Textiles and textile products - Organic fluorine - Part 1: Determination of non-volatile compounds by extraction method using liquid chromatography

This part of the standard specifies a test method (using liquid chromatography, LC) for detection and quantification of all extractable neutral, ionic, perfluorinated and polyfluorinated non-volatile substances in textile products (for example, in fabrics treated with fluorochemical finishes and in coated fabrics).
Classes of volatile and non volatile compounds (regulated and of concern) in Table 1 include acids, salt acids, esters, amides, telomers, sulfonates, sulfonamides and sulfonamidalcohols.

Textilien und textile Erzeugnisse - Organisches Fluor - Teil 1: Bestimmung des Gehaltes an nichtflüchtigen Verbindungen durch Extraktionsverfahren mittels Flüssigkeitschromatographie

Dieses Dokument legt ein Prüfverfahren (unter Anwendung von Flüssigkeitschromatographie, LC (en: liquid chromatography)) zum Nachweis und zur quantitativen Bestimmung von ausgewählten extrahierbaren perfluorierten und polyfluorierten Verbindungen in textilen Materialien (Fasern, Garne, textile Flächengebilde) und beschichteten textilen Flächengebilden fest.
ANMERKUNG 1 CEN/TR 16741 legt fest, welche Materialien für diese Bestimmung anzuwenden sind.
Ein Prüfverfahren (unter Anwendung von Gaschromatographie, GC (en: gas chromatography)) zum Nachweis und zur quantitativen Bestimmung von ausgewählten extrahierbaren perfluorierten und polyfluorierten Verbindungen ist in EN 17681-2 festgelegt.
ANMERKUNG 2 Sowohl dieses Dokument als auch EN 17681-2 werden für die Bestimmung und Totalisierung der PFOA verwandten Verbindungen benötigt.
Die Klassen regulierter Verbindungen sind in Tabelle 2 aufgeführt. Klassen anderer, nichtregulierter Verbindungen, die nach diesem Dokument bestimmt werden können, sind in Anhang C, Tabelle C.1, festgelegt. Dieses Dokument ist auch anzuwenden für weitere PFAS Verbindungen, vorausgesetzt, dass das Verfahren mit den zusätzlichen Verbindungen validiert wird.
ANMERKUNG 3 Die delegierte Verordnung (EU) 2020/784 der Kommission zur Änderung des Anhangs I der Verordnung (EU) 2019/1021 des Europäischen Parlaments und des Rates hinsichtlich der Aufnahme von Perfluoroctansäure (PFOA), ihrer Salze und von PFOA-verwandten Verbindungen legt u. a. fest, dass „PFOA verwandte Verbindungen umfasst: ...alle Stoffe (...), die zu PFOA abgebaut werden, einschließlich aller Stoffe (auch Salze und Polymere), die eine lineare oder verzweigte Perfluorheptylgruppe mit dem Bestandteil (C7F15)C als Strukturelement aufweisen.“ Um festzustellen, ob ihre Anwesenheit beabsichtigt ist, könnte die Aufnahme eines alkalischen Hydrolyseverfahrens zur Entfernung der Seitenkette des Polymers erforderlich sein. Nach Verordnung (EU) 2021/1297 der Kommission [7] trifft dies gleichermaßen auf C9-C14 PFCA-verwandte Stoffe zu. Eine zukünftige Überarbeitung dieses Dokumentes wird diesen Gesichtspunkt berücksichtigen.

Textiles et produits textiles - Fluor organique - Partie 1 : Détermination de composés non volatils par une méthode d’extraction utilisant la chromatographie en phase liquide

Le présent document spécifie une méthode d'essai (par chromatographie en phase liquide, LC) pour la détection et la quantification, dans des matières textiles (fibres, fils, étoffes) et des supports textiles revêtus, de substances perfluorées et polyfluorées extractibles sélectionnées.
NOTE 1 Le CEN/TR 16741 définit les matériaux auxquels s'applique cette détermination.
Une méthode d'essai (par chromatographie en phase gazeuse, GC) pour la détection et la quantification de substances perfluorées et polyfluorées extractibles sélectionnées est spécifiée dans l'EN 17681-2.
NOTE 2 Le présent document et l'EN 17681-2 sont tous les deux nécessaires pour les substances apparentées au PFOA.
Les classes de composés réglementés sont répertoriées dans le Tableau 2. Les classes d'autres composés, non réglementés, qui peuvent être déterminés en appliquant le présent document sont définies dans le Tableau C.1 (Annexe C). Le présent document est également applicable à d'autres PFAS, à condition que la méthode soit validée avec les composés additionnels.
NOTE 3 Le règlement délégué (UE) 2020/784 de la Commission modifiant l'annexe I du règlement (UE) 2019/1021 concernant les polluants organiques persistants aux fins d’y inscrire l’acide perfluorooctanoïque (PFOA), ses sels et les composés apparentés au PFOA stipule, entre autres, ce qui suit : « par " composés apparentés au PFOA ", il est entendu : … toutes les substances qui se dégradent en PFOA, y compris les substances (sels et polymères compris) qui comportent, parmi leurs éléments structurels, un groupe fonctionnel perfluoroheptyle (C7F15)C linéaire ou ramifié. » Pour déterminer si leur présence est intentionnelle, il pourrait s'avérer nécessaire d'introduire une méthode d'hydrolyse alcaline pour supprimer la chaîne latérale du polymère. Conformément au règlement (UE) 2021/1297[7] de la Commission, ceci s'applique de manière similaire aux composés apparentés aux PFCA en C9-C14. Le sujet sera abordé dans une future révision du présent document.

Tekstil in tekstilni izdelki - Organski fluor - 1. del: Določevanje nehlapnih spojin z ekstrakcijsko metodo s tekočinsko kromatografijo

General Information

Status
Published
Public Enquiry End Date
30-Jun-2021
Publication Date
11-Oct-2022
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
11-Oct-2022
Due Date
16-Dec-2022
Completion Date
12-Oct-2022

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SLOVENSKI STANDARD
SIST EN 17681-1:2022
01-december-2022

Tekstil in tekstilni izdelki - Organski fluor - 1. del: Določevanje nehlapnih spojin z

ekstrakcijsko metodo s tekočinsko kromatografijo

Textiles and textile products - Organic fluorine - Part 1: Determination of non-volatile

compounds by extraction method using liquid chromatography

Textilien und textile Erzeugnisse - Organisches Fluor - Teil 1: Bestimmung des Gehaltes

an nichtflüchtigen Verbindungen durch Extraktionsverfahren mittels
Flüssigkeitschromatographie

Textiles et produits textiles - Fluor organique - Partie 1 : Détermination de composés non

volatils par une méthode d’extraction utilisant la chromatographie en phase liquide

Ta slovenski standard je istoveten z: EN 17681-1:2022
ICS:
59.080.01 Tekstilije na splošno Textiles in general
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
SIST EN 17681-1:2022 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN 17681-1:2022
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SIST EN 17681-1:2022
EN 17681-1
EUROPEAN STANDARD
NORME EUROPÉENNE
September 2022
EUROPÄISCHE NORM
ICS 59.080.01
English Version
Textiles and textile products - Organic fluorine - Part 1:
Determination of non-volatile compounds by extraction
method using liquid chromatography

Textiles et produits textiles - Fluor organique - Partie 1 Textilien und textile Erzeugnisse - Organisches Fluor -

: Détermination de composés non volatils par une Teil 1: Bestimmung des Gehaltes an nichtflüchtigen

méthode d'extraction utilisant la chromatographie en Verbindungen durch Extraktionsverfahren mittels

phase liquide Flüssigkeitschromatographie
This European Standard was approved by CEN on 24 July 2022.

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

© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17681-1:2022 E

worldwide for CEN national Members.
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SIST EN 17681-1:2022
EN 17681-1:2022 (E)
Contents Page

European foreword ............................................................................................................................................. 3

Introduction .......................................................................................................................................................... 4

1 Scope ........................................................................................................................................................11

2 Normative references ........................................................................................................................11

3 Terms and definitions .......................................................................................................................11

4 Principle of method ............................................................................................................................12

5 Reagents .................................................................................................................................................12

6 Equipment .............................................................................................................................................12

7 Sampling .................................................................................................................................................13

7.1 General ....................................................................................................................................................13

7.2 Sampling based on area ....................................................................................................................13

7.3 Sampling based on mass ...................................................................................................................13

7.4 Preparation of test specimen ..........................................................................................................13

8 Procedure...............................................................................................................................................14

8.1 Preparation of stock solutions .......................................................................................................14

8.2 Preparation of the check solution .................................................................................................14

8.3 Preparation of calibration solutions ............................................................................................14

8.4 Extraction ...............................................................................................................................................14

8.5 Analysis ...................................................................................................................................................14

9 Expression of results ..........................................................................................................................15

9.1 Calibration .............................................................................................................................................15

9.2 Calculation of the results ..................................................................................................................15

9.3 Calculation of the sums of certain PFAS ......................................................................................16

9.4 Limit of detection (LoD) and limit of quantification (LoQ) ..................................................16

9.5 Reliability of the method ..................................................................................................................16

10 Test report .............................................................................................................................................18

Annex A (normative) Usable ions and reachable quantification limits for PFAS analysis by

LC/MS/MS ..............................................................................................................................................19

Annex B (informative) Interferences with LC/MS/MS ........................................................................21

Annex C (informative) Non-regulated PFAS ...........................................................................................22

Annex D (informative) Chromatographic conditions ..........................................................................23

D.1 General ....................................................................................................................................................23

D.2 Chromatographic conditions ..........................................................................................................23

D.3 LC/MS/MS conditions ........................................................................................................................23

Bibliography ........................................................................................................................................................24

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SIST EN 17681-1:2022
EN 17681-1:2022 (E)
European foreword

This document (EN 17681-1:2022) has been prepared by Technical Committee CEN/TC 248 “Textiles

and textile products”, the secretariat of which is held by BSI.

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 March 2023, and conflicting national standards shall be

withdrawn at the latest by March 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.

Any feedback and questions on this document should be directed to the users’ national standards body.

A complete listing of these bodies can be found on the CEN website.

According to the CEN-CENELEC Internal Regulations, the national standards organisations 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.
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SIST EN 17681-1:2022
EN 17681-1:2022 (E)
Introduction

In the European Union, according to Regulation (EU) 2019/1021 on persistent organic pollutants (POP),

Article 3, Clause 1, in connection with Annex I, amended by Commission Delegated Regulation

(EU) 2020/784, the manufacturing, placing on the market and use of perfluorooctanoic acid (PFOA), its

salts and PFOA-related compounds, whether on their own, in mixtures or in articles, is prohibited. This

is in addition to the existing prohibition of perfluorooctane sulfonic acid and its derivatives (PFOS).

According to Article 4 Clause 1. (b) this does not apply in the case of a substance present as an

unintentional trace contaminant, as specified in the relevant entries of Annex I in substances, mixtures

or articles.

Annex I Part A, describing perfluorooctane sulfonic acid and its derivatives (PFOS), contains the specific

exemption (Point 2) to concentrations of PFOS in semi-finished products or articles, or parts thereof, if

the concentration of PFOS is lower than 0,1 % mass fraction calculated with reference to the mass of

structurally or micro-structurally distinct parts that contain PFOS or, for textiles or other coated

materials, if the amount of PFOS is lower than 1 μg/m of the coated material. PFOS compounds have the

formula C F SO X where X = OH, Metal salt (O-M ), halide, amide and other derivatives, including

8 17 2
polymers.

In Annex I Part A, describing perfluorooctanoic acid (PFOA), its salts and PFOA-related compounds,

contains the specific exemption (Point 1) to concentrations of PFOA or any of its salts equal to or below

0,025 mg/kg (0,000 002 5 % mass fraction), where they are present in substances, mixtures or articles.

In addition, (Point 2) Article 4(1) applies to concentrations of any individual PFOA-related compound or

a combination of PFOA-related compounds equal to or below 1 mg/kg (0,000 1 % mass fraction) where

they are present in substances, mixtures or articles.
PFOA, its salts and PFOA-related compounds means the following:
i) perfluorooctanoic acid, including any of its branched isomers;
ii) its salts;

iii) PFOA-related compounds which, for the purposes of the Convention, are any substances that degrade

to PFOA, including any substances (including salts and polymers) having a linear or branched

perfluoroheptyl group with the moiety (C F )C as one of the structural elements.
7 15
The following compounds are not included as PFOA-related compounds:
iv) C F -X, where X = F, Cl, Br;
8 17

v) fluoropolymers that are covered by CF [CF ] -R’, where R’ = any group, n > 16;

3 2 n

vi) perfluoroalkyl carboxylic acids (including their salts, esters, halides and anhydrides) with ≥ 8

perfluorinated carbons;

vii) perfluoroalkane sulfonic acids and perfluoro phosphonic acids (including their salts, esters, halides

and anhydrides) with ≥ 9 perfluorinated carbons;

viii) perfluorooctane sulfonic acid and its derivatives (PFOS), as listed in Annex I.

As a further exemption in Annex I Part A (Point 5 c) the manufacturing, placing on the market and use of

PFOA, its salts and PFOA-related compounds is allowed in textiles for oil and water repellency for the

protection of workers from dangerous liquids that comprise risks to their health and safety, until 4 July

2023.
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SIST EN 17681-1:2022
EN 17681-1:2022 (E)

Commission Regulation (EU) 2021/1297 amending Regulation (EC) No 1907/2006 (REACH), Annex

XVII [7] restricts perfluorocarboxylic acids containing 9 to 14 carbon atoms in the chain (C9-C14 PFCAs),

their salts and C9-C14 PFCA-related substances from 25 February 2023.
This restriction concerns the following substances:

Linear and branched perfluorocarboxylic acids of the formula C F -C(= O)OH where n = 8, 9, 10, 11,

n 2n+1
12, or 13 (C9-C14 PFCAs), including their salts, and any combinations thereof;

Any C9-C14 PFCA-related substance having a perfluoro group with the formula C F - directly attached

n 2n+1

to another carbon atom, where n = 8, 9, 10, 11, 12, or 13, including their salts and any combinations

thereof;

Any C9-C14 PFCA-related substance having a perfluoro group with the formula C F - that it is not

n 2n+1

directly attached to another carbon atom, where n = 9, 10, 11, 12, 13 or 14 as one of the structural

elements, including their salts and any combinations thereof.
The following substances are excluded from this designation:
C F -X, where X = F, Cl, or Br
n 2n+1
where n = 9, 10, 11, 12, 13 or 14, including any combinations thereof,
C F -C(= O)OX' where n > 13 and X' = any group, including salts.
n 2n+1

Several per- and poly-fluorinated alkylated substances (PFAS), which are not restricted under the POP

Regulation have been added as Substances of Very High Concern (SVHC) to the Candidate List according

to Regulation (EC) No 1907/2006 (REACH), Article 59.

Per- and poly-fluorinated compounds from C4 – C14 (PFAS) occur, for example, in soil and water repellent

finishes within textiles or can be introduced as contaminants (for example from water sources).

Categories of PFAS are shown in Table 1. Table 2 lists classes of regulated compounds (i.e. listed in a

Regulation) including acids, telomers, sulfonates and sulfonamidalcohols. Compounds of concern (i.e. not

listed yet in a Regulation) are shown in the informative Annex C.
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SIST EN 17681-1:2022
EN 17681-1:2022 (E)
Table 1 — Categories of PFAS
Applications
Type of PFAS Sub-group Category
Use
Sources of contamination
Surfactant in fire-fighting foam, emulsifier in
+ +
K , Li , diethanolamine
floor polish, mist suppressant for metal plating
Surfactant for alkaline
(DEA) salt
baths, surfactant for etching acids for circuit A
cleaners
boards, pesticide active ingredient for ant bait
analysed as acids
traps
PFAS salts
Amines - Mist suppressant for metal plating baths B
Ammonium salts
- Emulsifier for fluoropolymer production C
analysed as acids
Water/solvent repellence
Amphoterics - D
for leather/paper
Carboxylates - Antistatic agent in photographic paper E
PFAS substances Amides - Pesticide active ingredient F
Oxazolidinones - Waterproofing casts (electronics) G
Alcohols, silanes, Soil and water repellence
alkoxylates, fatty acid esters, for carpets, fabrics,
- H
adipates, urethanes, upholstery, apparel,
polyesters, acrylates leather, metal, glass
PFAS
polymers/oligomers
Water repellence for
Soil/oil/water repellence for plates, food
Copolymers, phosphate carpets, fabrics, upholstery,
containers, bags, wraps, folding cartons, I
esters apparel, leather, metal,
containers, carbonless forms, masking papers
glass

These substances are not relevant in the manufacturing process of textiles but it is possible to find them as contaminants.

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SIST EN 17681-1:2022
EN 17681-1:2022 (E)
Table 2 — Regulated PFAS
PFAS
Applicable test method category
CAS Registry
regulation
(Table 1)
No. Substance Number®
(CAS RN®)
EN 17681-1 EN 17681-2
Perfluorinated carboxylic acids
under
1 PFHxA Perfluoro-n-hexanoic acid 307–24–4 x evaluation A and C
(REACH)
POP and
2 PFOA Perfluoro-n-octanoic acid 335–67–1 x A and C
REACH (SVHC)
APFO C
Perfluoro-n-octanoic acid salts
- Ammonium pentadecafluorooctanoate 3825–26–1
Na-PFO A
- Sodium perfluorooctanoate 335–95–5
K-PFO x POP A
2.2
- Potassium perfluorooctanoate 2395–00–8
Ag-PFO A
- Silver perfluorooctanoate 335–93–3
F-PFO - Perfluorooctanoyl fluoride 335–66–0 A
8:2 FTS 1H,1H,2H,2H-Perfluorodecanesulfonic acid 39108–34–4 x POP A
Me-PFOA Methyl perfluorooctanoate 376–27–2 x POP H
5 Et-PFOA Ethyl perfluorooctanoate 3108–24–5 x POP H
REACH
6 PFNA Perfluoro-n-nonanoic acid 375–95–1 x Annex XVII and
SVHC
Perfluoro-n-nonanoic acid salts REACH
NH -PFN
6.2 - Ammonium perfluorononanoate 4149–60–4 x Annex XVII and
Na-PFN
- Sodium perfluorononanoate 21049–39–8 SVHC

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 CEN of the product named. Equivalent products may be used if they can be shown to lead to the same results.

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SIST EN 17681-1:2022
EN 17681-1:2022 (E)
PFAS
Applicable test method category
CAS Registry
regulation
(Table 1)
No. Substance Number®
(CAS RN®)
EN 17681-1 EN 17681-2
REACH
Annex XVII and
7 PFDA Perfluoro-n-decanoic acid 335–76–2 x
SVHC
Perfluoro-n-decanoic acid salts REACH
NH -PFD
7.2 - Ammonium perfluorodecanoate 3830–45–3 x Annex XVII and
Na-PFD
- Sodium perfluorodecanoate 3108–42–7 SVHC
REACH
8 PFUnA Perfluoroundecanoic acid 2058–94–8 x Annex XVII and
SVHC
REACH
9 PFDoA Perfluorododecanoic acid 307–55–1 x Annex XVII and
SVHC
REACH
10 PFTrDA Perfluorotridecanoic acid 72629–94–8 x
Annex XVII and
SVHC
REACH
11 PFTeDA Perfluorotetradecanoic acid 376–06–7 x Annex XVII and
SVHC
REACH
12 PF-3,7-DMOA Perfluoro(3,7-dimethyloctanoic acid) 172155–07–6 x
Annex XVII
13 4HPFUnA 2H,2H,3H,3H-Heptadecafluoroundecanoic acid 34598–33–9 x POP
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SIST EN 17681-1:2022
EN 17681-1:2022 (E)
PFAS
Applicable test method category
CAS Registry
regulation
(Table 1)
No. Substance Number®
(CAS RN®)
EN 17681-1 EN 17681-2
Perfluorinated sulfonic acids
REACH
14 PFBS Perfluorobutanesulfonic acid 375–73–5 x A
(SVHC)
REACH
15 PFHxS Perfluorohexanesulfonic acid 355–46–4 x H
(SVHC)
16 PFOS Perfluorooctanesulfonic acid 1763–23–1 x POP H
Perfluorooctane sulfonic acid salts C F SO X
8 17 2
2795–39–3 A
- Potassium perfluorooctane sulfonate
29457–72–5 A
- Lithium perfluorooctane sulfonate
PFOS-X x POP
16.2
29081–56–9 A
- Ammonium perfluorooctane sulfonate
70225–14–8 A
- Bis2(hydroxyethyl)ammonium perfluorooctane sulfonate
56773–42–3 A
- Tetraethyl ammonium heptadecafluorooctane sulfonate
Perfluoro-octanesulfonamides (FOSA)
PFOSA Perfluorooctane sulfonamide 754–91–6 x POP F
N-MeFOSA N-Methylperfluoro-1-octanesulfonamide 31506–32–8 x POP F
19 N-EtFOSA N-Ethylperfluoro-1-octanesulfonamide 4151–50–2 x POP F
Perfluoro-octanesulfonamido ethanol (FOSE)

20 N-MeFOSE 2-(N-methylperfluoro-1-octanesulfonamideo)-ethanol 24448–09–7 x x POP H

N-EtFOSE 2-(N-Ethylperfluoro-1-octanesulfonamido)-ethanol 1691–99–2 x x POP H
Fluorinated telomer alcohols (FTOH)
22 8:2 FTOH 2-Perfluorooctylethanol 678–39–7 x POP H
REACH
23 10:2 FTOH 2-Perfluorodecylethanol 865–86–1 x H
Annex XVII
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SIST EN 17681-1:2022
EN 17681-1:2022 (E)
PFAS
Applicable test method category
CAS Registry
regulation
(Table 1)
No. Substance Number®
(CAS RN®)
EN 17681-1 EN 17681-2
Fluorinated telomer acrylates
24 8:2 FTA 1H,1H,2H,2H-Perfluorodecyl acrylate 27905–45–9 x POP H
REACH
25 10:2 FTA 1H,1H,2H,2H-Perfluorododecyl acrylate 17741–60–5 x H
Annex XVII
Other
26 PFOSF Heptadecafluorooctanesulfonyl fluoride 307–35–7 x POP
27 8:2 FTMA 1H,1H,2H,2H-heptadecafluorodecylmethacrylate 1996–88–9 x POP
1-decanaminium, N-decyl-N, N dimethyl-
28 0,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluoro-1- 251099–16–8 x POP A
octanesulfonate
REACH

29 HPFO-DA 2,3,3,3-tetrafluoro-2-(heptafluoropropoxy)propionic acid 13252–13–6 x A and C

(SVHC)
2,3,3,3-tetrafluoro-2-(heptafluoropropoxy)propionic acid
salts and acyl halides
REACH
X = F
HPFO-DA -X 21062–98–8 x A and C
29.2
(SVHC)
X = NH
62037–80–3 x
67118–55–2 x
X = K

Table 2 states the situation of the regulated PFAS on 2022–06–23 and might not be exhaustive. Readers should pay attention for updated information. Regulation (EU)

2021/1297 on C -C carboxylic acid substances will be enforced in 02/2023.
9 14
The results of PFOA and related substances to be summed up.

The results of PFOS and related substances to be summed up – calculated as PFOS.

For the halides a hydrolysation with water from the methanol extract is necessary.

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SIST EN 17681-1:2022
EN 17681-1:2022 (E)
1 Scope

This document specifies a test method (using liquid chromatography, LC) for detection and quantification

of selected extractable perfluorinated and polyfluorinated substances in textile materials (fibres, yarns,

fabrics) and coated fabrics.

NOTE 1 CEN/TR 16741 defines which materials are applicable to this determination.

A test method (using gas chromatography, GC) for detection and quantification of selected extractable

perfluorinated and polyfluorinated substances is specified in EN 17681-2.

NOTE 2 Both this document and EN 17681-2 are needed for the determination and totalization of the PFOA

related substances.

Classes of regulated compounds are listed in Table 2. Classes of other non-regulated compounds that can

be determined by this document are defined in Annex C, Table C.1. This document is also applicable for

further PFAS substances provided that the method is validated with the additional compounds.

NOTE 3 Commission Delegated Regulation (EU) 2020/784 amending Annex I to the POP Regulation (EU)

2019/1021 as regards the listing of perfluorooctanoic acid (PFOA), its salts and PFOA-related compounds defines

among other that “’…PFOA-related compounds’ means the following: … any substances that degrade to PFOA,

including any substances (including salts and polymers) having a linear or branched perfluoroheptyl group with

the moiety (C F )C as one of the structural elements.” To determine whether these are intentionally present it

7 15

could be necessary to introduce an alkaline hydrolysis method to remove the side-chain from the polymer.

According to Commission Regulation (EU) 2021/1297 [7], this applies similarly to C9-C14 PFCAs-related

compounds. A future revision of this document will address this aspect.
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.

EN 17681-2, Textiles and textile products - Organic fluorine - Part 2: Determination of volatile compounds

by extraction method using gas chromatography

EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696)

EN ISO 4787, Laboratory glass and plastic ware - Volumetric instruments - Methods for testing of capacity

and for use (ISO 4787)

EN ISO 5089, Textiles - Preparation of laboratory test samples and test specimens for chemical testing

(ISO 5089)
3 Terms and definitions
No terms and definitions are listed in this document.

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/
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SIST EN 17681-1:2022
EN 17681-1:2022 (E)
4 Principle of method

The selected compounds listed in Table 2 and in Table C.1 are extracted in an ultrasonic bath with

methanol and the extract is analysed by liquid chromatography 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 Methanol, LC-MS grade, CAS RN® 67-56-1
5.2 Check standards
5.2.1 Perfluoro-n-[1,2,3,4- C ]-octanoic-acid, CAS RN® 960315-48-4.

5.2.2 Other validated check standards can be used, for example C -PFOS, Sodium perfluoro-1-

13 18

[1,2,3,4- C]octanesulfonate (CAS RN® 960315-53-1); O -PFOS; 1H,1H,2H,2H-Perfluor(9-

4 x
methyldecan)-1-ol (CAS RN® 31200-98-2).
5.3 Water, grade 1 according to EN ISO 3696 or LC-MS grade
5.4 Selected PFAS, listed in Table 2 and Table C.1

Target compounds are available commercially as certified solutions, or a solution of target compounds

may be made.
6 Equipment
6.1 General

If possible, use equipment free from all types of fluoropolymer plastics, including polytetrafluoroethylene

(PTFE). For example, use equipment made of polypropylene (PP) or polyethylene (PE). The usual

laboratory apparatus and laboratory glassware according to EN ISO 4787 shall be used, in addition to the

following:

6.2 Test specimen containers, for example made from glass, PP, or PE. Re-used containers shall be

rinsed thoroughly with methanol (5.1) prior to use. Containers shall be checked for possible background

contamination before use.
6.3 Cutting die or template and cutting tool, to measure and cut area materials.

6.4 Extraction vials (glass, polypropylene), for example 40 ml, free from interfering compounds.

NOTE Further information about interferences can be found in Annex B.

6.5 LC Vials of glass, polypropylene or polyethylene, free from interfering compounds.

NOTE Further information about interferences can be found in Annex B.

6.6 Ultrasonic bath, equipped with heater (bath temperature to be set at (60 ± 5) °C).

6.7 Concentration equipment, for example rotavapor. Other apparatus for concentrating the sample

may be used, for example, a water bath with regulated nitrogen flow over the liquid.

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SIST EN 17681-1:2022
EN 17681-1:2022 (E)

6.8 Liquid chromatograph, temperature-controlled and with all required accessories, including

gases, LC columns, injector and a mass spectrometric detector with MS-MS, free from all types of

fluoropolymer plastics, including polytetrafluoroethene (PTFE).
6.9 Balance, with a resolution of 1 mg or better.
6.10 Analytical balance, with a resolution of at least 0,1 mg.

6.11 Filter, cellulosic filter, 0,45 µm pore size or polypropylene filter 0,2µm pore size.

NOTE It is possible that filters can be contaminated with PFAS. A check can be made by washing the filter with

a solvent corresponding to the extraction solvent and analysing the washing.
7 Sampling
7.1 General

The chosen sample shall be representative of the lot it is taken from. If possible, sampling shall be carried

out according to EN ISO 5089. When the sampling is being performed on products that have separate

distinct parts, the product shall be deconstructed and each part shall be treated according to the

applicable subclause 7.2 or 7.3.

NOTE The same method of preparation can be used for testing according to EN 17681-2 and this document, to

avoid duplication of effort.
7.2 Sampling based on area

When determining PFOS-related compounds using this document the result shall be reported as

mass/unit area. Take a fabric test specimen in order to get at least 1 g of material and an area of at least

100 cm .

Cut out using a cutting die or applicable tool and template (6.3) avoiding distortion of the fabric, to

determine the test specimen area to the nearest 0,1 cm each side. When using the cutting die, use the area

of the die for the calculation. Weigh the test specimen and record the mass to the nearest 10 mg using a

balance (6.9).

Determination of both area and mass allows expression of the results in both units of mg/kg and µg/m .

NOTE If less than 1 g of sample is available the volume of extraction solvent and check solution can be reduced

proportionately.
7.3 Sampling based on mass
If the material is no
...

SLOVENSKI STANDARD
oSIST prEN 17681-1:2021
01-junij-2021

Tekstil in tekstilni izdelki - Organski fluor - 1. del: Določevanje nehlapnih spojin z

ekstrakcijsko metodo s tekočinsko kromatografijo

Textiles and textile products - Organic fluorine - Part 1: Determination of non-volatile

compounds by extraction method using liquid chromatography

Textilien und textile Erzeugnisse - Organisches Fluor - Teil 1: Bestimmung des Gehaltes

an nichtflüchtigen Verbindungen durch Extraktionsverfahren mittels
Flüssigkeitschromatographie
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
oSIST prEN 17681-1:2021 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
oSIST prEN 17681-1:2021
---------------------- Page: 2 ----------------------
oSIST prEN 17681-1:2021
DRAFT
EUROPEAN STANDARD
prEN 17681-1
NORME EUROPÉENNE
EUROPÄISCHE NORM
June 2021
ICS 59.080.01
English Version
Textiles and textile products - Organic fluorine - Part 1:
Determination of non-volatile compounds by extraction
method using liquid chromatography
Textilien und textile Erzeugnisse - Organisches Fluor -
Teil 1: Bestimmung des Gehaltes an nichtflüchtigen
Verbindungen durch Extraktionsverfahren mittels
Flüssigkeitschromatographie

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, Turkey 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

© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 17681-1:2021 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
oSIST prEN 17681-1:2021
prEN 17681-1:2021 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

Introduction .................................................................................................................................................................... 4

1 Scope .................................................................................................................................................................... 9

2 Normative references .................................................................................................................................... 9

3 Terms and definitions ................................................................................................................................... 9

4 Principle of method ........................................................................................................................................ 9

5 Reagents ............................................................................................................................................................. 9

5.4 Selected PFAS listed in Table 2 and Table C.1 .................................................................................... 10

6 Equipment ...................................................................................................................................................... 10

7 Sampling .......................................................................................................................................................... 10

7.1 General ............................................................................................................................................................. 10

7.2 Sampling based on area ............................................................................................................................. 10

7.3 Sampling based on mass ............................................................................................................................ 11

7.4 Preparation .................................................................................................................................................... 11

7.4.1 Preparation of test specimen ................................................................................................................... 11

8 Procedure........................................................................................................................................................ 11

8.1 Preparation of stock solutions ................................................................................................................ 11

8.2 Preparation of the check solution .......................................................................................................... 11

8.3 Preparation of calibration solutions ..................................................................................................... 11

8.4 Extraction ........................................................................................................................................................ 11

8.5 Analysis ............................................................................................................................................................ 12

9 Expression of results ................................................................................................................................... 12

9.1 Calibration ...................................................................................................................................................... 12

9.2 Calculation of the results ........................................................................................................................... 12

9.3 Calculation of the results of a sum ......................................................................................................... 13

9.4 Limit of detection (LoD) and limit of quantification (LoQ) ........................................................... 13

10 Test report ...................................................................................................................................................... 13

Annex A (normative) Usable ions and LOQ for PFAS analysis by LC/MS/MS ....................................... 14

Annex B (informative) Interferences with LC/MS/MS ................................................................................. 16

Annex C (informative) Non-regulated PFAS .................................................................................................... 17

Annex D (informative) Chromatographic conditions ................................................................................... 19

D.1 General ............................................................................................................................................................. 19

D.2 Chromatographic conditions ................................................................................................................... 19

D.3 LC/MS/MS conditions ................................................................................................................................. 19

Bibliography ................................................................................................................................................................. 20

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oSIST prEN 17681-1:2021
prEN 17681-1:2021 (E)
European foreword

This document (prEN 17681-1:2021) 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.
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oSIST prEN 17681-1:2021
prEN 17681-1:2021 (E)
Introduction

In the European Union, according to Regulation (EU) 2019/1021 persistent organic pollutants (POP), Article

3, Clause 1, in connection with Annex I, amended by COMMISSION DELEGATED REGULATION (EU) 2020/784,

the manufacturing, placing on the market and use of perfluorooctanoic acid (PFOA), its salts and PFOA-related

compounds, whether on their own, in mixtures or in articles, shall be prohibited. This is in addition to the

existing prohibition of perfluorooctane sulfonic acid and its derivatives (PFOS).

According to Article 4 Clause 1. (b) this shall not apply in the case of a substance present as an unintentional

trace contaminant, as specified in the relevant entries of Annex I in substances, mixtures or articles.

Annex I Part A, describing perfluorooctane sulfonic acid and its derivatives (PFOS), contains the specific

exemption (Point 2) to concentrations of PFOS in semi-finished products or articles, or parts thereof, if the

concentration of PFOS is lower than 0,1 % by weight calculated with reference to the mass of structurally or

micro-structurally distinct parts that contain PFOS or, for textiles or other coated materials, if the amount of

PFOS is lower than 1 μg/m of the coated material. PFOS compounds have the formula C F SO X where

8 17 2

X = OH, Metal salt (O-M ), halide, amide and other derivatives, including polymers.

Annex I also states (point 5) that once standards are adopted by the European Committee for Standardization

(CEN) they shall be used as the analytical test methods for demonstrating the conformity of articles to point

In Annex I Part A, describing perfluorooctanoic acid (PFOA), its salts and PFOA-related compounds, contains

the specific exemption (Point 1) to concentrations of PFOA or any of its salts equal to or below 0,025 mg/kg

(0,000 002 5 % by weight) where they are present in substances, mixtures or articles. In addition, (Point 2)

Article 4(1) shall apply to concentrations of any individual PFOA-related compound or a combination of PFOA-

related compounds equal to or below 1 mg/kg (0,000 1 % by weight) where they are present in substances,

mixtures or articles.
PFOA, its salts and PFOA-related compounds means the following:
(i) perfluorooctanoic acid, including any of its branched isomers;
(ii) its salts;

(iii) PFOA-related compounds which, for the purposes of the Convention, are any substances that degrade to

PFOA, including any substances (including salts and polymers) having a linear or branched perfluoroheptyl

group with the moiety (C F )C as one of the structural elements.
7 15
The following compounds are not included as PFOA-related compounds:
(i) C F -X, where X = F, Cl, Br;
8 17

(ii) fluoropolymers that are covered by CF [CF ]n-R’, where R’ = any group, n > 16;

3 2

(iii) perfluoroalkyl carboxylic acids (including their salts, esters, halides and anhydrides) with ≥ 8

perfluorinated carbons;

(iv) perfluoroalkane sulfonic acids and perfluoro phosphonic acids (including their salts, esters, halides and

anhydrides) with ≥ 9 perfluorinated carbons;

(v) perfluorooctane sulfonic acid and its derivatives (PFOS), as listed in Annex I.

As a further exemption in Annex I Part A (Point 5 c) the manufacturing, placing on the market and use of PFOA,

its salts and PFOA-related compounds shall be allowed in textiles for oil and water repellency for the

protection of workers from dangerous liquids that comprise risks to their health and safety, until 4 July 2023.

Several per- and poly-fluorinated alkylated substances (PFAS), which are not restricted under the POP

regulation have been added as Substances of Very High Concern (SVHC) to the Candidate List according to

Regulation (EC) No 1907/2006 (REACH), Article 59.
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oSIST prEN 17681-1:2021
prEN 17681-1:2021 (E)

Per- and poly-fluorinated compounds from C4 – C14 (PFAS) occur, for example, in soil and water repellent

finishes within textiles or can be introduced as contaminants (e.g. from water sources). Categories of PFAS

are shown in Table 1. Table 2 lists classes of regulated compounds (i.e. listed in regulation) including acids,

telomers, sulfonates and sulfonamidalcohols. Compounds of concern (i.e. not listed yet in regulation) are

shown in the informative Annex C.
Table 1 — Categories of PFAS
Applications
Type of PFAS Sub-group Category
Sources of contamination
Use
Surfactant in fire-fighting
foam, emulsifier in floor
+ +
K , Li ,
polish mist, suppressant
diethanolamine
Surfactant for alkaline for metal plating baths,
(DEA) salt
cleaners surfactant for etching acids
for circuit boards, pesticide
Analysed as acids
active ingredient for ant
bait traps
PFAS salts
Mist suppressant for metal
Amines B
plating baths
Ammonium salts
Emulsifier for
C
fluoropolymer production
Analysed as acids
Water/solvent
Amphoterics repellence for D
leather/paper
Antistatic agent in
Carboxylates E
photographic paper
PFAS substances Amides Pesticide active ingredient F
Waterproofing casts
Oxazolidinones G
(electronics)
Alcohols, silanes,
alkoxylates, fatty Soil/water repellence
acid esters, for carpets,
H
adipates, fabric/upholstery,
urethanes, apparel, leather,
polyesters, metal/glass
PFAS
acrylates
polymers/oligomers
Soil/oil/water repellence
Water repellence for
for plates, food containers,
carpet,
Copolymers, bags, wraps, folding
fabric/upholstery, I
phosphate esters cartons, containers,
apparel, leather,
carbonless forms, masking
metal/glass
papers

These substances are not relevant in the manufacturing process of textiles but it is possible to find them as contaminants.

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oSIST prEN 17681-1:2021
prEN 17681-1:2021 (E)
Table 2 — Regulated PFAS
PFAS
No Chemicals CAS No. LC GC category
law (§)
(Table 1)
Perfluorinated carboxylic acids
under
1 PFHxA Perfluoro-n-hexanoic acid 307-24-4 x evaluation A and C
(REACh)
2 PFOA Perfluoro-n-octanoic acid 335-67-1 x POP A and C
Perfluoro-n-octanoic salts
APFO C
- Ammonium pentadecafluorooctanoate
3825-26-1
Na-PFO A
- Sodium perfluorooctanoate
335-95-5
2.2 x POP
- Potassium perfluorooctanoate
K-PFO 2395-00-8 A
- Silver perfluorooctanoate
335-93-3
Ag-PFO A
- Perfluorooctanoyl fluoride
335-60-0
F-PFO A
3 8:2 FTS 1H,1H,2H,2H-Perfluorodecanesulfonic acid 39108-34-4 x POP A
4 Me-PFOA Methyl perfluorooctanoate 376-27-2 x POP H
5 Et-PFOA Ethyl perfluorooctanoate 3108-24-5 x POP H
Reach
6 PFNA Perfluoro-n-nonanoic acid 375-95-1 x
(SVHC)
Reach
7 PFDA Perfluoro-n-decanoic acid 335-76-2 x
(SVHC)
Reach
8 PFUnA Perfluoroundecanoic acid 2058-94-8 x
(SVHC)
Reach
9 PFDoA Perfluorododecanoic acid 307-55-1 x
(SVHC)
Reach
10 PFTrA Perfluorotridecanoic acid 72629-94-8 x
(SVHC)
Reach
11 PFTeA Perfluorotetradecanoic acid 376-06-7 x
(SVHC)
12 PF-3,7-DMOA Perfluoro(3,7-dimethyloctanoic acid) 172155-07-6 x POP
2H,2H,3H,3H-Heptadecafluoroundecanoic
13 4HPFUnA 34598-33-9 x POP
Acid
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oSIST prEN 17681-1:2021
prEN 17681-1:2021 (E)
PFAS
No Chemicals CAS No. LC GC category
law (§)
(Table 1)
Perfluorinated sulfonic acids
Reach
14 PFBS Perfluorobutanesulfonic acid 375-73-5 x A
(SVHC)
Reach
15 PFHxS Perfluorohexanesulfonic acid 355-46-4 x H
(SVHC)
16 PFOS Perfluoro octanesulfonic acid 1763-23-1 x POP H
Perfluorooctane sulfonic acid salts
C8F17SO2X
- potassium Perfluorooctane sulfonate
2795-39-3
- lithium Perfluorooctane sulfonate
29457-72-5
16.2 PFOS-X - ammonium Perfluorooctane sulfonate x POP
29081-56-9 A
- bis2(hydroxyethyl)ammonium
70225-14-8
Perfluorooctane sulfonate
56773-42-3
- tetraethyl ammonium
heptadecafluorooctane sulfonate
Perfluoro-octanesulfonamides (FOSA)
17 PFOSA Perfluorooctane sulfonamide 754-91-6 x POP F
18 N-MeFOSA N-Methylperfluoro-1-octanesulfonamide 31506-32-8 x POP F
19 N-EtFOSA N-Ethylperfluoro-1-octanesulfonamide 4151-50-2 x POP F
Perfluoro-octanesulfonamido ethanol (FOSE)
2-(N-methylperlfuoro-1-
20 N-MeFOSE 24448-09-7 x x POP H
octanesulfonamideo)-ethanol
2-(N-Ethylperfluoro-1-
21 N-EtFOSE 1691-99-2 x x POP H
octanesulfonamido)-ethanol
Fluorinated telomer alcohols (FTOH)
b
22 8:2 FTOH 2-Perfluorooctylethanol 678-39-7 x POP H
Fluorinated telomer acrylate (FTA)
b
23 8:2 FTA 1H,1H,2H,2H-Perfluorodecyl acrylate 27905-45-9 x POP H
Other
24 PFOSF Heptadecafluorooctanesulfonyl fluoride 307-35-7 x POP
1H,1H,2H,2H-
25 8:2 FTMA 1996-88-9 x POP
heptadecafluorodecylmethacrylate
1-decanaminium, N-decyl-N, N dimethyl-
0,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-
26 251099-16-8 x POP A
heptadecafluoro-1-
octanesulfonate
Reach
2,3,3,3-tetrafluoro-2-
27 HPFO-DA 13252-13-6 x A and C
(heptafluoropropoxy)propionic acid
(SVHC)
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oSIST prEN 17681-1:2021
prEN 17681-1:2021 (E)
PFAS
No Chemicals CAS No. LC GC category
law (§)
(Table 1)
2,3,3,3-tetrafluoro-2-
(heptafluoropropoxy)propionic acid salts
and acyl halides
Reach
27.2 HPFO-DA -X 21062-98-8 x A and C
X = F
(SVHC)
62037-80-3 x
X = NH
67118-55-2 x
X = K

Table 2 states the situation of the regulated PFAS on 2021-03-1. Readers should pay attention to update the information.

The results of PFOA related substances to be summed up.

For the halides a hydrolysation with water from the methanol extract is necessary.

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oSIST prEN 17681-1:2021
prEN 17681-1:2021 (E)
1 Scope

This document specifies a test method (using liquid chromatography, LC) for detection and quantification of

selected extractable perfluorinated and polyfluorinated substances in textile materials (fibres, yarns, fabrics)

and coated fabrics.
NOTE CEN/TR 16741 defines which materials are applicable to this determination.

A test method (using gas chromatography, GC) for detection and quantification of selected extractable

perfluorinated and polyfluorinated substances is specified in prEN 17681-2.

Classes of regulated compounds are listed in Table 2. Classes of other non-regulated

...

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