EPA Method 8080A Organochlorine Pesticides and Polychlorinated Biphenyls by Gas Chromatography - Revision 1
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65C29F6BBBC64E0FA05501D969000056 |
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文件大小(MB)： |
0.2 |
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页数： |
28 |
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日期： |
2008-2-26 |
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CD-ROM 8080A - 1 Revision 1,September 1994,METHOD 8080A,ORGANOCHLORINE PESTICIDES AND POLYCHLORINATED BIPHENYLS,BY GAS CHROMATOGRAPHY,1.0 SCOPE AND APPLICATION,1.1 Method 8080 is used to determine the concentration of various,organochlorine pesticides and polychlorinated biphenyls (PCBs). The following,compounds can be determined by this method:,___________________________________________________________________,Compound Name CAS No.a,Aldrin 309-00-2,-BHC 319-84-6,-BHC 319-85-7,-BHC 319-86-8,-BHC (Lindane) 58-89-9,Chlordane (technical) 12789-03-6,4,4'-DDD 72-54-8,4,4'-DDE 72-55-9,4,4'-DDT 50-29-3,Dieldrin 60-57-1,Endosulfan I 959-98-8,Endosulfan II 33212-65-9,Endosulfan sulfate 1031-07-8,Endrin 72-20-8,Endrin aldehyde 7421-93-4,Heptachlor 76-44-8,Heptachlor epoxide 1024-57-3,4,4'-Methoxychlor 72-43-5,Toxaphene 8001-35-2,Aroclor-1016 12674-11-2,Aroclor-1221 1104-28-2,Aroclor-1232 11141-16-5,Aroclor-1242 53469-21-9,Aroclor-1248 12672-29-6,Aroclor-1254 11097-69-1,Aroclor-1260 11096-82-5,__________________________________________________________________,a Chemical Abstract Services Registry Number.,1.2 Table 1 lists the method detection limit for each compound in,organic-free reagent water. Table 2 lists the estimated quantitation limit (EQL),for other matrices.,CD-ROM 8080A - 2 Revision 1,September 1994,2.0 SUMMARY OF METHOD,2.1 Method 8080 provides gas chromatographic conditions for the detection,of ppb concentrations of certain organochlorine pesticides and PCBs. Prior to,the use of this method, appropriate sample extraction techniques must be used.,Both neat and diluted organic liquids (Method 3580, Waste Dilution) may be,analyzed by direct injection. A 2 to 5 μL sample is injected into a gas,chromatograph (GC) using the solvent flush technique, and compounds in the GC,effluent are detected by an electron capture detector (ECD) or an electrolytic,conductivity detector (HECD).,2.2 The sensitivity of Method 8080 usually depends on the concentration,of interferences rather than on instrumental limitations. If interferences,prevent detection of the analytes, Method 8080 may also be performed on samples,that have undergone cleanup. Method 3620, Florisil Column Cleanup, by itself or,followed by Method 3660, Sulfur Cleanup, may be used to eliminate interferences,in the analysis.,3.0 INTERFERENCES,3.1 Refer to Methods 3500, 3600, and 8000.,3.2 Interferences by phthalate esters can pose a major problem in,pesticide determinations when using the electron capture detector. These,compounds generally appear in the chromatogram as large late-eluting peaks,especially in the 15% and 50% fractions from the Florisil cleanup. Common,flexible plastics contain varying amounts of phthalates. These phthalates are,easily extracted or leached from such materials during laboratory operations.,Cross contamination of clean glassware routinely occurs when plastics are handled,during extraction steps, especially when solvent-wetted surfaces are handled.,Interferences from phthalates can best be minimized by avoiding contact with any,plastic materials. Exhaustive cleanup of reagents and glassware may be required,to eliminate background phthalate contamination. The contamination from,phthalate esters can be completely eliminated with a microcoulometric or,electrolytic conductivity detector.,4.0 APPARATUS AND MATERIALS,4.1 Gas chromatograph,4.1.1 Gas Chromatograph: Analytical system complete with gas,chromatograph suitable for on-column injections and all required,accessories, including detectors, column supplies, recorder, gases, and,syringes. A data system for measuring peak heights and/or peak areas is,recommended.,4.1.2 Columns,4.1.2.1 Column 1: Supelcoport (100/120 mesh) coated with,1.5% SP-2250/1.95% SP-2401 packed in a 1.8 m x 4 mm ID glass column,or equivalent.,CD-ROM 8080A - 3 Revision 1,September 1994,4.1.2.2 Column 2: Supelcoport (100/120 mesh) coated with,3% OV-1 in a 1.8 m x 4 mm ID glass column or equivalent.,4.1.3 Detectors: Electron capture (ECD) or electrolytic,conductivity detector (HECD).,4.2 Kuderna-Danish (K-D) apparatus:,4.2.1 Concentrator tube: 10 mL, graduated (Kontes K-570050-1025 or,equivalent). A ground-glass stopper is used to prevent evaporation of,extracts.,4.2.2 Evaporation flask: 500 mL (Kontes K-570001-500 or,equivalent). Attach to concentrator tube with springs, clamps, or,equivalent.,4.2.3 Snyder column: Three ball macro (Kontes K-503000-0121 or,equivalent).,4.2.4 Snyder column: Two ball micro (Kontes K-569001-0219 or,equivalent).,4.2.5 Springs - 1/2 inch (Kontes K-662750 or equivalent).,4.3 Boiling chips: Solvent extracted, approximately 10/40 mesh (silicon,carbide or eq……
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