EPA Method 617 Organophosphorus Pesticides and PCBs

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067046F5D1614CC6A8007C289226CE81

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0.18

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32

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pdf

日期:

2008-2-26

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Method 617,The Determination of,Organohalide Pesticides and,PCBs in Municipal and,Industrial Wastewater,Method 617,The Determination of Organohalide Pesticides and PCBs in Municipal,and Industrial Wastewater,1. SCOPE AND APPLICATION,1.1 This method covers the determination of certain organohalide pesticides and PCBs. The,following parameters can be determined by this method:,Parameter Storet No. CAS No.,Aldrin 39330 309-00-2,"-BHC 39337 319-84-6,?BHC 39338 319-85-7,*-BHC 39259 319-86-8,(-BHC 39340 58-89-9,Captan 39640 133-06-2,Carbophenothion -- 786-19-6,Chlordane 39350 57-74-9,4,4¢-DDD 39310 72-54-8,4,4¢-DDE 39320 72-55-9,4,4¢-DDT 39300 50-29-3,Dichloran -- 99-30-9,Dicofol 39780 115-32-2,Dieldrin 39380 60-57-1,Endosulfan I 34356 959-98-8,Endosulfan II 34361 33213-65-9,Endosulfan sulfate 34351 1031-07-8,Endrin 39390 72-20-8,Endrin aldehyde 34366 7421-93-4,Heptachlor 39410 76-44-8,Heptachlor epoxide 39420 1024-57-3,Isodrin 39430 465-73-6,Methoxychlor 39480 72-43-5,Mirex 39755 2385-85-5,PCNB 39029 82-68-8,Perthane 39034 72-56-0,Strobane -- 8001-50-1,Toxaphene 39400 8001-35-2,Trifluralin 39030 1582-09-8,PCB-1016 34671 12674-11-2,PCB-1221 39488 11104-28-2,PCB-1232 39492 11141-16-5,PCB-1242 39496 53469-21-9,PCB-1248 39500 12672-29-6,PCB-1254 39504 11097-69-1,PCB-1260 39508 11096-82-5,Method 617,1.2 This is a gas chromatographic (GC) method applicable to the determination of the,compounds listed above in industrial and municipal discharges as provided under,40 CFR 136.1. Any modification of this method beyond those expressly permitted shall,be considered a major modification subject to application and approval of alternative test,procedures under 40 CFR 136.4 and 136.5.,1.3 The method detection limit (MDL, defined in Section 15) for many of the parameters are,listed in Table 1. The MDL for a specific wastewater may differ from those listed,depending upon the nature of interferences in the sample matrix.,1.4 The sample extraction and concentration steps in this method are essentially the same as,in Method 614. Thus, a single sample may be extracted to measure the parameters,included in the scope of both of these methods. When cleanup is required, the,concentration levels must be high enough to permit selecting aliquots, as necessary, in,order to apply appropriate cleanup procedures. Under gas chromatography, the analyst,is allowed the latitude to select chromatographic conditions appropriate for the,simultaneous measurement of combinations of these parameters (see Section 12).,1.5 This method is restricted to use by or under the supervision of analysts experienced in,the use of gas chromatography and in the interpretation of gas chromatograms. Each,analyst must demonstrate the ability to generate acceptable results with this method,using the procedure described in Section 8.2.,1.6 When this method is used to analyze unfamiliar samples for any or all of the compounds,above, compound identifications should be supported by at least one additional,qualitative technique. This method describes analytical conditions for a second gas,chromatographic column that can be used to confirm measurements made with the,primary column. Section 14 provides gas chromatograph/mass spectrometer (GC/MS),criteria appropriate for the qualitative confirmation of compound identifications.,2. SUMMARY OF METHOD,2.1 A measured volume of sample, approximately 1 L, is extracted with 15% methylene,chloride in hexane using a separatory funnel. The extract is dried and concentrated to,a volume of 10 mL or less. Gas chromatographic conditions are described which permit,the separation and measurement of the compounds in the extract by electron capture gas,chromatography.,2.2 Method 617 represents an editorial revision of two previously promulgated U.S. EPA,methods for pesticides and for PCBs.1 While complete method validation data is not,presented herein, the method has been in widespread use since its promulgation, and,represents the state of the art for the analysis of such materials.,2.3 This method provides selected cleanup procedures to aid in the elimination of,interferences which may be encountered.,Method 617,3. INTERFERENCES,3.1 Method interferences may be caused by contaminants in solvents, reagents, glassware,and other sample processing apparatus that lead to discrete artifacts or elevated baselines,in gas chromatograms. All reagents and apparatus must be routinely demonstrated to,be free from interferences under the conditions of the analysis by running laboratory,reagent blanks as described in Section 8.5.,3.1.1 Glassware must be scrupulously cleaned.2 Clean all glassware as soon as possible,after use by……

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