prEN ISO 13646
(Main)Water quality - Determination of selected estrogens in whole water samples - Method using solid phase extraction (SPE) followed by liquid chromatography (LC) or gas chromatography (GC) coupled to mass spectrometry (MS) detection (ISO/DIS 13646:2023)
Water quality - Determination of selected estrogens in whole water samples - Method using solid phase extraction (SPE) followed by liquid chromatography (LC) or gas chromatography (GC) coupled to mass spectrometry (MS) detection (ISO/DIS 13646:2023)
This document specifies a method for the determination of 5 oestrogens, in whole water samples listed in Table 1. The method uses solid-phase extraction (SPE-disks and/or cartridges) followed by liquid or gas chromatography-mass spectrometry (tandem mass spectrometry and/or High resolution mass spectrometry). It is applicable to the analysis of selected estrogens in surface water containing suspended particulate matter (SPM) up to 50 mg/l , DOC content up to 7 mg/l (whole water samples), drinking water and groundwater.
Wasserbeschaffenheit - Bestimmung ausgewählter Estrogene in Gesamtwasserproben - Verfahren mittels Festphasenextraktion (SPE) und anschließender Flüssigkeitschromatographie (LC) oder Gaschromatographie (GC) gekoppelt mit massenspektrometrischer Detektion (MS) (ISO/DIS 13646:2024)
Dieses Dokument legt Verfahren für die Bestimmung von fünf ausgewählten Estrogenen in den in Tabelle 1 aufgeführten Vollwasserproben fest. Die Verfahren basieren auf der Festphasenextraktion (SPE-Disk und/oder Kartusche) und anschließendem Nachweis mittels Flüssigkeits- oder Gaschromatographie mit Massenspektrometrie-Kopplung (Tandem-Massenspektrometrie und/oder Hochauflösungsmassenspektrometrie). Je nach gewählter Probenvorbereitung ist er für die Analyse ausgewählter Estrogene in Trinkwasser, Grundwasser und Oberflächenwasser mit Schwebstoffen (SPM) bis zu 500 mg/l, DOC-Gehalt bis zu 14 mg/l (Gesamtwasserproben) geeignet.
Der untere Anwendungsbereich, der als nachgewiesene Bestimmungsgrenze definiert ist, kann je nach Verfahren, Empfindlichkeit der verwendeten Geräte und Matrix der Probe variieren. Der Bereich liegt bei 0,006 ng/l bis 1 ng/l für EE2 und 0,038 ng/l bis 1 ng/l für die anderen Estrogene in Trinkwasser, Grundwasser und Oberflächenwasser. Die Obergrenze des Arbeitsbereichs liegt bei etwa 10 ng/l.
Für Anwendungen, die auf die Messung sehr niedriger Konzentrationen abzielen (zwischen der niedrigsten LOQ und 0,1 ng/l), ist jeder einzelne Schritt des Verfahrens entscheidend und erfordert die Festlegung einiger zusätzlicher Anforderungen.
Das Verfahren kann zur Bestimmung weiterer Estrogene oder Hormone in anderen Wasserarten, z. B. in behandeltem Abwasser, verwendet werden, wenn die Genauigkeit in jedem Fall geprüft und verifiziert wurde und die Lagerungsbedingungen sowohl der Proben als auch der Referenzlösungen validiert wurden.
WARNUNG — Anwender dieses Dokuments sollten mit der üblichen Laborpraxis vertraut sein. Dieses Dokument gibt nicht vor, alle unter Umständen mit der Anwendung des Verfahrens verbundenen Sicherheitsaspekte anzusprechen. Es liegt in der Verantwortung des Arbeitgebers, angemessene Sicherheits- und Schutzmaßnahmen zu treffen.
WICHTIG — Es ist erforderlich, bei den Untersuchungen nach diesem Dokument Fachleute oder Facheinrichtungen einzuschalten
Qualité de l’eau - Dosage d'oestrogènes sélectionnés dans des échantillons d’eau totale - Méthode par extraction en phase solide (SPE) suivie d’une détection par chromatographie en phase liquide (CL) ou en phase gazeuse (CG) couplée à la spectrométrie de masse (SM) (ISO/DIS 13646:2023)
Kakovost vode - Določanje izbranih estrogenov v celotnem vzorcu vode - Metoda tekočinske kromatografije (LC) ali plinske kromatografije (GC) z masno selektivnim detektorjem po ekstrakciji na trdni fazi (SPE) (ISO/DIS 13646:2023)
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-februar-2024
Kakovost vode - Določanje izbranih estrogenov v celotnem vzorcu vode - Metoda
tekočinske kromatografije (LC) ali plinske kromatografije (GC) z masno
selektivnim detektorjem po ekstrakciji na trdni fazi (SPE) (ISO/DIS 13646:2023)
Water quality - Determination of selected estrogens in whole water samples - Method
using solid phase extraction (SPE) followed by liquid chromatography (LC) or gas
chromatography (GC) coupled to mass spectrometry (MS) detection (ISO/DIS
13646:2023)
Wasserbeschaffenheit - Bestimmung ausgewählter Estrogene in Gesamtwasserproben -
Verfahren mittels Festphasenextraktion (SPE) und anschließender
Flüssigkeitschromatographie (LC) oder Gaschromatographie (GC) gekoppelt mit
massenspektrometrischer Detektion (MS) (ISO/DIS 13646:2024)
Qualité des eaux - Dosage destrogènes sélectionnés dans des échantillons d'eau totale -
Méthode par extraction en phase solide (SPE), avec analyse par couplage
chromatographie-spectrométrie de masse (SM) (ISO/DIS 13646:2023)
Ta slovenski standard je istoveten z: prEN ISO 13646
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.
DRAFT INTERNATIONAL STANDARD
ISO/DIS 13646
ISO/TC 147/SC 2 Secretariat: DIN
Voting begins on: Voting terminates on:
2024-01-01 2024-03-25
Water quality — Determination of selected estrogens
in whole water samples — Method using solid phase
extraction (SPE) followed by liquid chromatography (LC)
or gas chromatography (GC) coupled to mass spectrometry
(MS) detection
ICS: 13.060.50
This document is circulated as received from the committee secretariat.
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENT AND APPROVAL. IT IS
ISO/CEN PARALLEL PROCESSING
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 13646:2024(E)
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. © ISO 2024
ISO/DIS 13646:2024(E)
DRAFT INTERNATIONAL STANDARD
ISO/DIS 13646
ISO/TC 147/SC 2 Secretariat: DIN
Voting begins on: Voting terminates on:
Water quality — Determination of selected estrogens
in whole water samples — Method using solid phase
extraction (SPE) followed by liquid chromatography (LC)
or gas chromatography (GC) coupled to mass spectrometry
(MS) detection
ICS: 13.060.50
This document is circulated as received from the committee secretariat.
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENT AND APPROVAL. IT IS
© ISO 2024
ISO/CEN PARALLEL PROCESSING
THEREFORE SUBJECT TO CHANGE AND MAY
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
NOT BE REFERRED TO AS AN INTERNATIONAL
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on STANDARD UNTIL PUBLISHED AS SUCH.
the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below
IN ADDITION TO THEIR EVALUATION AS
or ISO’s member body in the country of the requester. BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
ISO copyright office
USER PURPOSES, DRAFT INTERNATIONAL
CP 401 • Ch. de Blandonnet 8
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
CH-1214 Vernier, Geneva
POTENTIAL TO BECOME STANDARDS TO
Phone: +41 22 749 01 11
WHICH REFERENCE MAY BE MADE IN
Reference number
Email: copyright@iso.org
NATIONAL REGULATIONS.
Website: www.iso.org ISO/DIS 13646:2023(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
Published in Switzerland
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
ii
PROVIDE SUPPORTING DOCUMENTATION. © ISO 2023
ISO/DIS 13646:2023(E)
Contents Page
Foreword .v
Introduction . vi
1 Scope . 1
2 Normative references . 2
3 Terms and definitions . 3
4 Principle . 5
5 Interferences . 5
5.1 General . 5
5.2 Interferences with sampling, extraction and concentration . . 5
5.3 Interferences during high performance liquid chromatography and mass
spectrometry . 6
5.4 Interferences during gas phase chromatography and mass spectrometry . 7
5.5 Interferences coming from internal standards . 7
6 Reagents . 8
7 Apparatus .14
8 Sampling .16
9 Procedure .16
9.1 General . 16
9.2 Sample preparation and extraction . 18
9.2.1 General . 18
9.2.2 Sample preparation . 18
9.2.3 SPE cartridge extraction . 19
9.2.4 SPE disk Extraction .20
9.3 Sample Clean-up (purification) . 21
9.3.1 General . 21
9.3.2 Principles . 21
9.3.3 Procedures . 21
9.4 Reconcentration . 21
9.5 Liquid chromatography coupled to mass spectrometry .22
9.5.1 High performance liquid chromatography (LC) .22
9.5.2 Detection . 22
9.5.3 Derivatization .23
9.6 Gas chromatography coupled to mass spectrometry . 24
9.6.1 Derivatization . 24
9.6.2 Gas chromatography (GC) . 25
9.6.3 Detection . 25
10 Calibration .26
10.1 General . 26
10.2 Calibration by isotope dilution . 27
10.3 Calibration check .28
11 QA/QC .28
11.1 Identification of the substances .28
11.2 Blanks .28
12 Limit of quantification (LOQ) .28
13 Calculation of recovery .29
13.1 General .29
13.2 Calculation of analyte recovery using samples .29
13.3 Recovery rates from internal standards .29
iii
ISO/DIS 13646:2023(E)
14 Calculation of the concentration in the sample .30
15 Expression of results .31
16 Test reports .31
17 Performance Data .31
Annex A (in
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.