prEN ISO 18475

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)

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)

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)

General Information

• Status: Not Published
• Publication Date: 21-Apr-2027
• ICS: 13.080.10 - Chemical characteristics of soils
• Technical Committee: CEN/TC 444 - Environmental characterization
• Drafting Committee: CEN/TC 444/WG 2 - Organic analysis
• Current Stage: 4010 - Start of draft translation - Enquiry
• Start Date: 20-Jan-2025
• Due Date: 20-Jan-2025
• Completion Date: 20-Jan-2025
• Ref Project: oSIST prEN ISO 18475:2025 - 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)

Relations

• Revises: EN 17322:2020 - Environmental Solid Matrices - Determination of polychlorinated biphenyls (PCB) by gas chromatography - mass selective detection (GC-MS) or electron-capture detection (GC-ECD)
• Effective Date: 11-Dec-2024

Standards Content (Sample)

SLOVENSKI STANDARD
01-april-2025
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)
Ta slovenski standard je istoveten z: prEN ISO 18475
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.

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
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or ISO’s member body in the country of the requester.
ISO copyright office
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Phone: [phone]
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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 d
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