EPA Method 1613 Tetra- through Octa-Chlorinated Dioxins and Furans by Dilution HRGC_HRMS
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1EBA337C8E374F2A8302BEA3FC1C8B2D |
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0.41 |
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89 |
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日期： |
2008-2-26 |
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Method 1613,Tetra- through Octa-Chlorinated Dioxins and Furans by Isotope,Dilution HRGC/HRMS,October 1994,U.S. Environmental Protection Agency,Office of Water,Engineering and Analysis Division (4303),401 M Street S.W.,Washington, D.C. 20460,Acknowledgments,This method was prepared under the direction of William A. Telliard of the Engineering and,Analysis Division within the EPA Office of Water. This document was prepared under EPA,Contract No. 68-C3-0337 by DynCorp Environmental Services Division with assistance from,its subcontractor Interface, Inc.,Disclaimer,This method has been reviewed by the Engineering and Analysis Division, U.S.,Environmental Protection Agency, and approved for publication. Mention of trade names or,commercial products does not constitute endorsement or recommendation for use.,Method 1613,October 1994 iii,Introduction,Method 1613 was developed by the United States Environmental Protection Agency's Office,of Science and Technology for isomer-specific determination of the 2,3,7,8-substituted, tetrathrough,octa-chlorinated, dibenzo-p-dioxins and dibenzofurans in aqueous, solid, and tissue,matrices by isotope dilution, high resolution capillary column gas chromatography,(HRGC)/high resolution mass spectrometry (HRMS).,Questions concerning this method or its application should be addressed to:,W.A. Telliard,US EPA Office of Water,Analytical Methods Staff,Mail Code 4303,401 M Street, SW,Washington, D.C. 20460,202/260-7120,Requests for additional copies should be directed to:,Water Resource Center,Mail Code RC-4100,401 M Street, SW,Washington, D.C. 20460,202/260-7786 or 202/260-2814,Method 1613,October 1994 1,Method 1613, Revision B,Tetra- through Octa-Chlorinated Dioxins and Furans by Isotope,Dilution HRGC/HRMS,1.0 Scope and Application,1.1 This method is for determination of tetra- through octa-chlorinated dibenzo-p-dioxins,(CDDs) and dibenzofurans (CDFs) in water, soil, sediment, sludge, tissue, and other,sample matrices by high resolution gas chromatography/high resolution mass,spectrometry (HRGC/HRMS). The method is for use in EPA's data gathering and,monitoring programs associated with the Clean Water Act, the Resource Conservation,and Recovery Act, the Comprehensive Environmental Response, Compensation and,Liability Act, and the Safe Drinking Water Act. The method is based on a compilation,of EPA, industry, commercial laboratory, and academic methods (References 1-6).,1.2 The seventeen 2,3,7,8-substituted CDDs/CDFs listed in Table 1 may be determined by,this method. Specifications are also provided for separate determination of,2,3,7,8-tetrachloro-dibenzo-p-dioxin (2,3,7,8-TCDD) and 2,3,7,8-tetrachloro-dibenzofuran,(2,3,7,8-TCDF).,1.3 The detection limits and quantitation levels in this method are usually dependent on the,level of interferences rather than instrumental limitations. The minimum levels (MLs),in Table 2 are the levels at which the CDDs/CDFs can be determined with no,interferences present. The Method Detection Limit (MDL) for 2,3,7,8-TCDD has been,determined as 4.4 pg/L (parts-per-quadrillion) using this method.,1.4 The GC/MS portions of this method are for use only by analysts experienced with,HRGC/HRMS or under the close supervision of such qualified persons. Each laboratory,that uses this method must demonstrate the ability to generate acceptable results using,the procedure in Section 9.2.,1.5 This method is "performance-based". The analyst is permitted to modify the method to,overcome interferences or lower the cost of measurements, provided that all performance,criteria in this method are met. The requirements for establishing method equivalency,are given in Section 9.1.2.,1.6 Any modification of this method, beyond those expressly permitted, shall be considered,a major modification subject to application and approval of alternate test procedures,under 40 CFR 136.4 and 136.5.,2.0 Summary of Method,Flow charts that summarize procedures for sample preparation, extraction, and analysis,are given in Figure 1 for aqueous and solid samples, Figure 2 for multi-phase samples,and Figure 3 for tissue samples.,Method 1613,2 October 1994,2.1 Extraction,2.1.1 Aqueous samples (samples containing less than 1% solids)—Stable isotopically,labeled analogs of 15 of the 2,3,7,8-substituted CDDs/CDFs are spiked into a 1 L,sample, and the sample is extracted by one of three procedures:,2.1.1.1 Samples containing no visible particles are extracted with methylene,chloride in a separatory funnel or by the solid-phase extraction technique,summarized in Section 2.1.1.3. The extract is concentrated for cleanup.,2.1.1.2 Samples containing visible particles are……
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