EPA Method 8315A Determination of Carbonyl Compounds by High Performance Liquid Chromatography (HPLC)
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9AB2901F4AF840718D4155885037AACF |
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文件大小(MB)： |
0.18 |
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页数： |
34 |
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日期： |
2009-12-11 |
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CD-ROM 8315A - 1 Revision 1,December 1996,METHOD 8315A,DETERMINATION OF CARBONYL COMPOUNDS,BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC),1.0 SCOPE AND APPLICATION,1.1 This method provides procedures for the determination of free carbonyl compounds in,various matrices by derivatization with 2,4-dinitrophenylhydrazine (DNPH). The method utilizes high,performance liquid chromatography (HPLC) with ultraviolet/visible (UV/vis) detection to identify and,quantitate the target analytes. This method includes two procedures encompassing all aspects of,the analysis (extraction to determination of concentration). Procedure 1 is appropriate for the,analysis of aqueous, soil and waste samples and stack samples collected by Method 0011.,Procedure 2 is appropriate for the analysis of indoor air samples collected by Method 0100. The list,of target analytes differs by procedure. The appropriate procedure for each target analyte is listed,in the table below.,Compound CAS No.a Proc. 1b Proc. 2b,Acetaldehyde 75-07-0 X X,Acetone 67-64-1 X,Acrolein 107-02-8 X,Benzaldehyde 100-52-7 X,Butanal (Butyraldehyde) 123-72-8 X X,Crotonaldehyde 123-73-9 X X,Cyclohexanone 108-94-1 X,Decanal 112-31-2 X,2,5-Dimethylbenzaldehyde 5779-94-2 X,Formaldehyde 50-00-0 X X,Heptanal 111-71-7 X,Hexanal (Hexaldehyde) 66-25-1 X X,Isovaleraldehyde 590-86-3 X,Nonanal 124-19-6 X,Octanal 124-13-0 X,Pentanal (Valeraldehyde) 110-62-3 X X,Propanal (Propionaldehyde) 123-38-6 X X,m-Tolualdehyde 620-23-5 X X,o-Tolualdehyde 529-20-4 X,p-Tolualdehyde 104-87-0 X,a Chemical Abstract Service Registry Number.,b The two procedures have overlapping lists of target compounds that have been,evaluated using modifications of the analysis. Refer to the respective procedure number,when choosing the appropriate analysis technique for a particular compound.,1.2 Method detection limits (MDL) using procedure 1 are listed in Tables 1 and 2. Sensitivity,data for sampling and analysis by use of Method 0100 (procedure 2) are given in Table 3. The MDL,CD-ROM 8315A - 2 Revision 1,December 1996,for a specific sample may differ from the listed value, depending upon the interferences in the,sample matrix and the volume of sample used in the procedure.,1.3 The extraction procedure for solid samples is outlined in Sec. 7.1 of this method.,1.4 When this method is used to analyze unfamiliar sample matrices, compound identification,should be supported by at least one additional qualitative technique. A gas chromatograph/mass,spectrometer (GC/MS) may be used for the qualitative confirmation of results for the target analytes,using the extract produced by this method.,1.5 This method is restricted to use by, or under the supervision of, analysts experienced in,the use of chromatography and in the interpretation of chromatograms. Each analyst must,demonstrate the ability to generate acceptable results with this method.,2.0 SUMMARY OF METHOD,This method contains two procedures dealing with different sample types.,2.1 Liquid and Solid Samples (Procedure 1),2.1.1 For wastes comprised of solids, and aqueous wastes containing greater than one,percent solid material, the aqueous phase should be separated from the solid phase and,stored, according to Sec. 6.2, for possible later analysis. If necessary, the particle size of the,solids in the waste is reduced. The solid phase is extracted with a volume of fluid equal to 20,times the sample's weight. The extraction fluid employed is a function of the alkalinity of the,solid phase of the waste. A special extractor is used when volatiles are being extracted.,Following extraction, the extract is filtered through a 0.6 - 0.8 μm glass fiber filter.,2.1.2 If compatible (i.e., multiple phases will not form on combination), the initial,aqueous phase of the waste is added to the aqueous extract, and these liquids are analyzed,together. If incompatible, the liquids are analyzed separately and the results are,mathematically combined to yield a volume-weighted average concentration.,2.1.3 A measured volume of aqueous sample (approx. 100 mL) or an appropriate,amount of solids extract (approx. 25 g), is buffered to pH 3 and derivatized with 2,4-,dinitrophenylhydrazine (DNPH), using either the appropriate solid-phase or a liquid-liquid,extraction technique. If the solid-phase extraction (SPE) option is used, the derivatized,compound is extracted using solid sorbent cartridges, then eluted with ethanol. If the liquidliquid,option is used, the derivatized compound is serially extracted three (3) times with,methylene chloride. The methylene chloride extracts are concentrated using the appropriate,procedure 3500 series method and exchanged wi……
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