SIST EN ISO 6145-9:2011

Gas analysis - Preparation of calibration gas mixtures using dynamic volumetric methods - Part 9: Saturation method (ISO 6145-9:2009)

This part of ISO 6145 is one of a series of International Standards dealing with various dynamic volumetric methods used for the preparation of calibration gas mixtures. This part specifies a method for continuous production of calibration gas mixtures containing one or more readily condensable components. A relative expanded uncertainty of measurement, U, obtained by multiplying the relative combined standard uncertainty by a coverage factor k = 2, of not greater than ± 1 %, can be obtained using this method. Unlike the methods presented in the other parts of ISO 6145, the method described in this part does not require accurate measurement of flow rates since flow rates do not appear in the equations for calculation of the volume fraction. Readily condensable gases and vapours commonly become adsorbed on surfaces, and it is therefore difficult to prepare stable calibration gas mixtures of accurately known composition, containing such components, by means of static methods. In addition, these calibration gas mixtures cannot be maintained under a pressure near the saturation limit without the occurrence of condensation. The saturation method can be employed to prepare mixtures of this type.

Gasanalyse - Herstellung von Kalibriergasgemischen mit Hilfe von dynamisch-volumetrischen Verfahren - Teil 9: Sättigungsverfahren (ISO 6145-9:2009)

Dieser Teil von ISO 6145 ist Teil einer Reihe Internationaler Normen, die die verschiedenen dynamisch-volumetrischen Verfahren zur Herstellung von Kalibriergasgemischen behandelt. Der vorliegende Teil legt ein Verfahren zur kontinuierlichen Herstellung von Kalibriergasgemischen mit einer oder mehreren leicht kondensierbaren Komponenten fest. Mithilfe dieses Verfahrens kann eine relative erweiterte Unsicherheit der Messung, U , die durch Multiplizieren der relativen kombinierten Standardunsicherheit mit einem Überdeckungsfaktor von k = 2 erhalten wird, von nicht mehr als  1 % erreicht werden.
Im Unterschied zu den in den anderen Teilen von ISO 6145 vorgestellten Verfahren, ist für das im vorliegenden Teil beschriebene Verfahren keine genaue Messung der Durchflussraten erforderlich, da in den Gleichungen zur Berechnung des Volumenanteils keine Durchflussraten vorkommen.
Leicht kondensierbare Gase und Dämpfe werden im Allgemeinen auf Oberflächen adsorbiert, wodurch es schwierig ist, mithilfe statischer Verfahren stabile Kalibriergasgemische mit genau bekannter Zusammensetzung, die eine oder mehrere derartige Komponenten enthalten, herzustellen. Außerdem können diese Kalibriergasgemische nicht unter einem Druck nahe der Sättigungsgrenze gehalten werden, ohne dass Kondensation auftritt. Das Sättigungsverfahren kann zur Herstellung von Gemischen dieser Art angewendet werden.

Analyse des gaz - Préparation des mélanges de gaz pour étalonnage à l'aide de méthodes volumétriques dynamiques - Partie 9: Méthode par saturation (ISO 6145-9:2009)

L'ISO 6145-9:2009 fait partie d'une série de Normes internationales qui traitent des diverses méthodes volumétriques dynamiques utilisées pour la préparation des mélanges de gaz d'étalonnage. La présente partie spécifie une méthode pour la production continue de mélanges de gaz d'étalonnage contenant un ou plusieurs constituants facilement condensables. Une incertitude élargie relative, U, obtenue en multipliant l'incertitude-type composée relative par un coefficient d'élargissement k = 2, inférieure ou égale à ± 1 % peut être obtenue à l'aide de la présente méthode.
Contrairement aux méthodes présentées dans les autres parties de l'ISO 6145, la méthode décrite dans la présente partie ne demande pas un mesurage précis des débits puisque ceux-ci n'apparaissent pas dans les équations qui servent à calculer la fraction volumique.
Les gaz et vapeurs facilement condensables peuvent généralement s'adsorber sur les surfaces. Il est donc difficile de préparer, à l'aide de méthodes statiques, des mélanges de gaz d'étalonnage contenant ces constituants qui soient stables et dont la composition soit connue précisément. En outre, ces mélanges de gaz d'étalonnage ne peuvent être conservés à une pression proche de la limite de saturation sans que la condensation ait lieu. La méthode par saturation peut donc être utilisée pour la préparation de ce type de mélanges.

Analiza plinov - Priprava kalibracijskih plinskih zmesi z uporabo dinamičnih volumetričnih metod - 9. del: Metoda nasičenja (ISO 6145-9:2009)

Ta del ISO 6145 je eden izmed serije mednarodnih standardov, ki se ukvarjajo z različnimi dinamičnimi volumetričnimi metodami, uporabljenimi za pripravo kalibracijskih plinskih zmesi. Ta del določa metodo za neprekinjeno proizvodnjo kalibracijskih plinskih zmesi, ki vsebujejo eno ali več takoj zgostljivih komponent. Negotovost relativnega širjenja meritve U, pridobljene z množenjem združene standardne negotovosti s faktorjem pokritja k = 2, ki ni večji kot 1 %, je lahko pridobljena z uporabo te metode. V primerjavi z metodami, predstavljenimi v drugih delih ISO 6145, metoda, opisana v tem delu, ne potrebuje natančne meritve ocenjenih pretokov, zato ker se ocenjeni pretoki ne pojavljajo v enačbah za izračun masnega deleža. Takoj zgostljivi plini in hlapi se pogosto absorbirajo na površinah, zato je težko pripraviti stabilne zmesi kalibracijskih plinov natančno znanih sestavov, ki vsebujejo take komponente, na način statičnih metod. Poleg tega teh kalibracijskih plinskih zmesi ni mogoče vzdrževati pod pritiskom blizu meje nasičenosti brez kondenzacije. Metoda nasičenosti je lahko uporabljena za pripravo zmesi te vrste.

General Information

• Status: Published
• Publication Date: 08-Feb-2011
• ICS: 71.040.40 - Chemical analysis
• Technical Committee: NAD - Petroleum products, lubricants and related products
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 12-Jan-2011
• Due Date: 19-Mar-2011
• Completion Date: 09-Feb-2011
• Ref Project: EN ISO 6145-9:2010 - Gas analysis - Preparation of calibration gas mixtures using dynamic volumetric methods - Part 9: Saturation method (ISO 6145-9:2009)

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN ISO 6145-9:2011
01-marec-2011
$QDOL]DSOLQRY3ULSUDYDNDOLEUDFLMVNLKSOLQVNLK]PHVL]XSRUDERGLQDPLþQLK
YROXPHWULþQLKPHWRGGHO0HWRGDQDVLþHQMD,62
Gas analysis - Preparation of calibration gas mixtures using dynamic volumetric methods
- Part 9: Saturation method (ISO 6145-9:2009)
Gasanalyse - Herstellung von Kalibriergasgemischen mit Hilfe von dynamisch-
volumetrischen Verfahren - Teil 9: Sättigungsverfahren (ISO 6145-9:2009)
Analyse des gaz - Préparation des mélanges de gaz pour étalonnage à l'aide de
méthodes volumétriques dynamiques - Partie 9: Méthode par saturation (ISO 6145-
9:2009)
Ta slovenski standard je istoveten z: EN ISO 6145-9:2010
ICS:
71.040.40 Kemijska analiza Chemical analysis
SIST EN ISO 6145-9:2011 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------

SIST EN ISO 6145-9:2011

---------------------- Page: 2 ----------------------

SIST EN ISO 6145-9:2011


EUROPEAN STANDARD
EN ISO 6145-9

NORME EUROPÉENNE

EUROPÄISCHE NORM
December 2010
ICS 71.040.40
English Version
Gas analysis - Preparation of calibration gas mixtures using
dynamic volumetric methods - Part 9: Saturation method (ISO
6145-9:2009)
Analyse des gaz - Préparation des mélanges de gaz pour Gasanalyse - Herstellung von Kalibriergasgemischen mit
étalonnage à l'aide de méthodes volumétriques Hilfe von dynamisch-volumetrischen Verfahren - Teil 9:
dynamiques - Partie 9: Méthode par saturation (ISO 6145- Sättigungsverfahren (ISO 6145-9:2009)
9:2009)
This European Standard was approved by CEN on 11 December 2010.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same
status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.





EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2010 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 6145-9:2010: E
worldwide for CEN national Members.

---------------------- Page: 3 ----------------------

SIST EN ISO 6145-9:2011
EN ISO 6145-9:2010 (E)
Contents Page
Foreword .3

2

---------------------- Page: 4 ----------------------

SIST EN ISO 6145-9:2011
EN ISO 6145-9:2010 (E)
Foreword
The text of ISO 6145-9:2009 has been prepared by Technical Committee ISO/TC 158 “Analysis of gases” of
the International Organization for Standardization (ISO) and has been taken over as EN ISO 6145-9:2010.
This European Standard shall be given the status of a national standard, either by publication of an identical
text or by endorsement, at the latest by June 2011, and conflicting national standards shall be withdrawn at
the latest by June 2011.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech
Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,
Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
Sweden, Switzerland and the United Kingdom.
Endorsement notice
The text of ISO 6145-9:2009 has been approved by CEN as a EN ISO 6145-9:2010 without any modification.

3

---------------------- Page: 5 ----------------------

SIST EN ISO 6145-9:2011

---------------------- Page: 6 ----------------------

SIST EN ISO 6145-9:2011

INTERNATIONAL ISO
STANDARD 6145-9
Second edition
2009-10-01

Gas analysis — Preparation of calibration
gas mixtures using dynamic volumetric
methods —
Part 9:
Saturation method
Analyse des gaz — Préparation des mélanges de gaz pour étalonnage
à l'aide de méthodes volumétriques dynamiques —
Partie 9: Méthode par saturation




Reference number
ISO 6145-9:2009(E)
©
ISO 2009

---------------------- Page: 7 ----------------------

SIST EN ISO 6145-9:2011
ISO 6145-9:2009(E)
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but
shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In
the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.


COPYRIGHT PROTECTED DOCUMENT


©  ISO 2009
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or
ISO's member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail [e-mail]
Web www.iso.org
Published in Switzerland

ii © ISO 2009 – All rights reserved

---------------------- Page: 8 ----------------------

SIST EN ISO 6145-9:2011
ISO 6145-9:2009(E)
Contents Page
Foreword .iv
1 Scope.1
2 Normative references.1
3 Terms and definitions .1
4 Principle.1
5 Equipment .2
5.1 Set up.2
5.2 Gas preparation .2
5.3 Compatibility of the apparatus.2
5.4 Selection of the apparatus.2
5.5 Pressure measurement.2
5.6 Temperature control.3
5.7 Instrumentation .3
5.8 Purity.4
6 Procedure.4
6.1 Installation.4
6.2 Operation of a direct system.4
6.3 Operation of a closed circulation system.4
7 Uncertainty of measurement.5
Annex A (normative) Overview of vapour pressure data for various substances.7
Annex B (informative) Examples of uncertainty estimations.11
Bibliography.14

© ISO 2009 – All rights reserved iii

---------------------- Page: 9 ----------------------

SIST EN ISO 6145-9:2011
ISO 6145-9:2009(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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
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.
ISO 6145-9 was prepared by Technical Committee ISO/TC 158, Analysis of gases.
This second edition cancels and replaces the first edition (ISO 6145-9:2001) and ISO 6145-9:2001/Cor 1:2002,
which have been technically revised. As Annex B is purely informative, and included as a guide to the
methods of calculation of the volume fractions, the numerical examples which are presented in it have been
carried forward verbatim from ISO 6145-9:2001 to this updated standard. Although some references have
been updated in the present bibliography to the most recent editions, the tables in Annex A have also been
reproduced verbatim and are based on data from the earlier editions of the relevant publications (References
[3], [4] and [7] to [10] in the Bibliography). In the application of this updated standard, it is firmly recommended
that the more recent versions of the publications be consulted, even though it is anticipated that any
amendments to the earlier versions will be minor ones. For example, the 15th edition of Reference [4] was
published in 1999 and the 2nd edition of Reference [8] was published in 1984.
ISO 6145-9 also cancels and replaces ISO 6147, which has the same subject. In comparison with ISO 6147,
ISO 6145-9 gives more detailed information on the use of the apparatus and a clause on the uncertainty of
measurement has been added. The estimated uncertainties in the calibration methods and techniques have
now been combined in a square-root sum-of-squares manner to form the relative combined standard
uncertainty.
ISO 6145 consists of the following parts, under the general title Gas analysis — Preparation of calibration gas
mixtures using dynamic volumetric methods:
⎯ Part 1: Methods of calibration
⎯ Part 2: Volumetric pumps
⎯ Part 4: Continuous syringe injection method
⎯ Part 5: Capillary calibration devices
⎯ Part 6: Critical orifices
⎯ Part 7: Thermal mass-flow controllers
⎯ Part 8: Diffusion method
iv © ISO 2009 – All rights reserved

---------------------- Page: 10 ----------------------

SIST EN ISO 6145-9:2011
ISO 6145-9:2009(E)
⎯ Part 9: Saturation method
⎯ Part 10: Permeation method
⎯ Part 11: Electrochemical generation
ISO 6145-3, entitled Periodic injections into a flowing gas stream, has been withdrawn.
© ISO 2009 – All rights reserved v

---------------------- Page: 11 ----------------------

SIST EN ISO 6145-9:2011

---------------------- Page: 12 ----------------------

SIST EN ISO 6145-9:2011
INTERNATIONAL STANDARD ISO 6145-9:2009(E)

Gas analysis — Preparation of calibration gas mixtures using
dynamic volumetric methods —
Part 9:
Saturation method
1 Scope
This part of ISO 6145 is one of a series of International Standards dealing with various dynamic volumetric
methods used for the preparation of calibration gas mixtures. This part specifies a method for continuous
production of calibration gas mixtures containing one or more readily condensable components. A relative
expanded uncertainty of measurement, U, obtained by multiplying the relative combined standard uncertainty
by a coverage factor k = 2, of not greater than ± 1 %, can be obtained using this method.
Unlike the methods presented in the other parts of ISO 6145, the method described in this part does not
require accurate measurement of flow rates since flow rates do not appear in the equations for calculation of
the volume fraction.
Readily condensable gases and vapours commonly become adsorbed on surfaces, and it is therefore difficult
to prepare stable calibration gas mixtures of accurately known composition, containing such components, by
means of static methods. In addition, these calibration gas mixtures cannot be maintained under a pressure
near the saturation limit without the occurrence of condensation. The saturation method can be employed to
prepare mixtures of this type.
2 Normative references
The following referenced documents are indispensable for the application 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 7504, Gas analysis — Vocabulary
ISO 16664, Gas analysis — Handling of calibration gases and gas mixtures — Guidelines
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 7504 apply.
4 Principle
The vapour pressure of a pure substance in equilibrium with its condensed phase depends on the
temperature only. At pressures close to the prevailing barometric pressure, and in the absence of significant
© ISO 2009 – All rights reserved 1

---------------------- Page: 13 ----------------------

SIST EN ISO 6145-9:2011
ISO 6145-9:2009(E)
gas phase interactions, such as occur with hydrocarbon mixtures, the volume fraction of the constituent can
be calculated from knowledge of the temperature and pressure of the system.
If a complementary gas is simply brought into contact with the condensed phase of a volatile component at a
given temperature with no external agency, the equilibrium (saturation) condition is reached quite slowly. In
order to accelerate the process, the complementary gas is passed through the condensed phase at an
elevated temperature, T , following which the gas mixture thus obtained is cooled to a lower temperature, T ,
1 2
which is below the dew-point. To ensure that saturation is attained, the difference in temperature (T − T )
1 2
should be at least 5 K.
The volume fraction ϕ of the constituent x is, to a good approximation, equal to the ratio of the vapour
x
pressure p of the calibration component at temperature T to the total pressure p of the gas mixture at the
x 2
same temperature in the condenser:
p
x
ϕ = (1)
x
p
The value of the relevant partial pressure (vapour pressure) of the constituent at temperature T can be found
2
in tables or diagrams in References [1] to [4] in the Bibliography.
5 Equipment
5.1 Set up
An overview of the equipment that shall be used for producing calibration gas mixtures by the saturation
method is shown in Figure 1.
A continuous flow of complementary gas from the supply (item 1 in Figure 1) is passed firstly through a filter
(item 2 in Figure 2) containing quartz fibre material to remove suspended particles.
NOTE Items 11 and 12 in Figure 1 are required only when a recycling system of calibration gas is employed.
The procedure specified in 5.2 to 5.8 shall be followed for the assembly and use of the equipment in order to
minimize uncertainty in the volume fraction of the components.
5.2 Gas preparation
Clean and dry the complementary gas before it is introduced into the saturator.
5.3 Compatibility of the apparatus
In the apparatus, use components, particularly sample lines, constructed exclusively in materials which are
known to exhibit negligible interaction with the components of the calibration gas mixture. Avoid materials
which may be permeable to the component gases and/or the gas mixture, or upon which adsorption could
take place. If in doubt, the compatibility of sample lines shall be checked before they are used for the
preparation of the sample gas mixture.
5.4 Selection of the apparatus
Use sample lines of which the cross-sectional areas are of sufficient magnitude to ensure that the pressure
drop resulting from the resistance to flow remains negligibly small.
5.5 Pressure measurement
Measure the total pressure at the outlet of the pressure-equalizing vessel.
2 © ISO 2009 – All rights reserved

---------------------- Page: 14 ----------------------

SIST EN ISO 6145-9:2011
ISO 6145-9:2009(E)

Key
1 supply of complementary gas 7 constant-temperature control (T )
1
2 filter for suspended particles 8 constant-temperature control (T )
2
3 saturator 9 condensate outlet
4 condenser, constructed of a material that is of adequate 10 calibration-gas-mixture outlet
thermal conductivity (e.g. copper or stainless steel)
11 circulation system
5 pressure-equalizing vessel with baffles
12 circulation pump
6 pressure gauge
Figure 1 — Schema of equipment for producing calibration gas mixtures by the saturation method

5.6 Temperature control
This shall comply with the specification for transfer of calibration gas mixtures in ISO 16664.
Ensure that the temperature of the gas line is sufficiently higher than T so as to prevent condensation; when
2
necessary, a heated connecting line shall be provided.
5.7 Instrumentation
Use exclusively instruments of high accuracy for measurement: thermometers with an error of measurement
less than ± 0,05 K, and pressure-measuring devices with an error of measurement less than ± 1 hPa
1)
[1mbar] .

5 2
1) 1 bar = 10 N/m = 0,1 MPa
© ISO 2009 – All rights reserved 3

---------------------- Page: 15 ----------------------

SIST EN ISO 6145-9:2011
ISO 6145-9:2009(E)
5.8 Purity
Use exclusively components of purity W 99,99 %, because certain impurities, if present, affect the vapour
pressure.
NOTE It is possible that components of such purity cannot be acquired. If it is desired to apply the method in such
[5]
cases, attention is drawn to 8.2.5 of ISO 6144:2003 which outlines the additional factors to be considered relative to the
estimate of the expanded relative uncertainty.
6 Procedure
6.1 Installation
Arrange the cooling surfaces so as to obtain identical temperatures of the gas and the condenser at the
condensate outlet. Place the pressure-equalizing vessel with baffles after the condenser in order to remove
aerosols from the gas stream. Maintain the pressure-equalizing vessel at the same temperature as the
condenser. Ensure that the temperature of the cooling medium in the vessel, holding the condenser and the
pressure-equalizing vessel, remains constant by means of suitable cooling and heating elements via a control
circuit.
In addition to the temperature T , maintain the pressure, p, of the gas mixture constant in the condenser and
2
display it. Collect the condensate produced in the condenser in a condensate receiver or remove it
continuously by pumping.
6.2 Operation of a direct syst
...