EPA Method 8041 Phenols by Gas Chromatography
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463730E1BAF04727970962B1AB7C704C |
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文件大小(MB)： |
0.15 |
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页数： |
26 |
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日期： |
2009-12-11 |
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CD-ROM 8041 - 1 Revision 0,December 1996,METHOD 8041,PHENOLS BY GAS CHROMATOGRAPHY,1.0 SCOPE AND APPLICATION,1.1 Method 8041 describes open-tubular, capillary column gas chromatography procedures,for the analysis of phenols, using both single-column and dual-column/dual-detector approaches.,The following RCRA target analytes can be determined by this method:,______________________________________________________________________________,Appropriate Technique,Compound Name CAS No.a 3510 3520 3540 3550 3580,4-Chloro-3-methylphenol 59-50-7 X X X X X,2-Chlorophenol 95-57-8 X X X X X,2-Cyclohexyl-4,6-dinitrophenol 131-89-5 X ND ND ND LR,2,4-Dichlorophenol 120-83-2 X X X X X,2,6-Dichlorophenol 87-65-0 X ND ND ND X,2,4-Dimethylphenol 105-67-9 X X X X X,Dinoseb (DNBP) 88-85-7 X ND ND ND X,2,4-Dinitrophenol 51-28-5 X X X X X,2-Methyl-4,6-dinitrophenol 534-52-1 X X X X X,2-Methylphenol (o-Cresol) 95-48-7 X ND ND ND X,3-Methylphenol (m-Cresol) 108-39-4 X ND ND ND X,4-Methylphenol (p-Cresol) 106-44-5 X ND ND ND X,2-Nitrophenol 88-75-5 X X X X X,4-Nitrophenol 100-02-7 X X X X X,Pentachlorophenol 87-86-5 X X X X X,Phenol 108-95-2 DC(28) X X X X,2,3,4,5-Tetrachlorophenol 4901-51-3 ND ND ND ND ND,2,3,4,6-Tetrachlorophenol 58-90-2 X ND ND ND X,2,3,5,6-Tetrachlorophenol 935-95-5 ND ND ND ND ND,2,4,5-Trichlorophenol 95-95-4 X X ND X X,2,4,6-Trichlorophenol 88-06-2 X X X X X,a Chemical Abstract Service Registry Number.,DC = Unfavorable distribution coefficient (number in parenthesis is percent recovery).,LR = Low response.,ND = Not determined.,X = Greater than 70 percent recovery by this technique.,1.2 The single-column approach involves the use of a wide-bore fused-silica open tubular,column for analysis. The fused-silica, open-tubular wide-bore column offers improved resolution,better selectivity, increased sensitivity, and faster analysis than packed columns.,1.3 The dual-column/dual-detector approach involves the use of two wide-bore fused-silica,open-tubular columns of different polarities. The columns are connected to an injection tee and two,identical detectors.,CD-ROM 8041 - 2 Revision 0,December 1996,1.4 Phenols may be analyzed underivatized by FID, although the sensitivity of the method,may not be suitable for all needs.,1.5 This method also includes a procedure for the derivatization of the phenols and,identification of the target phenols as methylated phenols (anisoles) and as pentafluorobenzylbromo,ether derivatives (PFBBr). Three phenols failed to derivatize under the PFBBr method protocol: 2,4-,dinitrophenol, 2-methyl-4,6- dinitrophenol, and Dinoseb.,1.6 The following non-RCRA analytes may also be analyzed by this method:,Compound CAS No.,2-Chloro-5-methylphenol 615-74-7,4-Chloro-2-methylphenol 1570-64-5,3-Chlorophenol 108-43-0,4-Chlorophenol 106-48-9,2,3-Dichlorophenol 576-24-9,2,5-Dichlorophenol 583-78-8,3,4-Dichlorophenol 95-77-2,3,5-Dichlorophenol 591-35-5,2,3-Dimethylphenol 526-75-0,2,5-Dimethylphenol 95-87-4,2,6-Dimethylphenol 576-26-1,3,4-Dimethylphenol 95-65-8,2,5-Dinitrophenol 329-71-5,3-Nitrophenol 554-84-7,2,3,4-Trichlorophenol 15950-66-0,2,3,5-Trichlorophenol 933-78-8,2,3,6-Trichlorophenol 933-75-5,1.7 This method is restricted to use by or under the supervision of analysts experienced in,the use of a gas chromatograph and in the interpretation of gas chromatograms. Each analyst must,demonstrate the ability to generate acceptable results with this method.,1.8 Only experienced analysts should be allowed to work with diazomethane due to the,potential hazards associated with its use (explosive, carcinogenic).,2.0 SUMMARY OF METHOD,2.1 Samples are extracted using an appropriate sample preparation method. Prior to,analysis, the extracts are cleaned up, as necessary, and the solvent exchanged to 2-propanol.,2.2 Underivatized phenols may be analyzed by FID, using either the single-column or dualcolumn,approach.,2.3 The target phenols also may be derivatized with diazomethane or pentafluorobenzyl,bromide (PFBBr) and analyzed by gas chromatography.,CD-ROM 8041 - 3 Revision 0,December 1996,3.0 INTERFERENCES,3.1 Contamination by carryover can occur whenever high-concentration and lowconcentration,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,is encountered, it should be followed by the analysis of a solvent blank to check for crosscontamination.,Column blanks should be analyzed whenever the analysis of a solvent blank,indicates cross-contamination.,3.2 In certain cases some compounds coelute on either one or both columns. In these cases,the compo……
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