EPA Method 8141A Organophosphorus Compounds by Gas Chromatography_ Capillary Column Technique - Revision 1
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1D9EEE88C9D94DBD99CE3161D5E2D778 |
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0.23 |
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35 |
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日期： |
2003-1-16 |
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CD-ROM 8141A - 1 Revision 1,September 1994,METHOD 8141A,ORGANOPHOSPHORUS COMPOUNDS BY GAS CHROMATOGRAPHY:,CAPILLARY COLUMN TECHNIQUE,1.0 SCOPE AND APPLICATION,1.1 Method 8141 is a capillary gas chromatographic (GC) method used to,determine the concentration of organophosphorus (OP) compounds. The fusedsilica,open-tubular columns specified in this method offer improved resolution,better selectivity, increased sensitivity, and faster analysis than packed,columns. The compounds listed in the table below can be determined by GC using,capillary columns with a flame photometric detector (FPD) or a nitrogenphosphorus,detector (NPD). Triazine herbicides can also be determined with this,method when the NPD is used. Although performance data are presented for each,of the listed chemicals, it is unlikely that all of them could be determined in,a single analysis. This limitation results because the chemical and,chromatographic behavior of many of these chemicals can result in co-elution.,The analyst must select columns, detectors and calibration procedures for the,specific analytes of interest in a study. Any listed chemical is a potential,method interference when it is not a target analyte.,Compound Name CAS Registry No.,OP Pesticides,Aspon,b 3244-90-4,Azinphos-methyl 86-50-0,Azinphos-ethyla 2642-71-9,Bolstar (Sulprofos) 35400-43-2,Carbophenothiona 786-19-6,Chlorfenvinphosa 470-90-6,Chlorpyrifos 2921-88-2,Chlorpyrifos methyla 5598-13-0,Coumaphos 56-72-4,Crotoxyphosa 7700-17-6,Demeton-Oc 8065-48-3,Demeton-Sc 8065-48-3,Diazinon 333-41-5,Dichlorofenthiona 97-17-6,Dichlorvos (DDVP) 62-73-7,Dicrotophosa 141-66-2,Dimethoate 60-51-5,Dioxathiona,c 78-34-2,Disulfoton 298-04-4,EPN 2104-64-5,Ethiona 563-12-2,Ethoprop 13194-48-4,Famphura 52-85-7,Fenitrothiona 122-14-5,Fensulfothion 115-90-2,CD-ROM 8141A - 2 Revision 1,September 1994,Compound Name CAS Registry No.,Fonophosa 944-22-9,Fenthion 55-38-9,Leptophosa,d 21609-90-5,Malathion 121-75-5,Merphosc 150-50-5,Mevinphose 7786-34-7,Monocrotophos 6923-22-4,Naled 300-76-5,Parathion, ethyl 56-38-2,Parathion, methyl 298-00-0,Phorate 298-02-2,Phosmeta 732-11-6,Phosphamidona 13171-21-6,Ronnel 299-84-3,Stirophos (Tetrachlorovinphos) 22248-79-9,Sulfotepp 3689-24-5,TEPPd 21646-99-1,Terbufosa 13071-79-9,Thionazina,b (Zinophos) 297-97-2,Tokuthionb (Protothiofos) 34643-46-4,Trichlorfona 52-68-6,Trichloronateb 327-98-0,Industrial Chemicals,Hexamethylphosphoramidea (HMPA) 680-31-9,Tri-o-cresylphosphatea,d (TOCP) 78-30-8,Triazine Herbicides (NPD only),Atrazinea 1912-24-9,Simazinea 122-34-9,a This analyte has been evaluated using a 30-m column only.,b Production discontinued in the U.S., standard not readily available.,c Standards may have multiple components because of oxidation.,d Compound is extremely toxic or neurotoxic.,e Adjacent major/minor peaks can be observed due to cis/trans isomers.,1.2 A dual-column/dual-detector approach may be used for the analysis of,relatively clean extracts. Two 15- or 30-m x 0.53-mm ID fused-silica, opentubular,columns of different polarities are connected to an injection tee and,each is connected to a detector. Analysts are cautioned regarding the use of a,dual column configuration when their instrument is subject to mechanical stress,CD-ROM 8141A - 3 Revision 1,September 1994,when many samples are analyzed over a short time, or when extracts of,contaminated samples are analyzed.,1.3 Two detectors can be used for the listed OP chemicals. The FPD works,by measuring the emission of phosphorus- or sulfur-containing species. Detector,performance is optimized by selecting the proper optical filter and adjusting the,hydrogen and air flows to the flame. The NPD is a flame ionization detector with,a rubidium ceramic flame tip which enhances the response of phosphorus- and,nitrogen-containing analytes. The FPD is more sensitive and more selective, but,is a less common detector in environmental laboratories.,1.4 Table 1 lists method detection limits (MDLs) for the target analytes,using 15-m columns and FPD, for water and soil matrices. Table 2 lists the,estimated quantitation limits (EQLs) for other matrices. MDLs and EQLs using 30-,m columns will be very similar to those obtained from 15-m columns.,1.5 The use of a 15-m column system has not been fully validated for the,determination of the following compounds. The analyst must demonstrate,chromatographic resolution of all analytes, recoveries of greater than 70,percent, with precision of no more than 15 percent RSD, before data generated on,the 15-m column system can be reported for these, or any additional, analytes:,Azinphos-ethyl Ethion Phosmet,Carbophenothion Famphur Phosphamidon,Ch……
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