EPA Method 1671 Volatile Organic Compounds Specific to the Pharmaceutical Manufacturing Industry by GC_FID
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9AA3B9C5DA254FD68826E695A5292189 |
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文件大小(MB)： |
0.04 |
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页数： |
19 |
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日期： |
2008-2-26 |
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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）：
Method 1671,Volatile Organic Compounds Specific to the Pharmaceutical,Manufacturing Industry by GC/FID,Revision A, July 1998,2,Method 1671, Revision A,Volatile Organic Compounds Specific to the Pharmaceutical,Manufacturing Industry by GC/FID,1.0 Scope and Application,1.1 This method is for surveying and monitoring under the Clean Water Act. The method is used to,determine certain non-purgeable volatile organic pollutants specific to the pharmaceutical,manufacturing industry (PMI) that are amenable to direct aqueous injection gas chromatography,(GC) and detection by a flame ionization detector (FID).,1.2 The PMI analytes listed in Table 1 may be determined in waters, soils, and municipal sludges by this,method.,1.3 The detection limits of Method 1671 are usually dependent on the level of interferences rather than,instrumental limitations. The minimum levels (MLs) in Table 2 are the level that can be attained,with no interferences present.,1.4 This method is recommended for use by, or under the supervision of, analysts experienced in the,operation of gas chromatographs and in the interpretation of chromatograms.,1.5 This method is performance-based. The analyst is permitted to modify the method to overcome,interferences or to lower the cost of measurements, provided that all performance criteria in this,method are met. The requirements for establishing method equivalency are given in Section 9.2.,2.0 Summary of the Method,2.1 The percent solids content of the sample is determined. If the solids content is less than 1%, an,internal standard(s) is added to a 5-mL sample. If the solids content of the sample is greater than,1%, 5 mL of reagent water and an internal standard(s) is added to a 5-g aliquot of sample.,The mixture is sonicated in a centrifuge tube with little or no headspace for 5 minutes. During this,period the analytes and the internal standard will equilibrate between the solid and aqueous phases.,In some cases, additional sonication will be necessary to establish equilibrium. The resulting,suspension is centrifuged and the supernatant liquid analyzed.,2.2 An appropriate amount of the aqueous solution (or supernate) is injected into the GC. The,compounds are separated by the GC and detected by the FID.,3.0 Definitions,There are no definitions specific to this method.,Method 1671, Revision A,3,4.0 Interferences,4.1 Impurities in the carrier gas, organic compounds outgassing from the GC plumbing, and solvent,vapors in the laboratory account for the majority of contamination problems encountered with this,method. The analytical system is demonstrated to be free from interferences under conditions of the,analysis by analyzing reagent water blanks initially and with each sample batch (samples analyzed,on the same 12-hour shift), as described in Section 9.4.,4.2 Samples can be contaminated by diffusion of volatile organic compounds through the bottle seal,during shipment and storage. A field blank prepared from reagent water and carried through the,sampling and handling protocol may serve as a check on such contamination.,4.3 Contamination by carryover can occur when high-level and low-level samples are analyzed,sequentially. To reduce carryover, the syringe is cleaned or replaced with a new syringe after each,sample is analyzed. When an unusually concentrated sample is encountered, it is followed by,analysis of a reagent water blank to check for carryover. Syringes are cleaned by washing with soap,solution, rinsing with tap and distilled water, and drying in an oven at 100-125EC. Other parts of,the system are also subject to contamination; therefore, frequent bakeout and purging of the entire,system may be required.,4.4 Interferences resulting from samples will vary considerably from source to source, depending on the,diversity of the site being sampled.,5.0 Safety,The toxicity or carcinogenicity of each analyte, compound, or reagent used in this method has not,been precisely determined; however, each chemical compound should be treated as a potential health,hazard. Exposure to these compounds should be reduced to the lowest possible level. The,laboratory is responsible for maintaining a current awareness file of OSHA regulations regarding,the safe handling of the chemicals specified in this method. A reference file of material safety data,sheets should also be made available to all personnel involved in these analyses. Additional,information on laboratory safety can be found in References 2-4.,6.0 Equipment and Supplies,6.1 Sample bottles and septa,6.1.1 BottlesS25- to 40-mL with polytetrafluoroethylene (PTFE)-lined screw-cap (Pierce 13075,or equivalent). Detergent wash……
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