EPA Method 1614 Brominated diphenyl ethers in Water, Soil, Sediment, and Tissue by HRGC_HRMS

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E3100EFE0E3C4F29B000081EF706F44F

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2008-2-26

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Method 1614,Brominated Diphenyl Ethers in Water Soil,Sediment and Tissue by HRGC/HRMS,August 2007,U.S. Environmental Protection Agency,Office of Water,Office of Science and Technology,Engineering and Analysis Division (4303T),1200 Pennsylvania Avenue, NW,Washington, DC 20460,EPA-821-R-07-005,EPA Method 1614, August 2007,Method 1614,Brominated Diphenyl Ethers in Water, Soil, Sediment, and Tissue by,HRGC/HRMS,August 2007,Introduction,EPA Method 1614 was developed by the Office of Water’s Office of Science and Technology (OST),to determine polybrominated diphenyl ether (PBDE) congeners in aqueous, solid, tissue, and multi-phase,matrices. These ethers are used in brominated flame retardants. The method uses isotope dilution and,internal standard high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS).,This version revises the August 2003 version to include use of a temperature programmed,injector/vaporizer and a short column to improve recoveries of the octa-, nona- and decabrominated,diphenyl ethers.,Acknowledgments,EPA Method 1614 was developed under EPA contract by DynCorp Environmental and Interface, Inc.,Data were provided by Axys Analytical Services, Ltd., Sidney, BC, Canada.,Disclaimer,This PBDE-congener method is patterned after the EPA PCB-congener Method 1668A. The method,specifications are based on data from Axys Analytical. Method 1614 has been reviewed by the,Engineering and Analytical Support Branch in the Engineering and Analysis Division (EAD) of OST.,The method is available for general use, but has not been published in 40 CFR Part 136. Mention of trade,names or commercial products does not constitute endorsement or recommendation for use.,Please address your questions or comments to:,CWA Methods Team,Engineering and Analytical Support Branch/EAD (4303T),Office of Science and Technology,U.S. Environmental Protection Agency,1200 Pennsylvania Avenue,Washington, DC 20460,E-mail: OSTCWAMethods@epa.gov,EPA Method 1614, August 2007 1,Method 1614,Brominated Diphenyl Ether Congeners in Water, Soil, Sediment, Biosolids and,Tissue by HRGC/HRMS,August 2007,1.0 Scope and application,1.1 EPA Method 1614 ("Method 1614"; the "Method") is for determination of brominated diphenyl,ether (BDE) congeners in water, soil, sediment, biosolids, tissue, and other sample matrices by,high resolution gas chromatography combined with high resolution mass spectrometry,(HRGC/HRMS).,1.1.1 The 209 BDE congeners are listed in Table 1. The 8 congeners of primary interest,("BDEs of primary interest"; Reference 1) are shown in boldface type. Congeners that,have been reported as being found in environmental samples (References 2 and 3) are,shown in italics. Congeners that allow determination of BDEs at those levels of,bromination not found in environmental samples (References 2 and 3) are shown by,footnote in Table 1. Other congeners in Table 1 may be determined as standards become,available and as needs arise. Data are provided in Tables 2 - 6 for congeners that have,been tested.,1.1.2 This Method can also be used to test for other brominated flame retardants (BFR) and,brominated organic compounds in the event that new products come on the market.,1.2 This method is based on EPA Method 1668A (Reference 4) and a method developed by a,commercial testing laboratory (Reference 5).,1.3 The detection and quantitation limits in this Method are usually dependent on the level of,interferences and laboratory backgrounds rather than instrumental limitations. The method,detection limits and (MDLs) and minimum levels of quantitation (MLs) in Table 2 are the levels,at which the BDEs can be determined with laboratory contamination present. The estimated,MDL for BDE 99 in water is 5 pg/L (picograms-per-liter (pg/L); parts-per-quadrillion (ppq)) with,no interferences present.,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 laboratory is permitted to omit any step or modify any,procedure (e.g., to overcome interferences or lower the cost of measurements), provided that all,performance requirements in this method are met. Requirements for establishing equivalency are,given in Section 9.1.2, and additionally for Clean Water Act (CWA) uses, at 40 CFR 136.6. For,use in regulatory programs, such as the CWA, any modification beyond the modifications,expressly permitted in this method, or at 40 CFR 136.6 is a modification ……

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