ISO/TS 2610:2022
(Main)Analysis of natural gas — Biomethane — Determination of amines content
Analysis of natural gas — Biomethane — Determination of amines content
This document specifies the determination of the concentration of alkanolamines in biomethane. The measurement method involves thermal desorption gas chromatography with flame ionization and/or mass spectrometry detectors (TD-GC-MS/FID). The described method is specifically developed for the analysis of five amine compounds, namely: — monoethanolamine (MEA); — diglycolamine (DGA); — diethanolamine (DEA); — N-methyldiethanolamine (MDEA); — piperazine (PZ). Information about the compounds is given in Annex A.
Analyse du gaz naturel — Biométhane — Détermination de la teneur en amines
Le présent document traite de la détermination de la concentration en alcanolamines dans le biométhane. La méthode de mesure utilise la chromatographie en phase gazeuse à désorption thermique avec détecteurs à ionisation de flamme et/ou spectrométrie de masse (TD-CG-FID/SM). La méthode décrite est spécifiquement développée pour l'analyse de 5 composés aminés, à savoir: — la monoéthanolamine (MEA); — la diglycolamine (DGA); — la diéthanolamine (DEA); — la N-méthyldiéthanolamine (MDEA); — la pipérazine (PZ). Des informations sur les composés figurent à l’Annexe A.
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Standards Content (Sample)
TECHNICAL ISO/TS
SPECIFICATION 2610
First edition
2022-08
Analysis of natural gas — Biomethane
— Determination of amines content
Analyse du gaz naturel — Biométhane — Détermination de la teneur
en amines
Reference number
ISO/TS 2610:2022(E)
© ISO 2022
---------------------- Page: 1 ----------------------
ISO/TS 2610:2022(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2022
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below
or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii
© ISO 2022 – All rights reserved
---------------------- Page: 2 ----------------------
ISO/TS 2610:2022(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Reference conditions .2
5 Principle . 2
6 Reagents and equipment . 2
7 Sampling . 3
8 Preparation of the calibration tubes .3
9 Analysis . . 4
9.1 Thermal desorption . 4
9.2 Program temperature of the GC separation . 4
9.3 Sample analysis . . 4
9.4 Quantification method . 5
10 Performance characteristics . 5
11 Calculations . 5
12 Test report . 6
Annex A (informative) Characteristics of the amines to be quantified . 8
Bibliography . 9
iii
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ISO/TS 2610:2022(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 World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see
www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 193, Natural gas, Subcommittee SC 1,
Analysis of natural gas.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.
iv
© ISO 2022 – All rights reserved
---------------------- Page: 4 ----------------------
ISO/TS 2610:2022(E)
Introduction
[7]
This document was developed in response to biomethane specifications such as EN 16723 (all parts) .
In other regions, other specifications can apply for biomethane.
In the process of biogas upgrading into biomethane, alkanolamines are used for removing of sulphur-
containing components and carbon dioxide. Due to this reason, trace level of these components can
be present in biomethane. This method is suited for the detection of these components as well as the
determination of their concentration. To inject biomethane into natural gas grids and to use it as an
automotive fuel, it needs to meet specifications. For amines the maximum limit value in biomethane is
3 [7]
set as 10 mg/m is set in EN 16723 (all parts) . Other specifications can state other thresholds.
v
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TECHNICAL SPECIFICATION ISO/TS 2610:2022(E)
Analysis of natural gas — Biomethane — Determination of
amines content
1 Scope
This document specifies the determination of the concentration of alkanolamines in biomethane. The
measurement method involves thermal desorption gas chromatography with flame ionization and/or
mass spectrometry detectors (TD-GC-MS/FID). The described method is specifically developed for the
analysis of five amine compounds, namely:
— monoethanolamine (MEA);
— diglycolamine (DGA);
— diethanolamine (DEA);
— N-methyldiethanolamine (MDEA);
— piperazine (PZ).
Information about the compounds is given in Annex A.
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 10715, Natural gas — Sampling guidelines
ISO 14532, Natural gas — Vocabulary
ISO 16000-6, Indoor air — Part 6: Determination of organic compounds (VVOC, VOC, SVOC) in indoor and
test chamber air by active sampling on sorbent tubes, thermal desorption and gas chromatography using
MS or MS FID
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 14532 and the following apply.
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 https:// www .electropedia .org/
3.1
amine
chemical compound consisting nitrogen atoms bound to hydrogen and/or carbon atoms having the
general formula R N
3
[SOURCE: ISO/TR 27912:2016, 3.5]
1
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ISO/TS 2610:2022(E)
3.2
gas chromatography-mass spectrometry
GC-MS
method that combines the features of gas-liquid chromatography and mass spectrometry to
qualitatively and quantitatively analyse volatile compounds within a test sample
[SOURCE: ISO/TS 16550:2014, 2.3]
4 Reference conditions
Unless stated otherwise, all volumes and concentrations in this document are for real dry gas at
ISO Standard Reference conditions of 15 °C and 101,325 kPa (see ISO 13443).
Other reference conditions may be chosen if the context in which the measurements are performed, or
the results to be used, dictate to do so.
5 Principle
A known volume of biomethane is actively sampled on a sorbent tube. Amines compounds are then
trapped on the sorbent and tubes are analysed in laboratory. Analysis is performed by thermal
desorption at high temperature. When desorbed, compounds are sent on a cold trap prior to their
transport in the gas chromatograph column and their detection by flame ionisation detector and/or
mass spectrometry.
6 Reagents and equipment
6.1 Calibration standards.
6.1.1 Amine standards, pure amine components shall be used, and their purity shall be assessed in
accordance with ISO 19229. Amines (except DGA) should be at least 99 % purity grade. For DGA, purity
should be at least 98 %.
6.1.2 Reference standard, N-octane of at least 99 % purity grade.
6.2 Dilution solvent, methanol (chromatographic quality) shall be used as dilution solvent for the
preparation of calibration standards.
6.3 Sorbent tubes, equipped with a suitable sorbent. It is also recommended to use stainless steel
tubes with proper coating treatment (amines are photosensitive).
®1)
EXAMPLE Tenax TA based polymer (2,6-diphelylene oxide polymer).
6.4 Gas chromatograph (GC), equipped with a flame ionization detector (FID) and/or a mass
spectrometer (MS). Moreover, the GC shall be equipped with a thermal desorption system associated to
a cryogenic trap.
If an FID is used, the selectivity of the method regarding amines shall be established (see ISO 6974-1).
As biomethane composition regarding trace compounds (e.g., terpenes) is related to the nature of the
inputs, the method shall be tested towards a real
...
SPÉCIFICATION ISO/TS
TECHNIQUE 2610
Première édition
2022-08
Analyse du gaz naturel — Biométhane
— Détermination de la teneur en
amines
Analysis of natural gas — Biomethane — Determination of amines
content
Numéro de référence
ISO/TS 2610:2022(F)
© ISO 2022
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ISO/TS 2610:2022(F)
DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2022
Tous droits réservés. Sauf prescription différente ou nécessité dans le contexte de sa mise en œuvre, aucune partie de cette
publication ne peut être reproduite ni utilisée sous quelque forme que ce soit et par aucun procédé, électronique ou mécanique,
y compris la photocopie, ou la diffusion sur l’internet ou sur un intranet, sans autorisation écrite préalable. Une autorisation peut
être demandée à l’ISO à l’adresse ci-après ou au comité membre de l’ISO dans le pays du demandeur.
ISO copyright office
Case postale 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Genève
Tél.: +41 22 749 01 11
E-mail: copyright@iso.org
Web: www.iso.org
Publié en Suisse
ii
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ISO/TS 2610:2022(F)
Sommaire Page
Avant-propos .iv
Introduction .v
1 Domaine d’application . 1
2 Références normatives .1
3 Termes et définitions . 1
4 Conditions de référence .2
5 Principe. 2
6 Réactifs et matériel . 2
7 Échantillonnage .3
8 Préparation des tubes d’étalonnage .4
9 Analyse . 4
9.1 Désorption thermique . . 4
9.2 Programme de température de la séparation par CG . 5
9.3 Analyse des échantillons . 5
9.4 Méthode de quantification . 5
10 Caractéristiques de performance .6
11 Calculs . 6
12 Rapport d’essai . 7
Annexe A (informative) Caractéristiques des amines à quantifier . 8
Bibliographie . 9
iii
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ISO/TS 2610:2022(F)
Avant-propos
L'ISO (Organisation internationale de normalisation) est une fédération mondiale d'organismes
nationaux de normalisation (comités membres de l'ISO). L'élaboration des Normes internationales est
en général confiée aux comités techniques de l'ISO. Chaque comité membre intéressé par une étude
a le droit de faire partie du comité technique créé à cet effet. Les organisations internationales,
gouvernementales et non gouvernementales, en liaison avec l'ISO participent également aux travaux.
L'ISO collabore étroitement avec la Commission électrotechnique internationale (IEC) en ce qui
concerne la normalisation électrotechnique.
Les procédures utilisées pour élaborer le présent document et celles destinées à sa mise à jour sont
décrites dans les Directives ISO/IEC, Partie 1. Il convient, en particulier, de prendre note des différents
critères d'approbation requis pour les différents types de documents ISO. Le présent document
a été rédigé conformément aux règles de rédaction données dans les Directives ISO/IEC, Partie 2
(voir www.iso.org/directives).
L'attention est appelée sur le fait que certains des éléments du présent document peuvent faire l'objet de
droits de propriété intellectuelle ou de droits analogues. L’ISO ne saurait être tenue pour responsable
de ne pas avoir identifié de tels droits de propriété. Les détails concernant les références aux droits
de propriété intellectuelle ou autres droits analogues identifiés lors de l'élaboration du document
sont indiqués dans l'Introduction et/ou dans la liste des déclarations de brevets reçues par l'ISO
(voir www.iso.org/brevets).
Les appellations commerciales éventuellement mentionnées dans le présent document sont données
pour information, par souci de commodité, à l'intention des utilisateurs et ne sauraient constituer un
engagement.
Pour une explication de la nature volontaire des normes, la signification des termes et expressions
spécifiques de l'ISO liés à l'évaluation de la conformité, ou pour toute information au sujet de l'adhésion
de l'ISO aux principes de l’Organisation mondiale du commerce (OMC) concernant les obstacles
techniques au commerce (OTC), voir le lien suivant: www.iso.org/iso/avant-propos.html.
Le présent document a été élaboré par le comité technique ISO/TC 193, Gaz naturel, sous-comité SC 1,
Analyse du gaz naturel.
Il convient que l’utilisateur adresse tout retour d’information ou toute question concernant le présent
document à l’organisme national de normalisation de son pays. Une liste exhaustive desdits organismes
se trouve à l’adresse www.iso.org/members.html.
iv
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ISO/TS 2610:2022(F)
Introduction
Le présent document a été élaboré en réponse aux spécifications relatives au biométhane telles que
[7]
celles figurant dans l’EN 16723 (toutes les parties) . Dans d’autres régions, d’autres spécifications
peuvent s’appliquer au biométhane.
Le processus de traitement du biogaz en biométhane utilise des alcanolamines pour éliminer les
constituants soufrés et le dioxyde de carbone. C’est pourquoi des niveaux traces de ces constituants
peuvent être présents dans le biométhane. La présente méthode est adaptée à la détection de ces
constituants ainsi qu’à la détermination de leur concentration. Le biométhane doit répondre à des
spécifications pour pouvoir être injecté dans les réseaux de gaz naturel et être utilisé comme carburant
3
automobile. Pour les amines, la valeur limite maximale dans le biométhane est fixée à 10 mg/m dans
[7]
l’EN 16723 (toutes les parties) . D’autres spécifications peuvent indiquer d’autres seuils.
v
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SPÉCIFICATION TECHNIQUE ISO/TS 2610:2022(F)
Analyse du gaz naturel — Biométhane — Détermination de
la teneur en amines
1 Domaine d’application
Le présent document traite de la détermination de la concentration en alcanolamines dans le
biométhane. La méthode de mesure utilise la chromatographie en phase gazeuse à désorption
thermique avec détecteurs à ionisation de flamme et/ou spectrométrie de masse (TD-CG-FID/SM). La
méthode décrite est spécifiquement développée pour l'analyse de 5 composés aminés, à savoir:
— la monoéthanolamine (MEA);
— la diglycolamine (DGA);
— la diéthanolamine (DEA);
— la N-méthyldiéthanolamine (MDEA);
— la pipérazine (PZ).
Des informations sur les composés figurent à l’Annexe A.
2 Références normatives
Les documents suivants sont cités dans le texte de sorte qu’ils constituent, pour tout ou partie de leur
contenu, des exigences du présent document. Pour les références datées, seule l’édition citée s’applique.
Pour les références non datées, la dernière édition de la publication à laquelle il est fait référence
s'applique (y compris tous les amendements).
ISO 10715, Gaz naturel — Lignes directrices pour l’échantillonnage
ISO 14532, Gaz naturel — Vocabulaire
ISO 16000-6, Air intérieur — Partie 6: Dosage des composés organiques (COTV, COV, COSV) dans l'air
intérieur et l'air de chambre d'essai par prélèvement actif sur tubes à sorbant, désorption thermique et
chromatographie en phase gazeuse avec détection MS ou MS-FID
ISO 19229, Analyse des gaz — Analyse de pureté et traitement des données de pureté
3 Termes et définitions
Pour les besoins du présent document, les termes et définitions de l'ISO 14532 ainsi que les suivants
s'appliquent.
L'ISO et l'IEC tiennent à jour des bases de données terminologiques destinées à être utilisées en
normalisation, consultables aux adresses suivantes:
— ISO Online browsing platform: disponible à l'adresse https:// www .iso .org/ obp
— IEC Electropedia: disponible à l'adresse https:// www .electropedia .org/
1
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ISO/TS 2610:2022(F)
3.1
amine
composé chimique de formule générale R N, constitué d’atomes d’azote liés à des atomes d’hydrogène
3
et/ou de carbone
[SOURCE: ISO/TR 27912:2016, 3.5]
3.2
chromatographie en phase gazeuse couplée à la spectrométrie de masse
CG-SM
méthode qui combine les caractéristiques de la chromatographie gaz-liquide et de la spectrométrie de
masse pour l’analyse qualitative et quantitative des composés volatils dans un échantillon pour essai
[SOURCE: ISO/TS 16550:2014, 2.3]
4 Conditions de référence
Sauf indication contraire, tous les volumes et les concentrations figurant dans le présent document
sont pour le gaz sec réel à des conditions de référence standard ISO de 15 °C et de 101,325 kPa
(voir l’ISO 13443).
D'autres conditions de référence peuvent être choisies si le contexte dans lequel les mesurages sont
effectués, ou les résultats à utiliser, l'imposent.
5 Principe
Un volume connu de biométhane est activement prélevé sur un tube à sorbant. Les composés aminés
sont ensuite piégés sur le sorbant et les tubes sont analysés en laboratoire. L’analyse est réalisée par
désorption thermique à haute température. Une fois désorbés, les composés sont envoyés sur un piège
froid avant d’être transportés dans la colonne du chromatographe en phase gazeuse, puis détectés par
un détecteur à ionisation de flamme et/ou par spectrométrie de masse.
6 Réactifs et matériel
6.1 Étalons.
6.1.1 Étalons d’amines, des constituants aminés purs doivent être utilisés et leur pureté doit être
évaluée conformément à l’ISO 19229. Il convient que les amines (à l’exception de la DGA) aient une
pureté minimale de 99 %. Pour la DGA, il convient que la pureté soit au moins de 98 %.
6.1.2 Étalon de référence, N-octane, d’une pureté minimale de 99 %.
6.2 Solvant de dilution, du méthanol (de qualité chromatographique) doit être utilisé comme solvant
de dilution pour la préparation des étalons.
6.3 Tubes à sorbant, contenant un sorbant adapté. Il est également recommandé d’utiliser des tubes
en acier inoxydable avec un traitement de revêtement approprié (les amines sont photosensibles).
®1)
EXEMPLE Polymère à base de Tenax TA (polymère d’oxyde de 2,6-diphénylène).
1) Tenax® est une marque déposée de Buchem BV, Apeldoorn, Pays-Bas. Cette information est donnée à l’intention
des utilisateurs et ne signifie nullement que l’ISO approuve l’emploi du produit ainsi désigné.
2
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ISO/TS 2610:2022(F)
6.4 Chromatographe en phase gazeuse (CG), équipé d’un détecteur à ionisation de flamme (FID)
et/ou d’un spectromètre de masse (SM). De plus, le chromatographe en phase gazeuse doit être équipé
d’un système de désorption thermique associé à un piège cryogénique.
Si un FID est utilisé, la
...
ISO/TS 2610:2022(E)
ISO/TC 193/SC 1
Date: 2022-06-23xx
ISO/DTS 2610:2022(E)
ISO/TC 193/SC 1/WG 25
Secretariat: NEN
Analysis of natural gas — Biomethane — Determination of amines content
Analyse du gaz naturel — Biométhane — Détermination de la teneur en amine
---------------------- Page: 1 ----------------------
ISO/DTSTS 2610:2022(E)
COPYRIGHT PROTECTED DOCUMENT
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or
utilized otherwise in any form or by any means, electronic or mechanical, including photocopying,
or posting on the internet or an intranet, without prior written permission. Permission can be
requested from either ISO at the address below or ISO’s member body in the country of the
requester.
ISO copyright office
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2022 – All rights reserved
---------------------- Page: 2 ----------------------
ISO/DTSTS 2610:2022(E)
Contents Page
Foreword . iv
Introduction . v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Reference conditions . 2
5 Principle . 2
6 Reagents and equipment . 2
6.1 Calibration standards . 2
6.1.1 Amine standards . 2
6.1.2 Reference standard . 2
6.2 Dilution solvent . 3
6.3 Sorbent tubes . 3
6.4 Gas chromatograph (GC) . 3
6.5 Capillary column . 3
6.6 Thermal desorption (TD) system . 3
6.7 Precision syringes . 4
7 Conditioning of the sorbent tubes . 4
8 Sampling . 4
9 Preparation of the calibration tubes . 4
10 Analysis . 5
10.1 Thermal desorption . 5
10.2 Program temperature of the GC separation . 5
10.3 Sample analysis . 5
10.4 Quantification method . 5
11 Performance characteristics . 6
12 Calculations . 6
13 Test report . 7
Annex A (informative) Characteristics of the amines to be quantified . 9
Bibliography. 10
© ISO 2022 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO/DTSTS 2610:2022(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards Formatted: English (United States)
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
Formatted: Adjust space between Latin and Asian text,
through ISO technical committees. Each member body interested in a subject for which a technical
Adjust space between Asian text and numbers
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.
Formatted: English (United States)
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.
ln other circumstances, particularly when there is an urgent market requirement for such documents, a
technical committee may decide to publish other types of document:
— an ISO Publicly Available Specification (ISO/PAS) represents an agreement between technical
experts in an ISO working group and is accepted for publication if it is approved by more than 50 %
of the members of the parent committee casting a vote;
— an ISO Technical Specification (ISO/TS) represents an agreement between the members of a
technical committee and is accepted for publication if it is approved by 2/3 of the members of the
committee casting a vote.
An ISO/PAS or ISO/TS is reviewed after three years in order to decide whether it will be confirmed tor a
further three years, revised to become an International Standard, or withdrawn. lf the ISO/PAS or ISO/TS
is confirmed, it is reviewed again after a further three years, at which time it must either be transformed
into an International Standard or be withdrawn.
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 Formatted: English (United States)
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any
Formatted: Adjust space between Latin and Asian text,
patent rights identified during the development of the document will be in the Introduction and/or on
Adjust space between Asian text and numbers
the ISO list of patent declarations received (see www.iso.org/patents).
Formatted: English (United States)
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 World
Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see
www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 193, Natural gas, Subcommittee SC 1,
Analysis of natural gas.
iv © ISO 2022 – All rights reserved
---------------------- Page: 4 ----------------------
ISO/DTSTS 2610:2022(E)
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.
© ISO 2022 – All rights reserved v
---------------------- Page: 5 ----------------------
ISO/DTSTS 2610:2022(E)
Introduction
[7]
This document was developed in response to biomethane specifications such as EN 16723. (all parts) . Formatted: Pattern: Clear
In other regions, other specifications can apply for biomethane.
Formatted: Pattern: Clear
In the process of biogas upgrading into biomethane, alkanolamines are used for removing of sulphur-
containing components and carbon dioxide. Due to this reason, trace level of these components can be
present in biomethane. This method is suited for the detection of these components as well as the
determination of their concentration. To inject biomethane into natural gas grids and to use it as an
automotive fuel, it needs to meet specifications. For amines the maximum limit value in biomethane is
3 [7]
set as 10 mg/m is set in EN 16723. (all parts) . Other specifications can state other thresholds. Formatted: Pattern: Clear
Formatted: Pattern: Clear
vi © ISO 2022 – All rights reserved
---------------------- Page: 6 ----------------------
TECHNICAL SPECIFICATION ISO/DTSTS 2610:2022(E)
Formatted: Justified
Analysis of natural gas — Biomethane — Determination of
amines content
1 Scope
This document specifies the determination of the concentration of alkanolamines in biomethane. The
measurement method involve Thermal Desorption Gas Chromatographyinvolves thermal desorption gas
chromatography with Flame Ionizationflame ionization and/or Mass Spectrometrymass spectrometry
detectors (TD-GC-MS/FID). The described method is specifically developed for the analysis of five amine
compounds, namely:
— Monoethanolaminemonoethanolamine (MEA));
— Diglycolaminediglycolamine (DGA));
— Diethanolaminediethanolamine (DEA));
— N-methyldiethanolamine (MDEA)); Formatted: Font: Italic
— Piperazinepiperazine (PZ)).
Information about the compounds is given in Annex A. Formatted: Pattern: Clear
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 10715, Natural gas — Sampling guidelines
ISO 13443, Natural gas — Standard reference conditions
ISO 14532, Natural gas — Vocabulary
ISO 10715, Natural gas — Sampling guidelines
ISO 14532, Natural gas — Vocabulary
ISO 16000-6, Indoor air — Part 6: Determination of organic compounds (VVOC, VOC, SVOC) in indoor and Formatted: Pattern: Clear
test chamber air by active sampling on sorbent tubes, thermal desorption and gas chromatography using
Formatted: Pattern: Clear
MS or MS FID
Formatted: Pattern: Clear
Formatted: Pattern: Clear
ISO 19229, Gas analysis — Purity analysis and the treatment of purity data
Formatted: Pattern: Clear
ISO/TR 27912:2016, Carbon dioxide capture — Carbon dioxide capture systems, technologies and
Formatted: Pattern: Clear
processes
Formatted: Pattern: Clear
ISO/TS 16550:2014, Nanotechnologies — Determination of silver nanoparticles potency by release of
muramic acid from Staphylococcus aureus
© ISO 2022 – All rights reserved 1
---------------------- Page: 7 ----------------------
ISO/DTSTS 2610:2022(E)
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 14532 and the following apply. Formatted: Pattern: Clear
Formatted: Pattern: Clear
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
Formatted: English (United States)
— IEC Electropedia: available at https://www.electropedia.org/
Formatted: English (United States)
3.1
amine
chemical compound consisting nitrogen atoms bound to hydrogen and/or carbon atoms having the
general formula R N
3
[SOURCE: ISO/TR 27912:2016, 3.5] Formatted: Pattern: Clear
Formatted: Pattern: Clear
3.2
Formatted: Pattern: Clear
gas chromatography-mass spectrometry
Formatted: Pattern: Clear
GC-MS
method that combines the features of gas-liquid chromatography and mass spectrometry to qualitatively Formatted: Pattern: Clear
and quantitatively analyse volatile compounds within a test sample
[SOURCE: ISO/TS 16550:2014, 2.3]
Formatted: Pattern: Clear
Formatted: Pattern: Clear
4 Reference conditions
Formatted: Pattern: Clear
Formatted: Pattern: Clear
Unless stated otherwise, all volumes and concentrations in this document are for real dry gas at
ISO Standard Reference conditions of 15 °C and 101,325 kPa (see ISO 13443). Formatted: Pattern: Clear
Formatted: Pattern: Clear
Other reference conditions may be chosen if the context in which the measurements are performed, or
the results to be used, dictate to do so. Formatted: Pattern: Clear
5 Principle
A known volume of biomethane is actively sampled on a sorbent tube. Amines compounds are then
trapped on the sorbent and tubes are analysed in laboratory. Analysis is performed by thermal desorption
at high temperature. When desorbed, compounds are sent on a cold trap prior to their transport in the
gas chromatograph column and their detection by flame ionisation detector and/or mass spectrometry.
6 Reagents and equipment
6.1 6.1 Calibration standards. Formatted: p2, Adjust space between Latin and Asian
text, Adjust space between Asian text and numbers, Tab
stops: Not at 20 pt
6.1.1 6.1.1 Amine standards
Formatted: Font: Bold
Pure, pure amine components shall be used, and their purity shall be assessed in accordance with
Formatted: p3, Adjust space between Latin and Asian
ISO 19229. Amines (except DGA) should be at least 99 % purity grade. For DGA, purity should be at least
text, Adjust space between Asian text and numbers
98 %.
6.1.2 6.1.2 Reference standard
, N-Octaneoctane of at least 99 % purity grade.
Formatted: p3, Adjust space between Latin and Asian
text, Adjust space between Asian text and numbers
Formatted: Font: Italic
2 © ISO 2022 – All rights reserved
---------------------- Page: 8 ----------------------
ISO/DTSTS 2610:2022(E)
6.2 6.2 Dilution solvent
Methanol, methanol (chromatographic quality) shall be used as dilution solvent for the preparation of
Formatted: p2, Adjust space between Latin and Asian
text, Adjust space between Asian text and numbers
calibration standards.
6.3 6.3 Sorbent tubes
Sorbent tubes shall be, equipped with a suitable sorbent. It is also recommended to use stainless steel
Formatted: p2, Adjust space between Latin and Asian
text, Adjust space between Asian text and numbers
tubes with proper coating treatment (amines are photosensitive).
1
®
EXAMPLE Tenax TA based polymer (2,6-diphelylene oxide polymer).
6.4 6.4 Gas chromatograph (GC)
Gas chromatograph shall be), equipped with a flame ionization detector (FID) and/or a mass Formatted: p2, Adjust space between Latin and Asian
text, Adjust space between Asian text and numbers
spectrometer (MS). Moreover, the GC shall be equipped with a thermal desorption system associated to
a cryogenic trap.
[1]
If an FID is used, the selectivity of the method regarding amines shall be established (see ISO 6974-1 ).).
Formatted: Pattern: Clear
As biomethane composition regarding trace compounds (e.g., terpenes) is related to the nature of the
Formatted: Pattern: Clear
inputs, the method shall be tested towards a rea
...
TECHNICAL ISO/TS
SPECIFICATION 2610
First edition
Analysis of natural gas — Biomethane
— Determination of amines content
Analyse du gaz naturel — Biométhane — Détermination de la teneur
en amine
PROOF/ÉPREUVE
Reference number
ISO/TS 2610:2022(E)
© ISO/TS 2022
---------------------- Page: 1 ----------------------
ISO/TS 2610:2022(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2022
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below
or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii
PROOF/ÉPREUVE © ISO 2022 – All rights reserved
---------------------- Page: 2 ----------------------
ISO/TS 2610:2022(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Reference conditions .2
5 Principle . 2
6 Reagents and equipment . 2
7 Sampling . 3
8 Preparation of the calibration tubes .3
9 Analysis . . 4
9.1 Thermal desorption . 4
9.2 Program temperature of the GC separation . 4
9.3 Sample analysis . . 4
9.4 Quantification method . 5
10 Performance characteristics . 5
11 Calculations . 6
12 Test report . 6
Annex A (informative) Characteristics of the amines to be quantified . 8
Bibliography . 9
iii
© ISO 2022 – All rights reserved PROOF/ÉPREUVE
---------------------- Page: 3 ----------------------
ISO/TS 2610:2022(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 World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see
www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 193, Natural gas, Subcommittee SC 1,
Analysis of natural gas.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.
iv
PROOF/ÉPREUVE © ISO 2022 – All rights reserved
---------------------- Page: 4 ----------------------
ISO/TS 2610:2022(E)
Introduction
[7]
This document was developed in response to biomethane specifications such as EN 16723 (all parts) .
In other regions, other specifications can apply for biomethane.
In the process of biogas upgrading into biomethane, alkanolamines are used for removing of sulphur-
containing components and carbon dioxide. Due to this reason, trace level of these components can
be present in biomethane. This method is suited for the detection of these components as well as the
determination of their concentration. To inject biomethane into natural gas grids and to use it as an
automotive fuel, it needs to meet specifications. For amines the maximum limit value in biomethane is
3 [7]
set as 10 mg/m is set in EN 16723 (all parts) . Other specifications can state other thresholds.
v
© ISO 2022 – All rights reserved PROOF/ÉPREUVE
---------------------- Page: 5 ----------------------
TECHNICAL SPECIFICATION ISO/TS 2610:2022(E)
Analysis of natural gas — Biomethane — Determination of
amines content
1 Scope
This document specifies the determination of the concentration of alkanolamines in biomethane. The
measurement method involves thermal desorption gas chromatography with flame ionization and/or
mass spectrometry detectors (TD-GC-MS/FID). The described method is specifically developed for the
analysis of five amine compounds, namely:
— monoethanolamine (MEA);
— diglycolamine (DGA);
— diethanolamine (DEA);
— N-methyldiethanolamine (MDEA);
— piperazine (PZ).
Information about the compounds is given in Annex A.
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 10715, Natural gas — Sampling guidelines
ISO 14532, Natural gas — Vocabulary
ISO 16000-6, Indoor air — Part 6: Determination of organic compounds (VVOC, VOC, SVOC) in indoor and
test chamber air by active sampling on sorbent tubes, thermal desorption and gas chromatography using
MS or MS FID
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 14532 and the following apply.
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 https:// www .electropedia .org/
3.1
amine
chemical compound consisting nitrogen atoms bound to hydrogen and/or carbon atoms having the
general formula R N
3
[SOURCE: ISO/TR 27912:2016, 3.5]
1
© ISO 2022 – All rights reserved PROOF/ÉPREUVE
---------------------- Page: 6 ----------------------
ISO/TS 2610:2022(E)
3.2
gas chromatography-mass spectrometry
GC-MS
method that combines the features of gas-liquid chromatography and mass spectrometry to
qualitatively and quantitatively analyse volatile compounds within a test sample
[SOURCE: ISO/TS 16550:2014, 2.3]
4 Reference conditions
Unless stated otherwise, all volumes and concentrations in this document are for real dry gas at
ISO Standard Reference conditions of 15 °C and 101,325 kPa (see ISO 13443).
Other reference conditions may be chosen if the context in which the measurements are performed, or
the results to be used, dictate to do so.
5 Principle
A known volume of biomethane is actively sampled on a sorbent tube. Amines compounds are then
trapped on the sorbent and tubes are analysed in laboratory. Analysis is performed by thermal
desorption at high temperature. When desorbed, compounds are sent on a cold trap prior to their
transport in the gas chromatograph column and their detection by flame ionisation detector and/or
mass spectrometry.
6 Reagents and equipment
6.1 Calibration standards.
6.1.1 Amine standards, pure amine components shall be used, and their purity shall be assessed in
accordance with ISO 19229. Amines (except DGA) should be at least 99 % purity grade. For DGA, purity
should be at least 98 %.
6.1.2 Reference standard, N-octane of at least 99 % purity grade.
6.2 Dilution solvent, methanol (chromatographic quality) shall be used as dilution solvent for the
preparation of calibration standards.
6.3 Sorbent tubes, equipped with a suitable sorbent. It is also recommended to use stainless steel
tubes with proper coating treatment (amines are photosensitive).
®1)
EXAMPLE Tenax TA based polymer (2,6-diphelylene oxide polymer).
6.4 Gas chromatograph (GC), equipped with a flame ionization detector (FID) and/or a mass
spectrometer (MS). Moreover, the GC shall be equipped with a thermal desorption system associated to
a cryogenic trap.
If an FID is used, the selectivity of the method regarding amines shall be established (see ISO 6974-1).
As biomethane composition regarding trace compounds (e.g., terpenes) is related to the nature of the
inputs, the method shall be tested towards a real biomethane sample, and adapt it if necessary to avoid
coelution of components.
1) Tenax® is
...
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