SIST EN ISO 23702-1:2019

Leather - Organic fluorine - Part 1: Determination of non-volatile compounds by extraction method using liquid chromatography/tandem mass spectrometry detector (LC-MS/MS) (ISO 23702-1:2018)

This document specifies a test method for detection and quantification of extractable neutral, ionic,
long, medium and short chain perfluorinated and poly-fluorinated substances in leather and coated
leather.
This document, taking into account the three-dimensional distribution of the fibres within leather,
makes the evaluation of the perfluorinated and poly-fluorinated substances with respect to the mass.
Classes of regulated compounds listed in Annex A, Table A.1, include acids, telomers, sulfonates and
sulphonamide alcohols. Classes of other non-regulated compounds that can be determined by this
document are defined in Annex B, Table B.1.

Leder - Organisches Fluor - Teil 1: Bestimmung der nichtflüchtigen Verbindungen durch ein Extraktionsverfahren mit Flüssigkeitschromatographie/Tandem-Massenspektrometrie-Detektor (LC-MS/MS) (ISO 23702-1:2018)

Diese Norm legt ein Prüfverfahren für den Nachweis und die quantitative Bestimmung von extrahierbaren, neutralen, ionischen perfluorierten und polyfluorierten Substanzen mit kurzer und mittlerer Kettenlänge in Leder fest.
Unter Berücksichtigung der dreidimensionalen Faserverteilung innerhalb des Leders bewertet diese Norm die perfluorierten und polyfluorierten Substanzen im Hinblick auf die Masse.
Die in Tabelle A.1 des normativen Anhangs A angeführten Klassen der regulierten Verbindungen schließen Säuren, Telomere, Sulfonate und Sulfonamidalkohole ein. Die Klassen anderer, nicht regulierteer Verbindungen, die mit dieser Norm bestimmt werden können, sind in Anhang B, Tabelle B.1 festgelegt.

Cuir - Fluor organique - Partie 1: Détermination de la teneur en composés non volatils par une méthode d'extraction utilisant la chromatographie en phase liquide couplée à un détecteur par spectrométrie de masse en tandem (LC-MS/MS) (ISO 23702-1:2018)

Le présent document spécifie une méthode d'essai de détection et de quantification de substances perfluorées et polyfluorées neutres, ioniques, à chaîne longue, moyenne et courte, extractibles dans le cuir et le cuir verni.
Le présent document, tenant compte de la distribution tridimensionnelle des fibres dans le cuir, réalise l'évaluation des substances perfluorées et polyfluorées par rapport à la masse.
Les classes de composés réglementés répertoriés dans le Tableau A.1 de l'Annexe A comprennent des acides, des télomères, des sulfonates et des alcools sulfonamides. Les classes d'autres composés non réglementés qui peuvent être déterminés par le présent document sont définies dans le Tableau B.1 de l'Annexe B.

Usnje - Organski fluor - 1. del: Določevanje nehlapnih spojin z metodo ekstrakcije z uporabo tekoče kromatografije/tandemski masni spektrometer (LC-MS/MS) (ISO 23702-1:2018)

Ta dokument določa preskusno metodo za odkrivanje in kvantifikacijo izločljivih nevtralnih, ionskih, dolgoverižnih, srednjeverižnih in kratkoverižnih perfluoriranih in polifluoriranih snovi v usnju in premazanem usnju.
Ta dokument, upoštevajoč tridimenzionalno porazdelitev vlaken v usnju, vrednoti perfluorirane in polifluorirane snovi glede na maso.
Razredi predpisanih spojin, navedenih v preglednici A.1 dodatka A, vključujejo kisline, telomerje, sulfonate in sulfonamid alkohole. Razredi drugih nepredpisanih spojin, ki jih je mogoče določiti s tem dokumentov, so opredeljeni v preglednici B.1 dodatka B.

General Information

• Status: Withdrawn
• Public Enquiry End Date: 02-Oct-2017
• Publication Date: 06-Dec-2018
• Withdrawal Date: 06-Jul-2023
• ICS: 59.140.30 - Leather and furs
• Technical Committee: IUSN - Leather
• Current Stage: 9900 - Withdrawal (Adopted Project)
• Start Date: 07-Jul-2023
• Due Date: 30-Jul-2023
• Completion Date: 07-Jul-2023
• Ref Project: EN ISO 23702-1:2018 - Leather - Organic fluorine - Part 1: Determination of non-volatile compounds by extraction method using liquid chromatography/tandem mass spectrometry detector (LC-MS/MS) (ISO 23702-1:2018)

Relations

• Revises: SIST EN ISO 23702-1:2023 - Leather - Per- and polyfluoroalkyl substances - Part 1: Determination of non-volatile compounds by extraction method using liquid chromatography (ISO 23702-1:2023)
• Effective Date: 19-Jan-2023

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN ISO 23702-1:2019
01-januar-2019
8VQMH2UJDQVNLIOXRUGHO'RORþHYDQMHQHKODSQLKVSRMLQ]PHWRGRHNVWUDNFLMH
]XSRUDERWHNRþHNURPDWRJUDILMHWDQGHPVNLPDVQLVSHNWURPHWHU/&0606,62

Leather - Organic fluorine - Part 1: Determination of non-volatile compounds by
extraction method using liquid chromatography/tandem mass spectrometry detector (LC-
MS/MS) (ISO 23702-1:2018)
Leder - Organisches Fluor - Teil 1: Bestimmung der nichtflüchtigen Verbindungen durch
ein Extraktionsverfahren mit Flüssigkeitschromatographie/Tandem-Massenspektrometrie
-Detektor (LC-MS/MS) (ISO 23702-1:2018)
Cuir - Fluor organique - Partie 1: Détermination de la teneur en composés non volatils
par une méthode d'extraction utilisant la chromatographie en phase liquide couplée à un
détecteur par spectrométrie de masse en tandem (LC-MS/MS) (ISO 23702-1:2018)
Ta slovenski standard je istoveten z: EN ISO 23702-1:2018
ICS:
59.140.30 Usnje in krzno Leather and furs
SIST EN ISO 23702-1:2019 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 23702-1:2019

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SIST EN ISO 23702-1:2019


EN ISO 23702-1
EUROPEAN STANDARD

NORME EUROPÉENNE

November 2018
EUROPÄISCHE NORM
ICS 59.140.30
English Version

Leather - Organic fluorine - Part 1: Determination of non-
volatile compounds by extraction method using liquid
chromatography/tandem mass spectrometry detector (LC-
MS/MS) (ISO 23702-1:2018)
Cuir - Fluor organique - Partie 1: Détermination de la Leder - Organisches Fluor - Teil 1: Bestimmung der
teneur en composés non volatils par une méthode nichtflüchtigen Verbindungen durch ein
d'extraction utilisant la chromatographie en phase Extraktionsverfahren mit
liquide couplée à un détecteur par spectrométrie de Flüssigkeitschromatographie/Tandem-
masse en tandem (LC-MS/MS) (ISO 23702-1:2018) Massenspektrometrie-Detektor (LC-MS/MS) (ISO
23702-1:2018)
This European Standard was approved by CEN on 3 October 2018.

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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.





EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2018 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 23702-1:2018 E
worldwide for CEN national Members.

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SIST EN ISO 23702-1:2019
EN ISO 23702-1:2018 (E)
Contents Page
European foreword . 3

2

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SIST EN ISO 23702-1:2019
EN ISO 23702-1:2018 (E)
European foreword
This document (EN ISO 23702-1:2018) has been prepared by Technical Committee IULTCS
"International Union of Leather Technologists and Chemists Societies" in collaboration with Technical
Committee CEN/TC 289 “Leather” the secretariat of which is held by UNI.
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 May 2019, and conflicting national standards shall be
withdrawn at the latest by May 2019.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN 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, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Endorsement notice
The text of ISO 23702-1:2018 has been approved by CEN as EN ISO 23702-1:2018 without any
modification.


3

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SIST EN ISO 23702-1:2019

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SIST EN ISO 23702-1:2019
INTERNATIONAL ISO
STANDARD 23702-1
IULTCS/IUC 39-1
First edition
2018-09
Leather — Organic fluorine —
Part 1:
Determination of the non-volatile
compound content by extraction
method using liquid chromatography/
tandem mass spectrometry detector
(LC-MS/MS)
Cuir — Fluor organique —
Partie 1: Détermination de la teneur en composés non volatils par
une méthode d'extraction utilisant la chromatographie en phase
liquide couplée à un détecteur par spectrométrie de masse en tandem
(LC-MS/MS)
Reference numbers
ISO 23702-1:2018(E)
IULTCS/IUC 39-1:2018(E)
©
ISO 2018

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SIST EN ISO 23702-1:2019
ISO 23702-1:2018(E)
IULTCS/IUC 39-1:2018(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2018
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: [phone]
Fax: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland
ii © ISO 2018 – All rights reserved

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SIST EN ISO 23702-1:2019
ISO 23702-1:2018(E)
IULTCS/IUC 39-1:2018(E)
Contents  Page
Foreword .iv
Introduction .v
1  Scope .1
2  Normative references .1
3  Terms and definitions .1
4  Principle . 2
5  Reagents . 2
6  Apparatus . 3
7  Testing procedure . 4
7.1 Sampling and preparation of the sample . 4
7.2 Extraction procedure . 4
7.2.1 Extraction . 4
7.2.2 Interferences . 4
7.3 Analytical procedure . 4
8  Calculation and expression of results . 5
8.1 Calibration curve . 5
8.2 Calculation of the result . 5
9  Precision . 5
10  Test report . 6
Annex A (informative) Classes of highly fluorinated regulated compounds determinable by
this document . 7
Annex B (informative) Other relevant compounds of concern .8
Annex C (informative) LC-MS/MS chromatographic conditions .9
Annex D (informative) Interferences .16
Annex E (informative) Accuracy .17
Bibliography .19
© ISO 2018 – All rights reserved iii

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SIST EN ISO 23702-1:2019
ISO 23702-1:2018(E)
IULTCS/IUC 39-1:2018(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
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso
.org/iso/foreword .html.
This document was prepared by the Chemical Test Commission of the International Union of Leather
Technologists and Chemists Societies (IUC Commission, IULTCS) in collaboration with the European
Committee for Standardization (CEN) Technical Committee CEN/TC 289, Leather, the secretariat of
which is held by UNI, in accordance with the Agreement on technical cooperation between ISO and CEN
(Vienna Agreement).
IULTCS, originally formed in 1897, is a world-wide organization of professional leather societies to
further the advancement of leather science and technology. IULTCS has three Commissions, which
are responsible for establishing international methods for the sampling and testing of leather. ISO
recognizes IULTCS as an international standardizing body for the preparation of test methods for
leather.
A list of all parts in the ISO 23702 series can be found on the ISO website.
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 2018 – All rights reserved

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SIST EN ISO 23702-1:2019
ISO 23702-1:2018(E)
IULTCS/IUC 39-1:2018(E)
Introduction
The group of per- and poly-fluorinated compounds (PFC) consists of more than 800 substances. The
most well-known are perfluorooctanioc sulfonic acid (PFOS) and perfluorooctanooic acid (PFOA).
Perfluorooctanoic sulfonic acid (PFOS) is classified as persistent, bio-accumulative and toxic (PBT).
PFOS and its salts are restricted and regulated in many countries regarding its marketing and use (see
References [3] and [4]).
Perfluorooctanoic acid (PFOA) and its salts are suspected of having a similar risk profile to PFOS.
A number of long chain per- and poly-fluorinated compounds have been included in the EU Candidate
List of Substances of Very High Concern (SVHC), which is available at https: //echa .europa .eu/candidate
-list -table.
The regulatory thresholds for restricted per- and poly-fluorinated compounds limit the use to a level
below which they cannot be meaningfully used. The thresholds need to take into consideration the
possible presence of unavoidable impurities and unintentional trace contaminants.
The long chain, fully fluorinated anions are non-volatile. They are heat stable and resistant to breaking
down in the environment. The per- and poly-fluorinated compounds have been widely used in many
industries, including in oil-, soil- and water-repellent finishes for textiles, leather products, paper,
furniture and carpets.
© ISO 2018 – All rights reserved v

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SIST EN ISO 23702-1:2019

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SIST EN ISO 23702-1:2019
ISO 23702-1:2018(E)
INTERNATIONAL STANDARD
IULTCS/IUC 39-1:2018(E)
Leather — Organic fluorine —
Part 1:
Determination of the non-volatile compound content by
extraction method using liquid chromatography/tandem
mass spectrometry detector (LC-MS/MS)
1  Scope
This document specifies a test method for detection and quantification of extractable neutral, ionic,
long, medium and short chain perfluorinated and poly-fluorinated substances in leather and coated
leather.
This document, taking into account the three-dimensional distribution of the fibres within leather,
makes the evaluation of the perfluorinated and poly-fluorinated substances with respect to the mass.
Classes of regulated compounds listed in Annex A, Table A.1, include acids, telomers, sulfonates and
sulphonamide alcohols. Classes of other non-regulated compounds that can be determined by this
document are defined in Annex B, Table B.1.
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 2418, Leather — Chemical, physical and mechanical and fastness tests — Sampling location
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 4044:2017, Leather — Chemical tests — Preparation of chemical test samples
EN 15987, Leather — Terminology — Key definitions for the leather trade.
3  Terms and definitions
For the purposes of this document, the terms and definitions given in EN 15987 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 http: //www .electropedia .org/
3.1
analyte
substance or chemical constituent that is subjected to measurement
[SOURCE: CEN/TS 15968:2010, 3.1]
3.2
constituent
pure chemical material and substance of which a material is composed
© ISO 2018 – All rights reserved 1

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SIST EN ISO 23702-1:2019
ISO 23702-1:2018(E)
IULTCS/IUC 39-1:2018(E)
3.3
extract
concentrated preparation of the analytes isolated from the treated material
3.4
internal standard
compound different from the analyte, present in the sample with known content or added to the sample,
simultaneously detected with the analyte, with physical and chemical properties as similar as possible
to the analyte
4  Principle
The classes of regulated compounds listed in Annex A, Table A.1, are extracted with methanol and the
extract is analysed by high-performance liquid chromatograph with a tandem mass spectrometric
detector (LC-MS/MS).
NOTE The classes of non-regulated compounds listed in Annex B, Table B.1, are processed according to the
same principle as the regulated compounds.
5  Reagents
The chemicals used below shall be of the defined purity.
5.1  Distilled or deionized water, at least Grade 3 quality as specified in ISO 3696.
5.2  Methanol, CAS 67-56-1, HPLC grade.
5.3  Ammonium acetate, CAS 631-61-8, analytical grade.
5.4  Stock solutions of reference compounds, purity > 95 % for the pure substance.
Solutions of the reference compounds listed in Annex A and Annex B are available commercially. They
should be diluted to the required concentrations. If reference compounds are obtained pure, for example
weigh 100 mg of each standard separately into a 100 ml volumetric flask and make up to the mark with
methanol (5.2). Dilute this solution with methanol at a ratio of 1:1 000 to prepare a 1 000 µg/l stock
solution.
5.5  Target compound solutions.
Prepare a 500 µg/l solution of each target compound by diluting the 1 000 µg/l reference compound
stock solutions (5.3) with methanol.
For the preparation of the target compound solution, certified solutions are commercially available. The
purity level and the solvent shall be checked in order to be in accordance with the present standard.
5.6  Internal standard.
A suitable internal standard shall be used. The impurity level of the internal standard should be
determined prior to the use of every new lot.
...

SLOVENSKI STANDARD
oSIST prEN ISO 23702-1:2017
01-september-2017
8VQMH2UJDQVNLIOXRUGHO'RORþHYDQMHQHKODSQLKVSRMLQ]PHWRGRHNVWUDNFLMH
]XSRUDERWHNRþHNURPDWRJUDILMH,62',6
Leather - Organic fluorine - Part 1: Determination of non-volatile compounds by
extraction method using liquid chromatography (ISO/DIS 23702-1:2017)
Ta slovenski standard je istoveten z: prEN ISO 23702-1
ICS:
59.140.30 Usnje in krzno Leather and furs
oSIST prEN ISO 23702-1:2017 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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oSIST prEN ISO 23702-1:2017

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oSIST prEN ISO 23702-1:2017
DRAFT INTERNATIONAL STANDARD
ISO/DIS 23702-1
IULTCS/IUC 39-1
IULTCS Secretariat:
Voting begins on: Voting terminates on:
2017-06-06 2017-08-28
Leather - Organic fluorine —
Part 1:
Determination of non-volatile compounds by extraction
method using liquid chromatography
Titre manque
ICS: 59.140.30
THIS DOCUMENT IS A DRAFT CIRCULATED
This document is circulated as received from the committee secretariat.
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
ISO/CEN PARALLEL PROCESSING
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference numbers
NATIONAL REGULATIONS.
ISO/DIS 23702-1:2017(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
IULTCS/IUC 39-1:2017(E)
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
©
PROVIDE SUPPORTING DOCUMENTATION. ISO 2017

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oSIST prEN ISO 23702-1:2017
ISO/DIS 23702-1:2017(E)
IULTCS/IUC 39-1:2017(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2017, Published in Switzerland
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. [phone]
Fax [phone]
[e-mail]
www.iso.org
ii © ISO 2017 – All rights reserved

---------------------- Page: 4 ----------------------
oSIST prEN ISO 23702-1:2017
ISO/DIS 23702-1:2017(E)
IULTCS/IUC 39-1:2017(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Reagents . 2
6 Apparatus . 3
7 Testing procedure . 4
7.1 Sampling and preparation of the sample . 4
7.2 Extraction procedure . 4
7.2.1 Extraction . 4
7.2.2 Interferences . 4
7.3 Analytical procedure . 5
8 Calculation and expression of results . 5
9 Precision . 5
10 Test report . 5
Annex A (normative) Classes of highly fluorinated regulated compounds determinable by
this standard . 7
Annex B (informative) Other relevant compounds of concern . 8
Annex C (informative) LC-MS/MS chromatographic conditions . 9
Annex D (informative) Interferences .16
Bibliography .17
© ISO 2017 – All rights reserved iii

---------------------- Page: 5 ----------------------
oSIST prEN ISO 23702-1:2017
ISO/DIS 23702-1:2017(E)
IULTCS/IUC 39-1:2017(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 on 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 the following URL: www . i so .org/ iso/ foreword .html
ISO yyyyy was prepared by the Chemical Test Commission of the International Union of Leather
Technologists and Chemists Societies (IUC Commission, IULTCS) in collaboration with the European
Committee for Standardisation (CEN) Technical Committee CEN/TC 289, Leather, the secretariat of
which is held by UNI, in accordance with the agreement on technical co-operation between ISO and CEN
(Vienna Agreement).
IULTCS, originally formed in 1897, is a world-wide organization of professional leather societies to
further the advancement of leather science and technology. IULTCS has three Commissions, which
are responsible for establishing international methods for the sampling and testing of leather. ISO
recognizes IULTCS as an international standardizing body for the preparation of test methods for
leather.
Annexes A is a normative annex.
Annexes B, C and D are informative annexes.
iv © ISO 2017 – All rights reserved

---------------------- Page: 6 ----------------------
oSIST prEN ISO 23702-1:2017
ISO/DIS 23702-1:2017(E)
IULTCS/IUC 39-1:2017(E)
Introduction
The group of per- and poly-fluorinated compounds (PFC) consists of more than 800 substances. The
most well-known are perfluorooctanioc sulfonic acid (PFOS) and perfluorooctanooic acid (PFOA).
Perfluorooctanoic sulfonic acid (PFOS) is classified as persistent, bio-accumulative and toxic (PBT).
PFOS and its salts are restricted in the EU Regulation 1907/2006 (REACH) Annex XVII regarding its
marketing and use. PFOS and its salts were added to Annex B of the Stockholm Convention on Persistent
Organic Pollutants (POP) in May 2009. Consequently the use of PFOS and its salts are now restricted in
many national regulations, for example the EU Regulation 757/2010.
Perfluorooctanoic acid (PFOA) and its salts are suspected to have a similar risk profile to PFOS.
A number of long chain per- and poly-fluorinated compounds have been included in the EU Candidate
List of Substances of Very High Concern (SVHC), which is available at https:// echa .europa .eu/ candidate
-list -table.
The long chain, fully fluorinated anions are non-volatile. They are heat stable and resistant to breaking
down in the environment. The per- and poly-fluorinated compounds have been widely used in many
industries, including in oil, soil and water repellent finishes for textiles, leather products, paper,
furniture and carpets.
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oSIST prEN ISO 23702-1:2017
ISO/DIS 23702-1:2017(E)
DRAFT INTERNATIONAL STANDARD
IULTCS/IUC 39-1:2017(E)
Leather - Organic fluorine —
Part 1:
Determination of non-volatile compounds by extraction
method using liquid chromatography
1 Scope
This standard specifies a test method for detection and quantification of extractable neutral, ionic,
long, medium and short chain perfluorinated and poly-fluorinated substances in leather.
This standard, taking into account the three-dimensional distribution of the fibres within leather,
makes the evaluation of the perfluorinated and poly-fluorinated substances with respect to the mass.
Classes of regulated compounds listed in Table A.1 of the normative Annex A include acids, telomers,
sulfonates and sulphonamide alcohols. Classes of other non-regulated compounds that can be
determined by this standard are defined in Table B.1 in Annex B.
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 2418, Leather — Chemical, physical and mechanical and fastness tests — Sampling location
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 4044, Leather — Chemical tests — Preparation of chemical test samples
EN 15987, Leather — Terminology — Key definitions for the leather trade.
3 Terms and definitions
For the purposes of this document, the leather terms and definitions given in EN 15987 and the
following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at http:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
3.1
analyte
substance or chemical constituent that is subjected to measurement
[1]
[SOURCE: CEN/TS 15968:2010, 3.1]
3.2
blank matrix
matrix which is largely identical with the analytical one, but does not contain the analyte or contains it
in low and known content.
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oSIST prEN ISO 23702-1:2017
ISO/DIS 23702-1:2017(E)
IULTCS/IUC 39-1:2017(E)
[1]
[SOURCE: CEN/TS 15968:2010, 3.2]
3.3
constituents
all pure chemical materials and substances of which a material is composed.
3.4
extract
concentrated preparation of the analytes isolated from the treated material.
3.5
internal standard (IS)
compound different from the analyte, present in the sample with known content or added to the sample,
simultaneously detected with the analyte, with physical and chemical properties as similar as possible
to the analyte.
4 Principle
The classes of regulated compounds listed in Table A.1 in Annex A are extracted with methanol and
the extract is analyzed by high performance liquid chromatograph with a mass spectrometric detector
(LC-MS/MS).
NOTE The classes of non-regulated compounds listed in Table B.1 in Annex B are processed according to the
same principle as the regulated compounds.
5 Reagents
The chemicals used below shall be of the defined purity.
5.1 Distilled or deionized water, at least Grade 3 quality as specified in ISO 3696
5.2 Methanol, CAS 67-56-1, HPLC grade
5.3 Stock solutions of reference compounds, purity > 95 % for the pure substance.
Solutions of the reference compounds are available commercially. They should be diluted to the required
concentrations. If reference compounds are obtained pure, weigh 100 mg of each standard separately
into a 100 mL volumetric flask and make up to the mark with methanol (5.2). Dilute this solution with
methanol at a ratio 1:1 000 to prepare a 1 000 µg/L stock solution.
5.4 Target compound solutions
Prepare a 500 µg/L solution of each target compound by diluting the 1 000 µg/L reference compound
stock solutions (5.1) with methanol.
5.5 Preparation of calibration solutions
Materials and liquids shall be stored at 4 °C and in clean containers.
Prepare suitable calibration solutions using methanol (5.2), target compound solutions (5.4) and
the internal standard solution (5.6). At least four calibration solutions shall be prepared with a
concentration range to match the limits given. For example, prepare according to the volumes given in
Table 1.
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oSIST prEN ISO 23702-1:2017
ISO/DIS 23702-1:2017(E)
IULTCS/IUC 39-1:2017(E)
Table 1 — Calibration solutions
Concentration (µg/L) 2,5 5 10 20 30
Volume methanol (µL) 990 985 975 955 935
Volume Target compound (µL) 5 10 20 40 60
Volume Internal Standard (µL) 5 5 5 5 5
5.6 Internal Standard
A suitable internal standard is to be used. The impurity level of the internal standard should be
determined prior to the use of every new lot.
Examples of internal standards (IS) are:
1) perfluorononanoic-acid, PFNA.
2) suitable mass-labeled internal standard are:
13
— Perfluoro-[1,2,3,4- C ]-octanoic-acid, MPFOA [mass-labeled PFOA];
4
13 - + 13
— C -PFOS (e.g. [F(CF ) SO H ]-, 1,2,3,4- C );
x 2 8 3 4
18 - + 18
— O -PFOS (e.g. [F(CF ) SO H ]-, O ).
x 2 8 3 2
When other types of labelled internal standards become available, they may be used.
Prepare a 500 µg/L solution of the internal standard by diluting the commercial solution with methanol.
For the LC-MS/MS eluent, a 10 mM ammonium acetate solution is prepared by dissolving 0,771 g of
ammonium acetate (Table 3) in 1000 ml deionized water.
6 App
...