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 - Določevanje vsote perfluoriranih snovi (vsota PFAS) v pitni vodi - Metoda s tekočinsko kromatografijo in masno spektrometrijo (LC-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
oSIST prEN 17892:2022
01-september-2022
Kakovost vode - Določevanje vsote perfluoriranih snovi (vsota PFAS) v pitni vodi -
Metoda s tekočinsko kromatografijo in masno spektrometrijo (LC-MS)
Water quality - Determination of the sum of perfluorinated substances (Sum of PFAS) in
drinking water - Method using liquid chromatography/mass spectrometry (LC/MS)
Wasserqualität - Bestimmung der Summe der perfluorierten Substanzen (Summe der
PFAS) im Trinkwasser - Methode mittels Flüssigkeitschromatographie /
Massenspektrometrie (LC/MS)
Qualité de l'eau - Détermination de la somme des substances perfluorées (somme des
PFAS) dans l'eau potable - Méthode utilisant la chromatographie liquide / spectrométrie
de masse (LC / MS)
Ta slovenski standard je istoveten z: prEN 17892
ICS:
13.060.20 Pitna voda Drinking water
13.060.50 Preiskava vode na kemične Examination of water for
snovi chemical substances
oSIST prEN 17892:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

oSIST prEN 17892:2022
oSIST prEN 17892:2022
DRAFT
EUROPEAN STANDARD
prEN 17892
NORME EUROPÉENNE
EUROPÄISCHE NORM
August 2022
ICS 13.060.50
English Version
Water quality - Determination of the sum of perfluorinated
substances (Sum of PFAS) in drinking water - Method
using liquid chromatography/mass spectrometry (LC/MS)
Qualité de l'eau - Détermination de la somme des Wasserqualität - Bestimmung der Summe der
substances perfluorées (somme des PFAS) dans l'eau perfluorierten Substanzen (Summe der PFAS) im
potable - Méthode utilisant la chromatographie liquide Trinkwasser - Methode mittels
/ spectrométrie de masse (LC / MS) Flüssigkeitschromatographie / Massenspektrometrie
(LC/MS)
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 230.
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
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 17892:2022 E
worldwide for CEN national Members.

oSIST prEN 17892:2022
prEN 17892:2022 (E)
Contents Page
European foreword . 4
Introduction . 5
1 Scope . 6
2 Normative references . 6
3 Terms and definitions . 7
4 Principle . 7
Table 1 — Analytes for which a determination was validated in accordance with this
method . 8
5 Interferences . 10
5.1 Sampling . 10
5.2 Background contamination . 10
5.3 Interferences encountered during liquid chromatography and mass spectrometry 10
6 Reagents . 11
7 Apparatus . 13
8 Sampling . 14
9 Procedure . 15
9.1 Part A: Method using direct injection . 15
9.1.1 General. 15
9.1.2 Sampling . 15
9.1.3 Sample preparation . 15
9.2 Part B: Method using SPE . 15
9.2.1 General. 15
9.2.2 Sampling . 15
9.2.3 Sample preparation . 16
9.2.4 Extraction . 16
9.3 LC MS/MS operating conditions . 17
Table 2 — Selected diagnostic ions used in the determination (target substance) . 17
Table 3 — Selected diagnostic ions used in the determination of internal standards and
recommended corresponding analyte . 19
9.4 Blank determination . 20
9.5 Identification . 20
9.6 Calibration . 21
9.6.1 General requirements . 21
Table 4 — Explanation of subscripts . 22
9.6.2 Calibration using an external standard . 22
9.6.3 Calibration using an internal standard . 22
9.6.4 Calibration check . 23
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
oSIST prEN 17892:2022
prEN 17892:2022 (E)
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 . 28
Annex A (informative) Performance data . 29
Annex B . (informative) Instrumental conditions and chromatograms . 30
Table B.1 — Example of instrumental conditions LC-MS/MS . 30
Figure B.1 — Perfluoroalkyl carboxylic acids and perfluorooctane-sulfonamide . 31
Figure B.2 — Perfluoroalkane sulfonic acids, 6:2 fluorotelomer sulfonic acid and
hexafluoropropylene oxide dimer acid . 32
Bibliography . 33
oSIST prEN 17892:2022
prEN 17892:2022 (E)
European foreword
This document (prEN 17892:2022) has been prepared by the Technical Committee CEN/TC 230 “Water
analysis”, the secretariat of which is held by DIN.
This document is currently submitted to the CEN Enquiry.
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.
oSIST prEN 17892:2022
prEN 17892:2022 (E)
Introduction
Per- and polyfluoralkyl substances (PFAS) (Reference [1]) are industrially manufactured chemicals,
where some or all hydrogen atoms at the carbon skeleton have been replaced by fluorine atoms. PFAS is
a chemical family consisting of almost 5 000 individual substances. They are a group of widely used, man-
made chemicals. The perfluoralkyl substances are persistent and depending on their carbon chain length
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 foam or for
consumer products.
Due to the widespread usage and the resistance to biodegradation PFAS can now be found ubiquitous as
background contamination in the environment. Release during production processes or the application
of firefighting foams containing PFAS led to high local concentrations in some areas (Reference [2]).
In 2001 the largest producer of PFOS voluntarily phased the substance out and since 2011 respectively
2020 apart from a few exceptions, PFOS and PFOA as well as any compounds derived from these are no
longer permitted to be used or marketed in the European Union (Reference [4]). Despite these measures
PFAS represent a major legacy issue to be managed.
PFAS - especially the shorter-chain - can enter the water cycle as a result of manufacture, application and
disposal. In the EU Drinking Water Directive EU 2020/2184 (Reference [5]) PFAS are included 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 on the basis of epidemiological studies and the most sensitive effect on the
human immune system a tolerably weekly intake (TWI) for the sum of the four substances PFOA, PFNA,
PFHxS and PFOS of 4,4 ng/kg body weight (Reference [3]).
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, associ
...

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