EPA Method 633 Organonitrogen Pesticides
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ID： |
9BF60738D97D4F4990DE296E0F40B223 |
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文件大小(MB)： |
0.07 |
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页数： |
18 |
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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 633,The Determination of,Organonitrogen Pesticides in,Municipal and Industrial,Wastewater,Method 633,The Determination of Organonitrogen Pesticides in Municipal and,Industrial Wastewater,1. SCOPE AND APPLICATION,1.1 This method covers the determination of certain organonitrogen pesticides. The,following parameters can be determined by this method:,Parameter STORET No. CAS No.,Bromacil ) 314-40-9,Deet ) 134-62-3,Hexazinone ) 51235-04-2,Metribuzin 81408 21087-64-9,Terbacil ) 5902-51-2,Triadimefon ) 43121-43-3,Tricyclazole ) 41814-78-2,1.2 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 five 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 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.,1.5 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. 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 methylene,chloride using a separatory funnel. The methylene chloride extract is dried and,exchanged to acetone during concentration 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 gas chromatography with a,thermionic bead detector.1,Method 633,3. 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 15-30 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 interference,problems. Purification of solvents by distillation in all-glass systems may be,required.,3.2 Matrix interferences may be caused by contaminants that are coextracted from the,sample. The extent of matrix interferences will vary considerably from source to,source, depending upon the nature and diversity of the industrial complex or,municipality sampled. Unique samples may require special cleanup approaches to,achieve the MDL listed in Table 1.,4. SAFETY,4.1 The toxicity or carcinogenicity of each reagent used in this method has not been,precisely defined; however, each chemical compound must be treated as a potential,health hazard. From this viewpoint, exposure to these chemicals must be reduced to,the lowest possible level by whatever means available. The laboratory is responsible,for maintaining a current awareness file of OSHA regulations regarding the safe,handling of the chemicals specified in this method. A reference file of material data,handling sheets should also be made available to all personnel involved in the,chemical analysis. Additional references to laboratory safety are available and have,been identified3-5 for the information of the analyst.,5. APPARATUS AND MATERIALS,5.……
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