Water quality - Determination of selected per- and polyfluoroalkyl substances in drinking water - Method using liquid chromatography/tandem-mass spectrometry (LC-MS/MS)

This document specifies a method for the determination of the dissolved fraction of selected perfluoroalkyl and polyfluoroalkyl substances (PFAS) in non-filtrated drinking water using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The applicability of the method to other types of water like fresh waters (e.g. ground water, surface water) or treated wastewater can be validated separately for each individual case.
For each target compound both, eventually occurring branched isomers and the respective non-branched isomer, are quantified together. The selected set of substances determined by this method is representative for a wide variety of PFAS. This method has been validated for the analytes specified in Table 1. The list given in this table can be modified depending on the purpose and focus of the method. The lower application range of this method can vary depending on the sensitivity of the equipment used and the matrix of the samples. For many substances to which this document applies a limit of quantification (LOQ) of 1 ng/l can be achieved. Using high volume direct injection as described in part A or SPE as described in part B of the method allows lower LOQs. Analytical limitations can occur with short-chain PFAS or PFAS with more than ten carbon atoms in the carbon chain. Actual LOQs can depend on the blank values realized by individual laboratories as well.
NOTE   This document enables the analysis of those 20 PFAS which are listed in point 3 of Part B of Annex III of the EU Drinking Water Directive, EU 2020/2184 [4], for the surveillance of the parametric limit value of 0,10 µg/l for the sum of PFAS.
Furthermore, alternatives and substitutes for these PFAS substances can be analysed using this document as well.
Table 1 - Analytes for which a determination was validated in accordance with this method

Wasserbeschaffenheit - Bestimmung ausgewählter Per- und Polyfluoralkylsubstanzen in Trinkwasser - Verfahren mittels Flüssigkeitschromatographie/Tandem-Massenspektrometrie (LC-MS/MS)

Dieses Dokument legt ein Verfahren zur Bestimmung des gelösten Anteils ausgewählter Per- und Polyfluoralkylsubstanzen (PFAS) mittels Flüssigkeitschromatografie-Tandem-Massenspektrometrie (LC-MS/MS) in nicht filtriertem Trinkwasser fest. Die Anwendbarkeit des Verfahrens auf andere Wasserarten wie Süßwasser (z. B. Grundwasser, Oberflächenwasser) oder behandeltes Abwasser kann für jeden Einzelfall separat validiert werden.
Für jede Zielverbindung werden sowohl eventuell auftretende verzweigte Isomere als auch das jeweilige unverzweigte Isomer zusammen quantifiziert. Die mit diesem Verfahren ermittelte Stoffauswahl ist repräsentativ für eine Vielzahl von PFAS. Dieses Verfahren wurde für die in Tabelle 1 angegebenen Analyten validiert. Die Liste in dieser Tabelle kann je nach Zweck und Schwerpunkt des Verfahrens modifiziert werden. Der untere Anwendungsbereich dieses Verfahrens kann abhängig von der Empfindlichkeit der verwendeten Geräte und der Matrix der Proben variieren. Für zahlreiche Stoffe, für die diese Norm gilt, kann eine Bestimmungsgrenze (LOQ) von 1 ng/l erreicht werden. Die Verwendung einer Direktinjektion mit großem Probenvolumen, wie in Teil A beschrieben, oder von SPE, wie in Teil B beschrieben, ermöglicht niedrigere LOQs. Analytische Limitierungen können bei kurzkettigen PFAS oder PFAS mit mehr als zehn Kohlenstoffatomen in der Kohlenstoffkette auftreten. Tatsächlich erreichbare LOQs können auch von den Blindwerten abhängig sein, die in den einzelnen Laboren erzielt werden können.
ANMERKUNG   Dieses Dokument ermöglicht die Analyse der 20 PFAS, die in Anhang III Teil B Punkt 3 der EU-Trinkwasserrichtlinie EU 2020/2184 [4] zur Überwachung des maximal zulässigen Parameterwerts von 0,10 µg/l für die Summe der PFAS aufgeführt sind.
Darüber hinaus können mithilfe dieses Dokuments auch Alternativen und Ersatzstoffe für diese PFAS-Substanzen analysiert werden

Qualité de l'eau - Détermination de substances per- et polyfluoroalkylées sélectionnées dans l'eau potable - Méthode par chromatographie en phase liquide couplée à la spectrométrie de masse en tandem (LC-MS/MS)

Le présent document spécifie une méthode de détermination de la fraction dissoute de substances per-et polyfluoroalkylées (PFAS) sélectionnées dans l’eau potable non filtrée par chromatographie en phase liquide couplée à la spectrométrie de masse en tandem (LC-MS/MS). L’applicabilité de la méthode à d’autres types d’eau tels que les eaux douces (par exemple, eau souterraine, eau de surface) ou les eaux usées traitées, peut être validée séparément pour chaque cas individuel.
Pour chaque composé cible, les isomères ramifiés présents ainsi que les isomères non ramifiés correspondants sont quantifiés ensemble. Le groupe de substances sélectionné, déterminé par cette méthode, est représentatif d'une large gamme de PFAS. La méthode a été validée pour les analytes spécifiés dans le Tableau 1. La liste donnée dans ce tableau peut être modifiée en fonction des besoins et de l'objectif de la méthode. La limite inférieure d’application de cette méthode peut varier en fonction de la sensibilité de l’équipement utilisé et de la matrice des échantillons. Pour des nombreuses substances pour lesquelles le présent document s’applique, une limite de quantification (LQ) de 1 ng/l peut être atteinte. L’utilisation d’un grand volume en injection directe telle que décrite dans la partie A, ou de la SPE telle que décrite dans la partie B de la méthode, permet d'obtenir des LQ plus basses. Des limites analytiques peuvent survenir avec les PFAS à chaîne courte ou avec les PFAS ayant plus de dix atomes de carbone dans la chaîne carbonée. Les LQ réelles peuvent également dépendre des valeurs de blanc obtenues par chaque laboratoire.
NOTE   Le présent document permet d’analyser les 20 PFAS qui sont répertoriés au point 3 de la Partie B de l’Annexe III de la directive européenne eau potable UE 2020/2184 [4], pour la surveillance de la valeur paramétrique limite de 0,10 µg/l pour la somme des PFAS.
Par ailleurs, des alternatifs et des substituts de ces substances PFAS peuvent également être analysés en utilisant le présent document.
Tableau 1 - Analytes pour lesquels la présente méthode a été validée

Kakovost vode - Določanje izbranih perfluoroalkilnih in polifluoroalkilnih snovi (PFAS) v pitni vodi - Metoda s tekočinsko kromatografijo s tandemsko masno spektrometrijo (LC-MS/MS)

General Information

Status
Published
Publication Date
18-Jun-2024
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Start Date
19-Jun-2024
Due Date
31-Jan-2023
Completion Date
19-Jun-2024

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SLOVENSKI STANDARD
01-oktober-2024
Kakovost vode - Določanje izbranih perfluoroalkilnih in polifluoroalkilnih snovi
(PFAS) v pitni vodi - Metoda s tekočinsko kromatografijo s tandemsko masno
spektrometrijo (LC-MS/MS)
Water quality - Determination of selected per- and polyfluoroalkyl substances in drinking
water - Method using liquid chromatography/tandem-mass spectrometry (LC-MS/MS)
Wasserbeschaffenheit - Bestimmung ausgewählter Per- und Polyfluoralkylsubstanzen in
Trinkwasser - Verfahren mittels Flüssigkeitschromatographie/Tandem-
Massenspektrometrie (LC-MS/MS)
Qualité de l'eau - Détermination de substances per- et polyfluoroalkylées sélectionnées
dans l'eau potable - Méthode par chromatographie en phase liquide couplée à la
spectrométrie de masse en tandem (LC-MS/MS)
Ta slovenski standard je istoveten z: EN 17892:2024
ICS:
13.060.20 Pitna voda Drinking water
13.060.50 Preiskava vode na kemične Examination of water for
snovi chemical substances
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN 17892
EUROPEAN STANDARD
NORME EUROPÉENNE
June 2024
EUROPÄISCHE NORM
ICS 13.060.50
English Version
Water quality - Determination of selected per- and
polyfluoroalkyl substances in drinking water - Method
using liquid chromatography/tandem-mass spectrometry
(LC-MS/MS)
Qualité de l'eau - Détermination de substances per- et Wasserbeschaffenheit - Bestimmung ausgewählter
polyfluoroalkylées sélectionnées dans l'eau potable - Per- und Polyfluoralkylsubstanzen in Trinkwasser -
Méthode par chromatographie en phase liquide Verfahren mittels
couplée à la spectrométrie de masse en tandem (LC- Flüssigkeitschromatographie/Tandem-
MS/MS) Massenspektrometrie (LC-MS/MS)
This European Standard was approved by CEN on 19 May 2024.

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
© 2024 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17892:2024 E
worldwide for CEN national Members.

Contents Page
European foreword . 4
Introduction . 5
1 Scope . 6
2 Normative references . 8
3 Terms and definitions . 8
4 Principle . 9
5 Interferences . 9
5.1 Sampling . 9
5.2 Background contamination . 9
5.3 Interferences encountered during liquid chromatography and mass spectrometry 10
6 Reagents . 10
7 Apparatus . 12
8 Sampling . 14
9 Procedure . 14
9.1 Part A: Method using direct injection . 14
9.1.1 General. 14
9.1.2 Sampling . 14
9.1.3 Sample preparation . 14
9.2 Part B: Method using SPE . 15
9.2.1 General. 15
9.2.2 Sampling . 15
9.2.3 Sample preparation . 15
9.2.4 Extraction . 16
9.3 LC MS/MS operating conditions . 17
9.4 Blank determination . 20
9.4.1 General. 20
9.4.2 Method using direct injection. 20
9.4.3 Method using SPE . 20
9.5 Identification . 20
9.6 Calibration . 21
9.6.1 General requirements . 21
9.6.2 Calibration using an external standard . 22
9.6.3 Calibration using an internal standard . 23
9.6.4 Calibration check . 24
10 Calculation . 24
10.1 Use of a calibration curve to determine concentration . 24
10.2 Calculation of concentration using calibration with external standards . 24
10.3 Calculation of concentration using calibration with internal standards . 25
10.4 Treatment of results outside the calibration range . 25
10.5 Quantification of branched isomers . 25
11 Determination of analyte recovery . 26
11.1 Recovery . 26
11.2 Recovery of internal standards . 27
12 Expression of results . 27
13 Test report . 27
Annex A (informative) Performance data . 28
Annex B (informative) Instrumental conditions and chromatograms . 35
Bibliography . 41
European foreword
This document (EN 17892:2024) has been prepared by the Technical Committee CEN/TC 230 “Water
analysis”, the secretariat of which is held by DIN.
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 2024, and conflicting national standards shall
be withdrawn at the latest by December 2024.
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.
Introduction
Per- and polyfluoroalkyl substances (PFAS) are industrially manufactured chemicals, that contain at least
one fully fluorinated methyl or methylene carbon atom (without any H/Cl/Br/I atom attached to it) [1].
This definition is also chosen in the document (see 3.1). According to the United States Environmental
Protection Agency (U.S. EPA), PFAS is a chemical family consisting of more than 8 000 individual
substances [2]. They are a group of widely used man-made chemicals. The perfluoroalkyl substances are
persistent and can accumulate over time in humans and in the environment. Because of their special
properties and stability, some of these compounds were widely used in industry, as components in
firefighting foams or for consumer products and can now be found ubiquitous as background
contamination in the environment [3].
PFAS - especially the shorter-chain - can enter the water cycle as a result of manufacture, application and
disposal. PFAS are included in the EU Drinking Water Directive EU 2020/2184 [4] as parameter to be
under surveillance with a maximum parametric limit value of 0,10 µg/l for the sum of 20 selected PFAS,
i.e. the perfluorinated carbonic acids as well as the perfluorinated sulfonic acids with chain length of four
to thirteen carbon atoms.
Longer-chain compounds such as PFOA, PFNA, PFHxS, and PFOS accumulate in the blood and the liver,
and their half-lives in the human body amount to several years. In 2020 the European Food Safety
Authority (EFSA) has derived a tolerably weekly intake (TWI) for the sum of the four substances PFOA,
PFNA, PFHxS and PFOS of 4,4 ng/kg body weight based on epidemiological studies and the most sensitive
effect on the human immune system [5].
Due to the low TWI the EFSA recommends for the four substances PFOA, PFNA, PFHxS, and PFOS, the
analysis of at least these four EFSA-PFAS should be possible with a limit of detection far below the
maximum parametric limit value of 0,10 µg/l.
WARNING — Persons using this document should be familiar with usual laboratory practice. This
document does not purport to address all of the safety problems, if any, associated with its use. It is the
responsibility of the user to establish appropriate safety and health practices.
IMPORTANT — It is absolutely essential that tests conducted in accordance with this document be
carried out by suitably qualified staff.
1 Scope
This document specifies a method for the determination of the dissolved fraction of selected
perfluoroalkyl and polyfluoroalkyl substances (PFAS) in no
...

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