Analytical method for the determination of 2,3,7,8-substituted polychlorinated dibenzodioxins (PCDDs) and dibenzofurans (PCDFs)
Translation of DGUV Information 213-547 (former BGI 505-47 or ZH1/120.47)
CAS Number: 1746-01-6 (2,3,7,8-Tetrachlorodibenzodioxine)
Method 03 – GC/HRMS
Sampling with a pump, collection on a filter and adsorption on polyether urethan foam, gas chromatography after desorption by extraction and purification of the extract, detection by high-resolution mass spectrometry.
This method permits the determination of 2,3,7,8-substituted polychlorinated dibenzodioxin and dibenzofuran (PCDD/PCDF) concentrations in working areas averaged over the sampling time.
Principle
With a pump a measured air volume is drawn through an integrated collection system consisting of sampling inlet and glass-fibre deep bed filter followed by a section of toluene diisocyanate (TDI)-based polyether urethan foam (PUR foam). The inhalable fraction of particulate or particle-bound PCDDs/PCDFs is drawn in and collected on the filter or the fraction which passes the filter is adsorbed by the foam. Extraction is carried out with toluene in a Soxhlet extractor. The extracted PCDDs/PCDFs are separated from interfering components by a combination of preparation steps and then concentrated. The components of the purified extracts are separated by gas chromatography and the PCDDs/PCDFs are selectively determined using high-resolution mass spectrometry (HRMS). Sampling, sample preparation and analytical determination are checked by means of isotope labelled PCDD/PCDF standards (isotope-dilution method). Quantitative evaluation is carried out using these internal standards. The analytical results are expressed in toxicity equivalents (TEs) taking into account toxicity equivalent factors (TEFs).
Limit of quantification (LOQ)
Absolute: 0.3 pg TCDD/TCDF, PeCDDs/PeCDFs, HxCDDs/HxCDFs, 1 pg HpCDDs/HpCDFs and 3 pg OCDD/OCDF.
Relative: 0.15 pg/m3 TCDD/TCDF, PeCDDs/PeCDFs, HxCDDs/HxCDFs, 0.5 pg/m3 HpCDDs/HpCDFs and 1.5 pg/m3 OCDD/OCDF for an air sample volume of 20 m3, 30 µL sample solution and 3 µL injection volume.
Issue
July 1997
The complete measuring method is available in the Wiley Online Library: Method for the determination of 2,3,7,8-substituted polychlorinated dibenzodioxins (PCDDs) and dibenzofurans (PCDFs) (Analyses of Hazardous Substances in Air, Volume 5, 2002).
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