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
Technical Committee
Drafting Committee
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Due Date
20-Apr-2016
Completion Date
20-Apr-2016

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SLOVENSKI STANDARD
SIST EN ISO 18635:2017
01-junij-2017
.DNRYRVWYRGH'RORþHYDQMHSROLNORULUDQLKDONDQRYVNUDWNRYHULJR 6&&3 Y
VHGLPHQWXEODWXRGSDGQLKYRGLQVXVSHQGLUDQLKGHOFLK0HWRGDSOLQVNH
NURPDWRJUDILMHPDVQHVSHNWURPHWULMH *&06 ]QHJDWLYQRLRQL]DFLMRLQ]DMHPRP
HOHNWURQRY (&1,  ,62
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
SIST EN ISO 18635:2017 en,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 18635:2017
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SIST EN ISO 18635:2017
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.
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SIST EN ISO 18635:2017
EN ISO 18635:2016 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

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SIST EN ISO 18635:2017
EN ISO 18635:2016 (E)
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.

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SIST EN ISO 18635:2017
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SIST EN ISO 18635:2017
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
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SIST EN ISO 18635:2017
ISO 18635:2016(E)
COPYRIGHT PROTECTED DOCUMENT
© 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
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SIST EN ISO 18635:2017
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 2016 – All rights reserved iii
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SIST EN ISO 18635:2017
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 the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www.iso.org/patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation on the meaning of ISO specific terms and expressions related to conformity

assessment, as well as information about ISO’s adherence to the WTO principles in the Technical

Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information

The committee responsible for this document is ISO/TC 147, Water quality, Subcommittee SC 2, Physical,

chemical and biochemical methods.
iv © ISO 2016 – All rights reserved
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SIST EN ISO 18635:2017
ISO 18635:2016(E)
Introduction

The user should be aware that particular problems might require the specifications of additional

marginal conditions.
© ISO 2016 – All rights reserved v
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SIST EN ISO 18635:2017
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SIST EN ISO 18635:2017
INTERNATIONAL STANDARD ISO 18635:2016(E)
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)

WARNING — Persons using this document should be familiar with normal 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 and to

ensure compliance with any national regulatory conditions.

IMPORTANT — It is absolutely essential that tests conducted in accordance with this document

be carried out by suitably qualified staff.
1 Scope

This International Standard 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-C to n-C , inclusive in mixtures with chlorine mass fractions (“contents“)

10 13

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.
2 Normative references

The following documents, in whole or in part, are normatively referenced in this document and are

indispensable for its application. For dated references, only the edition cited applies. For undated

references, the latest edition of the referenced document (including any amendments) applies.

ISO 5667-12, Water quality — Sampling — Part 12: Guidance on sampling of bottom sediments

ISO 5667-13, Water quality — Sampling — Part 13: Guidance on sampling of sludges

ISO 5667-17, Water quality — Sampling — Part 17: Guidance on sampling of bulk suspended solids

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

ISO 12010, Water quality — Determination of short-chain polychlorinated alkanes (SCCPs) in water —

Method using gas chromatography-mass spectrometry (GC-MS) and negative-ion chemical ionization (NCI)

ISO/TS 13530, Water quality — Guidance on analytical quality control for chemical and physicochemical

water analysis
3 Principle

Determination of the sum of SCCPs in the carbon bond range, n-C to n-C , inclusive in technical and

10 13

environmental transposed mixtures with chlorine mass fractions (“contents“) between 50 % and 67 %

© ISO 2016 – All rights reserved 1
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SIST EN ISO 18635:2017
ISO 18635:2016(E)

(e.g. approximately 3 to 10 chlorine atoms per molecule) and independent of the C-number distribution

pattern of the congeners. No recognition of the chlorine content is necessary.

The samples are fortified with an internal standard and extracted using pressurized liquid extraction

with an organic solvent. The sample extraction procedure is followed by a clean-up procedure by

column chromatography and gel permeation chromatography to eliminate interfering compounds. Gas

chromatography (GC) is undertaken using a short capillary column within a short retention time range.

The detection of selected mass fragments is carried out using mass spectrometry (MS) in selected ion-

monitoring mode using electron capture negative ionization mode (ECNI). The mass fragments and

the compositions of the calibration solutions used in this International Standard are essential for the

analysis of the sum of SCCPs.

The selected ion chromatogram is integrated over the full retention time range of the SCCPs. The

quantification of the sum of SCCPs is carried out after establishing a calibration by a multiple linear

regression measuring solutions of different SCCP mixtures fortified with an internal standard.

The analysed sum of SCCPs includes the variety of SCCPs with their differing chlorine content and

C-number distribution patterns as found in technical mixtures, as well as compositions in the

environment. The calibration requires at least three differently composed standard mixtures.

These standard mixtures mimic different mixtures found in the environment. Only the multiple linear

regression quantification with these specific mixtures enables the quantification of the variety of

observed mixtures of SCCP in the environment and in technical compositions described in the scope

and in Reference [6]. It is not possible to use only one standard mixture for that complex task.

4 Interferences

Non-specific matrix interferences, as well as interferences from other environmental situations, are

dealt with using the given clean-up procedure. A further reduction of matrix effects can be achieved by

reducing the mass spectrometric resolution to, e.g., 0,4 amu, which is often possible with a quadrupole

mass spectrometer. The exact masses are 374,9588; 410,9169; and 422,9355 (see Reference [6]).

Applying the entire procedure, a selection of chlorinated pollutants has been tested and found not to

cause interferences below the concentrations given in Table 1.

Table 1 — Highest concentration level which causes no interferences higher than the limit of

quantification of 0,03 µg/g
Potential interfering compounds Highest concentration level which causes
no interferences higher than the limit of
quantification of 0,03 µg/g
Aroclor 1262 0,25 µg/g
Aroclor 1242 2 µg/g
Aroclor 1221 2 µg/g
Campheclor (toxaphene) 0,35 µg/g
Halowax 1014 2 µg/g
Halowax 1051 0,08 µg/g
MCCP (medium-chain chlorinated n-alkanes) 42 % 2 µg/g
MCCP (medium-chain chlorinated n-alkanes) 52 % 1,2 µg/g
MCCP (medium-chain chlorinated n-alkanes) 57 % 2 µg/g

Aroclor 1262, Aroclor 1242, Aroclor 1221, Halowax 1014, and Halowax 1051 are products commercially available. This

information is given for the convenience of users of this document and does not constitute an endorsement by ISO of these

products.
2 © ISO 2016 – All rights reserved
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SIST EN ISO 18635:2017
ISO 18635:2016(E)
5 Reagents

Use solvents and reagents of sufficient purity, i.e. with negligibly low concentrations of SCCPs, e.g. lower

than the limit of detection of the method.

Check blanks regularly over the entire procedure to establish proper analytical quality control.

5.1 Solvents for extraction, column chromatography, and preparation of stock solutions.

The solvent for extraction is n-heptane. Other non-polar solvents, e.g. n-hexane (C H ), cyclohexane

6 14

(C H ) can be used if the extraction efficiency is comparable with those of n-heptane.

6 12

For conditioning of the clean-up columns, use mixtures of n-heptane and propanone (acetone) as

described below.
5.2 Reference SCCP stock solutions.

Use commercially available solutions, e.g. in cyclohexane or n-hexane, of the single mixtures of SCCP

congeners with defined carbon chain length and with different defined chlorine contents (see Table 2,

first two columns). Alternatively, use commercially available ready mixed solutions with the same

composition.

Mixtures of synthetic solutions are used to simulate environmentally occurring SCCPs or technical

products of SCCPs. For example, the synthetic mixed calibration stock solution “Lake Ontario water” is

mixed to resemble a Lake Ontario water as reported in Reference [5]. Its characteristic is a relatively

high content of C to C , especially C and a low chlorine content as partly reported in water samples

10 12 12

too. The synthetic mixed calibration stock solution “Perch” simulates a C-number distribution found

in a perch (see Reference [6]). The standard mixture “Sediment Drevnice” simulates a natural mixture

reported about a sediment of the river Drevnice (see Reference [7]) with a high content of C and a

higher chlorine content.

The compositions of the calibration mixtures, as well as of the independent quality assurance solutions,

are mandatory to achieve the quantification of the variety of SCCP-mixtures. An example for recoveries

of quality assurance solutions is given in Annex H.

Prepare the solutions “Lake Ontario water”, “Perch”, and “Sediment Drevnice” according to Table 2.

Table 2 — Reference substances stock solutions
Standard solutions, e.g. in n-heptane Synthetic mixed standard solutions
which resemble environmental
mixtures
n-alkane Chlorine Mean “Lake “Perch” “Sediment
chain content (%) number Ontario Drevnice”
length of the of chlorines water”
individual in the
C-number molecules
mixtures (calculated)
Chlorine content calculated (%) 50,2 60,6 65,0
Composition, ng/ml
C 44,82 3,22
C 50,18 3,97 1 000
C 55,00 4,79 1 000
C 60,09 5,86 500
C 65,02 7,16 1 100 280
C 45,50 3,63 1 000
C 50,21 4,37 1 000
© ISO 2016 – All rights reserved 3
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SIST EN ISO 18635:2017
ISO 18635:2016(E)
Table 2 (continued)
Standard solutions, e.g. in n-heptane Synthetic mixed standard solutions
which resemble environmental
mixtures
n-alkane Chlorine Mean “Lake “Perch” “Sediment
chain content (%) number Ontario Drevnice”
length of the of chlorines water”
individual in the
C-number molecules
mixtures (calculated)
Chlorine content calculated (%) 50,2 60,6 65,0
Composition, ng/ml
C 55,20 5,31 600
C 60,53 6,55 1 000 500
C 65,25 7,94 3 000 660
C 45,32 3,93 2 000
C 50,18 4,76 2 000 800
C 55,00 5,74 2 000 2 000
C 65,08 8,59 900 1 000
C 69,98 10,62 830
C 44,90 4,19
C 50,23 5,16
C 55,03 6,22
C 59,98 7,56 100 730
C 65,18 9,34 6 000
Sum of SCCP (ng/ml) 10 000 10 000 10 000

The chlorine content (third column) of the mixtures is calculated as the weighted mean.

Store the prepared solutions in a refrigerator at 2 °C to 6 °C.
5.3 Internal standard stock solutions from individual congeners.

Use commercially available individual congener standard solutions and prepare a stock solution in

propanone (acetone) (5.1) at a concentration of, for example, 1 µg/ml.

— Individual SCCP congeners with chlorine contents of between 50 % and 67 % are suitable as internal

standards if the mass trace in mass spectrometric detection is not affected by matrix components,

e.g. 1,1,1,3,11,13,13,13-octachlorotridecane at e.g. 0,1 µg/ml.

NOTE 1 The different individual SCCP congeners used as internal standard substances probably contribute in

environmental samples to the sum of SCCPs. Nevertheless, the contribution is approximately <1 % which means

that the enhancement of the measurement uncertainty is negligible.

NOTE 2 Different individual SCCP congeners can produce different response factors, hence, it can be necessary

for different concentrations to be used.
The solutions should be stored in a refrigerator at 2 °C to 6 °C.
5.4 Calibration solutions.

Use the standard mixtures according to Table 2. Prepare a minimum of nine calibration solutions (see

Table 3) with concentrations according to the detection capability of the mass spectrometer. Combine

and dilute the solutions (5.2) and the internal standard stock solution (5.3) with n-heptane to produce

solutions for the calibration range, e.g. as shown in Table 3.
4 © ISO 2016 – All rights reserved
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SIST EN ISO 18635:2017
ISO 18635:2016(E)
Table 3 — Calibration solutions
Mixture “Lake “Perch” “Sediment Internal standard
Ontario” Drevnice”
water
1,1,1,3,11,13,13,13-octachlorotridecane
µg/ml µg/ml µg/ml µg/ml
Sum of SCCPs,
µg/ml
0,15 0,15 0,1
0,15 0,15 0,1
0,15 0,15 0,1
0,6 0,6 0,1
0,6 0,6 0,1
0,6 0,6 0,1
1 1 0,1
1 1 0,1
1 1 0,1
2 2 0,1
2 2 0,1
2 2 0,1
3 3 0,1
3 3 0,1
3 3 0,1

The solutions can be stored in a refrigerator, for at least four weeks. Check the concentration of the

calibration solutions against an independently prepared standard prior to use.

Quality control check solutions can be prepared to check the calibration independently. For that, use the

calibration mixtures as given in ISO 12010 (see Annex K). These mixtures are commercially available

(e.g. in cyclohexane or n-hexane).
5.5 Extraction auxiliary and clean-up materials.

5.5.1 High purity silica sand, grain size 600 µm to 850 µm, blank free from contamination.

5.5.2 Copper powder, grain size <63 µm.
5.5.3 2 mol/l hydrochloric acid.
5.5.4 Al O , neutral, high activity, (10 % water).
2 3
5.5.5 Glass wool.

5.6 Operating gases, for GC-MS of high purity and in accordance with manufacturer’s specifications.

5.7 Nitrogen, N , purity ≥99,996 % volume fraction for concentrating the solutions.

5.8 Sodium sulfate, anhydrous, Na SO , powdered.
2 4
© ISO 2016 – All rights reserved 5
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SIST EN ISO 18635:2017
ISO 18635:2016(E)
6 Apparatus
Clean all glassware by rinsing with acetone (propanone) (5.1).

6.1 Wide-necked bottle, 1 000 ml up to 5 000 ml capacity for wet sediment or sludge.

6.2 Freeze drying apparatus.
6.3 Deep freezer.
6.4 Mortar and pestle or a grinding mill.

6.5 Drying ovens, capable of maintaining temperatures in the ranges of 100 °C to 400 °C for baking

and storage of clean-up materials, for baking of glassware, an
...

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