EPA Method 632 Carbamate and Urea Pesticides

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FB589F174AAB4A55841675C37FE66103

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0.07

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19

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日期:

2008-2-26

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Method 632,The Determination of,Carbamate and Urea Pesticides,in Municipal and Industrial,Wastewater,Method 632,The Determination of Carbamate and Urea Pesticides in Municipal and,Industrial Wastewater,1. SCOPE AND APPLICATION,1.1 This method covers the determination of certain carbamate and urea pesticides. The,following parameters can be determined by this method:,Parameter STORET No. CAS No.,Aminocarb ) 2032-59-9,Barban ) 101-27-9,Carbaryl 39750 63-25-2,Carbofuran 81405 1563-66-2,Chlorpropham ) 101-21-3,Diuron 39650 330-54-1,Fenuron ) 101-42-8,Fenuron-TCA ) 4482-55-7,Fluometuron ) 2164-17-2,Linuron ) 330-55-2,Methiocarb ) 2032-65-7,Methomyl 39051 16752-77-5,Mexacarbate ) 315-18-4,Monuron ) 150-68-5,Monuron-TCA ) 140-41-0,Neburon ) 555-37-3,Oxamyl ) 23135-22-0,Propham 39052 122-42-9,Propoxur ) 114-26-1,Siduron ) 1982-49-6,Swep ) 1918-18-9,1.2 This method cannot distinguish monuron from monuron-TCA and fenuron from,fenuron-TCA. Results for the paired parameters are reported as monuron and fenuron,respectively.,1.3 This is a high-performance liquid chromatographic (HPLC) 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.,1.4 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.,Method 632,1.5 This method is restricted to use by or under the supervision of analysts experienced in,the use of liquid chromatography and in the interpretation of liquid 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.,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 concentrated to,a volume of 10 mL or less. HPLC chromatographic conditions are described which,permit the separation and measurement of the compounds in the extract by HPLC with,a UV detector.1,2,2.2 This method provides an optional Florisil column cleanup procedure to aid in the,elimination or reduction 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 liquid 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.3 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 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. The cleanup procedure in Section 11 can be used to overcome many of these,interferences, but unique samples may require additional cleanup approaches to achieve,the MDL listed in Table 1.,Method 632,4. 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……

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