FprEN 17681-1
(Main)Textiles and textile products - Per- and polyfluoroalkyl substances (PFAS) - Part 1: Analysis of an alkaline extract using liquid chromatography and tandem mass spectrometry
Textiles and textile products - Per- and polyfluoroalkyl substances (PFAS) - Part 1: Analysis of an alkaline extract using liquid chromatography and tandem mass spectrometry
This document specifies a test method, including the degradation of certain side-chain fluorinated polymers during the extraction with simultaneous alkaline hydrolysis, and using liquid chromatography (LC) and tandem mass spectrometry (MS/MS) for identification and quantification of certain per- and polyfluoroalkyl substances (PFAS). The document is applicable to all materials of textile products.
Table 2 indicates a list of target PFAS which can be analysed with this document. PFAS of Table 2 marked with the footnote e) and footnote f) undergo alkaline hydrolysis and only their per- or polyfluorinated degradation products such as PFOA or n:2 fluorotelomer alcohols (n:2 FTOHs, n = 4, 6, 8, 10) can be determined.
Through the methods outlined in the informative Annex E and Annex F, free n:2 FTOHs, PFOA and non-polymeric PFAS of Table 2 marked with the footnote e) and footnote f), that are not stable to alkaline hydrolysis, can be identified and quantified.
Certain side-chain fluorinated polymers release n:2 FTOHs (n = 4, 6, 8, 10) under the described extraction conditions. Since these side-chain fluorinated polymers can be PFOA or C9-C14 PFCA-related substances restricted by the EU-POPs [1] or EU-REACH [2] regulations, the amounts of released n:2 FTOHs can be used to indirectly assess whether the concentration of the aforementioned side-chain fluorinated polymers exceed limits for PFOA or C9-C14 PFCA-related substances.
This document is also applicable to the determination of further PFAS, provided that the method is validated with the additional substances and that these PFAS are stable to alkaline hydrolysis and dehydrofluorination.
Textilien und textile Erzeugnisse - Per- und polyfluorierte Alkylverbindungen (PFAS) - Teil 1: Untersuchung eines alkalischen Extraktes mittels Flüssigkeitschromatographie und Tandem-Massenspektrometrie
Dieses Dokument legt ein Prüfverfahren, einschließlich des Abbaus bestimmter fluorierter Polymere mit fluorierten Seitenketten während der Extraktion durch alkalische Hydrolyse, unter Verwendung von Flüssigkeitschromatographie (LC, en: liquid chromatography) und Tandem-Massenspektrometrie (MS/MS, en: tandem mass spectrometry) zur Identifizierung und quantitativen Bestimmung bestimmter PFAS fest.
Die Klassen der in der EU regulierten PFAS sind in Tabelle 2 aufgeführt. Sofern EU-Vorschläge zur Beschränkung bestimmter PFAS vorlagen, wurden diese Stoffe in diese Liste aufgenommen. Klassen anderer, nicht in der EU regulierter PFAS, die nach diesem Dokument bestimmt werden können, sind in Anhang C, Tabelle C.1, aufgeführt. Dieses Dokument ist auch anwendbar auf weitere PFAS-Verbindungen, vorausgesetzt, dass das Verfahren mit den zusätzlichen Verbindungen validiert wird.
Die Abbauprodukte, n:2 FTOH und PFOA, einiger in Tabelle 2 aufgeführter PFAS, die reguliert, aber nicht stabil gegenüber alkalischer Hydrolyse sind, werden anstelle dieser PFAS bestimmt. Diese PFAS sind in Tabelle 2 entsprechend gekennzeichnet. Anhang F enthält eine Beschreibung der Extraktion mit Methanol für die Prüfung auf diese PFAS. Ein Verfahren zum Nachweis und zur quantitativen Bestimmung der aufgeführten flüchtigen PFAS, die alle nicht stabil gegenüber alkalischer Hydrolyse sind, mittels Gaschromatographie (GC) ist in Anhang G beschrieben.
Textiles et produits textiles - Substances perfluoroalkylées et polyfluoroalkylées (PFAS) - Partie 1 : Analyse d’un extrait alcalin par chromatographie en phase liquide et spectrométrie de masse en tandem
Le présent document spécifie une méthode d’essai incluant la dégradation de certains polymères fluorés à chaîne latérale pendant l’extraction par hydrolyse alcaline et en utilisant la chromatographie en phase liquide (LC) et la spectrométrie de masse en tandem (MS/MS) pour l’identification et la quantification de certaines PFAS.
Les classes de PFAS réglementées dans l’UE sont répertoriées dans le Tableau 2. Lorsque des propositions de l’UE concernant des restrictions sur des PFAS données étaient disponibles, ces substances ont été incluses dans la liste. Les classes d’autres PFAS non réglementées dans l’UE qui peuvent être déterminés selon ce document sont répertoriées dans l’Annexe C, Tableau C.1. Le présent document est également applicable à d’autres PFAS, à condition que la méthode soit validée avec les composés additionnels.
Les produits de dégradation, n:2 FTOH et PFOA, de certaines PFAS répertoriées dans le Tableau 2 qui sont réglementés mais ne sont pas stables à l’hydrolyse alcaline seront déterminés à la place de ces PFAS. Ces PFAS sont marquées conformément au Tableau 2. Afin de soumettre ces PFAS à essai, une description de l’extraction au méthanol est fournie dans l’Annexe F. Une méthode utilisant la chromatographie en phase gazeuse (GC) pour détecter et quantifier les PFAS volatils énumérés, parmi lesquels aucun n’est stable à l’hydrolyse alcaline, est fournie dans l’Annexe G.
Tekstilje in tekstilni izdelki - Per- in polifluoroalkilne snovi (PFAS) - 1. del: Analiza alkalnega ekstrakta s tekočinsko kromatografijo in tandemsko masno spektrometrijo
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-januar-2024
Tekstilje in tekstilni izdelki - Per- in polifluoroalkilne snovi (PFAS) - 1. del: Analiza
alkalnega ekstrakta s tekočinsko kromatografijo in tandemsko masno
spektrometrijo
Textiles and textile products - Per- and polyfluoroalkyl substances (PFAS) - Part 1:
Analysis of an alkaline extract using liquid chromatography and tandem mass
spectrometry
Textilien und textile Erzeugnisse - Per- und polyfluorierte Alkylverbindungen (PFAS) -
Teil 1: Untersuchung eines alkalischen Extraktes mittels Flüssigkeitschromatographie
und Tandem-Massenspektrometrie
Textiles et produits textiles - Substances perfluoroalkylées et polyfluoroalkylées (PFAS) -
Partie 1 : Analyse d’un extrait alcalin par chromatographie en phase liquide et
spectrométrie de masse en tandem
Ta slovenski standard je istoveten z: prEN 17681-1
ICS:
59.080.01 Tekstilije na splošno Textiles in general
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
DRAFT
EUROPEAN STANDARD
prEN 17681-1
NORME EUROPÉENNE
EUROPÄISCHE NORM
November 2023
ICS 59.080.01 Will supersede EN 17681-1:2022
English Version
Textiles and textile products - Per- and polyfluoroalkyl
substances (PFAS) - Part 1: Analysis of an alkaline extract
using liquid chromatography and tandem mass
spectrometry
Textiles et produits textiles - Fluor organique - Partie 1 Textilien und textile Erzeugnisse - Per- und
: Détermination de composés non volatils par une Polyfluorierte Alkylverbindungen (PFAS) - Teil 1:
méthode d'extraction utilisant la chromatographie en Untersuchung eines alkalischen Extraktes mittels
phase liquide Flüssigkeitschromatographie und Tandem-
Massenspektrometrie
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 248.
If this draft becomes a European Standard, 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.
This draft European Standard was established by CEN 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.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are
aware and to provide supporting documentation.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.
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. prEN 17681-1:2023 E
worldwide for CEN national Members.
prEN 17681-1:2023 (E)
Contents Page
European foreword . 4
Introduction . 6
1 Scope .16
2 Normative references .16
3 Terms and definitions .16
4 Principle .16
5 Reagents .17
6 Equipment .17
7 Sampling .18
7.1 General .18
7.2 Sampling based on area .18
7.3 Sampling based on mass .18
7.4 Preparation of test specimen .18
8 Procedure.19
8.1 Preparation of stock solutions .19
8.2 Preparation of the check solution .19
8.3 Preparation of calibration solutions .19
8.4 Extraction .19
8.5 Analysis .19
9 Expression of results .20
9.1 Calibration .20
9.2 Calculation of the results of individual PFAS .20
9.3 Calculation of the sums of certain PFAS .21
9.4 Precision of the test method .21
10 Test report .21
Annex A (normative) Usable ions and reachable quantification limits for PFAS analysis of
sample matrix by LC-MS/MS .22
Annex B (informative) Interferences with LC-MS/MS .25
Annex C (informative) Non-regulated PFAS.26
Annex D (informative) Chromatographic conditions .27
D.1 General .27
D.2 Chromatographic conditions .27
D.3 MS/MS conditions .28
Annex E (informative) Reliability of the test method .29
Annex F (informative) Extraction with methanol .33
F.1 General .33
F.2 Procedure.33
Annex G (informative) Analysis with GC-MSD .34
prEN 17681-1:2023 (E)
G.1 General . 34
G.2 Reagents . 34
G.3 Equipment . 34
G.4 Procedure . 34
G.4.1 Preparation of stock solutions . 34
G.4.2 Preparation of internal standard solution . 34
G.4.3 Preparation of calibration solutions . 35
G.4.4 Analysis . 35
G.5 Expression of results . 35
G.5.1 Calibration. 35
G.5.2 Calculation of the results . 35
G.5.3 Reliability of the method . 36
G.6 Test report . 36
G.7 Usable ions and LOQ for PFAS analysis by GC . 37
G.7.1 Using GC-MS/MS . 37
G.7.2 Using GC-MS/PCI . 38
G.7.3 Using GC-MS/EI . 39
G.8 Interferences with GC . 40
G.9 Instrumental conditions . 40
G.9.1 General . 40
G.9.2 GC-PCI/MS . 41
G.9.3 GC-MS/EI . 42
G.10 Reliability of the method . 42
Bibliography . 43
prEN 17681-1:2023 (E)
European foreword
This document (prEN 17681-1:2023) has been prepared by Technical Committee CEN/TC 248 “Textiles
and textile products”, the secretariat of which is held by BSI.
This document is currently submitted to the CEN Enquiry.
This document will supersede EN 17681-1:2022.
prEN 17681-1:2023 includes the following significant technical changes with respect to EN 17681-
1:2022:
— Title has been changed;
— Introduction has been amended;
— Table 2 has been reordered and updated with regard to new EU regulations. The substance names
have largely been aligned with prEN 17892:2022 [10];
— Clause 1: The scope has been changed considering extraction by alkaline hydrolysis now;
— Clause 2: EN 17681-2 has been deleted;
— Terms and definitions 3.1 and 3.2 have been added;
— Clause 4 has been changed, describing extraction by alkaline hydrolysis now;
— Clause 5 has been amended and reorganised;
— Clause 6 has been amended by subclause 6.12;
— Subclause 7.1: The note has been deleted;
— Subclause 8.4 has been technically revised, describing extraction by alkaline hydrolysis now;
— Subclause 8.4 has been amended and technically revised;
— Subclause 9.3 has been rephrased and amended;
— Subclause 9.4: The title and the content have been revised;
— Subclause 9.5: The subclause has been deleted, statistical data on the reliability are presented in
Annex E now;
— Clause 10 has been rephrased;
— Table A.1: The substance names have largely
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