EPA Method 8316 Acrylamide, Acrylonitrile and Acrolein by High Performance Liquid Chromatography (HPLC) - Revision 0
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0D6EB690E1D3457EACDE0E6499005031 |
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0.03 |
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7 |
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日期： |
2003-1-16 |
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CD-ROM 8316 - 1 Revision 0,September 1994,METHOD 8316,ACRYLAMIDE, ACRYLONITRILE AND ACROLEIN BY HIGH PERFORMANCE,LIQUID CHROMATOGRAPHY (HPLC),1.0 SCOPE AND APPLICATION,1.1 The following compounds can be determined by this method:,____________________________________________________________________,Compound Name CAS No.a,Acrylamide 79-06-1,Acrylonitrile 107-13-1,Acrolein (Propenal) 107-02-8,____________________________________________________________________,a Chemical Abstract Services Registry Number.,1.2 The method detection limits (MDLs) for the target analytes in,organic-free reagent water are listed in Table 1. The method may be applicable,to other matrices.,1.3 This method is restricted to use by or under the supervision of,analysts experienced in the use of high performance liquid chromatographs and,skilled in the interpretation of high performance liquid chromatograms. Each,analyst must demonstrate the ability to generate acceptable results with this,method.,2.0 SUMMARY OF METHOD,2.1 Water samples are analyzed by high performance liquid chromatography,(HPLC). A 200 μL aliquot is injected onto a C-18 reverse-phase column, and,compounds in the effluent are detected with an ultraviolet (UV) detector.,3.0 INTERFERENCES,3.1 Contamination by carryover can occur whenever high-concentration and,low-concentration samples are sequentially analyzed. To reduce carryover, the,sample syringe must be rinsed out between samples with solvent. Whenever an,unusually concentrated sample is encountered, it should be followed by the,analysis of solvent to check for cross contamination.,CD-ROM 8316 - 2 Revision 0,September 1994,4.0 APPARATUS AND MATERIALS,4.1 HPLC system,4.1.1 One high pressure pump.,4.1.2 Octadecyl Silane (ODS, C-18) reverse phase HPLC column,25 cm x 4.6 mm, 10 μm, (Zorbax, or equivalent).,4.1.3 Variable wavelength UV detector.,4.1.4 Data system.,4.2 Other apparatus,4.2.1 Water degassing unit - 1 liter filter flask with stopper and,pressure tubing.,4.2.2 Analytical balance - + 0.0001 g.,4.2.3 Magnetic stirrer and magnetic stirring bar.,4.2.4 Sample filtration unit - syringe filter with 0.45 μm filter,membrane, or equivalent disposable filter unit.,4.3 Materials,4.3.1 Syringes - 10, 25, 50 and 250 μL and 10 mL.,4.3.2 Volumetric pipettes, Class A, glass - 1, 5 and 10 mL.,4.3.3 Volumetric flasks - 5, 10, 50 and 100 mL.,4.3.4 Vials - 25 mL, glass with Teflon lined screw caps or crimp,tops.,5.0 REAGENTS,5.1 Reagent grade inorganic 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 Acrylamide, CH2:CHCONH2, 99+% purity, electrophoresis reagent grade.,5.3 Acrylonitrile, H2C:CHCN, 99+% purity.,5.4 Acrolein, CH2:CHCHO, 99+% purity.,CD-ROM 8316 - 3 Revision 0,September 1994,5.5 Organic-free reagent water. All references to water in this method,refer to organic-free reagent water, as defined in Chapter One. Sparge with He,to eliminate O2 to prevent significant absorption interference from O2 at the 195,nm wavelength.,5.6 Stock standard solutions - Can be prepared from pure standard,materials or can be purchased as certified solutions. Commercially prepared,stock standards can be used if they are certified by the manufacturer and,verified against a standard made from pure material.,5.6.1 Acrylamide,5.6.1.1 Weigh 0.0100 g of acrylamide neat standard into a,100 mL volumetric flask, and dilute to the mark with organic-free,reagent water. Calculate the concentration of the standard solution,from the actual weight used. When compound purity is assayed to be,96% or greater, the weight can be used without correction to,calculate the concentration of the stock standard.,5.6.1.2 Transfer the stock solution into vials with Teflon,lined screw caps or crimp tops. Store at 4oC, protected from light.,5.6.1.3 Stock solutions must be replaced after six months,or sooner if comparison with the check standards indicates a,problem.,5.6.2 Acrylonitrile and Acrolein - Prepare separate stock solutions,for acrylonitrile and acrolein.,5.6.2.1 Place about 9.8 mL of organic-free reagent water,into a 10 mL volumetric flask before weighing the flask and stopper.,Weigh the flask and record the weight to the nearest 0.0001 g. Add,two drops of neat standard, using a 50 μL syringe, to the flask.,The liquid must fall directly into the water, wi……
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