ISO 18475
(Main)Environmental solid matrices — Determination of polychlorinated biphenyls (PCB) by gas chromatography - mass selective detection (GC-MS) or electron-capture detection (GC-ECD)
Environmental solid matrices — Determination of polychlorinated biphenyls (PCB) by gas chromatography - mass selective detection (GC-MS) or electron-capture detection (GC-ECD)
This document specifies methods for quantitative determination of seven selected polychlorinated biphenyls (PCB28, PCB52, PCB101, PCB118, PCB138, PCB153 and PCB180) in soil, sludge, sediment, treated biowaste, and waste using GC-MS and GC-ECD (see Table 2).
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ISO/PRF 18475:2023(E)
ISO/TC 190/SC 3/WG 6
Secretariat: DIN
Date: 2023-07-0108-10
Environmental solid matrices — Determination of
polychlorinated biphenyls (PCB) by gas chromatography - mass
selective detection (GC-MS) or electron-capture detection (GC-
ECD)
FDIS stage
---------------------- Page: 1 ----------------------
ISO/DISPRF 18475:2023(E)
© ISO 2023
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: + 41 22 749 01 11
EmailE-mail: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii
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ISO/FDISPRF 18475:2023(E)
Contents
Foreword . vi
Introduction . viii
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Principle . 4
5 Interferences . 4
5.1 Interference with sampling and extraction . 4
5.2 Interference with GC . 5
6 Safety remarks . 5
7 Reagents . 6
7.1 General . 6
7.2 Reagents for extraction . 6
7.3 Reagents for clean-up . 6
7.3.1 Clean-up A using aluminium oxide . 6
7.3.2 Clean-up B using silica gel 60 for column chromatography . 6
7.3.3 Clean-up C using gel permeation chromatography (GPC) . 7
®
7.3.4 Clean-up D using Florisil . 7
7.3.5 Clean-up E using silica H SO /silica NaOH . 7
2 4
7.3.6 Clean-up F using benzenesulfonic acid/sulfuric acid . 8
7.3.7 Clean-up G using TBA sulfite reagent . 8
7.3.8 Clean-up H using pyrogenic copper . 8
7.3.9 Clean-up I using silica/silver nitrate . 9
7.4 Gas chromatographic analysis . 9
7.5 Standards . 9
7.5.1 General . 9
7.5.2 Calibration standards . 9
7.5.3 Internal and injection standards. 10
7.6 Preparation of standard solutions . 11
7.6.1 Preparation of calibration standard solutions of PCBs . 11
7.6.2 Preparation of internal standard solution . 11
7.6.3 Preparation of injection standard solution . 11
8 Apparatus . 12
8.1 Extraction and clean-up procedures . 12
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ISO/DISPRF 18475:2023(E)
8.2 Gas chromatograph . 13
9 Sample storage and preservation . 13
9.1 Sample storage . 13
9.2 Sample pre-treatment . 13
10 Procedure . 14
10.1 Blank test . 14
10.2 Extraction . 14
10.2.1 General . 14
10.2.2 Extraction procedure 1: Samples using acetone/petroleum ether or hexane-like solvent and
agitation or sonication . 16
10.2.3 Extraction procedure 2: Samples using Soxhlet or pressurized liquid extraction . 16
10.2.4 Extraction procedure 3: Samples using acetone/petroleum ether or hexane-like
solvent/sodium chloride and agitation . 17
10.3 Concentration . 17
10.4 Clean-up of the extract . 17
10.4.1 General . 17
10.4.2 Clean-up A – Aluminium oxide . 18
10.4.3 Clean-up B – Silica gel . 19
10.4.4 Clean-up C – Gel permeation chromatography . 19
®
10.4.5 Clean-up D – Florisil . 20
10.4.6 Clean-up E – Silica H SO /silica NaOH . 20
2 4
10.4.7 Clean-up F – Benzenesulfonic acid/sulfuric acid . 20
10.4.8 Clean-up G – TBA sulfite reagent . 20
10.4.9 Clean-up H – Clean-up using pyrogenic copper to remove elemental sulfur and some other
organic sulfur compounds . 20
10.4.10 Clean up I – AgNO /silica . 21
3
10.5 Addition of the injection standard . 21
10.6 Gas chromatographic analysis (GC) . 21
10.6.1 General . 21
10.6.2 Setting the gas chromatograph . 21
10.7 Mass spectrometry (MS) . 21
10.7.1 Mass spectrometric conditions . 21
10.7.2 Calibration of the method using an internal standard . 22
10.7.3 Measurement . 23
10.7.4 Identification . 24
10.7.5 Check on method performance . 24
10.7.6 Calculation . 25
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ISO/FDISPRF 18475:2023(E)
10.8 Electron capture detection (ECD) . 26
10.8.1 General . 26
10.8.2 ECD conditions . 26
10.8.3 Calibration of the method using internal standards . 26
10.8.4 Measurement . 26
10.8.5 Identification . 26
10.8.6 Check on ECD method performance. 27
10.8.7 Calculation . 28
11 Performance characteristics . 28
12 Precision . 28
13 Test report . 28
Annex A (informative) Repeatability and reproducibility data . 29
Annex B (informative) Examples for gas chromatographic conditions and retention times of PCBs . 35
Annex C (informative) Calculation method for the estimation of total PCB content . 36
Bibliography . 44
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ISO/DISPRF 18475:2023(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 documentsdocument 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).
Field Code Changed
Attention is drawnISO draws attention to the possibility that some of the elementsimplementation of this
document may beinvolve the subjectuse of (a) patent(s). ISO takes no position concerning the evidence,
validity or applicability of any claimed patent rights in respect thereof. As of the date of publication of
this document, ISO had not received notice of (a) patent(s) which may be required to implement this
document. However, implementers are cautioned that this may not represent the latest information,
which may be obtained from the patent database available at www.iso.org/patents. 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 ).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of 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
www.iso.org/iso/foreword.html.
This document was prepared by the European Committee for Standardization (CEN) (as EN 17322:2020)
and was adopted, without modification other than those given below, by Technical Committee ISO/TC
190, Soil quality, Subcommittee SC 3, Chemical and physical characterization.
— — change of EN ISO 5667-15 reference to ISO 5667-15 reference;
— — change of EN ISO 16720 reference to ISO 16720 reference;
— — change of EN ISO 22892 reference to ISO 22892 reference;
— — change of EN ISO 5667-13 reference to ISO 5667-13 reference;
— — change of EN ISO 6468 reference to ISO 6468 reference;
— — uniform spelling of sulfate and sulfite;
— — editorially revised.
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ISO/FDISPRF 18475:2023(E)
This first edition cancels and replaces ISO 10382:2002 and ISO 13876:2013, which have been technically
revised.
The main changes are as follows:
— — deletion of OCP analysis (this document specifies methods for quantitative determination of
polychlorinated biphenyls);
— — addition of GC-MS as a detection method;
— — extension of the scope to sludge, sediment, treated biowaste and waste;
— — addition of modern extraction techniques and commonly used methods with optimized
extraction time, proven clean-up methods and state of the art quantification methods;
— — update of normative references.
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.
© ISO 2023 – All rights reserved vii
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ISO/DISPRF 18475:2023(E)
Introduction
Polychlorinated biphenyls (PCB) have been widely used as additives in industrial applications where
chemical stability has been required. This stability on the other hand creates environmental problems
when PCB are eventually released into the environment. Since some of these PCB compounds are highly
toxic, their presence in the environment (air, water, soil, sediment and waste) is regularly monitored and
controlled. At present determination of PCB is carried out in these matrices in most of the routine
laboratories following the preceding steps for sampling, pre-treatment, extraction and clean-up, by
measurement of specific PCB by means of gas chromatography in combination with mass spectrometric
detection (GC-MS) or gas chromatography with electron capture detector (GC-ECD).
This document was developed by merging of EN 16167:2018, initially elaborated as a CEN Technical
Specification in the European project 'HORIZONTAL' and validated by CEN/TC 400 with the support of
BAM, with EN 15308, published by CEN/TC 292.
Considered the different matrices and possible interfering compounds, this document does not contain
one single possible way of working. Several choices are possible, in particular relating to clean-up.
Detection with both MS-detection and ECD-detection is possible. Two different extraction procedures are
described and 9 clean-up procedures. The use of internal and injection standards is described in order to
have an internal check on choice of the extraction and clean-up procedure. The method is as far as
possible in agreement with the method described for PAH (EN 16181:2018 and EN 15527:2008). It has
been tested for ruggedness.
This document is applicable and validated for several types of matrices as indicated in Table 1Table 1
(see also Annex AAnnex A for the results of the validation).
Table 1 — Matrices for which this document Standard is applicable and validated
Matrix Materials used for validation
Soil Sandy soil
Mix of soil from the vicinity of Berlin, Germany and PCB-free
German reference soil
Sludge Mix of municipal waste water treatment plant sludge from North
Rhine Westphalia, Germany
Biowaste Mix of compost from the vicinity of Berlin, Germany and sludge
from North Rhine Westphalia, Germany
Waste Contaminated soil, building debris, waste wood, sealant waste,
electronic waste, shredder light fraction, cable shredder waste
WARNING — Persons using this document should be familiar with usual 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 according to this document be carried out
by suitably trained staff.
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DRAFT INTERNATIONAL STANDARD ISO/DIS 18475:2022(E)
Environmental Solid Matrices solid matrices — Determination of
polychlorinated biphenyls (PCB) by gas chromatography -
Massmass selective detection (GC-MS) or electron-capture
detection (GC-ECD)
1 Scope
This document specifies methods for quantitative determination of seven selected polychlorinated
biphenyls (PCB28, PCB52, PCB101, PCB118, PCB138, PCB153 and PCB180) in soil, sludge, sediment,
treated biowaste, and waste using GC-MS and GC-ECD (see Table 2Table 2).).
Table 2 — Target analytes of this document
a
Target analyte CAS-RN
PCB28 2,4,4'-trichlorobiphenyl 7012–37–5
PCB52 2,2',5,5'-tetrachlorobiphenyl 35693–99–3
PCB101 2,2',4,5,5'-pentachlorobiphenyl 37680–73–2
PCB118 2,3',4,4',5-pentachlorobiphenyl 31508–00–6
PCB138 2,2',3,4,4',5'-hexachlorobiphenyl 35065–28–2
PCB153 2,2',4,4',5,5'-hexachlorobiphenyl 35065–27–1
PCB180 2,2',3,4,4',5,5'-heptachlorobiphenyl 35065–29–3
a
CAS-RN Chemical Abstracts Service Registry Number.
The limit of detection depends on the determinants, the equipment used, the quality of chemicals used
for the extraction of the sample and the clean-up of the extract.
Under the conditions specified in this document, lower limit of application from 1 μg/kg (expressed as
dry matter) for soils, sludge and biowaste to 10 μg/kg (expressed as dry matter) for solid waste can be
achieved. For some specific samples the limit of 10 μg/kg cannot be reached.
Sludge, waste and treated biowaste may differ in properties, as well as in the expected contamination
levels of PCB and presence of interfering substances. These differences make it impossible to describe
one general procedure. This document contains decision tables based on the properties of the sample and
the extraction and clean-up procedure to be used.
NOTE The analysis of PCB in insulating liquids, petroleum products, used oils and aqueous samples is referred
to in EN 61619, EN 12766-1 and ISO 6468 respectively.
The method can be applied to the analysis of other PCB congeners not specified in the scope, provided
suitability is proven by proper in-house validation experiments.
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.
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ISO/DISPRF 18475:20222023(E)
ISO 5667--15, Water quality — Sampling — Part 15: Guidance on the preservation and handling of sludge
and sediment samples
ISO 8466--1, Water quality — Calibration and evaluation of analytical methods — Part 1: Linear
calibration function
ISO 16720, Soil quality — Pretreatment of samples by freeze-drying for subsequent analysis
ISO 18512, Soil quality — Guidance on long and short term storage of soil samples
ISO 22892, Soil quality — Guidelines for the identification of target compounds by gas chromatography and
mass spectrometry
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— — ISO Online browsing platform: available at https://www.iso.org/obp
— — IEC Electropedia: available at https://www.electropedia.org/
3.1
critical pair
pair of congeners that shall be separated to a predefined degree (e.g. R = 0,5) to ensure chromatographic
separation meets minimum quality criteria
𝛥𝛥𝛥𝛥
= 2× (𝑥𝑥) (1)
𝑌𝑌𝑌𝑌+𝑌𝑌𝑌𝑌
where
R resolution
Δt difference in retention times of the two peaks a and b in seconds (s)
Y peak width at the base of peak a in seconds (s)
a
Y peak width at the base of peak b in seconds (s)
b
2
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ISO/DISPRF 18475:20222023(E)
Figure 1 — Example of a chromatogram of a critical pair
3.2
congener
member of the same kind, class or group of chemicals, e.g. anyone of the two hundred and nine individual
PCB
Note 1 to entry: The IUPAC congener numbers are for easy identification; they do not represent the order of
chromatographic elution.
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ISO/DISPRF 18475:20222023(E)
3.3
injection standard
13
C12-labelled PCB or other PCB that is unlikely to be present in samples, added to the sample extract
before injection into the gas chromatograph, to monitor variability of instrument response and the
recovery of the internal standards
3.4
internal standard
13
C -labelled PCB or other PCB that are unlikely to be present in samples, added to the sample before
12
extraction and used for quantification of PCB content
3.5
polychlorinated biphenyl
PCB
biphenyl substituted with one to ten chlorine atoms
3.6
sediment
solid material, both mineral and organic, deposited in the bottom of a water body
[SOURCE: ISO 5667--12:2017]
4 Principle
Due to the multi-matrix character of this document, different procedures for different steps (modules)
are allowed. Which modules should be used depends on the sample. A recommendation is given in this
document. Performance criteria are described and it is the responsibility of the laboratories applying this
document to show that these criteria are met. Using of spiking standards (internal standards) allows an
overall check on the efficiency of a specific combination of modules for a specific sample. But it does not
necessarily give the information regarding the extensive extraction efficiency of the native PCB bonded
to the matrix.
After pre-treatment, the sample is extracted with a suitable solvent.
The extract is concentrated by evaporation. If necessary, interfering compounds are removed by a clean-
up method suitable for the specific matrix, before the concentration step.
The extract is analysed by gas chromatography. The various compounds are separated using a capillary
column with a stationary phase of low polarity. Detection occurs by mass spectrometry (MS) or an
electron capture detector (ECD).
PCB are identified and quantified by comparison of relative retention times and relative peak heights (or
peak areas) with respect to internal standards added.
...
INTERNATIONAL ISO
STANDARD 18475
First edition
Environmental solid matrices —
Determination of polychlorinated
biphenyls (PCB) by gas
chromatography - mass selective
detection (GC-MS) or electron-capture
detection (GC-ECD)
PROOF/ÉPREUVE
Reference number
ISO 18475:2023(E)
© ISO 2023
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ISO 18475:2023(E)
INTERNATIONAL ISO
STANDARD 18475
Second edition
Environmental solid matrices —
Determination of polychlorinated
biphenyls (PCB) by gas
chromatography - mass selective
detection (GC-MS) or electron-capture
detection (GC-ECD)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2023
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.
PROOF/ÉPREUVE
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Reference number
Email: copyright@iso.org
ISO 18475:2023(E)
Website: www.iso.org
Published in Switzerland
ii
PROOF/ÉPREUVE © ISO 2023 – All rights reserved
© ISO 2023
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ISO 18475:2023(E)
Contents Page
Foreword .v
Introduction .vii
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Principle . 3
5 Interferences . 4
5.1 Interference with sampling and extraction . 4
5.2 Interference with GC . 4
6 Safety remarks . 5
7 Reagents . 5
7.1 General . 5
7.2 Reagents for extraction . 5
7.3 Reagents for clean-up . 5
7.3.1 Clean-up A using aluminium oxide. 5
7.3.2 Clean-up B using silica gel 60 for column chromatography . 6
7.3.3 Clean-up C using gel permeation chromatography (GPC) . 6
®
7.3.4 Clean-up D using Florisil . 6
7.3.5 Clean-up E using silica H SO /silica NaOH . 7
2 4
7.3.6 Clean-up F using benzenesulfonic acid/sulfuric acid . 7
7.3.7 Clean-up G using TBA sulfite reagent . 7
7.3.8 Clean-up H using pyrogenic copper . 7
7.3.9 Clean-up I using silica/silver nitrate . 8
7.4 Gas chromatographic analysis . 8
7.5 Standards . 9
7.5.1 General . 9
7.5.2 Calibration standards . 9
7.5.3 Internal and injection standards . 9
7.6 Preparation of standard solutions . 10
7.6.1 Preparation of calibration standard solutions of PCBs . 10
7.6.2 Preparation of internal standard solution . 11
7.6.3 Preparation of injection standard solution . 11
8 Apparatus .11
8.1 Extraction and clean-up procedures . 11
8.2 Gas chromatograph .12
9 Sample storage and preservation .12
9.1 Sample storage .12
9.2 Sample pre-treatment . 13
10 Procedure .13
10.1 Blank test .13
10.2 Extraction . 13
10.2.1 General .13
10.2.2 Extraction procedure 1: Samples using acetone/petroleum ether or
hexane-like solvent and agitation or sonication . 14
10.2.3 Extraction procedure 2: Samples using Soxhlet or pressurized liquid
extraction. 15
10.2.4 Extraction procedure 3: Samples using acetone/petroleum ether or
hexane-like solvent/sodium chloride and agitation .15
10.3 Concentration . 16
10.4 Clean-up of the extract . 16
iii
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ISO 18475:2023(E)
10.4.1 General . 16
10.4.2 Clean-up A – Aluminium oxide . 17
10.4.3 Clean-up B – Silica gel. 17
10.4.4 Clean-up C – Gel permeation chromatography. 17
®
10.4.5 Clean-up D – Florisil . 18
10.4.6 Clean-up E – Silica H SO /silica NaOH . 18
2 4
10.4.7 Clean-up F – Benzenesulfonic acid/sulfuric acid . 18
10.4.8 Clean-up G – TBA sulfite reagent . 19
10.4.9 Clean-up H – Clean-up using pyrogenic copper to remove elemental sulfur
and some other organic sulfur compounds . 19
10.4.10 Clean up I – AgNO /silica . 19
3
10.5 Addition of the injection standard . 19
10.6 Gas chromatographic analysis (GC) . 19
10.6.1 General . 19
10.6.2 Setting the gas chromatograph . 19
10.7 Mass spectrometry (MS) . 20
10.7.1 Mass spectrometric conditions . 20
10.7.2 Calibration of the method using an internal standard .20
10.7.3 Measurement . 21
10.7.4 Identification .22
10.7.5 Check on method performance . 22
10.7.6 Calculation .23
10.8 Electron capture detection (ECD) . 24
10.8.1 General . 24
10.8.2 ECD conditions . 24
10.8.3 Calibration of the method using internal standards . 24
10.8.4 Measurement . 24
10.8.5 Identification . 24
10.8.6 Check on ECD method performance . 24
10.8.7 Calculation . 25
11 Performance characteristics .25
12 Precision .25
13 Test report .26
Annex A (informative) Repeatability and reproducibility data .27
Annex B (informative) Examples for gas chromatographic conditions and retention times
of PCBs .32
Annex C (informative) Calculation method for the estimation of total PCB content .33
Bibliography .40
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ISO 18475:2023(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 document 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).
ISO draws attention to the possibility that the implementation of this document may involve the use
of (a) patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed
patent rights in respect thereof. As of the date of publication of this document, ISO had not received
notice of (a) patent(s) which may be required to implement this document. However, implementers are
cautioned that this may not represent the latest information, which may be obtained from the patent
database available at www.iso.org/patents. ISO shall not be held responsible for identifying any or all
such patent rights.
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of 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
www.iso.org/iso/foreword.html.
This document was prepared by the European Committee for Standardization (CEN) (as EN 17322:2020)
and was adopted, without modification other than those given below, by Technical Committee
ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical and physical characterization.
— change of EN ISO 5667-15 reference to ISO 5667-15 reference;
— change of EN ISO 16720 reference to ISO 16720 reference;
— change of EN ISO 22892 reference to ISO 22892 reference;
— change of EN ISO 5667-13 reference to ISO 5667-13 reference;
— change of EN ISO 6468 reference to ISO 6468 reference;
— uniform spelling of sulfate and sulfite;
— editorially revised.
This first edition cancels and replaces ISO 10382:2002 and ISO 13876:2013, which have been technically
revised.
The main changes are as follows:
— deletion of OCP analysis (this document specifies methods for quantitative determination of
polychlorinated biphenyls);
— addition of GC-MS as a detection method;
— extension of the scope to sludge, sediment, treated biowaste and waste;
v
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ISO 18475:2023(E)
— addition of modern extraction techniques and commonly used methods with optimized extraction
time, proven clean-up methods and state of the art quantification methods;
— update of normative references.
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.
vi
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ISO 18475:2023(E)
Introduction
Polychlorinated biphenyls (PCB) have been widely used as additives in industrial applications where
chemical stability has been required. This stability on the other hand creates environmental problems
when PCB are eventually released into the environment. Since some of these PCB compounds are highly
toxic, their presence in the environment (air, water, soil, sediment and waste) is regularly monitored
and controlled. At present determination of PCB is carried out in these matrices in most of the routine
laboratories following the preceding steps for sampling, pre-treatment, extraction and clean-up, by
measurement of specific PCB by means of gas chromatography in combination with mass spectrometric
detection (GC-MS) or gas chromatography with electron capture detector (GC-ECD).
This document was developed by merging of EN 16167:2018, initially elaborated as a CEN Technical
Specification in the European project 'HORIZONTAL' and validated by CEN/TC 400 with the support of
BAM, with EN 15308, published by CEN/TC 292.
Considered the different matrices and possible interfering compounds, this document does not contain
one single possible way of working. Several choices are possible, in particular relating to clean-up.
Detection with both MS-detection and ECD-detection is possible. Two different extraction procedures
are described and 9 clean-up procedures. The use of internal and injection standards is described in
order to have an internal check on choice of the extraction and clean-up procedure. The method is as far
as possible in agreement with the method described for PAH (EN 16181:2018 and EN 15527:2008). It
has been tested for ruggedness.
This document is applicable and validated for several types of matrices as indicated in Table 1 (see also
Annex A for the results of the validation).
Table 1 — Matrices for which this document is applicable and validated
Matrix Materials used for validation
Soil Sandy soil
Mix of soil from the vicinity of Berlin, Germany and PCB-free Ger-
man reference soil
Sludge Mix of municipal waste water treatment plant sludge from North
Rhine Westphalia, Germany
Biowaste Mix of compost from the vicinity of Berlin, Germany and sludge
from North Rhine Westphalia, Germany
Waste Contaminated soil, building debris, waste wood, sealant waste,
electronic waste, shredder light fraction, cable shredder waste
WARNING — Persons using this document should be familiar with usual 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 according to this document be carried
out by suitably trained staff.
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INTERNATIONAL STANDARD ISO 18475:2023(E)
Environmental solid matrices — Determination of
polychlorinated biphenyls (PCB) by gas chromatography
- mass selective detection (GC-MS) or electron-capture
detection (GC-ECD)
1 Scope
This document specifies methods for quantitative determination of seven selected polychlorinated
biphenyls (PCB28, PCB52, PCB101, PCB118, PCB138, PCB153 and PCB180) in soil, sludge, sediment,
treated biowaste, and waste using GC-MS and GC-ECD (see Table 2).
Table 2 — Target analytes of this document
a
Target analyte CAS-RN
PCB28 2,4,4'-trichlorobiphenyl 7012–37–5
PCB52 2,2',5,5'-tetrachlorobiphenyl 35693–99–3
PCB101 2,2',4,5,5'-pentachlorobiphenyl 37680–73–2
PCB118 2,3',4,4',5-pentachlorobiphenyl 31508–00–6
PCB138 2,2',3,4,4',5'-hexachlorobiphenyl 35065–28–2
PCB153 2,2',4,4',5,5'-hexachlorobiphenyl 35065–27–1
PCB180 2,2',3,4,4',5,5'-heptachlorobiphenyl 35065–29–3
a
CAS-RN Chemical Abstracts Service Registry Number.
The limit of detection depends on the determinants, the equipment used, the quality of chemicals used
for the extraction of the sample and the clean-up of the extract.
Under the conditions specified in this document, lower limit of application from 1 μg/kg (expressed as
dry matter) for soils, sludge and biowaste to 10 μg/kg (expressed as dry matter) for solid waste can be
achieved. For some specific samples the limit of 10 μg/kg cannot be reached.
Sludge, waste and treated biowaste may differ in properties, as well as in the expected contamination
levels of PCB and presence of interfering substances. These differences make it impossible to describe
one general procedure. This document contains decision tables based on the properties of the sample
and the extraction and clean-up procedure to be used.
NOTE The analysis of PCB in insulating liquids, petroleum products, used oils and aqueous samples is
referred to in EN 61619, EN 12766-1 and ISO 6468 respectively.
The method can be applied to the analysis of other PCB congeners not specified in the scope, provided
suitability is proven by proper in-house validation experiments.
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 5667-15, Water quality — Sampling — Part 15: Guidance on the preservation and handling of sludge
and sediment samples
1
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ISO 18475:2023(E)
ISO 8466-1, Water quality — Calibration and evaluation of analytical methods — Part 1: Linear calibration
function
ISO 16720, Soil quality — Pretreatment of samples by freeze-drying for subsequent analysis
ISO 18512, Soil quality — Guidance on long and short term storage of soil samples
ISO 22892, Soil quality — Guidelines for the identification of target compounds by gas chromatography and
mass spectrometry
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
3.1
critical pair
pair of congeners that shall be separated to a predefined degree (e.g. R = 0,5) to ensure chromatographic
separation meets minimum quality criteria
Δ t
R =×2 ()x (1)
Ya +Yb
where
R resolution
Δt difference in retention times of the two peaks a and b in seconds (s)
Y peak width at the base of peak a in seconds (s)
a
Y peak width at the base of peak b in seconds (s)
b
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ISO 18475:2023(E)
Figure 1 — Example of a chromatogram of a critical pair
3.2
congener
member of the same kind, class or group of chemicals, e.g. anyone of the two hundred and nine individual
PCB
Note 1 to entry: The IUPAC congener numbers are for easy identification; they do not represent the order of
chromatographic elution.
3.3
injection standard
13
C -labelled PCB or other PCB that is unlikely to be present in samples, added to the sample extract
12
before injection into the gas chromatograph, to monitor variability of instrument response and the
recovery of the internal standards
3.4
internal standard
13
C -labelled PCB or other PCB that are unlikely to be present in samples, added to the sample before
12
extraction and used for quantification of PCB content
3.5
polychlorinated biphenyl
PCB
biphenyl substituted with one to ten chlorine atoms
3.6
sediment
solid material, both mineral and organic, deposited in the bottom of a water body
[SOURCE: ISO 5667-12:2017]
4 Principle
Due to the multi-matrix character of this document, different procedures for different steps (modules)
are allowed. Which modules should be used depends on the sample. A recommendation is given in this
document. Performance criteria are described and it is the responsibility of the laboratories applying
this document to show that these criteria are met. Using of spiking standards (internal standards)
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ISO 18475:2023(E)
allows an overall check on the efficiency of a specific combination of modules for a specific sample. But
it does not necessarily give the information regarding the extensive extraction efficiency of the native
PCB bonded to the matrix.
After pre-treatment, the sample is extracted with a suitable solvent.
The extract is concentrated by evaporation. If necessary, interfering compounds are removed by a
clean-up method suitable for the specific matrix, before the concentration step.
The extract is analysed by gas chromatography. The various compo
...
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