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BS ISO 18475:2023

$198.66

Environmental solid matrices. Determination of polychlorinated biphenyls (PCB) by gas chromatography. mass selective detection (GC-MS) or electron-capture detection (GC-ECD)

Published By Publication Date Number of Pages
BSI 2023 52
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PDF Catalog

PDF Pages PDF Title
2 undefined
7 Foreword
9 Introduction
11 1 Scope
2 Normative references
12 3 Terms and definitions
13 4 Principle
14 5 Interferences
5.1 Interference with sampling and extraction
5.2 Interference with GC
15 6 Safety remarks
7 Reagents
7.1 General
7.2 Reagents for extraction
7.3 Reagents for clean-up
7.3.1 Clean-up A using aluminium oxide
16 7.3.2 Clean-up B using silica gel 60 for column chromatography
7.3.3 Clean-up C using gel permeation chromatography (GPC)
7.3.4 Clean-up D using Florisil®
17 7.3.5 Clean-up E using silica H2SO4/silica NaOH
7.3.6 Clean-up F using benzenesulfonic acid/sulfuric acid
7.3.7 Clean-up G using TBA sulfite reagent
7.3.8 Clean-up H using pyrogenic copper
18 7.3.9 Clean-up I using silica/silver nitrate
7.4 Gas chromatographic analysis
19 7.5 Standards
7.5.1 General
7.5.2 Calibration standards
7.5.3 Internal and injection standards
20 7.6 Preparation of standard solutions
7.6.1 Preparation of calibration standard solutions of PCBs
21 7.6.2 Preparation of internal standard solution
7.6.3 Preparation of injection standard solution
8 Apparatus
8.1 Extraction and clean-up procedures
22 8.2 Gas chromatograph
9 Sample storage and preservation
9.1 Sample storage
23 9.2 Sample pre-treatment
10 Procedure
10.1 Blank test
10.2 Extraction
10.2.1 General
24 10.2.2 Extraction procedure 1: Samples using acetone/petroleum ether or hexane-like solvent and agitation or sonication
25 10.2.3 Extraction procedure 2: Samples using Soxhlet or pressurized liquid extraction
10.2.4 Extraction procedure 3: Samples using acetone/petroleum ether or hexane-like solvent/sodium chloride and agitation
26 10.3 Concentration
10.4 Clean-up of the extract
10.4.1 General
27 10.4.2 Clean-up A – Aluminium oxide
10.4.3 Clean-up B – Silica gel
10.4.4 Clean-up C – Gel permeation chromatography
28 10.4.5 Clean-up D – Florisil®
10.4.6 Clean-up E – Silica H2SO4/silica NaOH
10.4.7 Clean-up F – Benzenesulfonic acid/sulfuric acid
29 10.4.8 Clean-up G – TBA sulfite reagent
10.4.9 Clean-up H – Clean-up using pyrogenic copper to remove elemental sulfur and some other organic sulfur compounds
10.4.10 Clean up I – AgNO3/silica
10.5 Addition of the injection standard
10.6 Gas chromatographic analysis (GC)
10.6.1 General
10.6.2 Setting the gas chromatograph
30 10.7 Mass spectrometry (MS)
10.7.1 Mass spectrometric conditions
10.7.2 Calibration of the method using an internal standard
31 10.7.3 Measurement
32 10.7.4 Identification
10.7.5 Check on method performance
33 10.7.6 Calculation
34 10.8 Electron capture detection (ECD)
10.8.1 General
10.8.2 ECD conditions
10.8.3 Calibration of the method using internal standards
10.8.4 Measurement
10.8.5 Identification
10.8.6 Check on ECD method performance
35 10.8.7 Calculation
11 Performance characteristics
12 Precision
36 13 Test report
37 Annex A (informative) Repeatability and reproducibility data
42 Annex B (informative) Examples for gas chromatographic conditions and retention times of PCBs
43 Annex C (informative) Calculation method for the estimation of total PCB content
50 Bibliography
BS ISO 18475:2023
$198.66