EN ISO 18475:2025
(Main)Environmental solid matrices - Determination of polychlorinated biphenyls (PCB) by gas chromatography - mass selective detection (GC-MS) or electron-capture detection (GC-ECD) (ISO 18475:2023)
Environmental solid matrices - Determination of polychlorinated biphenyls (PCB) by gas chromatography - mass selective detection (GC-MS) or electron-capture detection (GC-ECD) (ISO 18475:2023)
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).
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.
Feststoffe in der Umwelt - Bestimmung von polychlorierten Biphenylen (PCB) mittels Gaschromatographie und massenspektrometrischer Detektion (GC-MS) oder Elektronen-Einfang-Detektion (GC-ECD) (ISO 18475:2023)
Dieses Dokument legt Verfahren für die quantitative Bestimmung von sieben ausgewählten polychlorierten Biphenylen (PCB 28, PCB 52, PCB 101, PCB 118, PCB 138, PCB 153 und PCB 180) in Boden, Schlamm, Sediment, behandeltem Bioabfall und Abfall unter Anwendung der GC MS und GC ECD fest (siehe Tabelle 2).
Tabelle 2 — Zielanalyten dieses Dokumentes
Zielanalyt CAS-RNa
PCB 28 2,4,4’ Trichlorbiphenyl 7012–37–5
PCB 52 2,2’,5,5’ Tetrachlorbiphenyl 35693–99–3
PCB 101 2,2’,4,5,5’ Pentachlorbiphenyl 37680–73–2
PCB 118 2,3’,4,4’,5 Pentachlorbiphenyl 31508–00–6
PCB 138 2,2’,3,4,4’,5’ Hexachlorbiphenyl 35065–28–2
PCB 153 2,2’,4,4’,5,5’ Hexachlorbiphenyl 35065–27–1
PCB 180 2,2’,3,4,4’,5,5’ Heptachlorbiphenyl 35065–29–3
a CAS-RN Chemical Abstracts Service Registry Number.
Die Nachweisgrenze hängt von den zu bestimmenden Stoffen, den verwendeten Geräten, der Qualität der für die Extraktion der Probe verwendeten Chemikalien und der Reinigung des Extrakts ab.
Unter den in diesem Dokument festgelegten Bedingungen kann eine untere Anwendungsgrenze zwischen 1 µg/kg (angegeben als Trockenmasse) für Böden, Schlamm und Bioabfall und 10 µg/kg (angegeben als Trockenmasse) für Feststoffabfall erreicht werden. Bei einigen speziellen Proben kann die Grenze von 10 µg/kg nicht erreicht werden.
Schlamm, Abfall und behandelter Bioabfall können sich hinsichtlich ihrer Eigenschaften sowie hinsichtlich der erwarteten Kontaminationsniveaus von PCB und der Anwesenheit von störenden Stoffen unterscheiden. Aufgrund dieser Unterschiede ist es unmöglich, ein allgemeines Verfahren zu beschreiben. Dieses Dokument enthält Entscheidungstabellen, die auf den Eigenschaften der Probe und den anzuwendenden Extraktions- und Aufreinigungsverfahren basieren.
ANMERKUNG Für die Analyse von PCB in Isolierflüssigkeiten, Mineralölerzeugnissen, Gebrauchtölen und wässrigen Proben wird jeweils auf EN 61619, EN 12766 1 bzw. ISO 6468 verwiesen.
Das Verfahren kann für die Analyse weiterer, nicht im Anwendungsbereich festgelegter PCB Kongenere angewendet werden, vorausgesetzt, seine Eignung wurde durch geeignete laborinterne Validierungs-untersuchungen nachgewiesen.
Matrices solides environnementales - Dosage des polychlorobiphenyles (PCB) par chromatographie en phase gazeuse-spectrometrie de masse (CG-SM) ou chromatographie en phase gazeuse avec detection par capture d'electrons (CG-ECD) (ISO 18475:2023)
Le présent document spécifie les méthodes de dosage, par CG-SM et CG-ECD, de sept polychlorobiphényles choisis (PCB28, PCB52, PCB101, PCB118, PCB138, PCB153 et PCB180) dans les sols, les boues, les sédiments, les biodéchets traités et les déchets (voir Tableau 2).
La limite de détection dépend des composés à analyser, de l’équipement utilisé, de la qualité des réactifs chimiques utilisés pour l’extraction de l’échantillon et la purification de l’extrait.
Dans les conditions spécifiées dans le présent document, il est possible d’atteindre une limite inférieure d’application de 1 μg/kg (exprimée sur matière sèche) pour les sols, les boues et les biodéchets à 10 μg/kg (exprimée sur matière sèche) pour les déchets solides. Pour certains échantillons spécifiques, la limite de 10 μg/kg ne peut pas être atteinte.
Les boues, les déchets et les biodéchets traités peuvent présenter des différences en termes de propriétés, de niveaux prévus de contamination par les PCB et de présence de substances interférentes. En raison de ces différences, il est impossible de décrire un mode opératoire général. Le présent document contient des tables de décision basées sur les propriétés de l’échantillon ainsi que sur le mode opératoire d’extraction et de purification à utiliser.
NOTE Pour l’analyse des PCB dans les liquides isolants, les produits pétroliers, les huiles usagées et les échantillons aqueux, se référer respectivement aux normes EN 61619, EN 12766-1 et ISO 6468.
La méthode peut être appliquée à l’analyse de congénères de PCB autres que ceux décrits dans le domaine d’application, à condition d’en définir l’applicabilité par des tests de validation internes adaptés.
Trdni matriksi v okolju - Določanje polikloriranih bifenilov (PCB) s plinsko kromatografijo z masno selektivnim detektorjem (GC-MS) ali s plinsko kromatografijo z detektorjem z zajetjem elektronov (GC-ECD) (ISO 18475:2023)
Ta dokument določa metodo za kvantitativno določevanje sedmih izbranih polikloriranih bifenilov (PCB28, PCB52, PCB101, PCB118, PCB138, PCB153 in PCB180) v tleh, blatu, obdelanih bioloških odpadkih in odpadkih s plinsko kromatografijo z masno selektivnim detektorjem (GC-MS) ali s plinsko kromatografijo z detektorjem z zajetjem elektronov (glej preglednico 2). Meja detekcije je odvisna od determinant, uporabljene opreme, kakovosti kemikalij, uporabljenih za ekstrakcijo vzorca, in čiščenja izvlečka. Pod pogoji, določenimi v tem dokumentu, je mogoče doseči spodnjo mejo uporabe od 1 μg/kg (izraženo kot suha snov) za tla, blato in biološke odpadke do 10 μg/kg (izraženo kot suha snov) za trdne odpadke. Za nekatere specifične vzorce ni mogoče doseči meje 10 μg/kg. Blato, odpadki in obdelani biološki odpadki se lahko razlikujejo glede lastnosti, predvidenih stopenj onesnaženja s polikloriranimi bifenili (PCB) ter prisotnosti motečih snovi. Zaradi teh razlik ni možen opis enotnega splošnega postopka. Ta dokument vključuje preglednice za odločanje na podlagi lastnosti vzorca ter postopek za ekstrakcijo in očiščenje, ki ga je treba uporabiti. OPOMBA: V zvezi z analizo polikloriranih bifenilov v izolacijskih tekočinah, naftnih proizvodih, rabljenih oljih in vodnih vzorcih se standard sklicuje na standarde EN 61619, EN 12766-1 in ISO 6468. Metodo je mogoče uporabiti za analizo drugih analogov polikloriranih bifenilov, ki ne spadajo na področje uporabe tega standarda, če je ustreznost dokazana s primernimi internimi poskusi za validacijo.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-september-2025
Nadomešča:
SIST EN 17322:2020
Trdni matriksi v okolju - Določanje polikloriranih bifenilov (PCB) s plinsko
kromatografijo z masno selektivnim detektorjem (GC-MS) ali s plinsko
kromatografijo z detektorjem z zajetjem elektronov (GC-ECD) (ISO 18475:2023)
Environmental solid matrices - Determination of polychlorinated biphenyls (PCB) by gas
chromatography - mass selective detection (GC-MS) or electron-capture detection (GC-
ECD) (ISO 18475:2023)
Feststoffe in der Umwelt - Bestimmung von polychlorierten Biphenylen (PCB) mittels
Gaschromatographie und massenspektrometrischer Detektion (GC-MS) oder
Elektronen-Einfang-Detektion (GC-ECD) (ISO 18475:2023)
Matrices solides environnementales - Dosage des polychlorobiphenyles (PCB) par
chromatographie en phase gazeuse-spectrometrie de masse (CG-SM) ou
chromatographie en phase gazeuse avec detection par capture d'electrons (CG-ECD)
(ISO 18475:2023)
Ta slovenski standard je istoveten z: EN ISO 18475:2025
ICS:
13.030.10 Trdni odpadki Solid wastes
13.080.10 Kemijske značilnosti tal Chemical characteristics of
soils
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN ISO 18475
EUROPEAN STANDARD
NORME EUROPÉENNE
July 2025
EUROPÄISCHE NORM
ICS 13.080.10 Supersedes EN 17322:2020
English Version
Environmental solid matrices - Determination of
polychlorinated biphenyls (PCB) by gas chromatography -
mass selective detection (GC-MS) or electron-capture
detection (GC-ECD) (ISO 18475:2023)
Matrices solides environnementales - Dosage des Feststoffe in der Umwelt - Bestimmung von
polychlorobiphenyles (PCB) par chromatographie en polychlorierten Biphenylen (PCB) mittels
phase gazeuse-spectrometrie de masse (CG-SM) ou Gaschromatographie und massenspektrometrischer
chromatographie en phase gazeuse avec detection par Detektion (GC-MS) oder Elektronen-Einfang-Detektion
capture d'electrons (CG-ECD) (ISO 18475:2023) (GC-ECD) (ISO 18475:2023)
This European Standard was approved by CEN on 13 July 2025.
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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2025 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 18475:2025 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
European foreword
The text of ISO 18475:2023 has been prepared by Technical Committee ISO/TC 190 "Soil quality” of the
International Organization for Standardization (ISO) and has been taken over as EN ISO 18475:2025 by
Technical Committee CEN/TC 444 “Environmental characterization of solid matrices” the secretariat of
which is held by NEN.
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 January 2026, and conflicting national standards shall
be withdrawn at the latest by January 2026.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN 17322:2020.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
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, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the
United Kingdom.
Endorsement notice
The text of ISO 18475:2023 has been approved by CEN as EN ISO 18475:2025 without any modification.
INTERNATIONAL ISO
STANDARD 18475
First edition
2023-10
Environmental solid matrices —
Determination of polychlorinated
biphenyls (PCB) by gas
chromatography - mass selective
detection (GC-MS) or electron-capture
detection (GC-ECD)
Reference number
ISO 18475:2023(E)
ISO 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
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii
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
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
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
iv
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
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
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.
vii
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
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
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
C -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
C -labelled PCB or other PCB that are unlikely to be present in samples, added to the sample before
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)
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 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. The efficiency of the procedure depends on
the composition of the matrix that is investigated.
5 Interferences
5.1 Interference with sampling and extraction
Use sampling containers of materials (preferably of steel, aluminium or glass) that do not affect the
sample during the contact time. Avoid plastics and other organic materials during sampling, sample
storage or extraction. Keep the samples from direct sunlight and prolonged exposure to light.
During storage of the samples, losses of PCB may occur due to adsorption on the walls of the containers.
The extent of the losses depends on the storage time.
5.2 Interference with GC
Substances that co-elute with the target PCB may interfere with the determination. These interferences
may lead to incompletely resolved signals and may, depending on their magnitude, affect accuracy
and precision of the analytical results. Peak overlap does not allow an interpretation of the result.
Asymmetric peaks and peaks being broader than the corresponding peaks of the reference substance
suggest interferences.
Chromatographic separation between the following pairs can be critical.
— PCB28 – PCB31
— PCB52 – PCB73
— PCB101 – PCB89 / PCB90
— PCB118 – PCB106
— PCB138 – PCB164 / PCB163
The critical pair PCB28 and PCB31 is used for selection of the capillary column (see 8.2.2). If molecular
mass differences are present, quantification can be made by mass selective detection. If not or using
ECD, the specific PCB is reported as the sum of all PCBs present in the peak. Typically, the concentrations
of the co-eluting congeners compared to those of the target congeners are low. When incomplete
resolution is encountered, peak integration shall be checked and, when necessary, corrected.
Presence of tetrachlorobenzyltoluene (TCBT)-mixtures or sulfur can disturb the determination of the
PCB with GC-ECD.
High mineral oil content can also disturb the determination of PCB with GC-MS.
ISO 18475:2023(E)
6 Safety remarks
PCBs are highly toxic and shall be handled with extreme care. Avoid contact with solid materials,
solvent extracts and solutions of standard PCB. Contact of solutions of standard with the body should
be prevented. It is strongly advised that standard solutions are prepared centrally in suitably equipped
laboratories or are purchased from suppliers specialized in their preparation.
Solvent solutions containing PCB and samples shall be disposed of in a manner approved for disposal of
toxic wastes.
For the handling of hexane precautions shall be taken because of its neurotoxic properties.
National regulations enforcing locally stricter requirements are used with respect to all hazards
associated with this method.
7 Reagents
7.1 General
All reagents shall be of recognized analytical grade. The purity of the reagents used shall be checked by
running a blank test as described in 10.1 The blank shall be less than 50 % of the lowest reporting limit.
7.2 Reagents for extraction
7.2.1 Acetone (2-propanone), (CH ) CO.
3 2
7.2.2 n-heptane, C H .
7 16
7.2.3 Petroleum ether, boiling range 40 °C to 60 °C.
Hexane-like solvents with a boiling range between 30 °C and 98 °C are allowed.
7.2.4 Sodium sulfate, Na SO . The anhydrous sodium sulfate shall be kept carefully sealed.
2 4
7.2.5 Distilled water or water of equivalent quality, H O.
7.2.6 Sodium chloride, NaCl,
7.2.7 Keeper substance. High boiling compound, i.e. octane, nonane.
7.3 Reagents for clean-up
7.3.1 Clean-up A using aluminium oxide
7.3.1.1 Aluminium oxide, Al O
2 3
2 [13]
Basic or neutral, specific surface 200 m /g, activity Super I .
7.3.1.2 Deactivated aluminium oxide
Deactivated with approximately 10 % water.
ISO 18475:2023(E)
Add approximately 10 g of water (7.2.5) to 90 g of aluminium oxide (7.3.1.1). Shake until all lumps have
disappeared. Allow the aluminium oxide to condition before use for some 16 h, sealed from the air, use
it for maximum two weeks.
NOTE 1 The activity depends on the water content. It can be necessary to adjust the water content.
NOTE 2 Commercially available aluminium oxides with 10 % mass fraction water can also be used.
7.3.2 Clean-up B using silica gel 60 for column chromatography
7.3.2.1 Silica gel 60, particle size 63 µm to 200 µm.
7.3.2.2 Silica gel 60, water content: mass fraction w(H O) = 10 %.
Silica gel 60 (7.3.2.1), heated for at least 3 h at 450 °C, cooled down and stored in a desiccator containing
magnesium perchlorate or a suitable drying agent. Before use heat at least for 5 h at 130 °C in a drying
oven. Then allow cooling in a desiccator and add 10 % water (mass fraction) (7.2.5) in a flask. Shake for
5 min intensively by hand until all lumps have disappeared and then for 2 h in a shaking device. Store
the deactivated silica gel in the absence of air, use it for maximum of two weeks.
1)
7.3.3 Clean-up C using gel permeation chromatography (GPC)
®2)
7.3.3.1 Bio-Beads S-X3.
7.3.3.2 Ethyl acetate, C H O .
4 8 2
7.3.3.3 Cyclohexane, C H .
6 12 ®
Preparation of GPC, for example: put 50 g Bio-Beads S-X3 (7.3.3.1) into a 500 ml Erlenmeyer flask and
add 300 ml elution mixture made up of cyclohexane (7.3.3.3) and ethyl acetate (7.3.3.2) 1:1 (volume
fraction) in order to allow the beads to swell; after swirling for a short time until no lumps are left,
maintain the flask closed for 24 h. Drain the slurry into the chromatography tube for GPC. After
approximately three days, push in the plungers of the column so that a filling level of approximately 35 cm
is obtained. To further compress the gel, pump approximately 2 l of elution mixture through the column
-1
at a flow rate of 5 ml · min and push in the plungers to obtain a filling level of approximately 33 cm.
®3)
7.3.4 Clean-up D using Florisil ®
7.3.4.1 Florisil , baked 2 h at 600 °C. Particle size 150 µm to 750 µm.
7.3.4.2 Iso-octane, C H .
8 18
7.3.4.3 Toluene, C H .
7 8
7.3.4.4 Iso-octane/Toluene 95/5 volumetric fraction
1) GPC is also known as SEC (size exclusion chromatography). ®
2) Bio-Beads 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. Equivalent
products can be used if they can be shown to lead to the same results. ®
3) Florisil is a trade name for a prepared diatomaceous substance, mainly consisting of anhydrous magnesium
silicate. This information is given for the convenience of users of this document and does not constitute an
endorsement by ISO of this product. Equivalent products can be used if they can be shown to lead to the same
results.
ISO 18475:2023(E)
7.3.5 Clean-up E using silica H SO /silica NaOH
2 4
7.3.5.1 Silica, SiO , particle size 70 µm to 230 µm, baked at 180 °C for a minimum of 1 h, and stored in
a pre-cleaned glass bottle with screw cap that prevents moisture from entering.
7.3.5.2 Sulfuric acid H SO 95 – 97 % percent mass fraction
2 4
7.3.5.3 Silica, treated with sulfuric acid.
Mix 56 g silica (7.3.5.1) and 44 g sulfuric acid (7.3.5.2).
7.3.5.4 Sodium hydroxide solution, c(NaOH) = 1 mol/l.
7.3.5.5 Silica, treated with sodium hydroxide.
Mix 33 g silica (7.3.5.1) and 17 g sodium hydroxide (7.3.5.4).
7.3.5.6 n-hexane, C H
6 14
7.3.6 Clean-up F using benzenesulfonic acid/sulfuric acid
7.3.6.1 silica gel with particle size between 40 µm to 200 µm.
7.3.6.2 benzenesulfonic acid C H O S > 98 % percent mass fraction
6 6 3
Mix 500 mg of silica gel with sulfuric acid (7.3.5.2) or benzenesulfonic acid (7.3.6.2) and add it into a
3 ml column
7.3.7 Clean-up G using TBA sulfite reagent
7.3.7.1 Tetrabutylammonium reagent (TBA sulfite reagent) 97 % percent mass fraction
7.3.7.2 2-Propanol, C H O.
3 8
7.3.7.3 Sodium sulfite, Na SO > 98 % percent mass fraction
2 3
Saturate a solution of tetrabutylammonium hydrogen sulphate in a mixture of equal volume of water
and 2-propanol, c((C H ) NHSO ) = 0,1 mol/l, with sodium sulphite.
4 9 4 4
NOTE 25 g of sodium sulphite might be sufficient for 100 ml of solution.
7.3.8 Clean-up H using pyrogenic copper
WARNING — Pyrogenic copper is spontaneously inflammable. Suitable precautions shall be
taken.
7.3.8.1 Copper(II)-sulfate pentahydrate, CuSO · 5 H O.
4 2
7.3.8.2 Hydrochloric acid, c(HCl) = 2 mol/l.
7.3.8.3 Zinc granules, Zn, particle size 0,3 mm to 1,4 mm.
7.3.8.4 Anionic detergent aqueous solution (e.g. 35 g/100 ml, n-
...
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