SIST EN ISO 12010:2019

Water quality - Determination of short-chain polychlorinated alkanes (SCCP) in water - Method using gas chromatography-mass spectrometry (GC-MS) and negative-ion chemical ionization (NCI) (ISO 12010:2019)

This document 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 unfiltered surface water, ground
water, drinking water and waste water using gas chromatography-mass spectrometry with electron
capture negative ionization (GC-ECNI-MS).
Depending on the capability of the GC-ECNI-MS instrument, the concentration range of the method
is from 0,1 μg/l or lower to 10 μg/l. Depending on the waste water matrix, the lowest detectable
concentration is estimated to be > 0,1 μg/l. The data of the interlaboratory trial concerning this method
are given in Annex I.

Wasserbeschaffenheit - Bestimmung von kurzkettigen Chloralkanen (SCCP) in Wasser - Verfahren mittels Gaschromatographie-Massenspektrometrie (GC-MS) und negativer chemischer Ionisation (NCI) (ISO 12010:2019)

Dieses Dokument 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 ungefiltertem Oberflächen-wasser, Grundwasser, Trinkwasser und Abwasser mittels Gaschromatographie Massenspektrometrie mit Elektroneneinfang nach negativer chemischer Ionisation (GC ECNI MS).
Abhängig von der Leistungsfähigkeit des GC ECNI MS liegt der Konzentrationsbereich des Verfahrens von 0,1 µg/l oder unter 10 µg/l. Abhängig von der Abwassermatrix wird die niedrigste nachweisbare Konzentration auf > 0,1 µg/l geschätzt. Die Daten des Ringversuchs zu diesem Verfahren sind im Anhang I dargestellt.

Qualité de l'eau - Détermination des alcanes polychlorés à chaîne courte (SCCP) dans l'eau - Méthode par chromatographie gazeuse-spectrométrie de masse (CG-SM) avec ionisation chimique négative (ICN) (ISO 12010:2019)

Le présent document spécifie une méthode de détermination quantitative de la somme des 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 % à 67 %, contenant environ 6 000 des environ 8 000 congénères.
Cette méthode est applicable à la détermination de la somme des SCCP dans les eaux de surface, les eaux souterraines, l'eau potable et les eaux usées non filtrées, par chromatographie en phase gazeuse couplée à la spectrométrie de masse (GC-MS) en mode d'ionisation négative par capture d'électrons (GC-ECNI-MS).
En fonction de la capacité de l'instrument de GC-ECNI-MS, la plage de concentration de la méthode se situe entre 0,1 µg/l ou inférieur et 10 µg/l. Selon la matrice de l'échantillon d'eau usée, la plus petite concentration détectable est estimée comme étant > 0,1 µg/l. Les données de l'essai interlaboratoires portant sur cette méthode sont présentés dans l'Annexe I.

Kakovost vode - Določevanje polikloriranih alkanov s kratko verigo (SCCP) v vodi - Metoda s plinsko kromatografijo z masno selektivnim detektorjem (GC-MS) in negativno kemijsko ionizacijo (NCI) (ISO 12010:2019)

Ta dokument določa metodo za kvantitativno določevanje vsote polikloriranih alkanov s kratko verigo (SCCP), znanih tudi kot poliklorirani parafini s kratko verigo, v razponu ogljikovih vezi od 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 nefiltrirani površinski vodi, podtalnici, pitni vodi in odpadni vodi na podlagi plinske kromatografije/masne spektrometrije (GC/MS) in negativne kemijske ionizacije z zajetjem elektronov (GC-ECNI-MS).
Glede na zmogljivost instrumenta GC-ECNI-MS je območje koncentracije metode
od 0,1 μg/l ali manj do 10 μg/l. Najnižja koncentracija, ki jo je še mogoče zaznati, je ocenjena na višjo od 0,1 μg/l, odvisno od matriksa odpadne vode. Podatki medlaboratorijskega preskušanja o tej metodi so navedeni v dodatku I.

General Information

• Status: Published
• Public Enquiry End Date: 01-Apr-2018
• Publication Date: 14-May-2019
• ICS: 13.060.50 - Examination of water for chemical substances
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: KAV - Water quality
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 20-Mar-2019
• Due Date: 25-May-2019
• Completion Date: 15-May-2019
• Directive: 2000/60/EC - Directive 2000/60/EC of the European Parliament and of the Council of 23 October 2000 establishing a framework for Community action in the field of water policy (substitutes Directive Reference 01/991 - Common Position on WFD)
• Mandate: M/424 - Mandate for standardisation addressed to CEN for the development or improvement standards in support of the water framework directive
• Ref Project: EN ISO 12010:2019 - Water quality - Determination of short-chain polychlorinated alkanes (SCCP) in water - Method using gas chromatography-mass spectrometry (GC-MS) and negative-ion chemical ionization (NCI) (ISO 12010:2019)

Relations

• Replaces: SIST EN ISO 12010:2014 - 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 12010:2012)
• Effective Date: 01-Jun-2019
• Replaces: SIST EN ISO 12010:2014 - 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 12010:2012)
• Effective Date: 08-Jun-2022

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN ISO 12010:2019
01-junij-2019
Nadomešča:
SIST EN ISO 12010:2014
Kakovost vode - Določevanje polikloriranih alkanov s kratko verigo (SCCP) v vodi
- Metoda s plinsko kromatografijo z masno selektivnim detektorjem (GC-MS) in
negativno kemijsko ionizacijo (NCI) (ISO 12010:2019)
Water quality - Determination of short-chain polychlorinated alkanes (SCCP) in water -
Method using gas chromatography-mass spectrometry (GC-MS) and negative-ion
chemical ionization (NCI) (ISO 12010:2019)
Wasserbeschaffenheit - Bestimmung von kurzkettigen Chloralkanen (SCCP) in Wasser -
Verfahren mittels Gaschromatographie-Massenspektrometrie (GC-MS) und negativer
chemischer Ionisation (NCI) (ISO 12010:2019)
Qualité de l'eau - Détermination des alcanes polychlorés à chaîne courte (SCCP) dans
l'eau - Méthode par chromatographie gazeuse-spectrométrie de masse (CG-SM) avec
ionisation chimique négative (ICN) (ISO 12010:2019)
Ta slovenski standard je istoveten z: EN ISO 12010:2019
ICS:
13.060.50 Preiskava vode na kemične Examination of water for
snovi chemical substances
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
SIST EN ISO 12010:2019 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 12010:2019

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SIST EN ISO 12010:2019


EN ISO 12010
EUROPEAN STANDARD

NORME EUROPÉENNE

April 2019
EUROPÄISCHE NORM
ICS 13.060.50 Supersedes EN ISO 12010:2014
English Version

Water quality - Determination of short-chain
polychlorinated alkanes (SCCP) in water - Method using
gas chromatography-mass spectrometry (GC-MS) and
negative-ion chemical ionization (NCI) (ISO 12010:2019)
Qualité de l'eau - Détermination des alcanes Wasserbeschaffenheit - Bestimmung von kurzkettigen
polychlorés à chaîne courte (SCCP) dans l'eau - Chloralkanen (SCCP) in Wasser - Verfahren mittels
Méthode par chromatographie gazeuse-spectrométrie Gaschromatographie-Massenspektrometrie (GC-MS)
de masse (CG-SM) avec ionisation chimique négative und negativer chemischer Ionisation (NCI) (ISO
(ICN) (ISO 12010:2019) 12010:2019)
This European Standard was approved by CEN on 18 February 2019.

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, Serbia, 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: Rue de la Science 23, B-1040 Brussels
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 12010:2019 E
worldwide for CEN national Members.

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SIST EN ISO 12010:2019
EN ISO 12010:2019 (E)
Contents Page
European foreword . 3

2

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SIST EN ISO 12010:2019
EN ISO 12010:2019 (E)
European foreword
This document (EN ISO 12010:2019) 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 2019, and conflicting national standards shall
be withdrawn at the latest by October 2019.
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.
This document supersedes EN ISO 12010:2014.
This document has been prepared under a mandate given to CEN by the European Commission and the
European Free Trade Association.
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, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Endorsement notice
The text of ISO 12010:2019 has been approved by CEN as EN ISO 12010:2019 without any modification.

3

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SIST EN ISO 12010:2019

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SIST EN ISO 12010:2019
INTERNATIONAL ISO
STANDARD 12010
Second edition
2019-03
Water quality — Determination of
short-chain polychlorinated alkanes
(SCCP) in water — Method using gas
chromatography-mass spectrometry
(GC-MS) and negative-ion chemical
ionization (NCI)
Qualité de l'eau — Détermination des alcanes polychlorés à
chaîne courte (SCCP) dans l'eau — Méthode par chromatographie
gazeuse-spectrométrie de masse (CG-SM) avec ionisation chimique
négative (ICN)
Reference number
ISO 12010:2019(E)
©
ISO 2019

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SIST EN ISO 12010:2019
ISO 12010:2019(E)

COPYRIGHT PROTECTED DOCUMENT
© ISO 2019
All rights reserved. Unless otherwise specified, or required in the context of its implementation, 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
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: [phone]
Fax: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved

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SIST EN ISO 12010:2019
ISO 12010:2019(E)

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Interferences . 2
6 Reagents and standards . 3
6.1 Solvents for extraction and preparation of stock solutions . 3
6.2 Reference SCCP stock solutions . 3
6.3 Internal standard stock solutions from individual congeners . 4
6.4 Calibration solutions . 5
6.5 Extraction auxiliary and clean-up materials . 5
7 Apparatus . 6
8 Sampling and sample pretreatment . 7
9 Procedure. 7
9.1 Extraction with liquid-liquid extraction . 7
9.2 Extraction with higher content of suspended matter . 7
9.3 Extract clean-up . 8
9.4 Measurement and integration of the chromatogram. 8
9.5 Calibration . 9
9.5.1 General. 9
9.5.2 Basic calibration .10
9.5.3 Identification and quantification with mass fragment combinations .11
9.5.4 Calculation of the results .11
9.5.5 Quality checks for internal standardization .12
10 Expression of results .12
11 Test report .12
Annex A (normative) Independent quality control check solutions .13
Annex B (informative) Explanation of the calibration of the sum of SCCPs with multiple
linear regression .15
Annex C (informative) Typical GC-MS conditions .21
Annex D (informative) Typical chromatograms of standard solutions and quality control
check solutions 1 µg/ml .24
Annex E (informative) Presentation of goodness of fit .31
Annex F (normative) Alternative clean-up with column chromatography .32
Annex G (informative) Alternative clean-up with gel chromatography .35
Annex H (informative) Chromatograms of real SPM samples .36
Annex I (informative) Performance data .40
Bibliography .42
© ISO 2019 – All rights reserved iii

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SIST EN ISO 12010:2019
ISO 12010:2019(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 voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following
URL: www .iso .org/iso/foreword .html.
This document was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2,
Physical, chemical and biochemical methods.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/members .html.
This second edition cancels and replaces the first edition (ISO 12010:2012), which has been technically
revised. The main changes compared to the previous edition are:
— the m/z values (mass/charge ratios) for quantification and identification;
— the calibration mixtures;
— the clean up procedure by gel chromatography;
— reduced interferences.
iv © ISO 2019 – All rights reserved

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SIST EN ISO 12010:2019
ISO 12010:2019(E)

Introduction
The user should be aware that particular problems might require the specifications of additional
marginal conditions.
This document achieves synergetic effects in the practical laboratory work. The following points
partially allow a combination of water and sediment analysis:
[2]
1) same mass combination as for sediment analysis (see ISO 18635 );
2) same calibration mixtures as for sediment analysis (see ISO 18635);
3) same GPC-clean up as for sediment analysis (see ISO 18635).
© ISO 2019 – All rights reserved v

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SIST EN ISO 12010:2019

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SIST EN ISO 12010:2019
INTERNATIONAL STANDARD ISO 12010:2019(E)
Water quality — Determination of short-chain
polychlorinated alkanes (SCCP) in water — Method using
gas chromatography-mass spectrometry (GC-MS) and
negative-ion chemical ionization (NCI)
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.
IMPORTANT — It is absolutely essential that tests conducted in accordance to this document be
carried out by suitably qualified staff.
1 Scope
This document 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”) between
10 13
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 unfiltered surface water, ground
water, drinking water and waste water using gas chromatography-mass spectrometry with electron
capture negative ionization (GC-ECNI-MS).
Depending on the capability of the GC-ECNI-MS instrument, the concentration range of the method
is from 0,1 µg/l or lower to 10 µg/l. Depending on the waste water matrix, the lowest detectable
concentration is estimated to be > 0,1 µg/l. The data of the interlaboratory trial concerning this method
are given in Annex I.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements 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.
ISO 5667-1, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes and
sampling techniques
ISO 5667-3, Water quality — Sampling — Part 3: Preservation and handling of water samples
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/TS 13530, Water quality — Guidance on analytical quality control for chemical and physicochemical
water analysis
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https: //www .iso .org/obp
— IEC Electropedia: available at http: //www .electropedia .org/
© ISO 2019 – All rights reserved 1

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SIST EN ISO 12010:2019
ISO 12010:2019(E)

4 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 %
(for example a mean of approximately 4 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 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 (References [5] to [9]).
SCCPs in whole water samples are fortified with an internal standard and extracted using liquid-
liquid extraction with an organic solvent. The sample enrichment procedure is followed by a clean-
up procedure 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 document are essential for the analysis of the sum of SCCPs (see References [3] and [4]).
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. The calibration requires the specified three differently composed standard mixtures
fortified with an internal standard.
These standard mixtures mimick different mixtures found in the environment. In this method, 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 Clause 1 and in References [3] and [4]. It is not possible to use only one reference mixture for that
complex task.
The method allows for a quantification of the sum of SCCPs expected to be within an expanded
measurement uncertainty of less than 50 %.
5 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 power to, for example, 0,4 u, which is often possible with
a quadrupole mass spectrometer. The exact m/z values are 374,958 8; 410,916 9; 422,935 5; 448,810 6
(see Reference [8]).
Applying the entire procedure using the clean up procedure given in 9.3, 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 0,1 µg/l
Highest concentration level which
causes no interferences higher
Potential interfering compounds
than the limit of quantification of
0,1 µg/l
a
Aroclor 1262 1,25 µg/l
a
Aroclor 1242 10 µg/l
a
Aroclor 1221 10 µg/l
a
Aroclor 1262, Aroclor 1242, Aroclor 1221, Halowax 1014 and Halowax 1051 are examples of suitable products
available commercially. These examples are given for the convenience of users of this document and do not constitute an
endorsement by ISO of these products.
2 © ISO 2019 – All rights reserved

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SIST EN ISO 12010:2019
ISO 12010:2019(E)

Table 1 (continued)
Highest concentration level which
causes no interferences higher
Potential interfering compounds
than the limit of quantification of
0,1 µg/l
Campheclor (toxaphene) 1,75 µg/l
a
Halowax 1014 10 µg/l
a
Halowax 1051 0,4 µg/l
MCCP (medium-chain chlorinated n-alkanes C -C ) 42 % chlorine 10 µg/l
14 17
MCCP (medium-chain chlorinated n-alkanes C -C ) 52 % chlorine 6 µg/l
14 17
MCCP (medium-chain chlorinated n-alkanes C -C ) 57 % chlorine 10 µg/l
14 17
a
Aroclor 1262, Aroclor 1242, Aroclor 1221, Halowax 1014 and Halowax 1051 are examples of suitable products
available commercially. These examples are given for the convenience of users of this document and do not constitute an
endorsement by ISO of these products.
6 Reagents and standards
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 ensure
they are suitable and establish proper analytical control.
6.1 Solvents for extraction 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
Use 2,2,4-trimethylpentane (C H , isooctane) for conditioning of the glass bottles (7.1).
8 18
For preparation of the stock solution and dilutions of the internal standard, use propanone
(acetone), C H O.
3 6
For conditioning of the clean-up columns, use mixtures of n-heptane and propanone (acetone).
For the first elution step of the filtrated suspended matter, use methanol (CH OH).
3
6.2 Reference SCCP stock solutions
Use commercially available solutions, such as 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 were 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 [6]. 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 [7]). The standard mixture “Sediment Drevnice” simulates a natural mixture
reported about a sediment of the river Drevnice (see Reference [8]) with a high content of C and a
13
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.
Prepare the solutions “Lake Ontario water”, ”Perch”, and “Sediment Drevnice” according to Table 2.
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ISO 12010:2019(E)

Table 2 — Reference substances stock solutions
Reference substances stock solutions in
accordance with 6.2
Commercially available standard solutions
(Synthetic mixed standard solutions, which
resemble environmental mixtures composi-
tion, ng/ml)
“Lake Ontario “Sediment
“Perch”
Chlorine content
water” Drevnice”
n-alkane
% of the individual Mean number of chlorines in
chain
Chlorine Chlorine Chlorine
C-number mixtures as the molecules (calculated)
length a a a
content content content
certified
50,2 % 60,6 % 65,0 %
C 50,18 3,97 1 000
10
C 55,00 4,79 1 000
10
C 60,09 5,86 500
10
C 65,02 7,16 1 100 280
10
C 45,50 3,63 1 000
11
C 50,21 4,37 1 000
11
C 55,20 5,31 600
11
C 60,53 6,55 1 000 500
11
C 65,25 7,94 3 000 660
11
C 45,32 3,93 2 000
12
C 50,18 4,76 2 000 800
12
C 55,00 5,74 2 000 2 000
12
C 65,08 8,59 900 1 000
12
C 69,98 10,62 830
12
C 59,98 7,56 100 730
13
C 65,18 9,34 6 000
13
Sum of SCCP (ng/ml) 10 000 10 000 10 000
a
The chlorine content of the mixtures is calculated as the weighted mean.
Store the prepared solutions in a refrigerator at 2 °C to 8 °C. Avoiding losses of the solvent by evaporation,
solutions can be used for five years.
Use as well commercially available solutions, e.g. in cyclohexane or n-hexane, of the reference substances
stock solutions (see Table 2, last three columns) of SCCP. See Reference [8].
1)
An example is DRE-ZS22102105HP . See Reference [8].
6.3 Internal standard stock solutions from individual congeners
Use commercially available individual congener standard solutions and prepare a stock solution in
propanone (acetone) (6.1) 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, for example:
— 1,1,1,3,10,11-hexachloroundecane, with e.g. 0,1 µg/ml;
— 1,1,1,3,11,13,13,13-octachlorotridecane, with e.g. 0,1 µg/ml;
— 1,2,5,5,6,9,10-heptachlorodecane, with e.g. 0,01 µg/ml.
1) DRE-ZS22102105HP is an example of a suitable product available commercially. These examples are given for
the con
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