EPA Method 607 Nitrosamines
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ID： |
560DBDCCDF07481EAEB8FF4E0004FDDE |
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文件大小(MB)： |
0.14 |
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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 607—NITROSAMINES,1. Scope and Application,1.1 This method covers the determination of certain nitrosamines. The following,parameters can be determined by this method:,Parameter Storet No. CAS No.,N-Nitrosodimethylamine . . . . . . . . . . . . . . . 34438 62-75-9,N-Nitrosodiphenylamine . . . . . . . . . . . . . . . 34433 86-30-6,N-Nitrosodi-n-propylamine . . . . . . . . . . . . . 34428 621-64-7,1.2 This is a gas chromatographic (GC) method applicable to the determination of the,parameters listed above in municipal and industrial discharges as provided under,40 CFR 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 N-nitrosodi-n-propylamine. In order to confirm the,presence of N-nitrosodiphenylamine, the cleanup procedure specified in Section 11.3,or 11.4 must be used. In order to confirm the presence of N-nitrosodimethylamine by,GC/MS, Column 1 of this method must be substituted for the column recommended,in Method 625. Confirmation of these parameters using GC-high resolution mass,spectrometry or a Thermal Energy Analyzer is also recommended.1,2,1.3 The method detection limit (MDL, defined in Section 14.1)3 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 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 extracted with methylene,chloride using a separatory funnel. The methylene chloride extract is washed with,dilute hydrochloric acid to remove free amines, dried, and concentrated to a volume,of 10 mL or less. After the extract has been exchanged to methanol, it is separated by,gas chromatography and the parameters are then measured with a,nitrogen-phosphorus detector.4,2.2 The method provides Florisil and alumina column cleanup procedures to separate,diphenylamine from the nitrosamines and 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.5 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. Solvent rinses with,acetone and pesticide quality hexane may be substituted for the muffle furnace,heating. 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 helps to minimize interference,problems. Purification of solvents by distillation in all-glass systems may be,required.,3.2 Matrix interferences may be caused by contaminants that are co-extracted from the,sample. The extent of matrix interferences will vary considerably from source to,source, depending upon the nature and diversity of the industrial complex or,municipality being sampled. The cleanup procedures in Section 11 can be used to,overcome many of the……
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