SIST EN ISO 18635:2017
(Main)Water quality - Determination of short-chain polychlorinated alkanes (SCCPs) in sediment, sewage sludge and suspended (particulate) matter - Method using gas chromatography-mass spectrometry (GC-MS) and electron capture negative ionization (ECNI) (ISO 18635:2016)
Water quality - Determination of short-chain polychlorinated alkanes (SCCPs) in sediment, sewage sludge and suspended (particulate) matter - Method using gas chromatography-mass spectrometry (GC-MS) and electron capture negative ionization (ECNI) (ISO 18635:2016)
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-C10 to n-C13 inclusive, in mixtures with chlorine mass fractions ("contents") between 50 % and 67 %, including approximately 6 000 of approximately 8 000 congeners.
This method is applicable to the determination of the sum of SCCPs in sediment and suspended, particulate matter and soil using gas chromatography mass spectrometry with electron capture negative ionization (GC ECNI MS).
Depending on the detection capabilities of the GC ECNI MS the method can be applied to samples containing e.g. 0,03 µg/g to 1 µg/g sum of SCCPs.
Wasserbeschaffenheit - Bestimmung kurzkettiger polychlorierter Alkane (SCCP) in Sediment, Klärschlamm und Schwebstoff - Gaschromatographisch-massenspektrometrisches Verfahren (GC-MS) unter Anwendung negativer chemischer Ionisation und Elektroneneinfang (ECNI) (ISO 18635:2016)
Diese Internationale Norm legt ein Verfahren zur quantitativen Bestimmung der Summe von kurzkettigen polychlorierten n-Alkanen fest. Diese werden auch als kurzkettige polychlorierte Paraffine (SCCP, en: short-chain polychlorinated paraffins) bezeichnet und haben Kohlenstoffkettenlängen von n-C10 bis einschließlich n-C13 in Gemischen mit Chlor-Massenanteilen („Gehalten“) zwischen 50 % und 67 %, die ungefähr 6 000 der etwa 8 000 Kongenere umfassen.
Dieses Verfahren ist anwendbar auf die Bestimmung der Summe von SCCP in Sediment, Schwebstoff, Klärschlamm und Boden mittels Gaschromatographie-Massenspektrometrie mit Elektroneneinfang nach negativer chemischer Ionisation (GC-ECNI-MS).
Abhängig von der Matrix und der Nachweisempfindlichkeit der GC-ECNI-MS kann das Verfahren auf Proben mit einer SCCP-Gesamtkonzentration von z. B. 0,03 µg/g bis 3 µg/g angewendet werden.
Qualité de l'eau - Détermination des alcanes polychlorés à chaîne courte dans les sédiments et matières en supsension (particules) - Méthode par chromatographie en phase gazeuse-spectrométrie de masse (CPG-SM) et ionisation chimique négative (ICN) (ISO 18635:2016)
L'ISO 18635:2016 spécifie une méthode de détermination quantitative de la somme de n-alcanes polychlorés à chaîne courte, également connus sous le nom de paraffines polychlorées à chaîne courte (SCCP), ayant une chaîne carbonée comprise entre n-C10 et n-C13 inclus, dans des mélanges dont la fraction massique («teneur») de chlore varie de 50 % et 67 %, englobant approximativement 6 000 des 8 000 congénères environ.
La présente méthode est applicable à la détermination de la somme des SCCP dans les sédiments et les matières en suspension (particules), les boues d'épuration et le sol, par chromatographie en phase gazeuse-spectrométrie de masse en mode d'ionisation négative par capture d'électrons (CG-INCE-SM).
Selon la matrice et les capabilités de détection de la CG-INCE-SM, la méthode peut être appliquée aux échantillons contenant, par exemple, de 0,03 µg/g à 3 µg/g de la somme des SCCP.
Kakovost vode - Določevanje polikloriranih alkanov s kratko verigo (SCCP) v sedimentu, blatu odpadnih vod in suspendiranih delcih - Metoda plinske kromatografije/masne spektrometrije (GC/MS) z negativno ionizacijo in zajemom elektronov (ECNI) (ISO 18635:2016)
Ta mednarodni standard določa metodo za kvantitativno določevanje vsote polikloriranih alkanov s kratko verigo (SCCP), znanih tudi kot poliklorirani parafini s kratko verigo, v razponu ogljikovih vezi n-C10 do vključno n-C13, v zmeseh z masnimi deleži klora (»vsebnost«) med 50 in 67 %, vključno s približno 6000 od približno 8000 analogov. Ta metoda se uporablja za določevanje vsote polikloriranih alkanov s kratko verigo v sedimentu ter suspendiranih delcih in zemlji z uporabo plinske kromatografije/masne spektrometrije (GC/MS) in negativno kemijsko ionizacijo z zajetjem elektronov (GC ECNI MS). Metodo je mogoče uporabiti za vzorce z vsoto polikloriranih alkanov npr. od 0,03 µg/g do 1 µg/g, odvisno od detekcijskih sposobnosti GC ECNI MS.
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 18635:2017
01-junij-2017
.DNRYRVWYRGH'RORþHYDQMHSROLNORULUDQLKDONDQRYVNUDWNRYHULJR 6&&3 Y
VHGLPHQWXEODWXRGSDGQLKYRGLQVXVSHQGLUDQLKGHOFLK0HWRGDSOLQVNH
NURPDWRJUDILMHPDVQHVSHNWURPHWULMH *&06 ]QHJDWLYQRLRQL]DFLMRLQ]DMHPRP
HOHNWURQRY (&1, ,62
Water quality - Determination of short-chain polychlorinated alkanes (SCCPs) in
sediment, sewage sludge and suspended (particulate) matter - Method using gas
chromatography-mass spectrometry (GC-MS) and electron capture negative ionization
(ECNI) (ISO 18635:2016)
Wasserbeschaffenheit - Bestimmung kurzkettiger polychlorierter Alkane (SCCP) in
Sediment, Klärschlamm und Schwebstoff - Gaschromatographisch-
massenspektrometrisches Verfahren (GC-MS) unter Anwendung negativer chemischer
Ionisation und Elektroneneinfang (ECNI) (ISO 18635:2016)
Qualité de l'eau - Détermination des alcanes polychlorés à chaîne courte dans les
sédiments et matières en supsension (particules) - Méthode par chromatographie en
phase gazeuse-spectrométrie de masse (CPG-SM) et ionisation chimique négative (ICN)
(ISO 18635:2016)
Ta slovenski standard je istoveten z: EN ISO 18635:2016
ICS:
13.060.50 3UHLVNDYDYRGHQDNHPLþQH Examination of water for
VQRYL chemical substances
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
SIST EN ISO 18635:2017 en,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 18635:2017
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SIST EN ISO 18635:2017
EN ISO 18635
EUROPEAN STANDARD
NORME EUROPÉENNE
April 2016
EUROPÄISCHE NORM
ICS 13.060.50
English Version
Water quality - Determination of short-chain
polychlorinated alkanes (SCCPs) in sediment, sewage
sludge and suspended (particulate) matter - Method using
gas chromatography-mass spectrometry (GC-MS) and
electron capture negative ionization (ECNI) (ISO
18635:2016)
Qualité de l'eau - Détermination des alcanes Wasserbeschaffenheit - Bestimmung kurzkettiger
polychlorés à chaîne courte dans les sédiments et polychlorierter Alkane (SCCP) in Sediment,
matières en supsension (particules) - Méthode par Klärschlamm und Schwebstoffen -
chromatographie en phase gazeuse-spectrométrie de Gaschromatographisch-massenspektrometrisches
masse (CPG-SM) et ionisation chimique négative (ICN) Verfahren (GC-MS) unter Anwendung negativer
(ISO 18635:2016) chemischer Ionisation und Elektroneneinfang (ECNI)
(ISO 18635:2016)
This European Standard was approved by CEN on 20 February 2016.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2016 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 18635:2016 E
worldwide for CEN national Members.
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SIST EN ISO 18635:2017
EN ISO 18635:2016 (E)
Contents Page
European foreword . 3
2
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SIST EN ISO 18635:2017
EN ISO 18635:2016 (E)
European foreword
This document (EN ISO 18635:2016) has been prepared by Technical Committee ISO/TC 147 “Water
quality” in collaboration with Technical Committee CEN/TC 230 “Water analysis” the secretariat of
which is held by DIN.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by October 2016, and conflicting national standards shall
be withdrawn at the latest by October 2016.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent
rights.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Endorsement notice
The text of ISO 18635:2016 has been approved by CEN as EN ISO 18635:2016 without any modification.
3
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SIST EN ISO 18635:2017
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SIST EN ISO 18635:2017
INTERNATIONAL ISO
STANDARD 18635
First edition
2016-04-01
Water quality — Determination
of short-chain polychlorinated
alkanes (SCCPs) in sediment, sewage
sludge and suspended (particulate)
matter — Method using gas
chromatography-mass spectrometry
(GC-MS) and electron capture
negative ionization (ECNI)
Qualité de l’eau — Détermination des alcanes polychlorés à chaîne
courte dans les sédiments et matières en supsension (particules) —
Méthode par chromatographie en phase gazeuse-spectrométrie de
masse (CPG-SM) et ionisation chimique négative (ICN)
Reference number
ISO 18635:2016(E)
©
ISO 2016
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SIST EN ISO 18635:2017
ISO 18635:2016(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2016, Published in Switzerland
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
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copyright@iso.org
www.iso.org
ii © ISO 2016 – All rights reserved
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SIST EN ISO 18635:2017
ISO 18635:2016(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Principle . 1
4 Interferences . 2
5 Reagents . 3
6 Apparatus . 6
7 Sampling and sample pretreatment . 7
8 Procedure. 7
8.1 Extraction . 7
8.2 Extract clean-up . 7
8.3 Measurement and integration of the chromatogram. 8
8.4 Calibration . 8
8.4.1 General. 8
8.4.2 Basic calibration . 9
8.4.3 Identification and quantification with mass fragment combinations .10
8.4.4 Calculation of the results .10
8.4.5 Quality checks for internal standardization .11
9 Expression of results .11
10 Test report .11
Annex A (normative) Programme for pressurized liquid extraction .12
Annex B (informative) Explanation of the calibration of the sum of SCCPs with multiple
linear regression .13
Annex C (informative) Examples of typical GC-MS conditions .18
Annex D (normative) Alternative clean-up with column chromatography .22
Annex E (informative) Alternative clean-up with gel chromatography .24
Annex F (informative) Typical chromatograms of standard solutions 1 µg/ml .25
Annex G (informative) Presentation of goodness of fit of the calibration .26
Annex H (informative) Example for recoveries of quality assurance solutions .27
Annex I (informative) Chromatograms of real samples.29
Annex J (informative) Performance data .31
Annex K (informative) Quality control check solutions .32
Bibliography .33
© ISO 2016 – All rights reserved iii
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SIST EN ISO 18635:2017
ISO 18635:2016(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical
Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information
The committee responsible for this document is ISO/TC 147, Water quality, Subcommittee SC 2, Physical,
chemical and biochemical methods.
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SIST EN ISO 18635:2017
ISO 18635:2016(E)
Introduction
The user should be aware that particular problems might require the specifications of additional
marginal conditions.
© ISO 2016 – All rights reserved v
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SIST EN ISO 18635:2017
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SIST EN ISO 18635:2017
INTERNATIONAL STANDARD ISO 18635:2016(E)
Water quality — Determination of short-chain
polychlorinated alkanes (SCCPs) in sediment, sewage
sludge and suspended (particulate) matter — Method
using gas chromatography-mass spectrometry (GC-MS) and
electron capture negative ionization (ECNI)
WARNING — Persons using this document should be familiar with normal laboratory practice.
This document does not purport to address all of the safety problems, if any, associated with its
use. It is the responsibility of the user to establish appropriate safety and health practices and to
ensure compliance with any national regulatory conditions.
IMPORTANT — It is absolutely essential that tests conducted in accordance with this document
be carried out by suitably qualified staff.
1 Scope
This International Standard specifies a method for the quantitative determination of the sum of short-
chain polychlorinated n-alkanes also known as short-chain polychlorinated paraffins (SCCPs) in the
carbon bond range, n-C to n-C , inclusive in mixtures with chlorine mass fractions (“contents“)
10 13
between 50 % and 67 %, including approximately 6 000 of approximately 8 000 congeners.
This method is applicable to the determination of the sum of SCCPs in sediment and suspended
(particulate) matter, sewage sludge, and soil using gas chromatography-mass spectrometry with
electron capture negative ionization (GC-ECNI-MS).
Depending on matrix and the detection capabilities of the GC-ECNI-MS, the method can be applied to
samples containing, e.g. 0,03 µg/g to 3 µg/g sum of SCCPs.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 5667-12, Water quality — Sampling — Part 12: Guidance on sampling of bottom sediments
ISO 5667-13, Water quality — Sampling — Part 13: Guidance on sampling of sludges
ISO 5667-17, Water quality — Sampling — Part 17: Guidance on sampling of bulk suspended solids
ISO 8466-1, Water quality — Calibration and evaluation of analytical methods and estimation of
performance characteristics — Part 1: Statistical evaluation of the linear calibration function
ISO 12010, Water quality — Determination of short-chain polychlorinated alkanes (SCCPs) in water —
Method using gas chromatography-mass spectrometry (GC-MS) and negative-ion chemical ionization (NCI)
ISO/TS 13530, Water quality — Guidance on analytical quality control for chemical and physicochemical
water analysis
3 Principle
Determination of the sum of SCCPs in the carbon bond range, n-C to n-C , inclusive in technical and
10 13
environmental transposed mixtures with chlorine mass fractions (“contents“) between 50 % and 67 %
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SIST EN ISO 18635:2017
ISO 18635:2016(E)
(e.g. approximately 3 to 10 chlorine atoms per molecule) and independent of the C-number distribution
pattern of the congeners. No recognition of the chlorine content is necessary.
The samples are fortified with an internal standard and extracted using pressurized liquid extraction
with an organic solvent. The sample extraction procedure is followed by a clean-up procedure by
column chromatography and gel permeation chromatography to eliminate interfering compounds. Gas
chromatography (GC) is undertaken using a short capillary column within a short retention time range.
The detection of selected mass fragments is carried out using mass spectrometry (MS) in selected ion-
monitoring mode using electron capture negative ionization mode (ECNI). The mass fragments and
the compositions of the calibration solutions used in this International Standard are essential for the
analysis of the sum of SCCPs.
The selected ion chromatogram is integrated over the full retention time range of the SCCPs. The
quantification of the sum of SCCPs is carried out after establishing a calibration by a multiple linear
regression measuring solutions of different SCCP mixtures fortified with an internal standard.
The analysed sum of SCCPs includes the variety of SCCPs with their differing chlorine content and
C-number distribution patterns as found in technical mixtures, as well as compositions in the
environment. The calibration requires at least three differently composed standard mixtures.
These standard mixtures mimic different mixtures found in the environment. Only the multiple linear
regression quantification with these specific mixtures enables the quantification of the variety of
observed mixtures of SCCP in the environment and in technical compositions described in the scope
and in Reference [6]. It is not possible to use only one standard mixture for that complex task.
4 Interferences
Non-specific matrix interferences, as well as interferences from other environmental situations, are
dealt with using the given clean-up procedure. A further reduction of matrix effects can be achieved by
reducing the mass spectrometric resolution to, e.g., 0,4 amu, which is often possible with a quadrupole
mass spectrometer. The exact masses are 374,9588; 410,9169; and 422,9355 (see Reference [6]).
Applying the entire procedure, a selection of chlorinated pollutants has been tested and found not to
cause interferences below the concentrations given in Table 1.
Table 1 — Highest concentration level which causes no interferences higher than the limit of
quantification of 0,03 µg/g
Potential interfering compounds Highest concentration level which causes
no interferences higher than the limit of
quantification of 0,03 µg/g
a
Aroclor 1262 0,25 µg/g
a
Aroclor 1242 2 µg/g
a
Aroclor 1221 2 µg/g
Campheclor (toxaphene) 0,35 µg/g
a
Halowax 1014 2 µg/g
a
Halowax 1051 0,08 µg/g
MCCP (medium-chain chlorinated n-alkanes) 42 % 2 µg/g
MCCP (medium-chain chlorinated n-alkanes) 52 % 1,2 µg/g
MCCP (medium-chain chlorinated n-alkanes) 57 % 2 µg/g
a
Aroclor 1262, Aroclor 1242, Aroclor 1221, Halowax 1014, and Halowax 1051 are products commercially available. This
information is given for the convenience of users of this document and does not constitute an endorsement by ISO of these
products.
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SIST EN ISO 18635:2017
ISO 18635:2016(E)
5 Reagents
Use solvents and reagents of sufficient purity, i.e. with negligibly low concentrations of SCCPs, e.g. lower
than the limit of detection of the method.
Check blanks regularly over the entire procedure to establish proper analytical quality control.
5.1 Solvents for extraction, column chromatography, and preparation of stock solutions.
The solvent for extraction is n-heptane. Other non-polar solvents, e.g. n-hexane (C H ), cyclohexane
6 14
(C H ) can be used if the extraction efficiency is comparable with those of n-heptane.
6 12
For conditioning of the clean-up columns, use mixtures of n-heptane and propanone (acetone) as
described below.
5.2 Reference SCCP stock solutions.
Use commercially available solutions, e.g. in cyclohexane or n-hexane, of the single mixtures of SCCP
congeners with defined carbon chain length and with different defined chlorine contents (see Table 2,
first two columns). Alternatively, use commercially available ready mixed solutions with the same
composition.
Mixtures of synthetic solutions are used to simulate environmentally occurring SCCPs or technical
products of SCCPs. For example, the synthetic mixed calibration stock solution “Lake Ontario water” is
mixed to resemble a Lake Ontario water as reported in Reference [5]. Its characteristic is a relatively
high content of C to C , especially C and a low chlorine content as partly reported in water samples
10 12 12
too. The synthetic mixed calibration stock solution “Perch” simulates a C-number distribution found
in a perch (see Reference [6]). The standard mixture “Sediment Drevnice” simulates a natural mixture
reported about a sediment of the river Drevnice (see Reference [7]) with a high content of C and a
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. An example for recoveries
of quality assurance solutions is given in Annex H.
Prepare the solutions “Lake Ontario water”, “Perch”, and “Sediment Drevnice” according to Table 2.
Table 2 — Reference substances stock solutions
Standard solutions, e.g. in n-heptane Synthetic mixed standard solutions
which resemble environmental
mixtures
n-alkane Chlorine Mean “Lake “Perch” “Sediment
chain content (%) number Ontario Drevnice”
length of the of chlorines water”
individual in the
C-number molecules
mixtures (calculated)
Chlorine content calculated (%) 50,2 60,6 65,0
Composition, ng/ml
C 44,82 3,22
10
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
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SIST EN ISO 18635:2017
ISO 18635:2016(E)
Table 2 (continued)
Standard solutions, e.g. in n-heptane Synthetic mixed standard solutions
which resemble environmental
mixtures
n-alkane Chlorine Mean “Lake “Perch” “Sediment
chain content (%) number Ontario Drevnice”
length of the of chlorines water”
individual in the
C-number molecules
mixtures (calculated)
Chlorine content calculated (%) 50,2 60,6 65,0
Composition, ng/ml
C 55,20 5,31 600
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 44,90 4,19
13
C 50,23 5,16
13
C 55,03 6,22
13
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
The chlorine content (third column) of the mixtures is calculated as the weighted mean.
Store the prepared solutions in a refrigerator at 2 °C to 6 °C.
5.3 Internal standard stock solutions from individual congeners.
Use commercially available individual congener standard solutions and prepare a stock solution in
propanone (acetone) (5.1) at a concentration of, for example, 1 µg/ml.
— Individual SCCP congeners with chlorine contents of between 50 % and 67 % are suitable as internal
standards if the mass trace in mass spectrometric detection is not affected by matrix components,
e.g. 1,1,1,3,11,13,13,13-octachlorotridecane at e.g. 0,1 µg/ml.
NOTE 1 The different individual SCCP congeners used as internal standard substances probably contribute in
environmental samples to the sum of SCCPs. Nevertheless, the contribution is approximately <1 % which means
that the enhancement of the measurement uncertainty is negligible.
NOTE 2 Different individual SCCP congeners can produce different response factors, hence, it can be necessary
for different concentrations to be used.
The solutions should be stored in a refrigerator at 2 °C to 6 °C.
5.4 Calibration solutions.
Use the standard mixtures according to Table 2. Prepare a minimum of nine calibration solutions (see
Table 3) with concentrations according to the detection capability of the mass spectrometer. Combine
and dilute the solutions (5.2) and the internal standard stock solution (5.3) with n-heptane to produce
solutions for the calibration range, e.g. as shown in Table 3.
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SIST EN ISO 18635:2017
ISO 18635:2016(E)
Table 3 — Calibration solutions
Mixture “Lake “Perch” “Sediment Internal standard
Ontario” Drevnice”
water
1,1,1,3,11,13,13,13-octachlorotridecane
µg/ml µg/ml µg/ml µg/ml
Sum of SCCPs,
µg/ml
0,15 0,15 0,1
0,15 0,15 0,1
0,15 0,15 0,1
0,6 0,6 0,1
0,6 0,6 0,1
0,6 0,6 0,1
1 1 0,1
1 1 0,1
1 1 0,1
2 2 0,1
2 2 0,1
2 2 0,1
3 3 0,1
3 3 0,1
3 3 0,1
The solutions can be stored in a refrigerator, for at least four weeks. Check the concentration of the
calibration solutions against an independently prepared standard prior to use.
Quality control check solutions can be prepared to check the calibration independently. For that, use the
calibration mixtures as given in ISO 12010 (see Annex K). These mixtures are commercially available
(e.g. in cyclohexane or n-hexane).
5.5 Extraction auxiliary and clean-up materials.
5.5.1 High purity silica sand, grain size 600 µm to 850 µm, blank free from contamination.
5.5.2 Copper powder, grain size <63 µm.
5.5.3 2 mol/l hydrochloric acid.
5.5.4 Al O , neutral, high activity, (10 % water).
2 3
5.5.5 Glass wool.
5.6 Operating gases, for GC-MS of high purity and in accordance with manufacturer’s specifications.
5.7 Nitrogen, N , purity ≥99,996 % volume fraction for concentrating the solutions.
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5.8 Sodium sulfate, anhydrous, Na SO , powdered.
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© ISO 2016 – All rights reserved 5
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SIST EN ISO 18635:2017
ISO 18635:2016(E)
6 Apparatus
Clean all glassware by rinsing with acetone (propanone) (5.1).
6.1 Wide-necked bottle, 1 000 ml up to 5 000 ml capacity for wet sediment or sludge.
6.2 Freeze drying apparatus.
6.3 Deep freezer.
6.4 Mortar and pestle or a grinding mill.
6.5 Drying ovens, capable of maintaining temperatures in the ranges of 100 °C to 400 °C for baking
and storage of clean-up materials, for baking of glassware, an
...
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