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BS EN 17503:2022:2023 Edition

BS EN 17503:2022:2023 Edition

$198.66

Soil, sludge, treated biowaste and waste. Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid chromatography (HPLC)

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BSI 2023 58
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This document specifies different methods for quantitative determination of 16 polycyclic aromatic hydrocarbons (PAH) (see Table 2) in soil, sludge, treated biowaste, and waste, using GC-MS or HPLC-UV-DAD/FLD covering a wide range of PAH contamination levels (see Table 2). NOTE The method can be applied to sediments provided that validity is demonstrated by the user. When using fluorescence detection, acenaphthylene cannot be measured. [Table 2 -Target analytes of this document] 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, the lower limit of application from 10 μg/kg (expressed as dry matter) for soils, sludge and biowaste to 100 μg/kg (expressed as dry matter) for solid waste can be achieved. For some specific samples (e.g. bitumen) the limit of 100 μg/kg cannot be reached. Sludge, waste and treated biowaste can differ in properties as well as in the expected contamination levels of PAH 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. The method can be applied to the analysis of other PAH not specified in the scope, provided suitability is proven by proper in-house validation experiments. Sampling is not part of this standard. In dependence of the materials, the following standards need to be considered, e.g. EN 14899, ISO 5667-12 and EN ISO 5667-13.

PDF Catalog

PDF Pages PDF Title
2 undefined
9 1 Scope
10 2 Normative references
3 Terms and definitions
12 4 Principle
5 Interferences
5.1 Interference with sampling and extraction
5.2 Interference with GC-MS
13 5.3 Interference with the HPLC
6 Safety remarks
14 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
7.3.2 Clean-up B using silica gel 60 for column chromatography
15 7.3.3 Clean-up C using gel permeation chromatography (GPC)
7.4 Reagents for chromatographic analysis
7.4.1 GC-Analysis
7.4.2 HPLC-analysis
7.5 Standards
7.5.1 General
7.5.2 Calibration substances and internal standards
16 7.5.3 Injection standard
17 7.6 Preparation of standard solutions
7.6.1 General
7.6.2 Preparation of calibration standard solutions for GC-MS
7.6.3 Preparation of internal standard solution for GC-MS
7.6.4 Preparation of injection standard solution for GC-MS
7.6.5 Preparation of calibration standard solutions for HPLC
18 7.6.6 Preparation of extraction standard solution for HPLC
8 Apparatus
8.1 Extraction and clean-up procedures
19 8.2 Gas chromatograph
8.2.1 General
8.2.2 Capillary columns
8.3 High-performance liquid chromatograph
8.3.1 General
8.3.2 Analytical separation column
9 Sample storage and preservation
9.1 Sample storage
20 9.2 Sample pre-treatment
10 Procedure
10.1 Blank test
10.2 Extraction
10.2.1 General
22 10.2.2 Extraction procedure 1: acetone/hexane-like solvent and agitation or sonication
10.2.3 Extraction procedure 2: Soxhlet extraction
10.2.4 Extraction procedure 3: Pressurized liquid extraction (PLE)
23 10.2.5 Extraction procedure 4: acetone/hexane-like solvent/sodium chloride and agitation
10.3 Concentration
10.3.1 General
24 10.3.2 For HPLC analysis
10.4 Clean-up of the extract
10.4.1 General
10.4.2 Clean-up A – Aluminium oxide
25 10.4.3 Clean-up B – Silica gel
10.4.4 Clean-up C – Gel permeation chromatography
10.5 Addition of the injection standard
26 10.6 GC-MS analysis
10.6.1 Settings of the gas chromatograph
10.6.2 Mass spectrometric (MS) conditions
27 10.6.3 Calibration of the method using an internal standard
10.6.3.1 General
28 10.6.3.2 Initial calibration
10.6.3.3 Calibration verification
10.6.4 Measurement
29 10.6.5 Identification
10.6.6 Check on method performance
30 10.6.7 Calculation
10.7 High-performance liquid chromatographic analysis (HPLC)
10.7.1 General
10.7.2 Setting the HPLC
31 10.7.3 Detection
10.7.3.1 General
10.7.3.2 Ultraviolet detector
10.7.3.3 Fluorescence detector
10.7.3.4 Identification of individual compounds
32 10.7.4 Calibration
10.7.4.1 General
10.7.4.2 Initial calibration
10.7.4.3 Calibration verification
10.7.5 Measurement
33 10.7.6 Calculation
11 Performance characteristics
12 Precision
34 13 Test report
35 Annex A (informative)Repeatability and reproducibility data
A.1 Materials used in the interlaboratory comparison study
36 A.2 Interlaboratory comparison results
43 Annex B (informative)Examples of instrumental conditions and chromatograms
B.1 Measurement of PAH with GC-MS
49 B.2 Measurement of PAH with HPLC fluorescence
55 B.3 Example for measurement conditions of PAH with GC-MS/MS

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BS EN 17503:2022
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