EN ISO 20596-2:2022
(Main)Water quality - Determination of cyclic volatile methylsiloxanes in water - Part 2: Method using liquid-liquid extraction with gas chromatography-mass spectrometry (GC-MS) (ISO 20596-2:2021)
Water quality - Determination of cyclic volatile methylsiloxanes in water - Part 2: Method using liquid-liquid extraction with gas chromatography-mass spectrometry (GC-MS) (ISO 20596-2:2021)
This document specifies a method for the determination of certain cyclic volatile methylsiloxanes (cVMS) in environmental water samples with low density polyethylene (LDPE) as a preservative and subsequent liquid-liquid extraction with hexane containing 13C-labeled cVMS as internal standards. The extract is then analysed by gas chromatography-mass spectrometry (GC-MS).
NOTE Using the 13C-labeled, chemically identical substances as internal standards with the same properties as the corresponding analytes, minimizes possible substance-specific discrimination in calibrations. Since these substances are least soluble in water, they are introduced via the extraction solvent hexane into the system.
Wasserbeschaffenheit - Bestimmung von cyclischen flüchtigen Methylsiloxanen in Wasser - Teil 2: Verfahren mittels Flüssig-Flüssig-Extraktion und Gaschromatographie-Massenspektrometrie (GC-MS) (ISO 20596‑2:2021)
Dieses Dokument legt ein Verfahren zur Bestimmung der wichtigsten cyclischen flüchtigen Methylsiloxane (cVMS, en: cyclic volatile methylsiloxanes) in Wasserproben fest. Polyethylen niedriger Dichte (LDPE, en: low density polyethylene) wird in dem beschriebenen Verfahren zur Vermeidung von Verlusten der cyclischen flüchtigen Methylsiloxane bei Probennahme und -verarbeitung verwendet. Die Proben werden mit Hexan extrahiert, das die einzelnen 13C-markierten cVMS enthält, die als interne Quantifizierungsstandards verwendet werden. Die Extrakte werden anschließend mittels Gaschromatographie-Massenspektrometrie (GC-MS) analysiert.
ANMERKUNG Durch die Verwendung von 13C-markierten – aber chemisch identischen – Substanzen als interne Standardmaterialien, die nahezu die gleichen physikochemischen Eigenschaften wie die entsprechenden Analyten haben, werden substanzspezifische Effekte bei der Kalibrierung im Wesentlichen vermieden. Da sie kaum wasserlöslich sind, werden sie über das Extraktionsmittel Hexan in das Analysensystem eingeführt.
Dieses Dokument ist anwendbar für die Bestimmung von Spurengehalten der im Folgenden aufgeführten cVMS in Oberflächenwässern (Flüsse, Ströme) sowie in Abwässern (Zu- und Ablauf von Klärwerken).
Tabelle 1 — Analyten, die mit dem hier beschriebenen Verfahren bestimmt werden können
Analyt Bruttoformel Übliche Abkürzung CASa-RN
Octamethylcyclotetrasiloxan C8H24O4Si4 D4 556-67-2
Decamethylcyclopentasiloxan C10H30O5Si5 D5 541-02-6
Dodecamethylcyclohexasiloxan C12H36O6Si6 D6 540-97-6
a CAS-RN Chemical Abstracts Services Registrierungsnummer
Mit diesem Verfahren können cVMS-Gehalte zwischen 0,1 µg/l bis 250 µg/l bestimmt werden. In besonders kontrollierten Laborumgebungen, in denen mögliche Kontaminationen minimiert werden können, kann die untere Bestimmungsgrenze, um bis zu einem Faktor 10 reduziert werden.
Qualité de l'eau - Détermination de méthylsiloxanes cycliques volatiles dans l'eau - Partie 2: Méthode par extraction liquide-liquide avec chromatographie en phase gazeuse-spectrométrie de masse (CG-SM) (ISO 20596-2:2021)
Le présent document spécifie une méthode de détermination de certains méthylsiloxanes cycliques volatils (cVMS) dans des échantillons d’eau environnementale avec du polyéthylène basse densité (LDPE) comme conservateur puis extraction liquide-liquide avec de l’hexane contenant des cVMS marqués au 13C comme étalons internes. L’extrait est ensuite analysé par chromatographie en phase gazeuse couplée à la spectrométrie de masse (CG-SM).
NOTE Le fait d’utiliser des substances chimiquement identiques marquées au 13C comme étalons internes qui ont les mêmes propriétés que les analytes correspondants, réduit au minimum les possibles discriminations substance spécifique lors des étalonnages. Étant donné que ces substances sont les moins solubles dans l’eau, elles sont introduites dans le système par le solvant d’extraction (hexane).
Kakovost vode - Določevanje hlapnih cikličnih metilsiloksanov v vodi - 2. del: Metoda s tekočinsko-tekočinsko ekstrakcijo in plinsko kromatografijo z masno spektrometrijo (GC-MS) (ISO 20596-2:2021)
Ta dokument določa metodo za določanje nekaterih cikličnih hlapnih metilsiloksanov (cVMS) v okoljskih vzorcih vode s polietilenom nizke gostote (LDPE) kot konzervansom in naknadno ekstrakcijo tekočina-tekočina s heksanom, ki vsebuje 13C-označene cVMS kot notranje standarde. Ekstrakt se nato analizira s plinsko kromatografijo z masno spektrometrijo (GC-MS).
OPOMBA: Uporaba kemično enakih snovi, označenih s 13C, kot notranjih standardov z enakimi lastnostmi kot ustrezni analiti, zmanjšuje morebitno razlikovanje na podlagi različnih lastnosti snovi pri kalibracijah. Ker so te snovi najmanj topne v vodi, jih v sistem vnesemo prek ekstrakcijskega topila heksana.
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-april-2023
Kakovost vode - Določevanje hlapnih cikličnih metilsiloksanov v vodi - 2. del:
Metoda s tekočinsko-tekočinsko ekstrakcijo in plinsko kromatografijo z masno
spektrometrijo (GC-MS) (ISO 20596-2:2021)
Water quality - Determination of cyclic volatile methylsiloxanes in water - Part 2: Method
using liquid-liquid extraction with gas chromatography-mass spectrometry (GC-MS) (ISO
20596-2:2021)
Wasserbeschaffenheit - Bestimmung von cyclischen flüchtigen Methylsiloxanen in
Wasser - Teil 2: Verfahren mittels Flüssig-Flüssig-Extraktion und Gaschromatographie
mit Massenspektrometrie (GC-MS) (ISO 20596-2:2021)
Qualité de l'eau - Détermination de méthylsiloxanes cycliques volatiles dans l'eau -
Partie 2: Méthode par extraction liquide-liquide avec chromatographie en phase
gazeuse-spectrométrie de masse (CG-SM) (ISO 20596-2:2021)
Ta slovenski standard je istoveten z: EN ISO 20596-2:2022
ICS:
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 ISO 20596-2
EUROPEAN STANDARD
NORME EUROPÉENNE
September 2022
EUROPÄISCHE NORM
ICS 13.060.50
English Version
Water quality - Determination of cyclic volatile
methylsiloxanes in water - Part 2: Method using liquid-
liquid extraction with gas chromatography-mass
spectrometry (GC-MS) (ISO 20596-2:2021)
Qualité de l'eau - Détermination de méthylsiloxanes Wasserbeschaffenheit - Bestimmung von cyclischen
cycliques volatiles dans l'eau - Partie 2: Méthode par flüchtigen Methylsiloxanen in Wasser - Teil 2:
extraction liquide-liquide avec chromatographie en Verfahren mittels Flüssig-Flüssig-Extraktion und
phase gazeuse-spectrométrie de masse (CG-SM) (ISO Gaschromatographie-Massenspektrometrie (GC-MS)
20596-2:2021) (ISO 20596-2:2021)
This European Standard was approved by CEN on 19 September 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.
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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.
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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 ISO 20596-2:2022 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
European foreword
The text of ISO 20596-2:2021 has been prepared by Technical Committee ISO/TC 147 "Water quality”
of the International Organization for Standardization (ISO) and has been taken over as EN ISO 20596-
2:2022 by 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 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 organizations 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.
Endorsement notice
The text of ISO 20596-2:2021 has been approved by CEN as EN ISO 20596-2:2022 without any
modification.
INTERNATIONAL ISO
STANDARD 20596-2
First edition
2021-01
Water quality — Determination of
cyclic volatile methylsiloxanes in
water —
Part 2:
Method using liquid-liquid extraction
with gas chromatography-mass
spectrometry (GC-MS)
Qualité de l'eau — Détermination de méthylsiloxanes cycliques
volatiles dans l'eau —
Partie 2: Méthode par extraction liquide-liquide avec
chromatographie en phase gazeuse-spectrométrie de masse (CG-SM)
Reference number
ISO 20596-2:2021(E)
©
ISO 2021
ISO 20596-2:2021(E)
© ISO 2021
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
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ISO 20596-2:2021(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Principle . 2
4.1 Principle of preservation and extraction . 2
5 Interferences . 2
5.1 Interferences with sampling and processing . 2
5.2 Interferences with GC-MS . 2
5.3 Interferences determination . 3
6 Reagents . 3
7 Apparatus . 5
8 Method detection limits . 6
9 Quality control . 6
10 Sampling and storage . 6
10.1 Sampling preparation . 6
10.2 Sample collection . 6
11 Extraction and analysis . 7
11.1 Extraction . 7
11.2 GC conditions and operation . 7
12 Calibration . 7
12.1 General requirements . 7
12.2 Calibration calculations . 8
12.3 Concentration calculations . 8
12.4 Calculation of results . 9
12.5 Treatment of results lying outside the calibration range . 9
13 Expression of results .10
14 Test report .10
Annex A (informative) GC-MS conditions .11
Annex B (informative) Method detection limit and limit of quantification .13
Annex C (informative) Example quality control samples .14
Annex D (informative) Performance data .15
Bibliography .16
ISO 20596-2:2021(E)
Foreword
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