oSIST prEN 17892:2022
(Main)Water quality - Determination of the sum of perfluorinated substances (Sum of PFAS) in drinking water - Method using liquid chromatography/mass spectrometry (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)
The proposed document will specify a method for the determination of the sum of selected perfluoroalkyl and polyfluoroalkyl substances (PFAS) in drinking water using liquid chromatography mass spectrometry (LC MS/MS).
The method covers at least the substances needed for the calculation of the 'Sum of PFASs ' according to Annex III, part B, point 3 of the new European drinking water directive (draft). Currently the DWD comprises the perfluoralkyl acids C4 to C13 as well as the perfluoralkyl sulfonic acids C4 to C13.
Other matrices like groundwater and additional substances like HFPO-DA (GenX) and ADONA or perfluoralkansulfonamides (FASA) will be included if possible. The lower application range of the method can vary depending on the sensitivity of the equipment used and the matrix of the sample. For most compounds to which this document applies ≥0,2 ng/l as limit of quantification can be achieved. Actual levels can depend on the blank levels realized by individual laboratory.
The applicability of the method to further substances, not listed in the annex of the DWD, or to further types of water is not excluded, but is intended to be validated separately for each individual case.
Wasserqualität - Bestimmung der Summe der perfluorierten Substanzen (Summe der PFAS) im Trinkwasser - Methode mittels Flüssigkeitschromatographie / Massenspektrometrie (LC/MS)
Dieses Dokument legt ein Verfahren zur Bestimmung des gelösten Anteils ausgewählter Per- und Polyfluoral
kylsubstanzen (PFAS) mittels Flüssigkeitschromatografie-Tandem-Massenspektrometrie (LC MS/MS) in nicht filtriertem Trinkwasser fest, welches weniger als 0,5g/l Feststoffpartikel (SPM) enthält. Die Anwendbarkeit des Verfahrens auf weitere Wasserarten wie Süßwasser (z.B. Grundwasser, Oberflächenwasser) oder
deltes Abwasser muss für jeden Einzelfall separat validiert werden.
Für jede Zielverbindung werden sowohl eventuell auftretende verzweigte Isomere als auch das jeweilige unver
zweigte Isomer zusammen quantifiziert. Die mit dieser Methode ermittelte Stoffauswahl ist repräsentativ für eine Vielzahl von PFAS. Die in Tabelle1 aufgeführten Analyten sind validiert und können mit dieser Methode bestimmt werden. Die Liste in dieser Tabelle kann je nach Zweck und Schwerpunkt der Methode modifiziert werden. Der untere Anwendungsbereich dieser Methode kann abhängig von der Empfindlichkeit der verwen
deten Geräte und der Matrix der Proben variieren. Für zahlreiche Stoffe, für die diese Norm gilt, kann eine Bestimmungsgrenze (LOQ) von 1ng/l erreicht werden. Die Verwendung einer Direktinjektion mit großem
benvolumen, 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 20PFAS, die in AnhangIII TeilB Punkt3 der EU- TrinkwasserrichtlinieEU2020/2184 zur Überwachung des maximal zulässigen Parameterwerts von 0,10μg/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 la somme des substances perfluorées (somme des PFAS) dans l'eau potable - Méthode utilisant la chromatographie liquide / spectrométrie de masse (LC / MS)
Le présent document spécifie une méthode de détermination de la fraction dissoute de substances per- et polyfluoroalkylées (PFAS) sélectionnées dans de l’eau potable non filtrée contenant moins de 0,5 g/l de matière en suspension (MES) par chromatographie liquide associée à une spectrométrie de masse en tandem (CL-SM/SM). L’applicabilité de la méthode à d’autres types d’eau tels que les eaux douces (par exemple, eau souterraine, eau de surface) ou, par exemple, les eaux usées traitées, doit 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 vaste gamme de PFAS. Les analytes spécifiés dans le Tableau 1 ont été validés et peuvent être déterminés par cette méthode. 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 courte chaîne 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 les laboratoires individuels.
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, 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.
Kakovost vode - Določevanje vsote perfluoriranih snovi (vsota PFAS) v pitni vodi - Metoda s tekočinsko kromatografijo in masno spektrometrijo (LC-MS)
General Information
Standards Content (Sample)
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.
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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.
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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
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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
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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.
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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, 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.
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1 Scope
This document specifies a method for the determination of the dissolved fraction of selected
perfluoroalkyl and polyfluoroalkyl substances (PFAS) in non-filtrated drinking water containing less
than 0,5 g/l solid particulate material (SPM) using liquid chromatography-tandem mass spectrometry
(LC-MS/MS). The applicability of the method to further types of water like fresh waters (e.g. ground
water, surface water) or e.g. treated waste water is 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. The analytes specified in Table 1 have been validated and can
be determined by this method. 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, 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.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 5667-1, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes and
sampling techniques
ISO 5667-3, Water quality — Sampling — Part 3: Preservation and handling of water samples
ISO 5667-5, Water quality — Sampling — Part 5: Guidance on sampling of drinking water from treatment
works and piped distribution systems
ISO 8466-1, Water quality — Calibration and evaluation of analytical methods — Part 1: Linear calibration
function
ISO 21253-1, Water quality — Multi-compound class methods — Part 1: Criteria for the identification of
target compounds by gas and liquid chromatography and mass spectrometry
ISO 21675, Water quality — Determination of perfluoroalkyl and polyfluoroalkyl substances (PFAS) in
water — Method using solid phase extraction and liquid chromatography-tandem mass spectrometry (LC-
MS/MS)
CEN/TS 16800, Guideline for the validation of physico-chemical analytical methods
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3 Terms and definitions
For the purposes of this document, the following terms and definitions apply
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/
3.1
per- and polyfluoroalkyl substances
PFAS
fluorinated substances that contain at least one fully fluorinated methyl or methylene carbon atom
Note 1 to entry: The term is used in the broader sense for substances that contain chlorine and oxygen in a
polyfluoroalkyl structure as well (Reference [1]).
Note 2 to entry There are a few noted exceptions, so that any chemical with at least a perfluorinated methyl group
(-CF3-) or a perfluorinated methylene group (–CF2–)
Note 3 to entry: Within legal regulations (e.g. European Drinking water Directive (Reference [5]) the definition of
PFAS might be different and for example be restricted to substances with a defined chain length.
4 Principle
Part A of this document comprises a method using direct injection LC-MS/MS: An aliquot of the
unfiltrated water sample is diluted with methanol and amended with a solution of isotopically labelled
internal standards. The diluted water sample is injected directly into the analysis system. The
identification and quantitative determination of the substances listed in Table 1 is performed using liquid
chromatography coupled with tandem mass-spectrometry detection (LC-MS/MS).
Part B of this document comprises a method using a solid-phase extraction protocol similar to ISO 21675
before LC-MS/MS measurement: The analytes listed in Table 1 are extracted from the water sample by
solid-phase extraction using a weak anion exchange sorbent. The identification and quantitative
determination of the substances in the extract is performed using liquid chromatography coupled with
tandem mass-spectrometry detection (LC-MS/MS).
The method can be used to determine additional PFAS substances provided that accuracy has been tested
and verified for each case as well as storage conditions of both samples and reference solutions have been
validated.
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Table 1 — Analytes for which a determination was validated in accordance with this method
a b
Analyte IUPAC name Formula Abbreviation CAS-RN
Perfluoro-n- 2,2,3,3,4,4,4-
HF O PFBA 375–22–4
C4 7 2
butanoic acid Heptafluorobutanoic acid
Perfluoro-n- 2,2,3,3,4,4,5,5,5-
C HF O PFPeA 2706–90–3
5 9 2
pentanoic acid Nonafluoropentanoic acid
Perfluoro-n- 2,2,3,3,4,4,5,5,6,6,6-
C6HF11O2 PFHxA 307–24–4
hexanoic acid Undecafluorohexanoic acid
Perfluoro-n- 2,2,3,3,4,4,5,5,6,6,7,7,7-
C HF O PFHpA 375–85–9
7 13 2
heptanoic acid Tridecafluoroheptanoic acid
Perfluoro-n- 2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-
C HF O PFOA 335–67–1
8 15 2
octanoic acid Pentadecafluorooctanoic acid
Perfluoro-n- 2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,9-
C HF O PFNA 375–95–1
9 17 2
nonanoic acid Heptadecafluorononanoic acid
Perfluoro-n- 2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,1
decanoic acid 0,
C HF O PFDA 335–76–2
10 19 2
10,10-
Nonadecafluorodecanoic acid
Perfluoro-n- 2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,1
undecanoic acid 0,
10,11,11,11- C HF O PFUnDA 2058–94–8
11 21 2
Heneicosafluoroundecanoic
acid
Perfluoro-n- 2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,1
dodecanoic acid 0,10,11,11,12,12,12- C HF O PFDoDA 307–55–1
12 23 2
Tricosafluorododecanoic acid
Perfluoro-n- 2,2,3,3,4,4,5,5,6,6,7,7,8,8,
tridecanoic acid 9,9,10,10,11,11,12,12,
C HF O PFTrDA 72629–94–8
13 25 2
13,13,13-Pentacosa-
fluorotridecanoic acid
Perfluoro-n- 1,1,2,2,3,3,4,4,4-
HF O S PFBS 375–73–5
butanesulfonic Nonafluorobutane-1-sulfonic C4 9 3
acid acid
Perfluoro-n- 1,1,2,2,3,3,4,4,5,5,5-
pentanesulfonic Undecafluoropentane-1- C HF O S PFPeS 2706–91–4
5 11 3
acid sulfonic acid
Perfluoro-n- 1,1,2,2,3,3,4,4,5,5,6,6,6-
hexanesulfonic Tridecafluorohexane-1- C HF O S PFHxS 355–46–4
6 13 3
acid sulfonic acid
Perfluoro-n- 1,1,2,2,3,3,4,4,5,5,6,6,7,7,7-
heptanesulfonic Pentadecafluoroheptane-1- C HF O S PFHpS 375–92–8
7 15 3
acid sulfonic acid
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a b
Analyte IUPAC name Formula Abbreviation CAS-RN
Perfluoro-n- 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-
octanesulfonic Heptadecafluorooctane-1- C HF O S PFOS 1763–23–1
8 17 3
acid sulfonic acid
Perfluoro-n- 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,
nonanesulfonic 9,9-Nonaadecafluorononane- C HF O S PFNS 68259–12–1
9 19 3
acid 1-sulfonic acid
Perfluoro-n- 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,
decanesulfonic 9,10,10,10-
C HF O S PFDS 335–77–3
10 21 3
acid Heneicosafluorodecane-1-
sulfonic acid
Perfluoro-n-
1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,
undecanesulfonic
9,9,10,10,11,11,11-
PFUnDS 749786-16-1
C HF O S
11 23 3
acid
Tricosafluoroundecane-1-
sulfonic acid
Perfluoro-n-
1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,
dodecanesulfonic
9,10,10,11,11,12,12,12-
PFDoDS 79780-39-5
C HF O S
12 25 3
acid
Pentacosafluorododecane-1-
sulfonic acid
Perfluoro-n-
1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,
tridecanesulfonic
10,10,11,11,12,12,12-
PFTrDS 791563-89-8
C HF O S
13 27 3
acid
Pentacosafluorodecane-1-
sulfonic acid
4:2 Fluorotelomer 3,3,4,4,5,5,6,6,6-
sulfonic acid Nonafluorohexane-1-sulfonic C H F O S 4:2 FTSA 27619–93–8
6 5 9 3
acid
6:2 Fluorotelomer 3,3,4,4,5,5,6,6,7,7,8,8,8-
sulfonic acid Tridecafluorooctane-1- C H F O S 6:2 FTSA 27619–97–2
8 5 13 3
sulfonic acid
8:2 Fluorotelomer 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10
sulfonic acid ,
C H F O S 8:2 FTSA 39108–34–4
10 5 17 3
10-Heptadecafluorodecane-1-
sulfonic acid
Perfluorooctanesu 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-
lfonamide Heptadecafluoro-1- C H F NO S FOSA 754–91–6
8 2 17 2
octanesulfonamide
N-ethyl 2-
perfluorooctanesu [Ethyl(1,1,2,2,3,3,4,4,5,5,6,6,7,
lfonamidoacetic 7,8,8,8- C H F NO S N-EtFOSAA 2991–50–6
12 8 17 4
acid heptadecafluorooctylsulfonyl)
amino]acetic acid
Hexafluoropropyle 2,3,3,3-Tetrafluoro-2-
ne oxide dimer (1,1,2,2,3,3,3-
C6HF11O3 HFPO-DA 13252–13–6
acid heptafluoropropoxy)propanoi
c acid
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a b
Analyte IUPAC name Formula Abbreviation CAS-RN
4,8-Dioxa-3H- 2,2,3-Trifluoro-3-[1,1, 2,2,3,3-
perfluorononanoic hexafluoro-3-(tri-
C H F O DONA 919005–14–4
7 2 12 4
acid fluoromethoxy)propoxy]
propanoic acid
Perfluoro-3- 2,2,3,3-Tetrafluoro-3-
PFMPA
methoxypropanoic (trifluoromethoxy)pro- C HF O 377–73–1
4 7 3
(PF4OPeA)
acid panoic acid
9-Chlorohexa- 2-(6-Chloro-1,1,2,2,
decafluoro-3- 3,3,4,4,5,5,6,6-dodeca-
C HClF O S 9Cl-PF3ONS 73606–19–6
8 16 4
oxanonane-1- fluorohexoxy)-1,1,2,2-
sulfonic acid tetrafluoroethanesulfonic acid
a
IUPAC: International Union of Pure and Applied Chemistry
b
CAS-RN: Chemical Abstract Services Registry Number
5 Interferences
5.1 Sampling
Long chain PFAS (e.g. perfluoralkyl carboxylic acids with x ≥ 7 and perfluoralkane sulfonic acids with
x ≥ 6, x being the number of perfluorinated C-atoms in the chain) may distribute to the water/vessel and
water/air interfaces. These interference depend on the geometry and material of the sample vessels and
can be minimized by minimizing the sample surface, e.g. by using narrow vessels with a small surface
area.
5.2 Background contamination
Efforts should be taken to minimize background levels in procedural blank materials such that the
procedural blank, including the instrumental blank, is at least one third below the limit of
quantification (9.4).
Low molecular residuals in fluoropolymer-containing materials such as polyvinylidene fluoride or
polyvinylidene difluoride (PVDF), polytetrafluoroethylene (PTFE) etc., which are often used in LC-
equipment, may cause blank values, e.g. in the case of PFOA. In order to avoid blank values, objects made
of glass, steel, polyether ether ketone (PEEK), polystyrene (PS), polypropylene (PP) or polyethylene (PE)
shall preferably be used for sampling, extraction and analysis. Sampling vessels (7.2) and sample
vials (7.12) shall be checked for possible background contamination before use.
Typical contamination sources in the LC-system include vacuum degassers, frits and hoses as well as
pump head seals. In the case of such interferences, degassing of the eluents, for example, can be carried
out using helium instead of vacuum degassers. Fluoropolymer frits and hoses shall be replaced by frits
and hoses made of stainless steel or PEEK. If available, pump head seals made of PE shall be used.
Background contamination, originating from the instrument and/or mobile phases can be controlled by
using a delay column (7.14.3).
5.3 Interferences encountered during liquid chromatography and mass spectrometry
Peak tailing, peak fronting and/or broadened peaks are indicative of interferences in chromatography.
Particles in the measurement solution, e.g. fine fractions of the SPE material in case of analytical
protocol B of this document or solid phase matter in the sample in case of analytical protocol A of this
document, can block the inlet sieves or frits, respectively, of the LC column and result in interferences
10
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oSIST prEN 17892:2022
prEN 17892:2022 (E)
due to the increase in pressure; in such cases the measurement solutions shall be centrifuged (7.11) prior
to the analysis.
Sample matrix components can affect the ionization of the target substances. This may result in
suppression or enhancement of the ionization. Such matrix interferences can be detected and corrected
by using authentic isotopically labelled internal standards or by the standard addition method.
Substances with similar retention times that can produce ions with similar mass to charge ratios (m/z)
to those produced by the target analytes may interfere with the determination. These interferences may
lead to incompletely resolved signals and/or additional signals in the mass chromatograms of target
substances. Depending on their levels in the sample, such substances may affect the accuracy and
precision of the results. As long as the peak of interest can be separately integrated from interferences, it
can be used.
6 Reagents
As far as available, analytical grade or residue-analytical grade reagents shall be used. The content of
impurities contributing to blank values or causing interfering signals shall be negligible. This shall be
checked in regular intervals (9.4).
Reagents, solvents and water used as eluents shall be suitable for LC and mass spectrometry.
6.1 Water, H O.
2
Purified laboratory water can be used. The quality of water is checked by the same procedure given in
9.4.
6.2 Methanol, CH OH.
3
6.3 Acetonitrile, CH CN.
3
6.4 Acetic acid, w(CH COOH) = 99,9 % mass fraction (999 g/kg).
3
6.5 Formic acid, w(HCOOH), minimum 98 %. (SPE alternative only)
6.6 Acetone, C H O (SPE alternative only).
3 6
6.7 Ammonia solution, w(NH ), minimum 25 % (SPE alternative only).
3
6.8 Ammonium acetate, CH COONH .
3 4
6.9 Solid phase material, mixed-mode material (weak anion exchanger on a polymer base with
reversed-phase moiety) (SPE alternative only).
6.10 Acetate buffer, for solid phase extraction only, 0,025 mol/l, pH 4.
Mix, for example, 0,
...
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