EPA Method 614 Organophosphorus Pesticides
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ID： |
03C513C4A69B4A1B8F39B9611648729E |
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文件大小(MB)： |
0.07 |
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页数： |
20 |
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文件格式： |
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日期： |
2008-2-26 |
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购买： |
文本摘录（文本识别可能有误，但文件阅览显示及打印正常，pdf文件可进行文字搜索定位）：
Method 614,The Determination of,Organophosphorus Pesticides in,Municipal and Industrial,Wastewater,Method 614,The Determination of Organophosphorus Pesticides in Municipal and,Industrial Wastewater,1. SCOPE AND APPLICATION,1.1 This method covers the determination of certain organophosphorus pesticides. The,following parameters can be determined by this method:,Parameter STORET No. CAS No.,Azinphos methyl 39580 86-50-0,Demeton 39560 8065-48-3,Diazinon 39570 333-41-5,Disulfoton 39010 298-04-4,Ethion ) 563-12-2,Malathion 39530 121-75-5,Parathion ethyl 39540 56-38-2,Parathion methyl 39600 298-00-0,1.2 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 several 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 617. 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,Method 614,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 flame photometric,or thermionic bead gas chromatography.,2.2 Method 614 represents an editorial revision of a previously promulgated U.S. EPA,method for organophosphorus pesticides.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.,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 thoroughly rinsing with the last solvent used in it. Follow by,washing with hot water and detergent and thorough rinsing with tap and reagent,water. Drain dry, and heat in an oven or muffle furnace at 400°C for 15 to 30,minutes. Do not heat volumetric ware. Thermally stable materials, such as PCBs,may not be eliminated by this treatment. Thorough rinsing with acetone and,pesticide-quality hexane may be substituted for the heating. After drying and,cooling, seal and store glassware in a clean environment to prevent any,accumulation of dust or other contaminants. Store inverted or capped with,aluminum foil.,3.1.2 The use of high-purity reagents and solvents helps to minimize interfere……
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