Water quality - Determination of short-chain polychlorinated alkanes (SCCPs) in sediment, sewage sludge and suspended (particulate) matter - Method using gas chromatography-mass spectrometry (GC-MS) and electron capture negative ionization (ECNI) (ISO 18635:2016)

ISO 18635:2016 specifies a method for the quantitative determination of the sum of short-chain polychlorinated n-alkanes also known as short-chain polychlorinated paraffins (SCCPs) in the carbon bond range, n-C10 to n-C13, inclusive in mixtures with chlorine mass fractions ("contents") between 50 % and 67 %, including approximately 6 000 of approximately 8 000 congeners.
This method is applicable to the determination of the sum of SCCPs in sediment and suspended (particulate) matter, sewage sludge, and soil using gas chromatography-mass spectrometry with electron capture negative ionization (GC-ECNI-MS).
Depending on matrix and the detection capabilities of the GC-ECNI-MS, the method can be applied to samples containing, e.g. 0,03 µg/g to 3 µg/g sum of SCCPs.

Wasserbeschaffenheit - Bestimmung kurzkettiger polychlorierter Alkane (SCCP) in Sediment, Klärschlamm und Schwebstoff - Gaschromatographisch-massenspektrometrisches Verfahren (GC-MS) unter Anwendung negativer chemischer Ionisation und Elektroneneinfang (ECNI) (ISO 18635:2016)

Diese Internationale Norm legt ein Verfahren zur quantitativen Bestimmung der Summe von kurzkettigen polychlorierten n-Alkanen fest. Diese werden auch als kurzkettige polychlorierte Paraffine (SCCP, en: short-chain polychlorinated paraffins) bezeichnet und haben Kohlenstoffkettenlängen von n-C10 bis einschließlich n-C13 in Gemischen mit Chlor-Massenanteilen („Gehalten“) zwischen 50 % und 67 %, die ungefähr 6 000 der etwa 8 000 Kongenere umfassen.
Dieses Verfahren ist anwendbar auf die Bestimmung der Summe von SCCP in Sediment, Schwebstoff, Klärschlamm und Boden mittels Gaschromatographie-Massenspektrometrie mit Elektroneneinfang nach negativer chemischer Ionisation (GC-ECNI-MS).
Abhängig von der Matrix und der Nachweisempfindlichkeit der GC-ECNI-MS kann das Verfahren auf Proben mit einer SCCP-Gesamtkonzentration von z. B. 0,03 µg/g bis 3 µg/g angewendet werden.

Qualité de l'eau - Détermination des alcanes polychlorés à chaîne courte dans les sédiments et matières en supsension (particules) - Méthode par chromatographie en phase gazeuse-spectrométrie de masse (CPG-SM) et ionisation chimique négative (ICN) (ISO 18635:2016)

L'ISO 18635:2016 spécifie une méthode de détermination quantitative de la somme de n-alcanes polychlorés à chaîne courte, également connus sous le nom de paraffines polychlorées à chaîne courte (SCCP), ayant une chaîne carbonée comprise entre n-C10 et n-C13 inclus, dans des mélanges dont la fraction massique («teneur») de chlore varie de 50 % et 67 %, englobant approximativement 6 000 des 8 000 congénères environ.
La présente méthode est applicable à la détermination de la somme des SCCP dans les sédiments et les matières en suspension (particules), les boues d'épuration et le sol, par chromatographie en phase gazeuse-spectrométrie de masse en mode d'ionisation négative par capture d'électrons (CG-INCE-SM).
Selon la matrice et les capabilités de détection de la CG-INCE-SM, la méthode peut être appliquée aux échantillons contenant, par exemple, de 0,03 µg/g à 3 µg/g de la somme des SCCP.

Kakovost vode - Določevanje polikloriranih alkanov s kratko verigo (SCCP) v sedimentu, blatu odpadnih vod in suspendiranih delcih - Metoda plinske kromatografije/masne spektrometrije (GC/MS) z negativno ionizacijo in zajemom elektronov (ECNI) (ISO 18635:2016)

Ta mednarodni standard določa metodo za kvantitativno določevanje vsote polikloriranih alkanov s kratko verigo (SCCP), znanih tudi kot poliklorirani parafini s kratko verigo, v razponu ogljikovih vezi n-C10 do vključno n-C13, v zmeseh z masnimi deleži klora (»vsebnost«) med 50 in 67 %, vključno s približno 6000 od približno 8000 analogov. Ta metoda se uporablja za določevanje vsote polikloriranih alkanov s kratko verigo v sedimentu ter suspendiranih delcih in zemlji z uporabo plinske kromatografije/masne spektrometrije (GC/MS) in negativno kemijsko ionizacijo z zajetjem elektronov (GC ECNI MS). Metodo je mogoče uporabiti za vzorce z vsoto polikloriranih alkanov npr. od 0,03 µg/g do 1 µg/g, odvisno od detekcijskih sposobnosti GC ECNI MS.

General Information

Status
Published
Publication Date
19-Apr-2016
Withdrawal Date
30-Oct-2016
Technical Committee
Drafting Committee
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Start Date
20-Apr-2016
Completion Date
20-Apr-2016

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SLOVENSKI STANDARD
01-junij-2017
.DNRYRVWYRGH'RORþHYDQMHSROLNORULUDQLKDONDQRYVNUDWNRYHULJR 6&&3 Y
VHGLPHQWXEODWXRGSDGQLKYRGLQVXVSHQGLUDQLKGHOFLK0HWRGDSOLQVNH
NURPDWRJUDILMHPDVQHVSHNWURPHWULMH *&06 ]QHJDWLYQRLRQL]DFLMRLQ]DMHPRP
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Water quality - Determination of short-chain polychlorinated alkanes (SCCPs) in
sediment, sewage sludge and suspended (particulate) matter - Method using gas
chromatography-mass spectrometry (GC-MS) and electron capture negative ionization
(ECNI) (ISO 18635:2016)
Wasserbeschaffenheit - Bestimmung kurzkettiger polychlorierter Alkane (SCCP) in
Sediment, Klärschlamm und Schwebstoff - Gaschromatographisch-
massenspektrometrisches Verfahren (GC-MS) unter Anwendung negativer chemischer
Ionisation und Elektroneneinfang (ECNI) (ISO 18635:2016)
Qualité de l'eau - Détermination des alcanes polychlorés à chaîne courte dans les
sédiments et matières en supsension (particules) - Méthode par chromatographie en
phase gazeuse-spectrométrie de masse (CPG-SM) et ionisation chimique négative (ICN)
(ISO 18635:2016)
Ta slovenski standard je istoveten z: EN ISO 18635:2016
ICS:
13.060.50 3UHLVNDYDYRGHQDNHPLþQH Examination of water for
VQRYL chemical substances
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN ISO 18635
EUROPEAN STANDARD
NORME EUROPÉENNE
April 2016
EUROPÄISCHE NORM
ICS 13.060.50
English Version
Water quality - Determination of short-chain
polychlorinated alkanes (SCCPs) in sediment, sewage
sludge and suspended (particulate) matter - Method using
gas chromatography-mass spectrometry (GC-MS) and
electron capture negative ionization (ECNI) (ISO
18635:2016)
Qualité de l'eau - Détermination des alcanes Wasserbeschaffenheit - Bestimmung kurzkettiger
polychlorés à chaîne courte dans les sédiments et polychlorierter Alkane (SCCP) in Sediment,
matières en supsension (particules) - Méthode par Klärschlamm und Schwebstoffen -
chromatographie en phase gazeuse-spectrométrie de Gaschromatographisch-massenspektrometrisches
masse (CPG-SM) et ionisation chimique négative (ICN) Verfahren (GC-MS) unter Anwendung negativer
(ISO 18635:2016) chemischer Ionisation und Elektroneneinfang (ECNI)
(ISO 18635:2016)
This European Standard was approved by CEN on 20 February 2016.

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.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2016 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 18635:2016 E
worldwide for CEN national Members.

Contents Page
European foreword . 3

European foreword
This document (EN ISO 18635:2016) has been prepared by Technical Committee ISO/TC 147 “Water
quality” in collaboration with 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 October 2016, and conflicting national standards shall
be withdrawn at the latest by October 2016.
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.
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, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Endorsement notice
The text of ISO 18635:2016 has been approved by CEN as EN ISO 18635:2016 without any modification.
INTERNATIONAL ISO
STANDARD 18635
First edition
2016-04-01
Water quality — Determination
of short-chain polychlorinated
alkanes (SCCPs) in sediment, sewage
sludge and suspended (particulate)
matter — Method using gas
chromatography-mass spectrometry
(GC-MS) and electron capture
negative ionization (ECNI)
Qualité de l’eau — Détermination des alcanes polychlorés à chaîne
courte dans les sédiments et matières en supsension (particules) —
Méthode par chromatographie en phase gazeuse-spectrométrie de
masse (CPG-SM) et ionisation chimique négative (ICN)
Reference number
ISO 18635:2016(E)
©
ISO 2016
ISO 18635:2016(E)
© ISO 2016, Published in Switzerland
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
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CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2016 – All rights reserved

ISO 18635:2016(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Principle . 1
4 Interferences . 2
5 Reagents . 3
6 Apparatus . 6
7 Sampling and sample pretreatment . 7
8 Procedure. 7
8.1 Extraction . 7
8.2 Extract clean-up . 7
8.3 Measurement and integration of the chromatogram. 8
8.4 Calibration . 8
8.4.1 General. 8
8.4.2 Basic calibration . 9
8.4.3 Identification and quantification with mass fragment combinations .10
8.4.4 Calculation of the results .10
8.4.5 Quality checks for internal standardization .11
9 Expression of results .11
10 Test report .11
Annex A (normative) Programme for pressurized liquid extraction .12
Annex B (informative) Explanation of the calibration of the sum of SCCPs with multiple
linear regression .13
Annex C (informative) Examples of typical GC-MS conditions .18
Annex D (normative) Alternative clean-up with column chromatography .22
Annex E (informative) Alternative clean-up with gel chromatography .24
Annex F (informative) Typical chromatograms of standard solutions 1 µg/ml .25
Annex G (informative) Presentation of goodness of fit of the calibration .26
Annex H (informative) Example for recoveries of quality assurance solutions .27
Annex I (informative) Chromatograms of real samples.29
Annex J (informative) Performance data .31
Annex K (informative) Quality control check solutions .32
Bibliography .33
ISO 18635:2016(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to th
...

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