ISO 18475:2023
(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). 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.
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)
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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 2023
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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
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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 .
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