EPA Method 609 Nitroaromatics and Isophorone
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ID： |
4E9D90C8E1C047028D6709B12D1166EF |
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文件大小(MB)： |
0.13 |
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页数： |
19 |
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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 609—NITROAROMATICS AND ISOPHORONE,1. Scope and Application,1.1 This method covers the determination of certain nitroaromatics and isophorone. The,following parameters may be determined by this method:,Parameter STORET No. CAS No.,2,4-Dinitrotoluene . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34611 121-14-2,2,6-Dinitrotoluene . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34626 606-20-2,Isophorone . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34408 78-59-1,Nitrobenzene . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34447 98-95-3,1.2 This is a gas chromatographic (GC) 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 a second gas chromatographic column that can be used to confirm measurements,made with the primary column. 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.,1.4 The sample extraction and concentration steps in this method are essentially the same,as in Methods 606, 608, 611, and 612. Thus, a single sample may be extracted to,measure the parameters included in the scope of each of these methods. When,cleanup is required, the concentration levels must be high enough to permit selecting,aliquots, as necessary, to apply appropriate cleanup procedures. The analyst is,allowed the latitude, under Section 12, to select chromatographic conditions,appropriate for the simultaneous measurement of combinations of these parameters.,1.5 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.,1.6 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 extracted with methylene,chloride using a separatory funnel. The methylene chloride extract is dried and,exchanged to hexane during concentration to a volume of 10 mL or less. Isophorone,and nitrobenzene are measured by flame ionization detector gas chromatography,(FIDGC). The dinitrotoluenes are measured by electron capture detector gas,chromatography (ECDGC).2,2.2 The method provides a Florisil column cleanup procedure to aid in the elimination of,interferences that may be encountered.,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,baseliles 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.3 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 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 with aluminum foil.,3.1.2 The use of……
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