EPA Method 8318 N-Methylcarbamates by High Performance Liquid Chromatography (HPLC) - Revision 0
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F8FBC41F6CA549AAA66B042991C3EA06 |
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0.13 |
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页数： |
18 |
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日期： |
2003-1-16 |
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CD-ROM 8318 - 1 Revision 0,September 1994,METHOD 8318,N-METHYLCARBAMATES BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC),1.0 SCOPE AND APPLICATION,1.1 Method 8318 is used to determine the concentration of,N-methylcarbamates in soil, water and waste matrices. The following compounds can,be determined by this method:,_______________________________________________________________________________,Compound Name CAS No.a,________________________________________________________________________________,Aldicarb (Temik) 116-06-3,Aldicarb Sulfone 1646-88-4,Carbaryl (Sevin) 63-25-2,Carbofuran (Furadan) 1563-66-2,Dioxacarb 6988-21-2,3-Hydroxycarbofuran 16655-82-6,Methiocarb (Mesurol) 2032-65-7,Methomyl (Lannate) 16752-77-5,Promecarb 2631-37-0,Propoxur (Baygon) 114-26-1,________________________________________________________________________________,a Chemical Abstract Services Registry Number.,1.2 The method detection limits (MDLs) of Method 8318 for determining the,target analytes in organic-free reagent water and in soil are listed in Table 1.,1.3 This method is restricted to use by, or under the supervision of,analysts experienced in the use of high performance liquid chromatography (HPLC),and skilled in the interpretation of chromatograms. Each analyst must,demonstrate the ability to generate acceptable results with this method.,2.0 SUMMARY OF METHOD,2.1 N-methylcarbamates are extracted from aqueous samples with methylene,chloride, and from soils, oily solid waste and oils with acetonitrile. The,extract solvent is exchanged to methanol/ethylene glycol, and then the extract,is cleaned up on a C-18 cartridge, filtered, and eluted on a C-18 analytical,column. After separation, the target analytes are hydrolyzed and derivatized,post-column, then quantitated fluorometrically.,2.2 Due to the specific nature of this analysis, confirmation by a,secondary method is not essential. However, fluorescence due to post-column,derivatization may be confirmed by substituting the NaOH and o-phthalaldehyde,solutions with organic-free reagent water and reanalyzing the sample. If,CD-ROM 8318 - 2 Revision 0,September 1994,fluorescence is still detected, then a positive interference is present and care,should be taken in the interpretation of the results.,2.3 The sensitivity of the method usually depends on the level of,interferences present, rather than on the instrumental conditions. Waste samples,with a high level of extractable fluorescent compounds are expected to yield,significantly higher detection limits.,3.0 INTERFERENCES,3.1 Fluorescent compounds, primarily alkyl amines and compounds which,yield primary alkyl amines on base hydrolysis, are potential sources of,interferences.,3.2 Coeluting compounds that are fluorescence quenchers may result in,negative interferences.,3.3 Impurities in solvents and reagents are additional sources of,interferences. Before processing any samples, the analyst must demonstrate,daily, through the analysis of solvent blanks, that the entire analytical system,is interference free.,4.0 APPARATUS AND MATERIALS,4.1 HPLC system,4.1.1 An HPLC system capable of injecting 20 μL aliquots and,performing multilinear gradients at a constant flow. The system must also,be equipped with a data system to measure the peak areas.,4.1.2 C-18 reverse phase HPLC column, 25 cm x 4.6 mm (5 μm).,4.1.3 Post Column Reactor with two solvent delivery systems (Kratos,PCRS 520 with two Kratos Spectroflow 400 Solvent Delivery Systems, or,equivalent).,4.1.4 Fluorescence detector (Kratos Spectroflow 980, or equivalent).,4.2 Other apparatus,4.2.1 Centrifuge.,4.2.2 Analytical balance - + 0.0001 g.,4.2.3 Top loading balance - + 0.01 g.,4.2.4 Platform shaker.,4.2.5 Heating block, or equivalent apparatus, that can accommodate,10 mL graduated vials (Sec. 4.3.11).,CD-ROM 8318 - 3 Revision 0,September 1994,4.3 Materials,4.3.1 HPLC injection syringe - 50 μL.,4.3.2 Filter paper, (Whatman #113 or #114, or equivalent).,4.3.3 Volumetric pipettes, Class A, glass, assorted sizes.,4.3.4 Reverse phase cartridges, (C-18 Sep-PakR [Waters Associates],or equivalent).,4.3.5 Glass syringes - 5 mL.,4.3.6 Volumetric flasks, Class A - Sizes as appropriate.,4.3.7 Erlenmeyer flasks with teflon-lined screw caps, 250 mL.,4.3.8 Assorted glass funnels.,4.3.9 Separatory funnels, with ground glass stoppers and teflon,stopcocks - 250 mL.,4.3.10 Graduated cylinders - 100 mL.,4.3.11 Graduated glass vials - 10 mL, 20 mL.,4.3.12 Centrifuge tubes - 250 mL.,4.3.13 Vials - 25 mL, glass with Teflon lined screw caps or,crimp tops.,4.3.14 Positive displacement micro-pipettor, 3 to 25 μL,displacement, (Gilson Microman [Rainin #M-25] with tips,……
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