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  • Title: Uncertainty assessment of polychlorinated dibenzo-p-dioxins and dibenzofuran and dioxin-like polychlorinated biphenyl analysis in stationary source sample emissions in accordance with the impending European standard EN-1948 using fly ashes.
    Author: Martínez K, Rivera-Austrui J, Adrados MA, Abalos M, Llerena JJ, van Bavel B, Rivera J, Abad E.
    Journal: J Chromatogr A; 2009 Jul 31; 1216(31):5888-94. PubMed ID: 19560773.
    Abstract:
    The analysis of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) and dioxin-like polychlorinated biphenyls (dl-PCBs) present in stack gas emissions and solid residues from incinerators will be mandatory in the foreseeable future. European standard EN-1948 is in the process of being updated through the addition of a new Part 4 related to the analysis of the 12 dl-PCBs. Therefore, either a comprehensive and reliable method capable of analyzing all of these 29 compounds (12 dl-PCBs and 17 2,3,7,8-PCDD/Fs) needs to be developed, or the existing PCDD/F analytical procedure must be adapted to include the dl-PCBs. This study has taken the latter approach of modifying PCDD/F methodology and in particular the fractionation step, by isolating dioxins and dl-PCBs into separate fractions ready for high resolution gas chromatography coupled to high resolution mass spectrometry (HRGC/HRMS) analysis. Results obtained from the analysis of Certified Reference Materials (CRM-490 and CRM-615) and fly ashes from the European Committee for Standardization (CEN) intercalibration study demonstrated that the proposed methodology is appropriate to determine the dl-PCBs in accordance with the impending European standard EN-1948. Uncertainty values obtained during the validation of the analytical methodology were 13% total I-TEQ (International Toxic Equivalent) for PCDD/Fs and 31% total WHO-TEQ (World Health Organization Toxic Equivalent) in the case of dl-PCBs. In addition, 'real' samples such as emissions and fly ashes were successfully analyzed following the proposed analytical method.
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