EPA Method 8100 Polynuclear Aromatic Hydrocarbons - Revision 0
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1DBE4E76DDE54CD4BDAFB40F5875FDE4 |
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0.1 |
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10 |
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2003-1-16 |
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8100 1,CD-ROM Revision 0,Date September 1986,METHOD 8100,POLYNUCLEAR AROMATIC HYDROCARBONS,1.0 SCOPE AND APPLICATION,1.1 Method 8100 is used to determine the concentration of certain,polynuclear aromatic hydrocarbons (PAH). Table 1 indicates compounds that may,be determined by this method.,1.2 The packed column gas chromatographic method described here cannot,adequately resolve the following four pairs of compounds: anthracene and,phenanthrene; chrysene and benzo(a)anthracene; benzo(b)fluoranthene and,benzo(k)fluoranthene; and dibenzo(a,h)anthracene and indeno(1,2,3-cd)pyrene. The,use of a capillary column instead of the packed column, also described in this,method, may adequately resolve these PAHs. However, unless the purpose of the,analysis can be served by reporting a quantitative sum for an unresolved PAH,pair, either liquid chromatography (Method 8310) or gas chroma-tography/mass,spectroscopy (Method 8270) should be used for these compounds.,2.0 SUMMARY OF METHOD,2.1 Method 8100 provides gas chromatographic conditions for the detection,of ppb levels of certain polynuclear aromatic hydrocarbons. Prior to use of this,method, appropriate sample extraction techniques must be used. Both neat and,diluted organic liquids (Method 3580, Waste Dilution) may be analyzed by direct,injection. A 2- to 5-uL aliquot of the extract is injected into a gas,chromatograph (GC) using the solvent flush technique, and compounds in the GC,effluent are detected by a flame ionization detector (FID).,2.2 If interferences prevent proper detection of the analytes of interest,the method may also be performed on extracts that have undergone cleanup using,silica gel column cleanup (Method 3630).,3.0 INTERFERENCES,3.1 Refer to Methods 3500, 3600, and 8000.,3.2 Solvents, reagents, glassware, and other sample processing hardware may,yield discrete artifacts and/or elevated baselines causing misinterpretation of,gas chromatograms. All of these materials must be demonstrated to be free from,interferences, under the conditions of the analysis, by analyzing method blanks.,Specific selection of reagents and purification of solvents by distillation in,all-glass systems may be required.,3.3 Interferences coextracted from samples will vary considerably from,source to source, depending upon the waste being sampled. Although general,cleanup techniques are recommended as part of this method, unique samples may,require additional cleanup.,8100 2,CD-ROM Revision 0,Date September 1986,TABLE 1. GAS CHROMATOGRAPHY OF POLYNUCLEAR AROMATIC HYDROCARBONSa,Compound Retention time (min),Acenaphthene 10.8,Acenaphthylene 10.4,Anthracene 15.9,Benzo(a)anthracene 20.6,Benzo(a)pyrene 29.4,Benzo(b)fluoranthene 28.0,Benzo(j)fluoranthene,Benzo(k)fluoranthene 28.0,Benzo(ghi)perylene 38.6,Chrysene 24.7,Dibenz(a,h)acridine,Dibenz(a,j)acridine,Dibenzo(a,h)anthracene 36.2,7H-Dibenzo(c,g)carbazole,Dibenzo(a,e)pyrene,Dibenzo(a,h)pyrene,Dibenzo(a,i)pyrene,Fluoranthene 19.8,Fluorene 12.6,Indeno(1,2,3-cd)pyrene 36.2,3-Methylcholanthrene,Naphthalene 4.5,Phenanthrene 15.9,Pyrene 20.6,aResults obtained using Column 1.,8100 3,CD-ROM Revision 0,Date September 1986,4.0 APPARATUS AND MATERIALS,4.1 Gas chromatograph:,4.1.1 Gas chromatograph: Analytical system complete with gas,chromatograph suitable for on-column injections and all required,accessories, including detectors, column supplies, recorder, gases, and,syringes. A data system for measuring peak areas and/or peak heights is,recommended.,4.1.2 Columns:,4.1.2.1 Column 1: 1.8-m x 2-mm I.D. glass column packed with 3%,OV-17 on Chromosorb W-AW-DCMS (100/120 mesh) or equivalent.,4.1.2.2 Column 2: 30-m x 0.25-mm I.D. SE-54 fused silica,capillary column.,4.1.2.3 Column 3: 30-m x 0.32-mm I.D. SE-54 fused silica,capillary column.,4.1.3 Detector: Flame ionization (FID).,4.2 Volumetric flask: 10-, 50-, and 100-mL, ground-glass stopper.,4.3 Microsyringe: 10-uL.,5.0 REAGENTS,5.1 Solvents: Hexane, isooctane (2,2,4-trimethylpentane) (pesticide,quality or equivalent).,5.2 Stock standard solutions:,5.2.1 Prepare stock standard solutions at a concentration of 1.00,ug/uL by dissolving 0.0100 g of assayed reference material in isooctane and,diluting to volume in a 10-mL volumetric flask. Larger volumes can be used,at the convenience of the analyst. When compound purity is assayed to be,96% or greater, the weight can be used without correction to calculate the,concentration of the stock standard. Commercially prepared stock standards,can be used at any concentration if they are certified by the manufacturer,or by an independent source.,5.2.2 Transfer the stock standard solutions into Teflon-sealed screwcap,bottles.……
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