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 \u03bcg\/kg (expressed as dry matter) for soils, sludge and biowaste to 100 \u03bcg\/kg (expressed as dry matter) for solid waste can be achieved. For some specific samples (e.g. bitumen) the limit of 100 \u03bcg\/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.<\/p>\n
| PDF Pages<\/th>\n | PDF Title<\/th>\n<\/tr>\n | ||||||
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| 2<\/td>\n | undefined <\/td>\n<\/tr>\n | ||||||
| 9<\/td>\n | 1 Scope <\/td>\n<\/tr>\n | ||||||
| 10<\/td>\n | 2 Normative references 3 Terms and definitions <\/td>\n<\/tr>\n | ||||||
| 12<\/td>\n | 4 Principle 5 Interferences 5.1 Interference with sampling and extraction 5.2 Interference with GC-MS <\/td>\n<\/tr>\n | ||||||
| 13<\/td>\n | 5.3 Interference with the HPLC 6 Safety remarks <\/td>\n<\/tr>\n | ||||||
| 14<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
| 15<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
| 16<\/td>\n | 7.5.3 Injection standard <\/td>\n<\/tr>\n | ||||||
| 17<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
| 18<\/td>\n | 7.6.6 Preparation of extraction standard solution for HPLC 8 Apparatus 8.1 Extraction and clean-up procedures <\/td>\n<\/tr>\n | ||||||
| 19<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
| 20<\/td>\n | 9.2 Sample pre-treatment 10 Procedure 10.1 Blank test 10.2 Extraction 10.2.1 General <\/td>\n<\/tr>\n | ||||||
| 22<\/td>\n | 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) <\/td>\n<\/tr>\n | ||||||
| 23<\/td>\n | 10.2.5 Extraction procedure 4: acetone\/hexane-like solvent\/sodium chloride and agitation 10.3 Concentration 10.3.1 General <\/td>\n<\/tr>\n | ||||||
| 24<\/td>\n | 10.3.2 For HPLC analysis 10.4 Clean-up of the extract 10.4.1 General 10.4.2 Clean-up A \u2013 Aluminium oxide <\/td>\n<\/tr>\n | ||||||
| 25<\/td>\n | 10.4.3 Clean-up B \u2013 Silica gel 10.4.4 Clean-up C \u2013 Gel permeation chromatography 10.5 Addition of the injection standard <\/td>\n<\/tr>\n | ||||||
| 26<\/td>\n | 10.6 GC-MS analysis 10.6.1 Settings of the gas chromatograph 10.6.2 Mass spectrometric (MS) conditions <\/td>\n<\/tr>\n | ||||||
| 27<\/td>\n | 10.6.3 Calibration of the method using an internal standard 10.6.3.1 General <\/td>\n<\/tr>\n | ||||||
| 28<\/td>\n | 10.6.3.2 Initial calibration 10.6.3.3 Calibration verification 10.6.4 Measurement <\/td>\n<\/tr>\n | ||||||
| 29<\/td>\n | 10.6.5 Identification 10.6.6 Check on method performance <\/td>\n<\/tr>\n | ||||||
| 30<\/td>\n | 10.6.7 Calculation 10.7 High-performance liquid chromatographic analysis (HPLC) 10.7.1 General 10.7.2 Setting the HPLC <\/td>\n<\/tr>\n | ||||||
| 31<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
| 32<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
| 33<\/td>\n | 10.7.6 Calculation 11 Performance characteristics 12 Precision <\/td>\n<\/tr>\n | ||||||
| 34<\/td>\n | 13 Test report <\/td>\n<\/tr>\n | ||||||
| 35<\/td>\n | Annex A (informative)Repeatability and reproducibility data A.1 Materials used in the interlaboratory comparison study <\/td>\n<\/tr>\n | ||||||
| 36<\/td>\n | A.2 Interlaboratory comparison results <\/td>\n<\/tr>\n | ||||||
| 43<\/td>\n | Annex B (informative)Examples of instrumental conditions and chromatograms B.1 Measurement of PAH with GC-MS <\/td>\n<\/tr>\n | ||||||
| 49<\/td>\n | B.2 Measurement of PAH with HPLC fluorescence <\/td>\n<\/tr>\n | ||||||
| 55<\/td>\n | B.3 Example for measurement conditions of PAH with GC-MS\/MS <\/td>\n<\/tr>\n<\/table>\n","protected":false},"excerpt":{"rendered":" Soil, sludge, treated biowaste and waste. Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid chromatography (HPLC)<\/b><\/p>\n |