INTERNATIONAL ISO

STANDARD 6145-7

Third edition
2018-12

Gas analysis — Preparation of

calibration gas mixtures using
dynamic methods —
Part 7:
Thermal mass-flow controllers
Analyse des gaz — Préparation
iTeh STANDARD PREVIEW des mélanges de gaz pour étalonnage
à l'aide de méthodes dynamiques —
(standards.iteh.ai)
Partie 7: Régulateurs thermiques de débit massique

ISO 6145-7:2018
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Reference number
ISO 6145-7:2018(E)

© ISO 2018
ISO 6145-7:2018(E)


iTeh STANDARD PREVIEW

(standards.iteh.ai)
ISO 6145-7:2018
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 ISO 6145-7:2018(E)


Contents Page

Foreword......................................................................................................................................................................................................................................... iv
1 Scope.................................................................................................................................................................................................................................. 1
2 Normative references....................................................................................................................................................................................... 1
3 Terms and definitions...................................................................................................................................................................................... 1
4 Symbols........................................................................................................................................................................................................................... 2
5 Principle......................................................................................................................................................................................................................... 2
6 Set-up................................................................................................................................................................................................................................. 2
6.1 General............................................................................................................................................................................................................ 2
6.2 Thermal mass-flow controller using a constant current supply................................................................... 3
6.3 Thermal mass-flow controller under constant temperature control....................................................... 3
7 Preparation of gas mixtures...................................................................................................................................................................... 4
7.1 Description of the experimental procedure.................................................................................................................... 4
7.2 Range of validity..................................................................................................................................................................................... 6
7.3 Operating conditions.......................................................................................................................................................................... 6
8 Calculations................................................................................................................................................................................................................ 7
8.1 Volume fraction....................................................................................................................................................................................... 7
8.2 Sources of uncertainty....................................................................................................................................................................... 7
8.3 Uncertainty of measurement....................................................................................................................................................... 8
iTeh STANDARD PREVIEW
Annex A (informative) Pre-mixed gases for the preparation of mixtures of high dilution........................... 9
Annex B (informative) Practical(standards.iteh.ai)
hints...............................................................................................................................................................10
Annex C (informative) Calculation of uncertainties ISO 6145-7:2018 ...........................................................................................................................12
Bibliography..............................................................................................................................................................................................................................
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ISO 6145-7:2018(E)


Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www​.iso​.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www​.iso​.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
iTeh STANDARD PREVIEW
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www​.iso​
.org/iso/foreword​.html. (standards.iteh.ai)
This document was prepared by Technical Committee ISO/TC 158, Analysis of gases.
ISO 6145-7:2018
Any feedback or questions on this document should be directed to the user’s national standards body. A
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complete listing of these bodies can be found at www​.iso​.org/members​.html.
d085bf377fb6/iso-6145-7-2018
This third edition cancels and replaces the second edition (ISO 6145-7:2009), which has been technically
revised. The main changes compared to the previous edition are as follows:
— correction of some errors in the formulae in Annexes A and C;
— minor editorial corrections.
A list of all parts in the ISO 6145 series can be found on the ISO website.

iv  © ISO 2018 – All rights reserved

INTERNATIONAL STANDARD ISO 6145-7:2018(E)

Gas analysis — Preparation of calibration gas mixtures

using dynamic methods —
Part 7:
Thermal mass-flow controllers

1 Scope
ISO 6145 is a series of documents dealing with various dynamic methods used for the preparation of
calibration gas mixtures. This document specifies a method for continuous preparation of calibration
gas mixtures, from nominally pure gases or gas mixtures by use of thermal mass-flow controllers. The
method is applicable to preparation of mixtures of non-reacting species, i.e. those which do not react
with any material of construction of the flow path in the thermal mass-flow controller or the ancillary
equipment.
If this method is employed for preparation of calibration gas mixtures the optimum performance is
as follows: the relative expanded measurement uncertainty U, obtained by multiplying the standard
uncertainty by a coverage factor k = 2, is not greater than 2 %.
iTeh STANDARD PREVIEW
If pre-mixed gases are used instead of pure gases, mole fractions below 10−6 can be obtained. The
measurement of mass flow is not absolute and the flow controller requires independent calibration.
(standards.iteh.ai)
The merits of the method are that a large quantity of the calibration gas mixture can be prepared on a
continuous basis and that multi-component ISO mixtures
6145-7:2018can be prepared as readily as binary mixtures if
the appropriate number of thermal mass-flow controllers is utilized.
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NOTE Gas blending systems, based upon thermal mass-flow controllers, and some including the facility of
computerization and automatic control, are commercially available.

2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 6143, Gas analysis — Comparison methods for determining and checking the composition of calibration
gas mixtures
ISO 6145-1, Gas analysis — Preparation of calibration gas mixtures using dynamic volumetric methods —
Part 1: Methods of calibration
ISO 7504, Gas analysis — Vocabulary
ISO 12963, Gas analysis — Comparison methods for the determination of the composition of gas mixtures
based on one- and two-point calibration
ISO 19229, Gas analysis — Purity analysis and the treatment of purity data

3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 7504 apply.

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ISO 6145-7:2018(E)


ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:​//www​.iso​.org/obp
— IEC Electropedia: available at: http:​//www​.electropedia​.org/

4 Symbols

Cp Heat capacity (at constant pressure)

i,k Indices for components in a gas or gas mixture

j Index for a parent gas

m Mass

p Pressure

q Number of components in the gas mixture

qm Mass flow rate

qV Volume flow rate

T Temperature

V Volume
iTeh STANDARD PREVIEW
Φ Heat flux
(standards.iteh.ai)
ISO 6145-7:2018
ϕ Volume fraction of a component in a parent gas
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φ Volume fraction of a component d085bf377fb6/iso-6145-7-2018
in a gas mixture

ρ Density

5 Principle
The continuous preparation of calibration gas mixtures from nominally pure gases or other gas
mixtures by the use of commercially available thermal mass-flow controllers is described. By
adjustment of the set-points on the mass flow controllers to pre-determined values, it is possible to
change the composition of the gas mixture rapidly and in a continuously variable manner. By selection
of appropriate combinations of thermal mass-flow controllers and with use of pure gases, the volume
fraction of the component of interest in the matrix gas can be varied by a factor of 1 000.

6 Set-up

6.1 General
To prepare a gas mixture, each gaseous component is passed through a calibrated thermal mass flow
controller (TMC) at a known and controlled flow rate and at constant pressure. Accurate flow meters
are used to measure the relevant flow rates in order to achieve an acceptable level of uncertainty
regardless of the setting of the mass flow controller (see also ISO 6145-1).
A TMC consists of a measuring unit for mass flow and a proportioning valve which is controlled by an
electronic unit (see also Reference [1] and [2]).

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 ISO 6145-7:2018(E)


6.2 Thermal mass-flow controller using a constant current supply

The flowing gas is passed through a heater connected to a constant current supply and the temperature
is sensed upstream and downstream from the heater.
Figure 1 shows the working principle of a TMC and its key parts: heater, temperature sensors and
associated circuitry. The two temperature sensors, one upstream and one downstream from the heater
form two arms of a Wheatstone bridge circuit, which is balanced to give zero reading when there is
no gas flow. When there is a gas flow through the system a temperature difference, ΔT, is established
between the two sensors such that the heat flux, Φ, is given by Formula (1):
Φ = C p ∆Tq m (1)

iTeh STANDARD PREVIEW

(standards.iteh.ai)
Key ISO 6145-7:2018
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1 temperature sensor 1 5 current supply
d085bf377fb6/iso-6145-7-2018
2 heater 6 wheatstone bridge
3 temperature sensor 2 7 differential amplifier
4 gas supply 8 signal readout

Figure 1 — Principle of a thermal mass-flow controller with constant current supply

The difference in temperature between sensors results in a potential difference across the Wheatstone
bridge circuit and thus a signal. The signal is compared with an adjustable reference voltage in a
differential amplifier. The resulting output signal is in turn used for operating a control valve to
regulate the flow of gas.

6.3 Thermal mass-flow controller under constant temperature control

In the system, shown in Figure 2, the parent gas passes through three heaters in sequence, each of
which is connected into an arm of a self-regulating Wheatstone bridge. Instead of the difference in
temperature being measured, the input to each heater is such that the temperature distribution along
the flow path is uniformly maintained. The Wheatstone bridge current is proportional to the heat loss
and therefore proportional also to the mass flow of the gas. The output signal is again used to operate a
solenoid valve to control the mass flow rate.

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ISO 6145-7:2018(E)


Key
1 heater 1 iTeh STANDARD
5 currentPREVIEW
supply
2 heater 2 6 wheatstone bridge
3 heater 3
(standards.iteh.ai)
7 differential amplifier
4 gas supply ISO 86145-7:2018
signal readout
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Figure 2 — Thermal mass-flowd085bf377fb6/iso-6145-7-2018
controller under constant temperature control

In the preparation of multicomponent mixtures, it is generally necessary to use one mass-flow controller
for each component. Dual-channel controllers are available and may be used in the preparation of
binary mixtures or, for example, preparation of mixtures of a given gas in air.

7 Preparation of gas mixtures

7.1 Description of the experimental procedure

A schematic diagram of the arrangement for preparation of binary mixtures is shown in Figure 3.
The pressure and temperature at the time of the calibration shall be recorded. Depending on the gases
to be mixed and their departure from ideality, the volume fraction can be somewhat influenced by the
ambient pressure and temperature. The pressure and temperature at the time of calibration of the
analyser should be as near as possible to those prevalent at the time the TMCs were checked by the
comparison method ISO 6143 or ISO 12963 (see 7.3).
Compositions of calibration gas mixtures are normally expressed by volume fractions but
manufacturers’ accuracy specifications for thermal mass-flow controllers are usually expressed in
terms of percentage of the full scale of the instrument. The relative expanded uncertainty of 2 %, which
is quoted in the Scope of this document, is 2 % of the volume fraction of the calibration component of
the mixture. This value assumes optimum use of each TMC in the system, which means that each is
operated at, or very near to, its maximum flow rate. Thus, if a TMC is operated at 10 % of full scale, the
expanded uncertainty expressed as percentage of maximum flow (as distinct from relative expanded
uncertainty) can be ±1 %, but if expressed instead as a percentage of the actual flow rate the relative
expanded uncertainty becomes 10 %.

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Key iTeh STANDARD PREVIEW

Matrix gas: (standards.iteh.ai) Calibration component:
1 cylinder of pressurized gas 7 cylinder of pressurized gas
2 pressure regulator 8 pressure regulator
ISO 6145-7:2018
3 shut-off valve 9 shut-off valve
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4 filter against contamination
d085bf377fb6/iso-6145-7-2018
10 filter against contamination
5 thermal mass-flow controller 11 thermal mass-flow controller
6 shut-off valve 12 shut-off valve
13 mixing vessel

Figure 3 — Mixing apparatus for preparation of binary gas mixtures

by means of thermal mass-flow controllers

A binary mixture containing the calibration component at volume fraction 1:11 could be prepared by
use of two TMCs each of full scale 1 000 mL/min by operating one at 100 mL/min and the other at
1 000 mL/min. However, the expanded uncertainty associated with the flow rate of the former would
be ±10 % of flow rate and the relative expanded uncertainty in the volume fraction would be ±9 %. Use
one TMC with a full scale range of 100 ml/min and a second one with a full scale range of 1 000 ml/min,
both being operated very close to full scale, so that the mixture has a volume fraction with a relative
expanded uncertainty of 2 %.
The same requirement shall be observed relative to preparation of multi component mixtures.
A method for which there is no requirement for calibration against external standards of gas flow rate
or volume fraction is described briefly in Annex B, and the reference to the publication which provides
the complete description is given in the bibliography.
As shown in Figure 3, gas cylinders (1) and (7)containing the matrix gas and the component of interest
respectively are connected to the thermal mass-flow controllers (5) and (11) through pressure
regulators (2) and (8) and shut-off valves (3) and (9). The two in-line filters (4) and (10) provide
protection against contamination. The gases from the flow controllers enter the mixing vessel (13).

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ISO 6145-7:2018(E)


The recommended working range for the pressure regulators is 60 kPa (0,6 bar) to 600 kPa (6,0 bar).
The pressure regulator for the “gaseous component” shall also be suitable for the particular component
involved (e.g. the diaphragm shall be of stainless steel or other corrosion resistant material). Similarly,
the thermal mass-flow controllers shall be suitable for use with the gaseous components and for the
requirements of the gas mixture.
Set the input pressures appropriate to the controllers using the pressure regulators and open the shut-
off valves (3), (6) and (9). Purge the inlet path of the gaseous component through the shut-off valve (12),
which shall be of a type which can be operated rapidly.
Adjust the set points of the controllers so as to obtain the respective flow rates in the correct ratio for
the desired composition of the binary gas mixture; meanwhile, continue the purging process of the
input tube for the component gas by multiple opening and closing of valve (12), until a total volume of
gas at least 10 times the volume of the flow path has been vented.
When the system has been thoroughly purged, feed the gases via the thermal mass-flow controllers
to the mixing vessel (13), constructed from inert materials. Provided that the resistance to flow
downstream of the mixing vessel (13) is low in relation to the flow being delivered at the source, the
mixture flows at ambient atmospheric pressure to the instrument.
Although for most applications the gas mixture will be transmitted at the prevailing ambient
atmospheric pressure, this method may also conceivably be applied to convey mixtures at elevated exit
pressures. However, in this case it would be necessary to give due consideration to changes in Cp and
density of the gaseous components with pressure in order to assess the validity of this procedure.

7.2 Range of validity iTeh STANDARD PREVIEW

(standards.iteh.ai)
As stated in the scope, this method is applicable to preparation of mixtures of non-reacting species, i.e.
those which do not react with any material of construction of the flow path in the thermal mass-flow
controller or the ancillary equipment. ParticularISO care shall be exercised if the method is considered as a
6145-7:2018
means of preparation of gaseous mixtures which contain components which form potentially explosive
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mixtures in air. Steps shall be taken to ensure that the apparatus is safe for example by means of in-line
d085bf377fb6/iso-6145-7-2018
flame arrestors in addition to the items listed in 6.1.
This method is not absolute and each thermal mass flow controller shall be calibrated for the particular
gas or gas mixture for which it is to be used.

7.3 Operating conditions

The conditions for efficient operation of the sensor system are that
— there shall be no heat loss or heat gain, other than that which results from the flow of gas, between
the region of the heater and that of the downstream sensor, and that
— there shall be uniform temperature distribution across the gas stream.
The assumption that Cp is constant is valid only over a restricted range of temperature. The general
precautions common to all dynamic techniques of preparation shall be observed. It is essential that
attention is paid to the materials used in the construction of the flow system. Only materials of low
porosity that do not cause adsorption of any of the components in the gases or gas mixture are suitable.
The tubing shall be clean and all unions secure.
Unless independence of the thermal mass-flow controller to its orientation has been established, it
shall be maintained in the orientation in which it was calibrated. Controllers shall be calibrated for the
components in question and it may be necessary to consult the manufacturer of the controller if the
type of gas is to be changed; it may be necessary for the sensor to be changed.

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 ISO 6145-7:2018(E)


8 Calculations

8.1 Volume fraction

Determine the volume fraction using any of the methods of calibration for the flow rates described in
ISO 6145-1. Due consideration shall be given to the uncertainty associated with the method selected.
Calibration of the TMC will define the mass flow rate, or the volume flow rate, dependent on the
method used.
Φ
qm = (2)
C p ∆T
Φ
qV = (3)
C p ρ∆T
The following calculation of the volume fractions is only valid if high-purity gases are used with
impurity fractions that are sufficiently low. The purity of the gases shall be evaluated in accordance
with ISO 19229 and the purity data shall be prepared accordingly. If impurity levels are too high to be
neglected in the calculation of the composition, an alternative calculation shall be used. One possibility
is given in Annex A.
The amount of substance fraction is calculated as:

( qm ) A iTeh STANDARD PREVIEW

MA
xA = (standards.iteh.ai) (4)
 ( qm ) ( qm ) B 
 A
+ 
 M A MB 
 ISO 6145-7:2018
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d085bf377fb6/iso-6145-7-2018
MA and MB are the molar masses of components A and B respectively;

(qm)A and (qm)B denote the values of mass flow rate, for components A and B respectively.
The corresponding volume fraction is:

( qV ) A
ϕA = (5)
( qV ) A + ( qV ) B
8.2 Sources of uncertainty
Commercially available thermal mass flow controllers indicate the gas flow rate usually in volume
units as an analogue or digital display. Typical claims for accuracy are ±1 % of full scale, provided that
the ambient temperature is maintained within ±5 °C of the temperature at which the instrument was
calibrated. The corresponding claims for set point repeatability are ±0,2 % full scale.
It is assumed that pressures and temperatures respectively are measured with the same instruments
during calibration and use, so that the standard uncertainties in these measurements are constant
throughout.
From Formulae (2) and (3):
1
u ( qm ) u Φ
=
( ) u ( ∆T ) u C p 
2
+ +
2 2
( ) 2
(6)
qm  Φ2 ∆T 2 C p2 
 

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