EPA Method 8131 Aniline and Selected Derivatives by Gas Chromatography - Revision 0
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ID： |
7A1EE6B6AE4549C28F15F6FA3CD991B3 |
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文件大小(MB)： |
0.1 |
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页数： |
13 |
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文件格式： |
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日期： |
2003-1-16 |
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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 8131 - 1 Revision 0,December 1996,METHOD 8131,ANILINE AND SELECTED DERIVATIVES BY GAS CHROMATOGRAPHY,1.0 SCOPE AND APPLICATION,1.1 Method 8131 is used to determine (by gas chromatography with a specific detector) the,concentration of aniline and certain derivatives of aniline in extracts prepared from environmental,samples and RCRA wastes. It has been validated for aqueous matrices. Application to other,matrices must be validated by developing spike recovery data. The following compounds can be,determined by this method:,Compound CAS No.a,Aniline 62-53-3,4-Bromoaniline 106-40-1,2-Bromo-6-chloro-4-nitroaniline 99-29-6,2-Bromo-4,6-dinitroaniline 1817-73-8,2-Chloroaniline 95-51-2,3-Chloroaniline 108-42-9,4-Chloroaniline 106-47-8,2-Chloro-4,6-dinitroaniline 3531-19-9,2-Chloro-4-nitroaniline 121-87-9,4-Chloro-2-nitroaniline 89-63-4,2,6-Dibromo-4-nitroaniline 827-94-1,3,4-Dichloroaniline 95-76-1,2,6-Dichloro-4-nitroaniline 99-30-9,2,4-Dinitroaniline 97-02-9,2-Nitroaniline 88-74-4,3-Nitroaniline 99-09-2,4-Nitroaniline 100-01-6,2,4,6-Trichloroaniline 634-93-5,2,4,5-Trichloroaniline 636-30-6,a Chemical Abstract Service Registry Number.,1.2 When this method is used to analyze unfamiliar samples for any or all of the target,analytes, compound identifications should be supported by at least one additional qualitative,technique. This method describes analytical conditions for a second gas chromatographic column,that can be used to confirm measurements made with the primary column. It is highly,recommended that gas chromatography/mass spectrometry be utilized for absolute analyte,identification when analyzing unfamiliar samples, if concentration permits. See Section 8.6 for,guidance. However, the use of the NPD minimizes the possibility of false positives.,1.3 The method detection limit (MDL) for each target analyte is given in Table 1. The MDL,for a specific sample may differ from those listed, depending upon the nature of interferences in the,CD-ROM 8131 - 2 Revision 0,December 1996,sample matrix. Table 2 provides guidance on the calculation of estimated quantitation limits (EQLs),for various matrices.,1.4 Aniline and many aniline derivatives often result in erratic responses, thereby requiring,frequent column maintenance and recalibration.,1.5 This method is restricted to use by or under the supervision of analysts experienced in,the use of gas chromatography and in the interpretation of gas chromatograms. Each analyst must,demonstrate the ability to generate acceptable results with this method using the procedure,described in Sec. 8.2.,2.0 SUMMARY OF METHOD,2.1 A measured volume of aqueous sample, approximately 1 liter, is solvent extracted at,basic pH according to Method 3510 (separatory funnel), Method 3520 (continuous liquid-liquid,extraction), or other appropriate technique. Extraction from solid matrices may be performed using,Methods 3540, 3541, 3545, or 3550, or other appropriate technique. Both neat and diluted organic,liquids may be prepared by Method 3580 (waste dilution) and analyzed by direct injection.,2.2 If interferences are present, the extract may be cleaned up according to Method 3620,Florisil Column Cleanup. Gel Permeation Chromatography Cleanup (Method 3640) has also been,validated for aniline and certain derivatives to remove high boiling material that causes,chromatography problems.,2.3 The target analytes in the extract are determined by capillary gas chromatography with,a nitrogen phosphorus detector (GC/NPD).,3.0 INTERFERENCES,3.1 Refer to Methods 3500, 3600, and 8000.,3.2 Solvents, reagents, glassware, and other sample processing hardware may yield discrete,artifacts and/or elevated baselines causing misinterpretation of gas chromatograms. All these,materials must be demonstrated to be free from interferences under the conditions of the analysis,by analyzing reagent blanks.,3.2.1 Volumetric flasks and glassware used for making up calibration standards must,be scrupulously cleaned. Clean all glassware as soon as possible after use by rinsing with,the last solvent used in it. This should be followed by detergent washing with hot water and,rinses with tap and distilled water. It should then be drained dry, and heated in a muffle,furnace at 400EC for 15 to 30 min.,3.2.2 Some thermally stable materials may not be eliminated by this treatment. Solvent,rinses with acetone and hexane may be substituted for the muffle furnace heating. Volumetric,ware should not be heated in a muffle furnace. After drying and cooling, glassware should be,sealed and stored in a clean environment to prevent any accumulation of dust or other,contaminants. Store inverted or capped ……
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