EPA Method 8061A Phthalate Esters by Gas Chromatography with Electron Capture Detection (GC_ECD) - Revision 1
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EA2C984BEB044498B8AFBEE4FA1DD281 |
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0.08 |
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页数： |
18 |
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日期： |
2003-1-16 |
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CD-ROM 8061A - 1 Revision 1,December 1996,METHOD 8061A,PHTHALATE ESTERS BY GAS CHROMATOGRAPHY,WITH ELECTRON CAPTURE DETECTION (GC/ECD),1.0 SCOPE AND APPLICATION,1.1 Method 8061 is used to determine the identities and concentrations of various phthalate,esters in aqueous and solid matrices including groundwater, leachate, soil, sludge and sediment.,The following compounds can be determined by this method:,______________________________________________________________________________,Compound Name CAS No.a,Benzyl benzoate (Int. Std.) 120-51-4,Bis(2-ethylhexyl) phthalate 117-81-7,Butyl benzyl phthalate 85-68-7,Di-n-butyl phthalate 84-74-2,Diethyl phthalate 84-66-2,Dimethyl phthalate 131-11-3,Di-n-octyl phthalate 117-84-0,______________________________________________________________________________,a Chemical Abstract Service Registry Number.,1.2 Table 1 lists the method detection limits (MDLs) for the target analytes in a water matrix.,The MDLs for the components of a specific sample may differ from those listed in Table 1 because,MDLs depend on the nature of interferences in the sample matrix. Table 2 lists the estimated,quantitation limits (EQLs) for other matrices.,1.3 The following compounds may also be analyzed by this procedure or may be used as,surrogates:,Compound Name CAS No.a,Bis(2-n-butoxyethyl) phthalate 117-83-9,Bis(2-ethoxyethyl) phthalate 605-54-9,Bis(2-methoxyethyl) phthalate 117-82-8,Bis(4-methyl-2-pentyl) phthalate 146-50-9,Diamyl phthalate 131-18-0,Dicyclohexyl phthalate 84-61-7,Dihexyl phthalate 84-75-3,Diisobutyl phthalate 84-69-5,Dinonyl phthalate 84-76-4,Hexyl 2-ethylhexyl phthalate 75673-16-4,1.4 When this method is used to analyze for any or all of the target analytes, compound,identification should be supported by at least one additional qualitative technique. This method,describes conditions for parallel column, dual electron capture detector analysis which fulfills the,above requirement. Retention time information obtained on two megabore fused-silica open tubular,CD-ROM 8061A - 2 Revision 1,December 1996,columns is given in Table 1. Alternatively, gas chromatography/mass spectrometry could be used,for compound confirmation.,1.5 Phthalate esters will hydrolyze below pH 5 and above pH 7. The amount of hydrolysis,will increase with increasing or decreasing pH and with longer contact times.,1.6 This method is restricted for use by, or under the supervision of, analysts experienced,in the use of gas chromatographs and skilled in the interpretation of gas chromatograms. Each,analyst must demonstrate the ability to generate acceptable results with this method.,2.0 SUMMARY OF METHOD,2.1 A measured volume or weight of sample (approximately 1 liter for liquids, 10 to 30 grams,for solids and sludges) is extracted using an appropriate 3500 series method.,2.1.1 Aqueous samples are extracted at a pH of 5 to 7, with methylene chloride, in a,separatory funnel (Method 3510). Alternatively, particulate-free aqueous samples can be,filtered through membrane disks that contain C -bonded silica (Method 3535). The phthalate 18,esters are retained by the bonded silica, eluted with acetonitrile, then exchanged to hexane.,Using either method, aqueous samples should not be adjusted to basic pH, as phthalate esters,will hydrolyze. Method 3520 is not recommended for the extraction of aqueous samples,containing phthalates because the longer chain esters (dihexyl phthalate, bis(2-ethylhexyl),phthalate, di-n-octyl phthalate, and dinonyl phthalate) tend to adsorb to the glassware and,consequently, their extraction recoveries are less than 40 percent.,2.1.2 Solid samples are extracted with methylene chloride/acetone (1:1) or,hexane/acetone (1:1) using an appropriate 3500 series method. After cleanup, the extract is,analyzed by gas chromatography with electron capture detection (GC/ECD).,The methylene chloride/acetone solvent system has generally been found to be more,effective at extracting the analytes of interest from solid matrices. The hexane/acetone solvent,system may be appropriate in instances where specific interferences are expected.,2.2 The sensitivity of Method 8061 usually depends on the level of interferences rather than,on instrumental limitations. If interferences prevent detection of the analytes, cleanup of the sample,extracts is necessary. Either Method 3610 or 3620 alone or followed by Method 3660, Sulfur,Cleanup, may be used to eliminate interferences in the analysis. Method 3640, Gel Permeation,Cleanup, is applicable for samples that contain high amounts of lipids and waxes.,3.0 INTERFERENCES,3.1 Refer to Methods 3500, 3600, and 8000.,3.2 Interferences coextra……
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