This draft European Standard 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 European Standard 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 European Standard, limits of detection better than 1 ng\/kg (expressed as dry matter) can be achieved. This method is “performance based”. It is allowed to modify the method 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 European Standard 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.<\/p>\n
| PDF Pages<\/th>\n | PDF Title<\/th>\n<\/tr>\n | ||||||
|---|---|---|---|---|---|---|---|
| 2<\/td>\n | undefined <\/td>\n<\/tr>\n | ||||||
| 8<\/td>\n | 1 Scope <\/td>\n<\/tr>\n | ||||||
| 9<\/td>\n | 2 Normative references 3 Terms and definitions 4 Abbreviations <\/td>\n<\/tr>\n | ||||||
| 10<\/td>\n | 5 Principle 6 Reagents <\/td>\n<\/tr>\n | ||||||
| 11<\/td>\n | 7 Apparatus and materials <\/td>\n<\/tr>\n | ||||||
| 12<\/td>\n | 8 Sample storage and sample pretreatment 8.1 Sample storage 8.2 Sample pretreatment <\/td>\n<\/tr>\n | ||||||
| 13<\/td>\n | 9 Extraction and clean-up 9.1 General 9.2 Extraction <\/td>\n<\/tr>\n | ||||||
| 15<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
| 16<\/td>\n | 9.5 Addition of recovery standard 10 HRGC\/HRMS analysis 10.1 General <\/td>\n<\/tr>\n | ||||||
| 17<\/td>\n | 10.2 Gas chromatographic analysis 10.3 Mass spectrometric detection <\/td>\n<\/tr>\n | ||||||
| 18<\/td>\n | 10.4 Minimum requirements for identification of PCDF\/PCDD and PCB <\/td>\n<\/tr>\n | ||||||
| 19<\/td>\n | 10.5 Minimum requirements for quantification of PCDF\/PCDD and PCB <\/td>\n<\/tr>\n | ||||||
| 20<\/td>\n | 10.6 Calibration of the HRGC\/HRMS system 10.6.1 General 10.6.2 Calibration for 2,3,7,8-congeners <\/td>\n<\/tr>\n | ||||||
| 21<\/td>\n | 10.6.3 Calibration for sum of homologue groups <\/td>\n<\/tr>\n | ||||||
| 22<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
| 23<\/td>\n | 10.7.3 Quantification of sum of homologue groups 10.7.4 Calculation of the toxic equivalent <\/td>\n<\/tr>\n | ||||||
| 24<\/td>\n | 10.7.5 Calculation of the limit of detection and the limit of quantification 10.7.5.1 Calculation of the limit of detection 10.7.5.2 Calculation of the limit of quantification 11 Expression of results 12 Precision <\/td>\n<\/tr>\n | ||||||
| 25<\/td>\n | 13 Test report <\/td>\n<\/tr>\n | ||||||
| 26<\/td>\n | Annex A (informative)Toxic equivalency factor (TEF) <\/td>\n<\/tr>\n | ||||||
| 28<\/td>\n | Annex B (informative)Examples of extraction and clean-up methods B.1 Example A B.1.1 General B.1.2 Chemicals <\/td>\n<\/tr>\n | ||||||
| 29<\/td>\n | B.1.3 Procedure B.1.3.1 Spiking of the sample <\/td>\n<\/tr>\n | ||||||
| 30<\/td>\n | B.1.3.2 Extraction <\/td>\n<\/tr>\n | ||||||
| 31<\/td>\n | B.1.3.3 Clean-up <\/td>\n<\/tr>\n | ||||||
| 34<\/td>\n | B.1.3.4 Preparation of sample solution for measurement B.2 Example B: Approved clean-up methods <\/td>\n<\/tr>\n | ||||||
| 36<\/td>\n | Annex C (informative)Examples of operation of GC\/HRMS determination \u2014 Example C.1 General C.2 Gas chromatographic analysis <\/td>\n<\/tr>\n | ||||||
| 37<\/td>\n | C.3 Mass spectrometric detection <\/td>\n<\/tr>\n | ||||||
| 40<\/td>\n | Annex D (informative)Repeatability and reproducibility data D.1 Materials used in the interlaboratory comparison study D.2 Interlaboratory comparison results <\/td>\n<\/tr>\n | ||||||
| 45<\/td>\n | D.3 Calculation of toxicity factors on the basis of interlaboratory data <\/td>\n<\/tr>\n<\/table>\n","protected":false},"excerpt":{"rendered":" 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)<\/b><\/p>\n |