EPA Method 8032A Acrylamide by Gas Chromatography - Revision 1
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C2A67D6E6CA54D7496E87E858E2D3361 |
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0.08 |
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页数： |
14 |
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日期： |
2003-1-16 |
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CD-ROM 8032A - 1 Revision 1,December 1996,METHOD 8032A,ACRYLAMIDE BY GAS CHROMATOGRAPHY,1.0 SCOPE AND APPLICATION,1.1 Method 8032 is used to determine trace amounts of acrylamide monomer (CAS No. 79-,06-1) in aqueous matrices. This method may be applicable to other matrices and to other similar,analytes.,1.2 The method detection limit (MDL) in an aqueous matrix is 0.032 μg/L.,1.3 This method is restricted for use by, or under the supervision of, analysts experienced,in the use of gas chromatographs and skilled in the interpretation of gas chromatograms. Each,analyst must demonstrate the ability to generate acceptable results with this method.,2.0 SUMMARY OF METHOD,2.1 Method 8032 is based on bromination of the acrylamide double bond. The reaction,product (2,3-dibromopropionamide) is extracted from the reaction mixture with ethyl acetate, after,salting out with sodium sulfate. The extract is cleaned up using a Florisil column, and analyzed by,gas chromatography with electron capture detection (GC/ECD).,2.2 Compound identification should be supported by at least one additional qualitative,technique. Analysis using a second gas chromatographic column or gas chromatography/mass,spectrometry may be used for compound confirmation.,3.0 INTERFERENCES,3.1 No interference is observed from seawater or in the presence of 8.0% of ammonium ions,derived from ammonium bromide.,3.2 Impurities from potassium bromide are removed by the Florisil cleanup procedure.,4.0 APPARATUS AND MATERIALS,4.1 Gas chromatographic system,4.1.1 Gas chromatograph suitable for on-column injections with all required,accessories, including detector, analytical columns, recorder, gases, and syringes. A data,system for measuring peak heights and/or peak areas is recommended.,4.1.2 GC Column - 2 m x 3 mm glass column, 5% FFAP (free fatty acid polyester) on,60-80 mesh acid washed Chromosorb W, or equivalent.,4.1.3 Detector - electron capture detector.,4.2 Separatory funnel - 150-mL.,CD-ROM 8032A - 2 Revision 1,December 1996,4.3 Volumetric flask (Class A) - 100-mL, with ground-glass stopper; 25-mL, amber, with,ground-glass stopper.,4.4 Syringe - 5-mL.,4.5 Microsyringes - 5-μL, 100-μL.,4.6 Pipets (Class A).,4.7 Glass chromatography column (30 cm x 2 cm).,4.8 Mechanical shaker.,5.0 REAGENTS,5.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is,intended that all reagents shall conform to the specifications of the Committee on Analytical,Reagents of the American Chemical Society, where such specifications are available. Other grades,may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its,use without lessening the accuracy of the determination.,5.2 Organic-free reagent water. All references to water in this method refer to organic-free,reagent water, as defined in Chapter One.,5.3 Solvents - All solvent must be pesticide quality, or equivalent.,5.3.1 Ethyl acetate, C H CO C H 2 5 2 2 5,5.3.2 Diethyl ether, C H OC H . Must be free of peroxides as indicated by test strips 2 5 2 5,(EM Quant, or equivalent). Procedures for removal of peroxides are provided with the test,strips. After cleanup, 20 mL of ethyl alcohol preservative must be added to each liter of ether.,5.3.3 Methanol, CH OH 3,5.3.4 Benzene, C H 6 6,5.3.5 Acetone, CH COCH 3 3,5.4 Saturated bromine water - Prepare by shaking organic-free reagent water with bromine,and allowing to stand for 1 hour, in the dark, at 4EC. Use the aqueous phase.,5.5 Sodium sulfate (anhydrous, granular), Na SO . Purify this reagent by heating at 400EC 2 4,for 4 hours in a shallow tray, or by precleaning the sodium sulfate with methylene chloride. If the,sodium sulfate is precleaned with methylene chloride, a method blank must be analyzed,demonstrating that there is no interference from the sodium sulfate.,5.6 Sodium thiosulfate, Na S O , 1 M aqueous solution. 2 2 3,5.7 Potassium bromide, KBr, prepared for infrared analysis.,5.8 Concentrated hydrobromic acid, HBr, specific gravity 1.48.,CD-ROM 8032A - 3 Revision 1,December 1996,5.9 Acrylamide monomer, H C:CHCONH , electrophoresis reagent grade, minimum 95% 2 2,purity.,5.10 Dimethyl phthalate, C H (COOCH ) , 99.0% purity. 6 4 3 2,5.11 Florisil (60/100 mesh): Prepare Florisil by activating at 130EC for at least 16 hours.,Alternatively, store Florisil in an oven at 130EC. Before use, cool the Florisil in a desiccator. Pack,5 g of the Florisil, suspended in benzene, in a glass column (Sec. 4.8).,NOTE: Benzene is toxic, and should only be used in a ventilated laboratory hood.,5.12 Stock standard solution,Prepare a stock standard solution of acrylamide monomer……
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