EPA Method 8030A Acrolein and Acrylonitrile by Gas Chromatography - Revision 1
|
ID： |
C8FB6D1F12B3431486BBF7C49EC337E1 |
|
文件大小(MB)： |
0.06 |
|
页数： |
11 |
|
文件格式： |
|
|
日期： |
2008-2-26 |
|
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）：
CD-ROM 8030A - 1 Revision 1,July 1992,METHOD 8030A,ACROLEIN AND ACRYLONITRILE BY GAS CHROMATOGRAPHY,1.0 SCOPE AND APPLICATION,1.1 Method 8030 is used to determine the concentration of the following,volatile organic compounds:,_________________________________________________________________,Compound Name CAS No.a,Acrolein (Propenal) 107-02-8,Acrylonitrile 107-13-1,_________________________________________________________________,a Chemical Abstract Services Registry Number.,1.2 Table 1 lists chromatographic conditions and method detection limits,for acrolein and acrylonitrile in organic-free reagent water. Table 2 lists the,estimated quantitation limit (EQL) for other matrices.,2.0 SUMMARY OF METHOD,2.1 Method 8030 provides gas chromatographic conditions for the detection,of the target analytes. Samples can be analyzed using direct injection or purgeand-,trap (Method 5030). Tenax should be used as the trap packing material.,Ground water samples must be analyzed using Method 5030. A temperature program,is used in the gas chromatograph to separate the organic compounds. Detection,is achieved by a flame ionization detector (FID).,2.2 The method provides an optional gas chromatographic column that may,be helpful in resolving the analytes from co-eluting non-target compounds and for,analyte confirmation.,3.0 INTERFERENCES,3.1 Refer to Methods 5030 and 8000.,3.2 Samples can be contaminated by diffusion of volatile organics,(particularly chlorofluorocarbons and methylene chloride) through the sample,container septum during shipment and storage. A trip blank prepared from,organic-free reagent water and carried through sampling and subsequent storage,and handling can serve as a check on such contamination.,CD-ROM 8030A - 2 Revision 1,July 1992,4.0 APPARATUS AND MATERIALS,4.1 Gas chromatograph,4.1.1 Gas Chromatograph - Analytical system complete with gas,chromatograph suitable for on-column injections or purge-and-trap sample,introduction and all required accessories, including detectors, column,supplies, recorder, gases, and syringes. A data system for measuring peak,height and/or peak area is recommended.,4.1.2 Columns,4.1.2.1 Column 1 - 10 ft x 2 mm ID stainless steel or,glass packed with Porapak-QS (80/100 mesh) or equivalent.,4.1.2.2 Column 2 - 6 ft x 0.1 in. ID stainless steel or,glass packed with Chromosorb 101 (60/80 mesh) or equivalent.,4.1.3 Detector - Flame ionization (FID).,4.2 Sample introduction apparatus - Refer to Method 5030 for the,appropriate equipment for sample introduction purposes.,4.3 Syringes - A 5 mL Luer-lok glass hypodermic and a 5 mL, gas-tight,with shutoff valve.,4.4 Volumetric flasks, Class A - Appropriate sizes with ground glass,stoppers.,4.5 Microsyringes - 10 and 25 μL with a 0.006 in. ID needle,(Hamilton 702N, or equivalent) and a 100 μL.,4.6 Analytical balance - 0.0001 g.,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 Hydrochloric acid, HCl - 1:1 (v/v).,5.4 Sodium hydroxide, NaOH - 10N solution. Dissolve 40 g NaOH in,organic-free reagent water and dilute to 100 mL.,5.5 Stock standards - Stock solutions may be prepared from pure standard,CD-ROM 8030A - 3 Revision 1,July 1992,materials or purchased as certified solutions. Prepare stock standards in,organic-free reagent water using assayed liquids. Because acrolein and,acrylonitrile are lachrymators, primary dilutions of these compounds should be,prepared in a hood.,5.5.1 Place about 9.8 mL of organic-free reagent water,in a 10 mL tared ground-glass stoppered volumetric flask. For acrolein,standards the water must be adjusted to pH 4-5 using hydrochloric acid,(1:1 v/v) or sodium hydroxide (10N), if necessary. Weigh the flask to the,nearest 0.0001 g.,5.5.2 Using a 100 μL syringe, immediately add two or,more drops of assayed reference material to the flask, then reweigh. The,liquid must fall directly into the water without contacting the neck of,the flask.,5.5.3 Reweigh, dilute to volume, stopper, and then mix,by inverting the flask several times. Calculate the concentration in,milligrams per liter (mg/L) from the net gain in weight. When compound,purity is assay……
……