SIST EN ISO 12010:2014
(Main)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)
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
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 12010:2014
01-julij-2014
.DNRYRVWYRGH'RORþHYDQMHSROLNORULUDQLKDONDQRYVNUDWNRYHULJR 6&&3 YYRGL
0HWRGDVSOLQVNRNURPDWRJUDILMRPDVQRVSHNWURPHWULMR *&06 LQQHJDWLYQR
NHPLMVNRLRQL]DFLMR 1&, ,62
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
2
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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.
3
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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
a
Aroclor 1262 0,5 µg/l
a
Aroclor 1242 0,5 µg/l
a
Aroclor 1221 1 µg/l
Campheclor 0,2 µg/l
a
Halowax 1014 1 µg/l
a
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
a
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).
3
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,
1)
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)
2)
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
10
C 50,18 3,97 500 500 500
10
C 55,00 4,79 500 500
10
C 60,09 5,86 1 000 900
10
C 65,02 7,16 500 300 2 000
10
C 45,50 3,63 1 200
11
C 50,21 4,37 2 600 2 500 500 700
11
C 55,20 5,31 1 000 2 000 1 300 400
11
C 60,53 6,55 1 900 1 200 2 500
11
C 65,25 7,94 2 500 3 200
11
C 45,32 3,93 1 000
12
C 50,18 4,76 2 400 2 500 500
12
C 55,00 5,74 1 500 2 500 2 000 1 000
12
C 65,08 8,59 200 1 500 1 700
12
C 69,98 10,62 3 100
12
C 44,90 4,19 500
13
C 50,23 5,16 1 800 1 000
13
C 55,03 6,22 1 000 400
13
C 59,98 7,56 400 1 300 700
13
C 65,18 9,34 100 1 700
13
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
2
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
10
C 50,18 50 50
10
C 55 50 100 100
10
C 60,09 50 90 150
10
C 65,02 50 20
10
C 45,5 200 200 100
11
C 50,21 280 50
11
C 55,2 150 250 200
11
C 60,53 150 200 140 350 120
11
C 65,25 300 200
11
C 45,32 150 100 100
12
C 50,18 150 50 50 240 50
12
C 55 250 100 200
12
C 65,08 100 200 100 20 170 150
12
C 69,98 50
12
C 44,9 50
13
C 50,23 100 50 180
13
C 55,03 100 100
13
C 59,98 50 100 40 70 170
13
C 65,18 100
13
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 ).
4
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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