EN ISO 23702-1:2023
(Main)Leather - Per- and polyfluoroalkyl substances - Part 1: Determination of non-volatile compounds by extraction method using liquid chromatography (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)
This document specifies a test method for detection and quantification of extractable non-volatile per- and polyfluoroalkyl substances (PFAS) in leather and coated leather by solvent extraction and liquid chromatography coupled with mass spectrometry.
This document, taking into account the three-dimensional distribution of the fibres within leather, makes the evaluation of the PFAS with respect to the mass.
PFAS substances categories and applications are listed in Annex A, Table A.1. Classes of PFAS regulated compounds listed in Annex B, Table B.1, include acids, telomers, sulfonates and sulphonamide alcohols. Classes of other non-regulated compounds that can be determined by this document are listed in Annex C, Table C.1.
NOTE 1 By applying the method specified in this document, the concentration of free fluorotelomer alcohols (FTOH) in a sample cannot be correctly quantified if perfluoropolymers that release FTOH due to transesterification with the extraction solvent methanol are present in the sample.
NOTE 2 Some regulations (e.g. Reference [4]) also restrict perfluoropolymers having a linear or branched perfluoroheptyl group with the moiety (C7F15)C as one of the structural elements that can degrade to PFOA, e.g. polymers containing 2-perfluorooctylethanol (8:2 FTOH, CAS Registry Number® 678-39-7) bonded as esters. To determine whether these perfluoropolymers are intentionally present, it could be necessary to introduce an alkaline hydrolysis method to remove the 8:2 FTOH side-chain from the polymer. In addition, other FTOH, e.g. 6:2 FTOH or 10:2 FTOH, will be released from relevant perfluoropolymers by alkaline hydrolysis.
Leder - Per- und Polyfluoralkylsubstanzen - Teil 1: Bestimmung von nichtflüchtigen Verbindungen durch Extraktion mit Flüssigkeitschromatographie (ISO 23702‑1:2023)
Dieses Dokument legt ein Prüfverfahren zum Nachweis und zur quantitativen Bestimmung von extrahierbaren nichtflüchtigen Per- und Polyfluoralkylsubstanzen (PFAS) in Leder und beschichtetem Leder mittels Lösemittelextraktion und Flüssigkeitschromatographie in Verbindung mit Massenspektrometrie fest.
Unter Berücksichtigung der dreidimensionalen Faserverteilung innerhalb des Leders bewertet dieses Dokument die PFAS im Hinblick auf die Masse.
PFAS-Substanzkategorien und Anwendungen sind in Anhang A, Tabelle A.1, aufgeführt. Die Klassen der regulierten PFAS-Verbindungen, die in Anhang B, Tabelle B.1, aufgeführt sind, schließen Säuren, Telomere, Sulfonate und Sulfon¬amidalkohole ein. Die Klassen anderer, nichtregulierter Verbindungen, die nach diesem Dokument bestimmt werden können, sind in Anhang C, Tabelle C.1, aufgeführt.
ANMERKUNG 1 Bei Anwendung des in diesem Dokument festgelegten Verfahrens kann die Konzentration freier Fluortelomeralkohole (FTOH) in einer Probe nicht korrekt quantifiziert werden, wenn Perfluorpolymere, die FTOH durch Um¬esterung mit dem Extraktionslösemittel Methanol freisetzen, in der Probe vorhanden sind.
ANMERKUNG 2 Einige Verordnungen (z. B. Literaturhinweis [4]) beschränken auch Perfluorpolymere mit einer linearen oder verzweigten Perfluorheptylgruppe mit dem Bestandteil (C7F15)C als einem der Strukturelemente, die zu PFOA abgebaut werden können, z. B. Polymere, die als Ester gebundenes 2 Perfluoroctylethanol (8:2 FTOH, CAS-Registernummer® 678 39 7) enthalten. Um festzustellen, ob die Anwesenheit dieser Perfluorpolymere beabsichtigt ist, könnte die Aufnahme eines alkalischen Hydrolyseverfahrens zur Entfernung der 8:2 FTOH-Seitenkette des Polymers erforderlich sein. Darüber hinaus werden andere FTOH, z. B. 6:2 FTOH oder 10:2 FTOH, durch alkalische Hydrolyse aus entsprechenden Perfluor¬polymeren freigesetzt [3].
WARNUNG — Die Anwendung dieses Dokuments schließt gefährliche Substanzen ein. Es gibt nicht vor, alle mit seiner Anwendung verbundenen Sicherheits- oder Umweltprobleme zu behandeln. Es liegt in der Verantwortung der Personen, die dieses Dokument anwenden, vor dessen Anwendung geeignete Maßnahmen zu ergreifen, um die Sicherheit und Gesundheit von Personal sicherzustellen und die dafür maßgebenden Anforderungen zu erfüllen.
Cuir - Substances perfluoroalkylées et polyfluoroalkylées - Partie 1: Détermination des composés non volatils par une méthode d’extraction utilisant la chromatographie en phase liquide (ISO 23702-1:2023)
Le présent document spécifie une méthode d’essai de détection et de quantification des substances perfluoroalkylées et polyfluoroalkylées (PFAS) extractibles non volatiles dans le cuir et le cuir enduit, en utilisant l’extraction par solvant et la chromatographie en phase liquide couplée à la spectrométrie de masse.
Le présent document, tenant compte de la distribution tridimensionnelle des fibres dans le cuir, réalise l’évaluation des PFAS par rapport à la masse.
Une liste des catégories de substances PFAS et de leurs applications est fournie dans le Tableau A.1 de l’Annexe A. Les classes de composés PFAS réglementés répertoriés dans le Tableau B.1 de l’Annexe B 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 énumérées dans le Tableau C.1 de l’Annexe C.
NOTE 1 En appliquant la méthode spécifiée dans le présent document, la concentration en alcools de télomères fluorés (FTOH) libres dans un échantillon ne peut pas être déterminée correctement, si des polymères perfluorés qui libèrent des FTOH en raison de la transestérification avec le méthanol utilisé comme solvant d’extraction sont présents dans l’échantillon.
NOTE 2 Certaines réglementations (par exemple, référence [4]) soumettent également à des restrictions les polymères perfluorés ayant, parmi leurs éléments structurels pouvant être dégradés en PFOA, un groupe perfluoroheptyle linéaire ou ramifié avec la fraction (C7F15)C, par exemple des polymères contenant du 2-perfluorooctyléthanol [8:2 FTOH, CAS Registry Number® (numéro d’enregistrement CAS) 678-39-7], lié sous forme d’esters. Afin de déterminer si ces polymères perfluorés sont intentionnellement présents, il peut s’avérer nécessaire d’introduire une méthode d’hydrolyse alcaline pour supprimer la chaîne latérale 8:2 FTOH du polymère. En outre, d’autres FTOH, par exemple 6:2 FTOH ou 10:2 FTOH, seront libérés des polymères perfluorés concernés par l’hydrolyse alcaline.
Usnje - Per- in polifluoroalkil snovi - 1. del: Določevanje nehlapnih spojin z metodo ekstrakcije z uporabo tekoče kromatografije (ISO 23702-1:2023)
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 dokumentom, so opredeljeni v preglednici B.1 dodatka B.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-september-2023
Usnje - Per- in polifluoroalkil snovi - 1. del: Določevanje nehlapnih spojin z metodo
ekstrakcije z uporabo tekoče kromatografije (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)
Leder - Per- und Polyfluoralkylsubstanzen - Teil 1: Bestimmung von nichtflüchtigen
Verbindungen durch Extraktion mit Flüssigchromatographie (ISO 23702-1:2023)
Cuir - Substances perfluoroalkylées et polyfluoroalkylées - Partie 1: Détermination des
composés non volatils par une méthode d’extraction utilisant la chromatographie en
phase liquide (ISO 23702-1:2023)
Ta slovenski standard je istoveten z: EN ISO 23702-1:2023
ICS:
59.140.30 Usnje in krzno Leather and furs
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN ISO 23702-1
EUROPEAN STANDARD
NORME EUROPÉENNE
June 2023
EUROPÄISCHE NORM
ICS 59.140.30 Supersedes EN ISO 23702-1:2018
English Version
Leather - Per- and polyfluoroalkyl substances - Part 1:
Determination of non-volatile compounds by extraction
method using liquid chromatography (ISO 23702-1:2023)
Cuir - Substances perfluoroalkylées et Leder - Per- und Polyfluoralkylsubstanzen - Teil 1:
polyfluoroalkylées - Partie 1: Détermination des Bestimmung von nichtflüchtigen Verbindungen durch
composés non volatils par une méthode d'extraction Extraktion mit Flüssigchromatographie (ISO 23702-
utilisant la chromatographie en phase liquide (ISO 1:2023)
23702-1:2023)
This European Standard was approved by CEN on 19 June 2023.
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, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye 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
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 23702-1:2023 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
European foreword
This document (EN ISO 23702-1:2023) has been prepared by Technical Committee ISO/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 December 2023, and conflicting national standards
shall be withdrawn at the latest by December 2023.
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.
This document supersedes EN ISO 23702-1:2018.
Any feedback and questions on this document should be directed to the users’ national standards
body/national committee. A complete listing of these bodies can be found on the CEN website.
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, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the
United Kingdom.
Endorsement notice
The text of ISO 23702-1:2023 has been approved by CEN as EN ISO 23702-1:2023 without any
modification.
INTERNATIONAL ISO
STANDARD 23702-1
IULTCS
IUC 39-1
Second edition
2023-06
Leather — Per- and polyfluoroalkyl
substances —
Part 1:
Determination of non-volatile
compounds by extraction method
using liquid chromatography
Cuir — Substances perfluoroalkylées et polyfluoroalkylées —
Partie 1: Détermination des composés non volatils par une méthode
d’extraction utilisant la chromatographie en phase liquide
Reference numbers
ISO 23702-1:2023(E)
IULTCS/IUC 39-1:2023(E)
ISO 23702-1:2023(E)
IULTCS/IUC 39-1:2023(E)
© ISO 2023
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 23702-1:2023(E)
IULTCS/IUC 39-1:2023(E)
Contents Page
Foreword .iv
Introduction . vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Principle . 2
5 Reagents . 2
6 Apparatus . 3
7 Sampling . 4
8 Procedure .4
9 Expression of results . 5
9.1 Calibration . 5
9.2 Calculation of the result . 5
9.3 Calculation of the results of a sum . 5
9.4 Precision . . . 6
10 Test report . 6
Annex A (informative) PFAS substance categories and applications . 7
Annex B (informative) PFAS regulated substances . 8
Annex C (informative) PFAS non-regulated substances .11
Annex D (informative) Usable ions and possible quantification limits for PFAS analysis by
LC-MS/MS .12
Annex E (informative) LC-MS/MS chromatographic conditions .14
Annex F (informative) Interferences.22
Annex G (informative) Accuracy .23
Bibliography .25
iii
ISO 23702-1:2023(E)
IULTCS/IUC 39-1:2023(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.
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.
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, in accordance with
the Agreement on technical cooperation between ISO and CEN (Vienna Agreement).
This second edition cancels and replaces the first edition (ISO 23702-1:2018), which has been technically
revised.
The main changes are as follows:
— to clarify the relevant organic fluorine compounds, the title has been modified;
— the Introduction, Scope and Clauses 3 to 10 have been editorially and technically modified;
— the previous Clause 7 has been split into two separate clauses, Clause 7, “Sampling”, and Clause 8,
“Procedure”;
— the previous Clause 8 is now Clause 9, “Expression of results” and includes the previous Clause 9,
“Precision”, as 9.4;
— a new Annex A, listing the category of application of the per- and polyfluoroalkyl substances (PFAS),
has been inserted and the subsequent annexes relettered accordingly;
— Annexes B and C have been technically modified and are now lists of “PFAS regulated substances”
and “PFAS non-regulated substances”, respectively;
iv
ISO 23702-1:2023(E)
IULTCS/IUC 39-1:2023(E)
— a new Annex D, listing the usable ions and possible quantification limits for PFAS analysis by LC-MS/
MS, has been inserted and the subsequent annexes relettered accordingly;
— Annex E has been technically modified.
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.
v
ISO 23702-1:2023(E)
IULTCS/IUC 39-1:2023(E)
Introduction
The per- and polyfluoroalkyl substances (PFAS) consists of a large group of surface active compounds.
The most well-known are perfluorooctanoic sulfonic acid (PFOS) and perfluorooctanooic acid (PFOA).
Table A.1 presents PFAS substance categories and applications.
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 their marketing and use
(see References [4] and [7]).
Perfluorooctanoic acid (PFOA) and its salts and related substances are suspected of having a similar
risk profile to PFOS and are also restricted and regulated in many countries regarding their marketing
and use (see Reference [4]).
Furthermore, restrictions on perfluorocarboxylic acids containing 9 to 14 carbon atoms in the chain
(C -C PFCAs), their salts and C -C PFCA-related substances are restricted in some countries (see
9 14 9 14
References [5] and [8])
A number of long-chain per- and polyfluoroalkyl compounds have been included in the
EU Candidate List of Substances of Very High Concern (SVHC), which is available at:
[6]
https://echa.europa.eu/candidate-list-table.
The regulatory thresholds for restricted per- and polyfluoroalkyl compounds limit their use to a
level below which they cannot be meaningfully used. The thresholds must 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 polyfluoroalkyl compounds have been widely used in many
industries, including in oil-, soil- and water-repellent finishes for textiles, leather products, paper,
furniture and carpets.
vi
ISO 23702-1:2023(E)
INTERNATIONAL STANDARD
IULTCS/IUC 39-1:2023(E)
Leather — Per- and polyfluoroalkyl substances —
Part 1:
Determination of non-volatile compounds by extraction
method using liquid chromatography
WARNING — The use of this document involves hazardous materials. It does not purport
to address all of the safety or environmental problems associated with its use. It is the
responsibility of users of this document to take appropriate measures to ensure the safety and
health of personnel and the environment prior to application of this document and to fulfil the
relevant requirements for this purpose.
1 Scope
This document specifies a test method for detection and quantification of extractable non-volatile per-
and polyfluoroalkyl substances (PFAS) in leather and coated leather by solvent extraction and liquid
chromatography coupled with mass spectrometry.
This document, taking into account the three-dimensional distribution of the fibres within leather,
makes the evaluation of the PFAS with respect to the mass.
PFAS substances categories and applications are listed in Annex A, Table A.1. Classes of PFAS regulated
compounds listed in Annex B, Table B.1, include acids, telomers, sulfonates and sulphonamide alcohols.
Classes of other non-regulated compounds that can be determined by this document are listed in
Annex C, Table C.1.
NOTE 1 By applying the method specified in this document, the concentration of free fluorotelomer
alcohols (FTOH) in a sample cannot be correctly quantified if perfluoropolymers that release FTOH due to
transesterification with the extraction solvent methanol are present in the sample.
NOTE 2 Some regulations (e.g. Reference [4]) also restrict perfluoropolymers having a linear or branched
perfluoroheptyl group with the moiety (C F )C as one of the structural elements that can degrade to PFOA, e.g.
7 15
®1)
polymers containing 2-perfluorooctylethanol (8:2 FTOH, CAS Registry Number 678-39-7) bonded as esters.
To determine whether these perfluoropolymers are intentionally present, it could be necessary to introduce an
alkaline hydrolysis method to remove the 8:2 FTOH side-chain from the polymer. In addition, other FTOH, e.g. 6:2
[3]
FTOH or 10:2 FTOH, will be released from relevant perfluoropolymers by alkaline hydrolysis.
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, mechanical and fastness tests — Position and preparation of
specimens for testing
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.
® ®
1) CAS Registry Number (CAS RN ) is a trademark of CAS corporation. This information is given for the
convenience of users of this document and does not constitute an endorsement by ISO of the product named.
Equivalent products may be used if they can be shown to lead to the same results.
ISO 23702-1:2023(E)
IULTCS/IUC 39-1:2023(E)
3 Terms and definitions
For the purposes of this document, the terms and definitions given in EN 15987 apply.
ISO and IEC maintain terminology 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/
4 Principle
The PFAS substances listed in Annexes B and C are extracted in an ultrasonic bath with methanol
at 60 °C; the extract is analysed by high-performance liquid chromatograph with a tandem mass
spectrometric detector (LC-MS/MS).
5 Reagents
Unless otherwise specified, all reagents shall be of a recognized analytical grade.
5.1 Water, grade 1 (according to ISO 3696) or LC-MS grade. ®
5.2 Methanol, CAS RN 67-56-1, LC-MS grade. ®
5.3 Ammonium acetate, CAS RN 631-61-8.
5.4 Stock solutions of reference compounds, purity > 95 % for the pure substance.
Solutions of the reference compounds listed in Annex B and Annex C 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 fill up to the
mark with methanol (5.2). Dilute this solution with methanol (5.2) at a ratio of 1:1 000 to prepare a
1 000 µg/l stock solution.
5.5 Target compound solutions.
Prepare a 25 µg/l solution of each target compound by diluting the 1 000 µg/l reference compound
stock solutions (5.4) with methanol (5.2)
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 this document.
5.6 Internal standard.
5.6.1 Internal standard solution I (2 000 µg/l) (used for extraction).
At least two suitable internal standards for perflurooctane sulfonate (PFOS) and perfluoroactanoic
acid (PFOA) shall be used. The impurity level of the internal standard should be determined prior to the
use of every new lot.
Suitable mass-labelled internal standards are:
13 13 ®
— C -PFOA (e.g. perfluoro[1,2,3,4- C ]-octanoic-acid, CAS RN 960315-48-4);
x 4
13 13 ®
— C -PFOS (e.g. sodium perfluoro-1-[1,2,3,4- C ]-octanesulfonate, CAS RN 960315-53-1).
x 4
ISO 23702-1:2023(E)
IULTCS/IUC 39-1:2023(E)
Prepare a 2 000 µg/l solution of the internal standard by diluting the commercial solution with
methanol (5.2).
5.6.2 Internal standard solution II (100 µg/l) (used for preparation of calibration solutions).
Prepare a 100 µg/l solution of the internal standard by diluting the commercial solution with methanol
(5.2).
5.7 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 (5.5) and
the internal standard solution II (5.6.2). At least five 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 in a 1 000 µl flask.
Table 1 — Example of calibration solutions
Concentration (µg/l) 0,25 0,5 1 2,5 5 10
Volume methanol (µl) 940 930 910 850 750 550
Volume target compound solu- 10 20 40 100 200 400
tion at 25 µg/l (µl)
Volume internal standard 50 50 50 50 50 50
solution II at 100 µg/l (µl)
5.8 Eluent for the LC-MS/MS.
10 mM ammonium acetate solution is prepared by dissolving 0,771 g of ammonium acetate (5.3) in
1 000 ml deionized water (5.1).
6 Apparatus
The usual laboratory apparatus and, in particular, the following shall be used.
Equipment or any accessible part of it that could come into contact with the sample or the extract shall
be free from interfering compounds, see Annex F.
Use equipment free from all types of fluoropolymer plastics, including polytetrafluoroethene (PTFE)
and glassware. For example, use equipment made of polypropylene (PP) or polyethylene (PE).
Sample containers shall be rinsed thoroughly with water (5.1) and methanol (5.2) and checked for
possible background contamination before use.
6.1 Suitable device with a sharp blade to cut leather sample.
6.2 Volumetric flasks, PP or PE, with inert stopper may be used.
6.3 Extraction vials, suitable PP or PE vials, volume at least 20 ml and able to be used in a centrifuge.
6.4 Laboratory centrifuge, suitable for the extraction vials (6.3).
6.5 Ultrasonic bath, equipped with adjustable bath temperature control, up to at least 60 °C.
6.6 Analytical balance, weighing up to 0,001 g.
ISO 23702-1:2023(E)
IULTCS/IUC 39-1:2023(E)
6.7 High-performance liquid chromatograph coupled with a tandem mass spectrometric
detector, (LC-MS/MS), free from all types of fluoropolymer plastics, including polytetrafluoroethene
(PTFE).
6.8 Membrane filter equipment and polyamide or polypropylene membrane filter, for example
0,22 µm pore size.
7 Sampling
The chosen leather piece should be representative of the lot it is taken from. Cut a test specimen in
accordance with ISO 2418. If cutting a test specimen in accordance with ISO 2418 is not possible (e.g.
for leathers from finished products such as shoes or garments), details about the selection of the test
specimen shall be given in the report. When testing leather products that have separate distinct parts,
the product shall be taken apart and each part shall be analysed separately.
In the case of coated leather, separate, if possible, the coating from the leather substrate. The leather
substrate shall be analysed according to the procedure in this document. If separation of the coating
from the leather cannot be carried out, the entire article shall be analysed according to this procedure.
NOTE The coating can be analysed according to CEN/TS 15968.
Take a leather test piece by mass using ≥ 1 g of leather. The results shall be reported in units of mg/kg.
Cut (6.1) the leather into small pieces according to the method specified in ISO 4044.
8 Procedure
Accurately weigh 1,0 g ± 0,1 g of the leather pieces with the analytical balance (6.6) into an appropriate
extraction vial (6.3). Record the mass of the leather test sample, m.
Add 10 ml methanol (5.2) and 50 µl of the internal standard solution I (5.6.1) to the extraction vial
containing the leather pieces. Extract the test specimen in an ultrasonic bath (6.5) at a temperature
of (60 ± 5) °C for (120 ± 5) min. Let the solution cool down to room temperature and pipette 0,5 ml of
the residual extract plus 0,5 ml of water in the HPLC-vial and seal with a cap for LC-MS/MS analysis.
If necessary, the extracted solution can be filtrated with a membrane filter (6.8) or centrifuged before
taking the 0,5 ml aliquot.
This extract is analysed by LC-MS/MS (6.7). Examples of suitable conditions for LC-MS/MS analysis are
given in Annex E.
Matrix interferences can be caused by contaminants that are co-extracted from the samples. The extent
of matrix interferences varies considerably depending on the nature of the samples, see Annex F.
For measuring PFAS No 29.2 HFPO-DA-X (Table B.1), a hydrolysation step is necessary. Thus, the
methanol-water extract should remain for 24 h at room temperature.
If the extract is turbid, centrifuge and decant the supernatant or filter it (6.8) to a new vial (6.3) for
LC-MS/MS analysis. The recovery rate of check standards in the extract should be ≥ 60 % and the
check standards can be used in the calculation. If < 60 % then a dilution and/or a standard addition is
recommended to overcome matrix effects, with regard to ion suppression.
If dilution or repetition is needed, the methanol extract should be separated from the test specimen,
otherwise inconsistent results can occur, especially for the FTOH substances.
If a concentration step is necessary, the recovery rate shall be checked to be ≥ 60 %. Removal of the
solvent (e.g. by concentration in the rotary vacuum evaporator and evaporation to dryness) can lead to
substantial losses of FTOH.
ISO 23702-1:2023(E)
IULTCS/IUC 39-1:2023(E)
9 Expression of results
9.1 Calibration
For each of the target PFAS substances, set up individually the linear regression functi
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