EPA Method 8091 Nitroaromatics and Cyclic Ketones by Gas Chromatography - Revision 0
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42D32EC0E23F4D44814E7122713D30A1 |
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0.09 |
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17 |
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日期： |
2003-1-16 |
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CD-ROM 8091 - 1 Revision 0,December 1996,METHOD 8091,NITROAROMATICS AND CYCLIC KETONES BY GAS CHROMATOGRAPHY,1.0 SCOPE AND APPLICATION,1.1 Method 8091 is a gas chromatographic (GC) method used to determine the concentration,of nitroaromatics and cyclic ketones. It describes wide-bore, open-tubular, capillary column gas,chromatography procedures using either electron capture (ECD) or nitrogen-phosphorous (NPD),detectors. The following RCRA analytes can be determined by this method:,Compound CAS No.a,1,4-Dinitrobenzene 100-25-4,2,4-Dinitrotoluene 121-14-2,2,6-Dinitrotoluene 606-20-2,1,4-Naphthoquinone 130-15-4,Nitrobenzene 98-95-3,Pentachloronitrobenzene 82-68-8,a Chemical Abstract Service Registry Number.,1.2 The following non-RCRA analytes can also be determined by this method:,Compound CAS No.a,Benefin 1861-40-1,Butralin 33629-47-9,1-Chloro-2,4-dinitrobenzene 97-00-7,1-Chloro-3,4-dinitrobenzene 610-40-2,1-Chloro-2-nitrobenzene 88-73-3,1-Chloro-4-nitrobenzene 100-00-5,2-Chloro-6-nitrotoluene 83-42-1,4-Chloro-2-nitrotoluene 89-59-8,4-Chloro-3-nitrotoluene 89-60-1,2,3-Dichloronitrobenzene 3209-22-1,2,4-Dichloronitrobenzene 611-06-3,3,5-Dichloronitrobenzene 618-62-2,3,4-Dichloronitrobenzene 99-54-7,2,5-Dichloronitrobenzene 89-61-2,CD-ROM 8091 - 2 Revision 0,December 1996,Compound CAS No.a,Dinitramine 29091-05-2,1,2-Dinitrobenzene 528-29-0,1,3-Dinitrobenzene 99-65-0,Isopropalin 33820-53-0,1,2-Naphthoquinone 524-42-5,2-Nitrotoluene 88-72-2,3-Nitrotoluene 99-08-1,4-Nitrotoluene 99-99-0,Penoxalin (Pendimethalin) 40487-42-1,Profluralin 26399-36-0,2,3,4,5-Tetrachloronitrobenzene 879-39-0,2,3,5,6-Tetrachloronitrobenzene 117-18-0,1,2,3-Trichloro-4-nitrobenzene 17700-09-3,1,2,4-Trichloro-5-nitrobenzene 89-69-0,2,4,6-Trichloronitrobenzene 18708-70-8,Trifluralin 1582-09-8,1.3 This method is restricted to 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 8091 provides gas chromatographic conditions for the detection of ppb,concentrations of nitroaromatics and cyclic ketones in water and soil or ppm concentrations in waste,samples. Prior to use of this method, appropriate sample extraction techniques must be used for,environmental samples (refer to Chapter Two and Method 3500). Both neat and diluted organic,liquids (Method 3580) may be analyzed by direct injection. Analysis is accomplished by gas,chromatography utilizing an instrument equipped with wide bore capillary columns and one or more,electron capture detectors or nitrogen-phosphorus detectors (NPD).,3.0 INTERFERENCES,3.1 Refer to Method 3500, 3600, and 8000.,3.2 The electron capture detector responds to all electronegative compounds. Therefore,interferences are possible from other halogenated compounds, as well as phthalates and other,oxygenated compounds such as organonitrogen, organosulfur, and organophosphorus compounds.,Second column confirmation or GC/MS confirmation is necessary to ensure proper analyte,identification unless previous characterization of the sample source will ensure proper identification.,3.3 Contamination by carryover can occur whenever high-concentration and,low-concentration samples are sequentially analyzed. To reduce carryover, the syringe used for,injection must be thoroughly rinsed between samples with solvent. Whenever a highly concentrated,sample extract is encountered, it should be followed by the analysis of a solvent blank to check for,CD-ROM 8091 - 3 Revision 0,December 1996,cross-contamination. Additional solvent blanks interspersed with the sample extracts should be,considered whenever the analysis of a solvent blank indicates cross-contamination problems.,3.4 In certain cases some compounds coelute on either one or both columns. In these cases,the compounds must be reported as coeluting. The mixture can be reanalyzed by GC/MS,techniques if concentration permits (see Method 8270).,3.4.1 DB-5 column:,2,4,6-trichloronitrobenzene/1,3-dinitrobenzene,1-chloro-2,4-dinitrobenzene/1-chloro-3,4-dinitrobenzene/,1,2,3-trichloro-4-nitrobenzene,3.4.2 DB-1701 column:,2,4-dichloronitrobenzene/4-chloro-3-nitrotoluene,2,4,6-trichloronitrobenzene/1,4-naphthoquinone,1-chloro-2,4-dinitrobenzene/2,3,4,5-tetrachloronitrobenzene,3.4.3 In addition, on the DB-5 column, 2,5-dichloronitrobenzene is not well resolved,from 4-chloro-3-nitrotoluene. Also, Trifluralin is not well resolved from Benefin. On the,DB-1701 column, compound pairs that are not well resolved include,4-nitrotoluene/1-chloro-3-nitrobenz……
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