Development and validation of a method for analyzing polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans in sewage sludge samples

Autor: L. Comellas, R. Martí, L. Molina, M. C. Rodriguez-Larena, J. Díaz-Ferrero, F. Broto-Puig
Rok vydání: 2000
Předmět:
Zdroj: Chromatographia. 52:87-92
ISSN: 1612-1112
0009-5893
DOI: 10.1007/bf02490798
Popis: A method has been developed for the analysis of polychlorinated dibenzo-p-dioxins (PCDD) and dibenzofurans (PCDF) in sewage sludge samples. It was found that PCDD/F are best Soxhlet extracted from the matrix with toluene for 24h, after having tested other solvents (dichloromethane and hexane/acetone 41/59) and other extraction times. Several clean up steps (sulfuric acid, multilayer silica and Florisl columns) and concentration are required prior to analysis of the extract by high resolution gas chromatography-high resolution mass spectrometry (HRGC-HRMS). The complete procedure has been validated and the accuracy and precision data (repeatability and reproducibility) are given. The method is linear in the range studied and the limit of detection ranges between 0.2 and 2.2 pg g−1 of dry matter for the 2,3,7,8-substituted congeners. Moreover, the suitability of the method has been checked in an international interlaboratory comparison. The successful application of this method to several samples from Catalan and Dutch urban wastewater treatment plants was demonstrated.
Databáze: OpenAIRE
Externí odkaz: