CEN/TS 15968:2010
(Main)Determination of extractable perfluorooctanesulphonate (PFOS) in coated and impregnated solid articles, liquids and fire fighting foams - Method for sampling, extraction and analysis by LC-qMS or LC-tandem/MS
Determination of extractable perfluorooctanesulphonate (PFOS) in coated and impregnated solid articles, liquids and fire fighting foams - Method for sampling, extraction and analysis by LC-qMS or LC-tandem/MS
This Technical Specification describes the determination of perfluorooctanesulfonate (PFOS) in concentrated extracts from coated and impregnated solid articles, liquids and fire extinguishing foams using high performance liquid chromatography-tandem mass spectrometry (LC-tandemMS) or quadrupole mass spectrometry (LC-qMS).
The method is applicable for a concentration range for PFOS in the extract solution of 0,5 µg/l to 50 µg/l.
WARNING - Persons using this Technical Specification should be familiar with normal laboratory practice. This Technical Specification 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 and to ensure compliance with any national regulatory conditions.
IMPORTANT - It is absolutely essential that tests conducted in accordance with this Technical Specification be carried out by suitably qualified staff.
Bestimmung von extrahierbarem Perfluoroctansulfonat (PFOS) in beschichteten und imprägnierten Feststoffartikeln, Flüssigkeiten und Feuerlöschschäumen - Verfahren zur Probenahme, Extraktion und Analyse mittels LC-MS oder LC-MS
Die vorliegende Technische Spezifikation beschreibt die Bestimmung von Perfluoroctansulfo¬nat (PFOS) in konzentrierten Extrakten aus beschichteten und imprägnierten Feststoffartikeln, Flüssigkeiten und Feuerlöschschäumen unter Anwendung von Hochleistungs-Flüssigkeitschromatographie/Tandem-Massen-spektrometrie (LC tandem/MS) oder Quadrupol-Massenspektrometrie (LC qMS).
Das Verfahren ist anwendbar auf Konzentrationen von PFOS in der Extraktionslösung im Bereich zwischen 0,5 µg/l und 50 µg/l.
WARNUNG - Die Anwender dieser Technischen Spezifikation sollten mit der üblichen Laborpraxis vertraut sein. Diese Technische Spezifikation beansprucht nicht, sämtliche mit deren Anwendung verbundenen Sicherheitsprobleme, soweit solche gegeben sind, abzudecken. Es liegt in der Verantwortung des Anwenders, geeignete Maßnahmen für Gesundheits- und Arbeitsschutz einzuleiten und deren Übereinstimmung mit sämtlichen nationalen gesetzlichen Vorschriften sicherzustellen.
WICHTIG - Es ist unbedingt notwendig, dass Prüfungen nach dieser Technischen Spezifikation von entspre¬chend qualifizierten Personen durchgeführt werden.
Détermination du sulfonate de perfluorooctane (SPFO) extractible dans des articles solides couchés et imprégnés, des liquides et des mousses anti-incendie - Méthode d'échantillonnage, d'extraction et d'analyse par LC-MS ou LC-MS/MS
La présente Spécification technique européenne décrit la détermination du sulfonate de perfluorooctane (SPFO) dans un extrait concentré provenant d’articles solides couchés et imprégnés, de liquides et de mousses anti-incendie au moyen d’une chromatographie en phase liquide haute performance couplée à la spectrométrie de masse en tandem (LC-MS/MS) ou à une spectrométrie de masse quadripôle (LC-MS).
La méthode est applicable pour une plage de concentration de SPFO dans la solution d’extrait allant de 0,5 ng/ml à 50 ng/ml.
AVERTISSEMENT — Il convient que les utilisateurs de la présente Spécification technique soient familiarisés avec les pratiques courantes de laboratoire. La présente Spécification technique n’a pas pour objet de traiter tous les problèmes de sécurité qui sont, le cas échéant, liés à son utilisation. Il incombe à l’utilisateur d’établir des pratiques appropriées en matière d’hygiène et de sécurité et de s'assurer de la conformité à la réglementation nationale en vigueur.
IMPORTANT — Il est absolument essentiel que les essais menés conformément à la présente Spécification technique soient effectués par un personnel qualifié.
Določevanje izločljivega perfluorooktansulfonata (PFOS) v prevlečenih in impregniranih trdnih predmetih, tekočinah in protipožarnih penah - Metode vzorčenja, ekstrakcije in analize s pomočjo LC-MS ali LC-MS/MS
Ta tehnična specifikacija opisuje določevanje perfluorooktansulfonata (PFOS) v koncentriranih ekstraktih iz prevlečenih in impregniranih trdnih predmetov, tekočin in protipožarnih pen z uporabo tekočinske kromatografije visoke ločljivosti LC-MS ali LC-MS/MS. Metoda se uporablja za razpon koncentracije PFOS v raztopini ekstrakta od 0,5 μg/l do 50 μg/l.
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-december-2010
'RORþHYDQMHL]ORþOMLYHJDSHUIOXRURRNWDQVXOIRQDWD 3)26 YSUHYOHþHQLKLQ
LPSUHJQLUDQLKWUGQLKSUHGPHWLKWHNRþLQDKLQSURWLSRåDUQLKSHQDK0HWRGH
Y]RUþHQMDHNVWUDNFLMHLQDQDOL]HVSRPRþMR/&06DOL/&0606
Determination of extractable perfluorooctanesulphonate (PFOS) in coated and
impregnated solid articles, liquids and fire fighting foams - Method for sampling,
extraction and analysis by LC-qMS or LC-tandem/MS
%HVWLPPXQJYRQH[WUDKLHUEDUHP3HUIOXRURFWDQVXOIRQDW 3)26 LQEHVFKLFKWHWHQXQG
LPSUlJQLHUWHQ)HVWVWRIIDUWLNHOQ)OVVLJNHLWHQXQG)HXHUO|VFKVFKlXPHQ9HUIDKUHQ]XU
3UREHQDKPH([WUDNWLRQXQG$QDO\VH
PLWWHOV/&06RGHU/&0606
Détermination du sulfonate de perfluorooctane (SPFO) extractible dans des articles
solides couchés et imprégnés, des liquides et des mousses anti-incendie - Méthode
d'échantillonnage, d'extraction et d'analyse par LC-MS ou LC-MS/MS
Ta slovenski standard je istoveten z: CEN/TS 15968:2010
ICS:
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
71.080.20 Halogenirani ogljikovodiki Halogenated hydrocarbons
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
TECHNICAL SPECIFICATION
CEN/TS 15968
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
August 2010
ICS 71.040.50; 71.080.20
English Version
Determination of extractable perfluorooctanesulphonate (PFOS)
in coated and impregnated solid articles, liquids and fire fighting
foams - Method for sampling, extraction and analysis by LC-
qMS or LC-tandem/MS
Détermination du sulfonate de perfluorooctane (SPFO) Bestimmung von extrahierbarem Perfluoroctansulfonat
extractible dans des articles solides couchés et imprégnés,
(PFOS) in beschichteten und imprägnierten
des liquides et des mousses anti-incendie - Méthode Feststoffartikeln, Flüssigkeiten und Feuerlöschschäumen -
d'échantillonnage, d'extraction et d'analyse par LC-MS ou Verfahren zur Probenahme, Extraktion und Analyse mittels
LC-MS/MS LC-MS oder LC-MS
This Technical Specification (CEN/TS) was approved by CEN on 25 October 2009 for provisional application.
The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the CEN/TS can be converted into a European Standard.
CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available
promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)
until the final decision about the possible conversion of the CEN/TS into an EN is reached.
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, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2010 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 15968:2010: E
worldwide for CEN national Members.
Contents Page
Foreword .4
Introduction .5
1 Scope .6
2 Normative references .6
3 Terms and definitions .6
4 Symbols and abbreviations .7
5 Principle .7
6 Apparatus and Reagents .8
6.1 General .8
6.2 Equipment .9
6.3 Reagents for extraction .9
6.4 Reagents for LC and MS .9
7 Sampling . 10
7.1 General . 10
7.2 Conditioning samples . 10
7.3 Sampling solids . 10
7.4 Sampling products that have separate distinct parts . 10
7.5 Sampling liquids . 10
8 Sample pre-treatment . 11
9 Extraction . 11
9.1 Extraction method for textile, fabrics, leather and paper . 11
9.2 Clean-up method for textile, fabrics, leather and paper . 11
9.3 Dilution method for aqueous fire extinguishing foams . 11
9.4 Extraction method for other liquids . 12
10 Interference with LC-tandemMS . 12
11 Analysis . 12
11.1 LC-tandemMS operating conditions . 12
11.2 Blank determination . 12
11.3 Quality Control samples . 12
11.4 Identification . 12
12 System suitability test . 14
12.1 Calibration . 14
12.2 Recovery . 15
12.3 Blank measurement . 15
13 Calculation . 15
13.1 Calibration curve for quantification . 15
13.2 Calculation of results after calibration with reference compounds . 16
13.3 Calculation of results to PFOS equivalents . 17
14 Expression of results . 17
15 Test report . 18
Annex A (informative) LC-QMS and LC-TOFMS . 20
Annex B (informative) . 25
Annex C (informative) Confirmation of compound identity by MS methods . 26
Bibliography . 31
Foreword
This document (CEN/TS 15968:2010) has been prepared by Technical Committee CEN/TC 382 “Project
Committee - PFOS”, the secretariat of which is held by NEN.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
This document has been prepared under a mandate given to CEN by the European Commission and the
European Free Trade Association and supports essential requirements of REACH (1907/2006), annex XVII,
designation 53 [1].
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to announce this Technical Specification: 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, Romania, Slovakia, Slovenia,
Spain, Sweden, Switzerland and the United Kingdom.
Introduction
For implementation of REACH (1907/2006), annex XVII, designation 53 [1] the European Commission asked
CEN to develop an European Technical Specification with test methods for measuring levels of PFOS
containing compounds in preparations, semi-finished products and articles including textile and coated
materials.
REACH (1907/2006), annex XVII, designation 53 [1] states that the substances that are under the Directive
are perfluorooctanesulfonates (PFOS), that means substances with the formula C F SO X (where X=OH,
8 17 2
Metal salt (O-M+), halide, amide and other derivatives including polymers).
1 Scope
This Technical Specification describes the determination of perfluorooctanesulfonate (PFOS) in concentrated
extracts from coated and impregnated solid articles, liquids and fire extinguishing foams using high
performance liquid chromatography-tandem mass spectrometry (LC-tandemMS) or quadrupole mass
spectrometry (LC-qMS).
The method is applicable for a concentration range for PFOS in the extract solution of 0,5 µg/l to 50 µg/l.
WARNING ― Persons using this Technical Specification should be familiar with normal laboratory
practice. This Technical Specification 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 and to ensure compliance with any national regulatory conditions.
IMPORTANT ― It is absolutely essential that tests conducted in accordance with this Technical
Specification be carried out by suitably qualified staff.
2 Normative references
The following referenced documents are indispensable for the application 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 20187, Paper, board and pulps — Standard atmosphere for conditioning and testing and procedure for
monitoring the atmosphere and conditioning of samples (ISO 187:1990)
EN ISO 2419, Leather — Physical and mechanical tests — Sample preparation and conditioning
(ISO 2419:2006)
EN ISO 3696:1995, Water for analytical laboratory use — Specification and test methods (ISO 3696:1987)
EN ISO 8130-9, Coating powders — Part 9: Sampling (ISO 8130-9:1992)
EN ISO 15194, In vitro diagnostic medical devices — Measurement of quantities in samples of biological
origin ― Requirements for certified reference materials and the content of supporting documentation
(ISO 15194:2009)
ISO 8466-1, Water quality — Calibration and evaluation of analytical methods and estimation of performance
characteristics — Part 1: Statistical evaluation of the linear calibration function
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply
3.1
analyte
substance or chemical constituent that is subjected to measurement
3.2
blank matrix
matrix which is la
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.