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)

EN ISO 12010 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 49 % and 67 %, including approximately 6 300 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). The method can be applied to samples containing 0,1 μg/l to 10 μg/l. Depending on the waste water matrix, the lowest detectable concentration is estimated to be >0,1 μg/l.

Wasserbeschaffenheit - Bestimmung von kurzkettigen Chloralkanen (SCCP) in Wasser - Verfahren mittels Gaschromatographie-Massenspektrometrie (GC-MS) und negativer chemischer Ionisation (NCI) (ISO 12010:2012)

Diese Internationale Norm legt ein Verfahren zur quantitativen Bestimmung der Summe kurzkettiger polychlorierter n-Alkane (oder kurzkettiger polychlorierter Paraffine, Abk.: SCCP) mit einer Kohlenstoff-Kettenlänge zwischen n-C10 bis einschließlich n-C13 in Gemischen mit Chlorgehalten zwischen 49 % und 67 % fest, die ungefähr 6 300 der etwa 8 000 Kongenere umfassen.
Dieses Verfahren ist zur Bestimmung der Summe von SCCP in ungefiltertem Oberflächenwasser, Grund-wasser, Trinkwasser und Abwasser unter Verwendung der Gaschromatographie-Massenspektrometrie mit Elektroneneinfang nach negativer chemischer Ionisierung (GC-ECNI-MS) geeignet.
Das Verfahren kann für Proben mit einem Gehalt von 0,1 µg/l bis 10 µg/l angewendet werden. In Abhängigkeit von der Abwasser-Matrix ist die niedrigste nachweisbare Konzentration > 0,1 µg/l.

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 12010:2012)

Kakovost vode - Določevanje polikloriranih alkanov s kratko verigo (SCCP) v vodi - Metoda s plinsko kromatografijo/masno spektrometrijo (GC/MS) in negativno kemijsko ionizacijo (NCI) (ISO 12010:2012)

EN ISO 12010 podaja 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 49 in 67 %, vključno s približno 6300 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, z uporabo plinske kromatografije/masne spektrometrije (GC/MS) in negativno kemijsko ionizacijo z zajetjem elektronov (GC-ECNI-MS). Ta metoda se uporablja za vzorce, ki vsebujejo od 0,1 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.

General Information

Status
Withdrawn
Public Enquiry End Date
31-Jan-2014
Publication Date
09-Jun-2014
Withdrawal Date
09-May-2019
Technical Committee
Current Stage
9900 - Withdrawal (Adopted Project)
Start Date
09-May-2019
Due Date
01-Jun-2019
Completion Date
10-May-2019

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SLOVENSKI STANDARD
SIST EN ISO 12010:2014
01-julij-2014

.DNRYRVWYRGH'RORþHYDQMHSROLNORULUDQLKDONDQRYVNUDWNRYHULJR 6&&3 YYRGL

0HWRGDVSOLQVNRNURPDWRJUDILMRPDVQRVSHNWURPHWULMR *&06 LQQHJDWLYQR
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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)

Wasserbeschaffenheit - Bestimmung von kurzkettigen Chloralkanen (SCCP) in Wasser -

Verfahren mittels Gaschromatographie-Massenspektrometrie (GC-MS) und negativer
chemischer Ionisation (NCI) (ISO 12010:2012)

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 12010:2012)
Ta slovenski standard je istoveten z: EN ISO 12010:2014
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 12010:2014 en

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

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SIST EN ISO 12010:2014
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SIST EN ISO 12010:2014
EUROPEAN STANDARD
EN ISO 12010
NORME EUROPÉENNE
EUROPÄISCHE NORM
April 2014
ICS 13.060.50
English Version
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)

Qualité de l'eau - Détermination des alcanes polychlorés à Wasserbeschaffenheit - Bestimmung von kurzkettigen

chaîne courte (SCCP) dans l'eau - Méthode par Chloralkanen (SCCP) in Wasser - Verfahren mittels

chromatographie gazeuse-spectrométrie de masse (CG- Gaschromatographie-Massenspektrometrie (GC-MS) und

SM) avec ionisation chimique négative (ICN) (ISO negativer chemischer Ionisation (NCI) (ISO 12010:2012)

12010:2012)
This European Standard was approved by CEN on 11 April 2014.

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

© 2014 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 12010:2014 E

worldwide for CEN national Members.
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SIST EN ISO 12010:2014
EN ISO 12010:2014 (E)
Contents Page

Foreword ..............................................................................................................................................................3

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SIST EN ISO 12010:2014
EN ISO 12010:2014 (E)
Foreword

The text of ISO 12010:2012 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 12010:2014 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 October 2014, and conflicting national standards shall be withdrawn at

the latest by October 2014.

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.

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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.

Endorsement notice

The text of ISO 12010:2012 has been approved by CEN as EN ISO 12010:2014 without any modification.

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SIST EN ISO 12010:2014
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SIST EN ISO 12010:2014
INTERNATIONAL ISO
STANDARD 12010
First edition
2012-03-15
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)
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 12010:2012(E)
ISO 2012
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SIST EN ISO 12010:2014
ISO 12010:2012(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2012

All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,

electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISO’s

member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2012 – All rights reserved
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SIST EN ISO 12010:2014
ISO 12010:2012(E)
Contents Page

Foreword ............................................................................................................................................................................iv

Introduction ........................................................................................................................................................................ v

1 Scope ...................................................................................................................................................................... 1

2 Normative references ......................................................................................................................................... 1

3 Principle ................................................................................................................................................................. 1

4 Interferences ......................................................................................................................................................... 2

5 Reagents and standards ................................................................................................................................... 2

6 Apparatus .............................................................................................................................................................. 6

7 Sampling and sample pretreatment ............................................................................................................... 7

8 Procedure .............................................................................................................................................................. 7

8.1 Extraction with liquid-liquid extraction method .......................................................................................... 7

8.2 Extraction of samples with higher content of suspended matter .......................................................... 7

8.3 Extract clean-up ................................................................................................................................................... 8

8.4 Measurement and integration of the chromatogram ................................................................................. 9

8.5 Calibration ............................................................................................................................................................. 9

9 Expression of results .......................................................................................................................................12

10 Test report ...........................................................................................................................................................12

Annex A (informative) Additional quality control check solutions ......................................................................13

Annex B (informative) Explanation of the calibration of the sum of SCCPs with multiple

linear regression ................................................................................................................................................14

Annex C (informative) Typical GC-MS conditions ....................................................................................................19

Annex D (informative) Typical chromatograms of standard solutions 1 µg/ml ...............................................22

Annex E (informative) Presentation of goodness of fit ..........................................................................................23

Annex F (informative) Example for recoveries of quality assurance solutions ...............................................24

Annex G (informative) Chromatogram of a real water sample with a sum of SCCPs concentration of

2,59 µg/l ................................................................................................................................................................25

Annex H (informative) Precision data..........................................................................................................................27

Bibliography .....................................................................................................................................................................28

© ISO 2012 – All rights reserved iii
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SIST EN ISO 12010:2014
ISO 12010:2012(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.

International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.

The main task of technical committees is to prepare International Standards. Draft International Standards

adopted by the technical committees are circulated to the member bodies for voting. Publication as an

International Standard requires approval by at least 75 % of the member bodies casting a vote.

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.

ISO 12010 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical,

chemical and biochemical methods.
iv © ISO 2012 – All rights reserved
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SIST EN ISO 12010:2014
ISO 12010:2012(E)
Introduction

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

© ISO 2012 – All rights reserved v
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SIST EN ISO 12010:2014
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SIST EN ISO 12010:2014
INTERNATIONAL STANDARD ISO 12010:2012(E)
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)

WARNING — Persons using this International Standard should be familiar with normal laboratory

practice. This International Standard 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 to this International

Standard 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”) between 49 % and 67 %,

10 13
including approximately 6 300 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).

The method can be applied to samples containing 0,1 µg/l to 10 µg/l. Depending on the waste water matrix, the

lowest detectable concentration is estimated to be >0,1 µg/l.
2 Normative references

The following referenced documents are indispensable for the application 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 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 49 % and 67 %

(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.

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

© ISO 2012 – All rights reserved 1
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SIST EN ISO 12010:2014
ISO 12010:2012(E)

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 selection of

the mass fragments is specific for the variety of technical mixtures as well as for their chlorine content and

C-number distribution patterns. Alternative mass fragment combinations for qualification are also given in this

International Standard.

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 multiple linear regression, measuring

solutions of different technical mixtures fortified with an internal standard.

The calibration requires a minimum of three different composed standard mixtures, each of which resembles

the C-number distribution pattern and chlorine content of different technical mixtures. This is to reflect the

variety of chlorine contents and C-number distribution patterns of technical SCCP mixtures and SCCP levels

found in environmental samples, which cannot be described by a single defined standard substance.

The method allows a quantification of the sum of SCCPs expected to be within an expanded measurement

uncertainty of less than 50 %.
4 Interferences

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

with using the given clean-up procedure. Following the entire procedure, including the concentration factor of

approximately 5 000, the following pollutants have been tested and found not to cause interferences below the

following concentrations.

Potential interfering compounds Highest concentration level at which no interferences

higher than the limit of detection are detected
Aroclor 1262 0,5 µg/l
Aroclor 1242 0,5 µg/l
Aroclor 1221 1 µg/l
Campheclor 0,2 µg/l
Halowax 1014 1 µg/l
Halowax 1051 1 µg/l
Technical chlordane 0,5 µg/l
MCCP (medium-chain chlorinated n-alkanes) 42 % 0,2 µg/l
MCCP (medium-chain chlorinated n-alkanes) 52 % 0,2 µg/l
MCCP (medium-chain chlorinated n-alkanes) 57 % 0,2 µg/l

Product available commercially. This information is given for the convenience of users of this document and does not constitute an

endorsement by ISO of this product.
If the clean-up procedure is repeated, interferences can be further reduced.
5 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).

NOTE Check blanks regularly over the entire procedure to ensure they are suitable and establish proper analytical control.

2 © ISO 2012 – All rights reserved
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SIST EN ISO 12010:2014
ISO 12010:2012(E)

5.1 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 ) or cyclohexane (C H ), can be used if the extraction efficiency

6 14 6 12
is comparable with those of n-heptane.

Use 2,2,4-trimethylpentane (C H , isooctane) for conditioning of the glass bottles (6.1).

8 18

For preparation of the stock solutions, use dilutions in 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).

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 a defined carbon chain length and with different

defined chlorine contents (see Table 1, first two columns). Alternatively, use commercially available ready-mixed

solutions as described in Table 1.
1) 1) 1) 1)

Prepare the solutions Hordalub 17 -s1, SCCP 51,5 % -s1, Hordalub 80 -s1, Cereclor 60 -s1, Hordalub 500 -s1,

and Cereclor 70 -s1 according to Table 1. The suffix “-s1” denotes synthetically mixed standard solutions,

which resemble the technical mixtures.

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

Store the prepared solutions in a refrigerator at a temperature of 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 49 % and 67 % are suitable as internal standards, e.g.

— 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.

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

sum of SCCPs in environmental samples. 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 to

use different concentrations.

If validated, other individual SCCP congeners can be used as the internal standard if the congener shows the

same properties over the entire analytical process as the SCCPs being determined.

The solutions can be stored in a refrigerator at a temperature of 2 °C to 6 °C.

5.4 Copper powder, mesh size <63 µm. Copper powder is used in the clean-up procedure to remove sulfur

and sulfur-containing matrix components.

5.5 Hydrochloric acid, 2 mol/l. Used for copper activation in the clean-up column.

1) Product available commercially. This information is given for the convenience of users of this document and does

not constitute an endorsement by ISO of this product.
© ISO 2012 – All rights reserved 3
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SIST EN ISO 12010:2014
ISO 12010:2012(E)

5.6 Activated magnesium silicate, MgO/3,75 SiO /(x) H O, for column chromatography.

2 2

Activated magnesium silicate is used in the clean-up procedure to separate organohalogenic compounds like

polychlorinated biphenyls and naphthalenes.

Use activated magnesium silicate with the following characteristics: particle size 0,15 mm to 0,25 mm, of which

2 2

80 % >0,15 mm; surface area, determined according to the BET method, 170 m /g to 300 m /g; pH 9 to pH 10.

Activate the magnesium silicate by heating, for example, 200 g in a shallow dish at 140 °C for at least 4 h. Allow

the activated magnesium silicate to cool to room temperature in a desiccator. Activated magnesium silicate can

be stored in a closed bottle at room temperature for up to 1 month.
Table 1 — Reference substances stock solutions
Synthetic mixed standard solutions,
Standard solutions
which resemble technical mixtures
Chlorine Hordalub SCCP Hordalub Cereclor Hordalub Cereclor
Mean
content 17 -s1 51,5 % -s1 80 -s1 60 -s1 500 -s1 70 -s1
number
n-Alkane of the
Chlorine content calculated, %
of chlorines
chain individual
in the
49,0 51,5 56,0 59,0 62,0 66,7
length C-number
molecules
mixtures,
(calculated)
Composition, ng/ml
C 44,82 3,22 500
C 50,18 3,97 500 500 500
C 55,00 4,79 500 500
C 60,09 5,86 1 000 900
C 65,02 7,16 500 300 2 000
C 45,50 3,63 1 200
C 50,21 4,37 2 600 2 500 500 700
C 55,20 5,31 1 000 2 000 1 300 400
C 60,53 6,55 1 900 1 200 2 500
C 65,25 7,94 2 500 3 200
C 45,32 3,93 1 000
C 50,18 4,76 2 400 2 500 500
C 55,00 5,74 1 500 2 500 2 000 1 000
C 65,08 8,59 200 1 500 1 700
C 69,98 10,62 3 100
C 44,90 4,19 500
C 50,23 5,16 1 800 1 000
C 55,03 6,22 1 000 400
C 59,98 7,56 400 1 300 700
C 65,18 9,34 100 1 700
Sum of SCCPs, ng/ml 10 000 10 000 10 000 10 000 10 000 10 000
5.7 Sodium sulfate, Na SO , anhydrous, granular.
2 4

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

2) Florisil is an example of a suitable product available commercially. This information is given for the convenience of

users of this document and does not constitute an endorsement by ISO of this product.

4 © ISO 2012 – All rights reserved
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SIST EN ISO 12010:2014
ISO 12010:2012(E)

5.9 Nitrogen, N , purity ≥99,996 % volume fraction, for drying of the sorbent packing material and for

concentrating solutions.

5.10 Calibration working solutions. Use a minimum of three different composed standard mixtures according

to Table 1, Hordalub 17 -s1, Hordalub 80 -s1, and Cereclor 70 -s1. Prepare a minimum of nine calibration

solutions (see bold figures in Table 2) with concentrations that correspond the detection capability of the mass

spectrometer. Combine and dilute the solutions (5.2) and the internal standard solution (5.3) with n-heptane to

produce solutions for the calibration range, e.g. as shown in Table 2.

The solutions may be stored in a refrigerator for up to 4 weeks. Check the concentration of the calibration

solutions against an independently prepared standard prior to use.
Table 2 — Calibration working solutions
Internal standard:
Hordalub SCCP Hordalub Cereclor Hordalub Cereclor e.g. 1,1,1,10,11,13-
17 -s1 51,5 -s1 80 -s1 60 -s1 500 -s1 70 -s1 hexachloro-
Mixture
decane
µg/ml µg/ml µg/ml 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
0,15 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
0,6 0,6 0,1
0,6 0,6 0,1
0,6 0,6 0,1
1,0 1,0 0,1
1,0 1,0 0,1
1,0 1,0 0,1
1,0 1,0 0,1
1,0 1,0 0,1
1,0 1,0 0,1

5.11 Quality control multi-component stock solution of SCCP for assuring calibration procedure.

Quality control check solutions should be prepared to check the calibration independently. Prepare a minimum

of three different solutions; see Table 3 or Annex A. These mixtures are also commercially available (e.g. in

cyclohexane or n-hexane).
The solutions can be stored in a refrigerator for up to 4 weeks.

5.12 Test solution for checking linearity of internal standards. Prepare solutions of the internal standard

used at concentrations of 0,1 µg/ml, 0,5 µg/ml, and 1 µg/ml.
© ISO 2012 – All rights reserved 5
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SIST EN ISO 12010:2014
ISO 12010:2012(E)
6 Apparatus

Glassware and equipment which may come into contact with water samples or their extracts should be free

from interfering compounds.
Clean all glassware by rinsing with propanone (acetone) (5.1).

6.1 Flat-bottomed glass bottles, conical shoulder, 1 000 ml capacity, for collecting water samples, preferably

with glass stoppers.
The sample bottle shall enable direct extraction of the sample.

Before use, to condition it, rinse the dry sample bottle with e.g. 2 ml of isooctane (5.1), invert it and allow the

solvent to drain and evaporate from it.
Table 3 — Calibration assurance solutions
Chlorine SCCP SCCP SCCP Hordalub Hordalub Hordalub Cereclor
content of 51,5 -s2 55,5 -s2 63 -s2 17 -s2 80 -s2 500 -s2 60 -s2
the individual
Calculated mean chlorine content, %
n-Alkane C-number
51,45 55,77 63,22 49,07 55,91 61,87 59,07
chain mixtures
length according
to the
Composition, ng/ml
manufacturer,
C 44,82 50
C 50,18 50 50
C 55 50 100 100
C 60,09 50 90 150
C 65,02 50 20
C 45,5 200 200 100
C 50,21 280 50
C 55,2 150 250 200
C 60,53 150 200 140 350 120
C 65,25 300 200
C 45,32 150 100 100
C 50,18 150 50 50 240 50
C 55 250 100 200
C 65,08 100 200 100 20 170 150
C 69,98 50
C 44,9 50
C 50,23 100 50 180
C 55,03 100 100
C 59,98 50 100 40 70 170
C 65,18 100
Sum of SCCPs, ng/ml 1 000 1 000 1 000 1 000 1 000 1 000 990
6.2 Evaporation device, e.g. rotary evaporator or nitrogen evaporating system.

6.3 Separator, for example micro-separator or other suitable device for phase separation.

6.4 Vials, compatible with the GC-autosampler (e.g. with a capacity of 1,5 ml).
6 © ISO 2012 – All rights reserved
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SIST EN ISO 12010:2014
ISO 12010:2012(E)
6.5 Chromatographic column, internal diameter (ID) 10 mm (empty) for clean-up.

6.6 Gas chromatograph, temperature-programmable, with all required accessories, including gases,

capillary column, split/splitless injector and mass spectrometer detector with negative-ion chemical ionization

option and appropriate reactant gas (CH ).
6.7 Volumetric flasks, 1 ml, 2 ml, 10 ml, and 25 ml.
6.8 Disposable glass Pasteur pipettes, e.g. 150 mm or 250 mm.
6.9 Syringes, 2 µl, 5 µl, 10 µl and 50 µl.

6.10 Analytical column. Fused silica column with non-polar low-bleed separating phase (see Annex C for

examples); e.g. ID <0,25 mm, length 15 m and film thickness 0,1 µm.
6.11 Glass fibre filter.
6.12 Vacuum filtration device, volume 1 l.
6.13 Shaking device or magnetic stirrer device (with a magnetic stir bar).
7 Sampling and sample pretreatment

Take samples as specified in ISO 5667-1 and ISO 5667-3. To collect water samples, use conditioned glass

bottle
...

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