EPA Method 611 Haloethers

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FB55D5A5FD35402FA79B30AE7B045204

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日期:

2003-1-16

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APPENDIX A TO PART 136,METHODS FOR ORGANIC CHEMICAL ANALYSIS OF MUNICIPAL AND,INDUSTRIAL WASTEWATER,METHOD 611—HALOETHERS,1. Scope and Application,1.1 This method covers the determination of certain haloethers. The following parameters,can be determined by this method:,Parameter STORET No. CAS No.,Bis(2-chloroethyl) ether . . . . . . . . . . . . . . . . . . . . . . . . . 34273 111-44-4,Bis(2-chloroethoxy) methane . . . . . . . . . . . . . . . . . . . . . 34278 111-91-1,Bis(2-chloroisopropyl) ether . . . . . . . . . . . . . . . . . . . . . . 34283 108-60-1,4-Bromophenyl phenyl ether . . . . . . . . . . . . . . . . . . . . . 34636 101-55-3,4-Chlorophenyl phenyl ether . . . . . . . . . . . . . . . . . . . . . 34641 7005-72-3,1.2 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, 609, 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. The extract,is separated by gas chromatography and the parameters are then measured with a,halide specific detector.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,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.3 Clean all glassware as soon as,possible after use by rinsing with the last solvent used in it. Solvent rinsing,should be followed be 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 high purity reagents and solvents hel……

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