ISO 13914:2023
Soil, treated biowaste and sludge — Determination of dioxins and furans and dioxin-like polychlorinated biphenyls by gas chromatography with high resolution mass selective detection (HR GC-MS)
This document specifies a method for quantitative determination of 17 2,3,7,8-chlorine substituted dibenzo-p-dioxins and dibenzofurans and dioxin-like polychlorinated biphenyls in sludge, treated biowaste and soil using liquid column chromatographic clean-up methods and GC/HRMS.
The analytes to be determined with this document are listed in Table 1.
The limit of detection depends on the kind of sample, the congener, the equipment used and the quality of chemicals used for extraction and clean-up. Under the conditions specified in this document, limits of detection better than 1 ng/kg (expressed as dry matter) can be achieved.
This method is “performance based”. The method can be modified if all performance criteria given in this method are met.
NOTE In principle, this method can also be applied for sediments, mineral wastes and for vegetation. It is the responsibility of the user of this document to validate the application for these matrices. For measurement in complex matrices like fly ashes adsorbed on vegetation, it can be necessary to further improve the clean-up. This can also apply to sediments and mineral wastes.
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Foreword
Introduction
1 Scope
2 Normative references
3 Terms and definitions
4 Abbreviated terms
5 Principle
6 Reagents
6.1 Chemicals
6.2 Standards
7 Apparatus and materials
7.1 Equipment for sample preparation
7.2 Soxhlet extractor
7.3 Clean-up apparatus
7.4 Concentration apparatus
7.5 Other equipment
8 Sample storage and sample pretreatment
8.1 Sample storage
8.2 Sample pretreatment
9 Extraction and clean-up
9.1 General
9.2 Extraction
9.3 Clean-up
9.3.1 General
9.3.2 Gel permeation chromatography
9.3.3 Multilayer column
9.3.4 Sulphuric acid treatment
9.3.5 Activated carbon column
9.3.6 Aluminium oxide column
9.3.7 Removal of sulphur
9.4 Final concentration of cleaned sample extract
9.5 Addition of recovery standard
10 HRGC/HRMS analysis
10.1 General
10.2 Gas chromatographic analysis
10.3 Mass spectrometric detection
10.4 Minimum requirements for identification of PCDF/PCDD and PCB
10.5 Minimum requirements for quantification of PCDF/PCDD and PCB
10.6 Calibration of the HRGC/HRMS system
10.6.1 General
10.6.2 Calibration for 2,3,7,8-congeners
10.6.3 Calibration for sum of homologue groups
10.7 Quantification of HRGC/HRMS results
10.7.1 Quantification of concentrations of 2,3,7,8-congeners
10.7.2 Quantification of recovery rates of 13C-labelled standards
10.7.3 Quantification of sum of homologue groups
10.7.4 Calculation of the toxic equivalent
10.7.5 Calculation of the limit of detection and the limit of quantification
11 Expression of results
12 Precision
13 Test report
Annex A (informative) Toxic equivalency factor (TEF)
Annex B (informative) Examples of extraction and clean-up methods
Annex C (informative) Examples of operation of GC/HRMS determination — Example
Annex D (informative) Repeatability and reproducibility data
Bibliography
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Foreword
Introduction
1 Scope
2 Normative references
3 Terms and definitions
4 Abbreviated terms
5 Principle
6 Reagents
6.1 Chemicals
6.2 Standards
7 Apparatus and materials
7.1 Equipment for sample preparation
7.2 Soxhlet extractor
7.3 Clean-up apparatus
7.4 Concentration apparatus
7.5 Other equipment
8 Sample storage and sample pretreatment
8.1 Sample storage
8.2 Sample pretreatment
9 Extraction and clean-up
9.1 General
9.2 Extraction
9.3 Clean-up
9.3.1 General
9.3.2 Gel permeation chromatography
9.3.3 Multilayer column
9.3.4 Sulphuric acid treatment
9.3.5 Activated carbon column
9.3.6 Aluminium oxide column
9.3.7 Removal of sulphur
9.4 Final concentration of cleaned sample extract
9.5 Addition of recovery standard
10 HRGC/HRMS analysis
10.1 General
10.2 Gas chromatographic analysis
10.3 Mass spectrometric detection
10.4 Minimum requirements for identification of PCDF/PCDD and PCB
10.5 Minimum requirements for quantification of PCDF/PCDD and PCB
10.6 Calibration of the HRGC/HRMS system
10.6.1 General
10.6.2 Calibration for 2,3,7,8-congeners
10.6.3 Calibration for sum of homologue groups
10.7 Quantification of HRGC/HRMS results
10.7.1 Quantification of concentrations of 2,3,7,8-congeners
10.7.2 Quantification of recovery rates of 13C-labelled standards
10.7.3 Quantification of sum of homologue groups
10.7.4 Calculation of the toxic equivalent
10.7.5 Calculation of the limit of detection and the limit of quantification
11 Expression of results
12 Precision
13 Test report
Annex A (informative) Toxic equivalency factor (TEF)
Annex B (informative) Examples of extraction and clean-up methods
Annex C (informative) Examples of operation of GC/HRMS determination — Example
Annex D (informative) Repeatability and reproducibility data
Bibliography