EPA Method 604 Phenols
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ID： |
9C4A7219CBF64CE79E3C3474D5B6AF6E |
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文件大小(MB)： |
0.2 |
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页数： |
22 |
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文件格式： |
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日期： |
2003-1-16 |
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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）：
APPENDIX A TO PART 136,METHODS FOR ORGANIC CHEMICAL ANALYSIS OF MUNICIPAL AND,INDUSTRIAL WASTEWATER,METHOD 604—PHENOLS,1. Scope and Application,1.1 This method covers the determination of phenol and certain substituted phenols. The,following parameters may be determined by this method:,Parameter STORET CAS No.,No.,4-Chloro-3-methylphenol . . . . . . . . . . . . . . . 34452 59-50-7,2—Chlorophenol . . . . . . . . . . . . . . . . . . . . . 34586 95-57-8,2,4-Dichlorophenol . . . . . . . . . . . . . . . . . . . 34601 120-83-2,2,4-Dimethylphenol. . . . . . . . . . . . . . . . . . . 34606 105-67-9,2,4-Dinitrophenol . . . . . . . . . . . . . . . . . . . . 34616 51-28-5,2-Methyl-4,6-dinitrophenol . . . . . . . . . . . . . 34657 534-52-1,2-Nitrophenol . . . . . . . . . . . . . . . . . . . . . . . 34591 88-75-5,4-Nitrophenol . . . . . . . . . . . . . . . . . . . . . . . 34646 100-02-7,Pentachlorophenol . . . . . . . . . . . . . . . . . . . . 39032 87-86-5,Phenol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34694 108-95-2,2,4,6-Trichlorophenol . . . . . . . . . . . . . . . . . . 34621 88-06-2,1.2 This is a flame ionization detector gas chromatographic (FIDGC) method applicable to,the determination of the compounds listed above in municipal and industrial discharges,as provided under 40 CFR Part 136.1. When this method is used to analyze unfamiliar,samples for any or all of the compounds above, compound identifications should be,supported by at least one additional qualitative technique. This method describes,analytical conditions for derivatization, cleanup, and electron capture detector gas,chromatography (ECDGC) that can be used to confirm measurements made by FIDGC.,Method 625 provides gas chromatograph/mass spectrometer (GC/MS) conditions,appropriate for the qualitative and quantitative confirmation of results for all of the,parameters listed above, using the extract produced by this method.,1.3 The method detection limit (MDL, defined in Section 14.1)1 for each parameter is listed,in Table 1. The MDL for a specific wastewater may differ from those listed, depending,upon the nature of interferences in the sample matrix. The MDL listed in Table 1 for,each parameter was achieved with a flame ionization detector (FID). The MDLs that,were achieved when the derivatization cleanup and electron capture detector (ECD) were,employed are presented in Table 2.,1.4 Any modification of this method, beyond those expressly permitted, shall be considered,as a major modification subject to application and approval of alternate test procedures,under 40 CFR Parts 136.4 and 136.5.,1.5 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,using the procedure described in Section 8.2.,2. Summary of Method,2.1 A measured volume of sample, approximately 1 L, is acidified and extracted with,methylene chloride using a separatory funnel. The methylene chloride extract is dried,and exchanged to 2-propanol during concentration to a volume of 10 mL or less. The,extract is separated by gas chromatography and the phenols are then measured with an,FID.2,2.2 A preliminary sample wash under basic conditions can be employed for samples having,high general organic and organic base interferences.,2.3 The method also provides for a derivatization and column chromatography cleanup,procedure to aid in the elimination of interferences.2,3 The derivatives are analyzed by,ECDGC.,3. Interferences,3.1 Method interferences may be caused by contaminants in solvents, reagents, glassware,and other sample processing hardware that lead to discrete artifacts and/or elevated,baselines in gas chromatograms. All of these materials must be routinely demonstrated,to be free from interferences under the conditions of the analysis by running laboratory,reagent blanks as described in Section 8.1.3.,3.1.1 Glassware must be scrupulously cleaned.4 Clean all glassware as soon as possible,after use by rinsing with the last solvent used in it. Solvent rinsing should be,followed by detergent washing with hot water, and rinses with tap water and,distilled water. The glassware should then be drained dry, and heated in a,muffle furnace at 400°C for 15-30 minutes. Some thermally stable materials, such,as PCBs, may not be eliminated by this treatment. Solvent rinses with acetone,and pesticide quality hexane may be substituted for the muffle furnace heating.,Thorough rinsing with such solvents usually eliminates PCB interference.,Volumetric w……
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