Description: "Size infor-
mation plus sample ID only". The list of parameters associated with the tem-

Page 9-8 MAN 0474

Advanced features Chapter 9

plate is displayed in the Parameters panel. Initially this consists of the whole
set of system parameters.
3. Click the Change selection and order button to show the Parameter
selection window, then select the required parameters as follows:
Locate parameters by manually expanding the tree structure in the Availa-
ble list, or search for them by typing their first few characters into the
Search... field.
Select a parameter in the Available list and then click the Add button to
transfer it to the Selected list. Similarly, select an item from the Selected
list and click the Remove button to transfer it to the Available list. It is
also possible to select multiple items using the standard Windows selection
methods (i.e. SHIFT and click, CTRL and click).
When all of the required parameters are shown in the Selected list, choose
an order of presentation so that they are shown in the desired left-to-right
order. Select a parameter and then click the up/down buttons to move its
position in the list. Items at the top of the list are shown on the left, items
at the bottom are shown on the right.
Click Apply to apply the settings without closing the window, or click OK
to apply the settings and also close the Parameter Selection window.
4. Choose either rows or columns from the Ordering selector to present the data
horizontally or vertically respectively.
5. From the Delimiter selection, choose either Comma separated (csv) or
Tab separated. Your choice will depend on the requirements of the target
application.
6. Use the Formatting option to select either Format values as displayed in
software, which displays numeric information to a limited number of decimal
places (this may be preferable for presentation purposes); or choose Unfor-
matted values to show all data as recorded by the system.
7. Select Header on/off to specify whether the export should contain the names
of the fields as a header row (or column).
8. Click Save when complete.

Deleting an export template

From the Export Data window, select the template you wish to remove and click
Remove. The software asks for confirmation of the action before permanently
removing the template.

Mastersizer 3000 Page 9-9

Chapter 9 Advanced features

Page 9-10 MAN 0474

Part 3 -
Appendices
 A

Setup reference
Introduction
This chapter provides the following information:
Software installation reference.
Connection reference.
Testing the system.

Installing the software

If the computer was supplied by Malvern, all software will be pre-installed. If not,
follow the procedure described in the Software Update Notification document
that was supplied with the software CD, which also details the minimum system
requirements. If this document is not present, contact Malvern Instruments.

Mastersizer 3000 Page A-1

A Appendix A Setup reference

Making connections
This section explains how to reconnect the system if it is moved after it has been
commissioned. Systems must be commissioned initially by a Malvern Instruments
representative. Commissioning is the process of ensuring a that a safe physical
installation of the Mastersizer 3000 has taken place together with a formal verifica-
tion process to ensure that measurements are accurate.

Connection prerequisites
Ensure that the new location of the system has the correct services and space
before attempting to move the system see the Basic Guide for site requirements
information.
Before moving the system, ensure that any wet dispersion units are drained, any air
lines for dry dispersion units vented, and the system allowed to cool. All pipes and
cables must be disconnected before moving a dispersion unit.

Post-connection verification
To verify that the system has not been affected by the move, make a measurement
of a standard sample before and after moving the system. If the results differ signif-
icantly, check the connections to see if any mistakes were made. Contact your Mal-
vern representative if the difference persists.

Page A-2 MAN 0474

Setup reference Appendix A

Connecting the optical unit and computer

1. With the computer switched off, connect one end of the USB cable to a free
USB port on the Computer and the other end to the USB port on the opti-
cal unit .
2. Connect the dispersion units CAN port to an available CAN port on the
optical unit (there are three CAN ports on the optical unit).

4 3 6 7
ill 8627
3. Plug the power cable into the power supply unit and connect the power
cable from the power supply unit to the optical bench power input but do
not connect to the mains power supply at this point.

Warning!
We recommend that the computer and waste sink are not adjacent.

4. Ensure the dispersion unit tubing is connected correctly, using the following
sections for reference.

Mastersizer 3000 Page A-3

Appendix A Setup reference

Connecting dispersion unit tubing

Refer to the Basic Guide or individual dispersion unit manuals for details on
tubing connection.

Testing the system

Use these checks to verify that the system is still working correctly after the move:
The indicator on the optical bench should be blue.
The indicator on a dispersion unit with its cell attached to the optical bench
should be blue.
The software should indicate that the USB connection to the instrument is
active (by showing this in green in the status bar) and also show any dispersion
unit connected to one of the instruments CAN ports.

To verify that the system is still working correctly, make another measurement
using the standard sample and compare the results to those obtained before moving
the system.

Page A-4 MAN 0474

 B

Specifications
Optical unit
All specifications correct at time of publication, but may be subject to alteration.

Size range 0.01 - 3500 microns*

Accuracy Better than 1%**
Measurement Mie and Fraunhofer scattering
principle
Detection systems Red light: Forward scattering, side scattering and
back scattering.
Blue light: Wide angle forward and back scattering.
Light sources Red light: Max. 4mW He-Ne, 632.8nm
Blue light: Max. 10mW LED, 470nm
Laser Class Class 1, EN 60825-1:2007 and CDRH
IP Rating Designed to meet IP41B
Lens arrangement Reverse Fourier (convergent beam).
Sample dispersion unit Sample dispersion units automatically recognised,
interchange system. configured and enabled on insertion of measurement
cell cassettes into optical bench.
Storage conditions -20 to +50C, 10%-80% RH (non-condensing)
Operational conditions +10 to +35C, 10%-80% RH (non-condensing)
Power 110/240V, 50/60Hz, 60VA
Dimensions Length: 690mm / Depth: 300mm / Height: 450mm
Weight 30kg
*Sample/preparation dependent. See dispersion unit guides for wet/dry size ranges.
**Accuracy defined for the recovery of the mean size of a narrow log-normal dis-
tribution. Sample and sample preparation dependent.

Mastersizer 3000 Page B-1

B Appendix B Specifications

Chemical compatibility
The Mastersizer and its dispersion units have been manufactured from materials
that are considered to give the widest protection from chemical attack. However, it
is important to check that any sample or dispersant you may use is chemically com-
patible with the materials that they will come in contact with within the system.
In normal operation the sample and dispersant should not come into contact with
any component of the optical bench (the sample path is contained within the dis-
persion unit and the sample cell). However, if a sample pipe or sealing ring should
fail then sample and dispersant may drip into the cell area of the optical bench. A
drain is fitted in the base of the cell area to limit the spread of any leak.
Should a small leak occur the sample/dispersant may come into contact with the
following materials:

Component Materials
Detector lens Glass
Protection window Glass
Cell bay walls Aluminium (hard anodised)
Cell bay base Aluminium (hard anodised)
Drain assembly Stainless steel, Tygon tubing
Cell and dispersion unit See applicable dispersion unit manuals

Caution!
The paint finish of the external covers may be permanently damaged if
samples or dispersants are spilt on them. Clean up any spillage immedi-
ately.

Remember to check the chemical compatibility of the sample dispersion units

before using a new sample and dispersant.

Page B-2 MAN 0474

Specifications Appendix B

Regulatory Information
Disposal of Electrical & Electronic Equipment
This regulation is applicable in the European Union and other European countries
with separate collection systems.

ill 7610
This symbol on the product or on its packaging indicates that when the last user
wishes to discard this product it must not be treated as general waste. Instead it
shall be handed over to the appropriate facility for the recovery and recycling of
electrical and electronic equipment.
By not discarding this product along with other household-type waste, the volume
of waste sent to incinerators or landfills will be reduced and natural resources will
be conserved. 0
For more detailed information about recycling of this product, please contact your
local city office, your waste disposal service, or Malvern Instruments.

Mastersizer 3000 Page B-3

Appendix B Specifications

CE Declaration of Conformity
The CE badge on this product signifies conformance to the following European
Directives:
EMC directive 2004/108/EC {BS EN 61326-1: 2006}
Low Voltage Directive 2006/95/EC {BS EN 61010-1: 2010}

FCC Notice (US only)

The Federal Communications Commission (FCC) mark on this product signifies
conformance to FCC regulations relating to Radio Frequency Devices. These have
been satisfied by testing the product against, and being found to be compliant with:
FCC CFR 47 Part 15:October 2010.Class A digital device.
The device complies with part 15 of the FCC Rules. Operation is subject to the
following two conditions:
1) This device may not cause harmful interference, and
2) This device must accept any interference received, including interference
that may cause undesired operation.

Note
This equipment has been tested and found to comply with the limits for a
Class A digital device, pursuant to part 15 of the FCC rules. These limits
are designed to provide reasonable protection against harmful interference
when the equipment is operated in a commercial environment.

This equipment generates, uses, and can radiate radio frequency energy
and, if not installed and used in accordance with the instruction manual,
may cause harmful interference to radio communications. Operation of
this equipment in a residential area is likely to cause harmful interference
in which case the user will be required to correct the interference at his
own expense.

Note
Changes or modifications not expressly approved by Malvern Instruments
Limited could void the users authority to operate the equipment.

Page B-4 MAN 0474

Specifications Appendix B

Canadian Regulatory Information

(This applies to Canada only.)
This digital apparatus does not exceed the Class A limits for radio noise emissions
from digital apparatus set out in the Radio Interference Regulations of the
Canadian Department of Communications.
Note that Canadian Department of Communications (DOC) regulations provide,
that changes or modifications not expressly approved by Malvern Instruments
Limited could void your authority to operate this equipment.
This Class A digital apparatus complies with Canadian ICES-003.
Cet appareil numrique de la classe A est conforme la norme NMB-003 du
Canada.

VCCI acceptance (Japan only)

The Voluntary Control Council for Interference (VCCI) mark on this product
signifies compliance to Japanese EMC regulations as specified by VCCI.

ill 8708
Translation:
This is a Class B product based on the standard of the Voluntary Control Council
for Interference from Information Technology Equipment (VCCI). If this is used
near a radio or television receiver in a domestic environment, it may cause radio
interference. Install and use the equipment according to the instruction manual.

Mastersizer 3000 Page B-5

Appendix B Specifications

Page B-6 MAN 0474

 Index
A Connecting dispersion unit tubing A-4
Connection panel 2-8
Access to the instrument 1-2 Control ribbon 3-3
Accessory controls (manual mode) 4-18
Admixtures 6-7 D
Aero S settings 4-22
Data Processing
All files 3-3, 5-5
analysis 4-40
Analysis report 7-2
User Sizes 4-41
Analysis settings
Advanced 4-41 Data Quality 3-3, 3-7
Data report 7-2
Ancillary switching unit 2-6
Degassing 6-9
Audit history 8-4
Dispersant
averaged record 5-6
choice and preparation 6-5
B contains impurities 6-10
Dispersion units 2-2
Beer-Lambert law 5-12 Distribution 5-11
Bubbles Drain 2-8
degassing 6-9 Dry dispersion unit 2-5
problems 6-9 Dry samples 6-4
sticking to windows 6-10
E
C
Editing results 9-6
CAN ports 2-9 Enable security features 8-1
Cell 2-2, 2-7 End panel 2-8, 2-9
about 2-2 Equivalent spheres 5-16
bay 2-8 Export Data window 9-7
dry 2-5 Export templates
eject button 2-10 about 9-8
handle 2-10 creating 9-8
inserting/removing 2-11 deleting 9-9
sample input (blue) 2-10 Exporting data 9-7
Sample output (yellow) 2-11
Temperature regulator throughput 2-11 F
wet 2-4
Federal Communications Commission B-4
windows 2-11
feet (instrument) 2-8
Concentration
at different obscurations 5-14 Fraunhofer model 5-19
calculating 5-12 G
definition 5-10
how calculated 5-12 General Preferences 3-11
volume calculation 5-12 Graphs 3-12
Condensation on cell windows 6-10

Mastersizer 3000 Page 1

 Index Mastersizer 3000

H P
Hydro EV 2-3 paging layout 7-3
Hydro EV settings 4-21 Parameter filters 5-3
Hydro LV/MV 2-3 Parameters report 7-2
Hydro LV/MV settings 4-19 Power input 2-9
Hygroscopic samples 6-4 Power switch 2-9
Protection window 2-8
I
Q
Installation
guidelines A-2 Quick Access Toolbar 3-13
software A-1
R
K
Record
Kurtosis 5-18 edit 9-6
Record View 3-3
L
filtering 5-3
LED (status) 2-8 Refractive index
licence common dispersants 6-6
about 8-2 Remote support 1-5
sharing 8-3 reports
Logs 3-16 about 7-2
add item 7-9
M Analysis 5-9, 7-2
Maintenance utilities 3-15 creating 7-8
Malvern Access Configurator 8-1 Data 7-2
Malvern personnel 1-2 displaying 7-2
Malvern reports 7-2 editing 7-8
manual measurements 4-14 graph 7-9
Measurement Duration 4-30 Malvern 7-2
Measurement Obscuration 4-32 parameter grid 7-9
Measurement Sequence 4-31 Parameters 7-2
Measurement settings reference 4-23 printing 7-7
Mie theory 5-16, 5-20 table 7-9
Model number 1-5 workspace 7-4
zoom 7-4
O Reports tab 3-7
Reports tabs 3-3
Obscuration 4-32
Representative sampling 6-3
mathematical expression 5-10
Operator tasks 1-3 S
Optical model
Fraunhofer 5-19 Sample
Mie theory 5-20 symptoms of poor preparation 6-10
Optical unit 2-4, 2-5 Sample Dispersant 4-28
about 2-2 Sample Dispersion Accessory 4-34
Optical unit components 2-7 Sample dissolving 6-10
Options 3-11 Sample floating on dispersant 6-10
Sample Identification 4-24

Page 2 MAN 0474

Mastersizer 3000 Index

Sample Instructions 4-29 optical unit 2-7

Sample Material 4-27 wet 2-3
Sample preparation flow chart 6-2 System usage 3-16
Sample sinks to bottom 6-10
T
Sampling
representative 6-3 Testing system after move A-4
unstable concentrations 6-8 Themes 3-12
Save My Layout 3-12 Transmission 5-13
Scrolling layout 7-3 Trend Graph
security editing 7-5
activating 8-1 trend graph
Serial number 1-5 adding 4-11
Shortcuts 3-10 Trend Graphs 7-5
size bands 4-42 trend view
Skewness 5-18 about 4-8
Slurries 6-8 selecting range 4-10
Software statistics 4-9
installing A-1 Tube/cable routing 2-8
licence 8-2 Tubing connection
SOP dispersion units A-4
about 4-2, 4-4
creating/editing 4-4 U
extract 9-2 Ultrasonics 6-8
running (Aero) 4-12 Uniformity 5-11
running (Hydro) 4-6 Unstable concentrations 6-8
SOP settings USB port 2-9
Aero S 4-34
Hydro LV/MV/EV 4-36 V
Span 5-10
Vacuum unit 2-6
Spinning rifflers 6-3
VCCI acceptance B-5
SSA (Specific Surface Area) 5-11
Volume concentration
Standard deviation 5-18
how calculated 5-12
Status bar 3-3
Volume Weighted Mean 5-10
status bar 3-2
Volume-based results 5-15
Supervisor tasks 1-2
Surface Weighted Mean 5-10, 5-14 Voluntary Control Council for Interference B-5
Surfactants 6-7 W
System health checks 3-16
System information 3-16 Website 1-6
System overview Wet samples 6-5
dry 2-5 Workspace Viewer 3-8

Mastersizer 3000 Page 3

Index Mastersizer 3000

Page 4 MAN 0474

 Mastersizer 3000 user manual
www.malvern.com
3000

User manual

Malvern Instruments Limited

Enigma Business Park
Grovewood Road, Malvern
Worcs, WR14 1XZ, U.K.
Tel: +44 (0) 1684 892456
MAN0474
Fax: +44 (0) 1684 892789 MRK1738-01