1、Designation: D 5831 03Standard Test Method forScreening Fuels in Soils1This standard is issued under the fixed designation D 5831; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses i
2、ndicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method is a screening procedure for determin-ing the presence of fuels containing aromatic compounds insoils. If the contaminant fuel is available
3、for calibration, theapproximate concentration of the fuel in the soil can becalculated. If the contaminant fuel type is known, but thecontaminant fuel is not available for calibration, an estimate ofthe concentration of the fuel in the soil can be determined usingaverage response factors. If the nat
4、ure of the contaminant fuelis unknown, this screening test method can be used to identifythe possible presence of contamination.1.2 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish
5、appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterE 131 Terminology Relating to Molecul
6、ar SpectroscopyE 169 Practices for General Techniques of Ultraviolet-Visible Quantitative AnalysisE 177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE 275 Practice for Describing and Measuring Performanceof Ultraviolet, Visible, and Near-Infrared Spectrophotom-etersE 691 Pract
7、ice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE 925 Practice for Monitoring the Calibration ofUltraviolet-Visible Spectrophotometers whose SpectralSlit Width does not Exceed 2 nm3. Terminology3.1 DefinitionsFor definitions of terms used in thisscreening test m
8、ethod, refer to Terminology E 131.4. Summary of Test Method4.1 Asample of soil is extracted with isopropyl alcohol, andthe extract is filtered. The ultraviolet absorbance of the extractis measured at 254 nm. If the contaminant fuel is available forcalibration, the approximate concentration of contam
9、ination iscalculated. If the contaminant fuel type is known, but thecontaminant fuel is not available for calibration, an estimate ofthe contaminant concentration is determined using averageresponse factors. If the nature of the contaminant fuel is notknown, the absorbance value is used to indicate
10、the presence orabsence of fuel contamination. Calcium oxide is added to thesoil as a conditioning agent to minimize interferences fromhumic materials and moisture present in the soil. Particulateinterferences are removed by passing the extract through afilter.5. Significance and Use5.1 This test met
11、hod is a screening procedure for determin-ing the presence of fuels containing aromatic compounds insoils. If the contaminant fuel is available for calibration, theapproximate concentration of the fuel in the soil can becalculated. If the fuel type is known, but the contaminant fuelis not available
12、for calibration, an estimate of the contaminantfuel concentration can be calculated using average responsefactors. If the nature of the contaminant fuel is unknown, acontaminant concentration cannot be calculated, and the testmethod can only be used only to indicate the presence orabsence of fuel co
13、ntamination.5.2 Fuels containing aromatic compounds, such as dieselfuel and gasoline, as well as other aromatic-containing hydro-carbon materials, such as crude oil, coal oil, and motor oil, canbe determined by this test method. The quantitation limit fordiesel fuel is about 75 mg/kg. Approximate qu
14、antitation limitsfor other aromatic-containing hydrocarbon materials that canbe determined by this screening test method are given in Table1. Quantitation limits for highly aliphatic materials, such asaviation gasoline and synthetic motor oil, are much higher thanthose for more aromatic materials, s
15、uch as coal oil and dieselfuel.1This test method is under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subcommittee D34.01.05 onScreening Methods.Current edition approved Aug. 10, 2003. Published September 2003. Originallyapproved in 1995. Last previo
16、us edition approved in 2002 as D 5831 02.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM Inte
17、rnational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.NOTE 1The quantitation limits listed in Table 1 are approximatevalues because in this test method, the quantitation limit can be influencedby the particular fuel type and soil background levels. For inform
18、ation onhow the values given in Table 1 were determined, see Appendix X1. Datagenerated during the development of this screening test method and otherinformation pertaining to this test method can be found in the researchreports. (1,2)35.3 When applying this test method to sites contaminated bydiese
19、l fuel, care should be taken in selecting the appropriateresponse factor from the list given in Table 2, with consider-ation given to whether or not the fuel contamination is fresh orhas undergone weathering/or biodegradation processes. SeeAppendix X2.5.4 A factor to consider in using this test meth
20、od is whetherthe contamination is a mixture of one or more fuel types. If thisis the case, and a site-specific response factor (see AppendixX2, Section X2.3) cannot be determined, the response factorsfor the individual fuel types in the mixture should be used toestimate contaminant concentrations.5.
21、5 Certain materials, such as asphalts and asphalt residualsand oils and pitch from trees and other vegetation, whichrespond as fuel when tested by the method giving high blankabsorbance values, may interfere with use of this test method.See 8.1.2.1 and Note 3 for information on determining if thetes
22、t method can be applied to a specific soil containing one ormore of these types of materials.5.6 Extractable material, which scatters or absorbs light at254 nm, is a potential interference for this screening testmethod.6. Apparatus6.1 Glass Bottles, wide-mouth, 125-mL (4-oz) withpolytetrafluoroethyl
23、ene-lined lids.6.2 Portable Scale, (for field testing) or laboratory balance,capable of weighing to 0.1 g.6.3 Portable Stirring Device, (for field testing) or magneticstir bar and stirrer, which result in motion of the solids duringstirring.6.4 Syringes, disposable, polyethylene or polypropylene,10-
24、mL capacity.6.5 Syringe Filters, disposable, polytetrafluoroethylene,0.45-m pore size, 25-mm diameter.6.6 Spectrometer, set at 254 nm with a 1-cm path length,quartz cell (cuvette).6.7 Volumetric Flasks and Pipets, for preparing standardsolutions.6.8 Laboratory Balance, capable of weighing to 0.0001
25、g.7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall beused in all screening tests. Unless otherwise indicated, it isintended that all reagents shall conform to the specifications ofthe Committee onAnalytical Reagents of theAmerican Chemi-cal Society where such specificatio
26、ns are available.4Othergrades may be used provided it is first ascertained that thereagent is of sufficiently high purity to permit its use withoutlessening the accuracy of the determination.7.2 Calcium Oxide Powder, Reagent GradeUse calciumoxide powder, reagent grade dried at 900C for 12 h and stor
27、edin a desiccator or tightly sealed glass container prior to use.This is a conditioning agent for removal of interferencescaused by the presence of humic material or moisture, or both,in the sample.7.3 Isopropyl Alcohol, Reagent GradeThe extraction sol-vent should have an absorbance value versus air
28、 that is lessthan 0.1. To maintain purity, the solvent should not be storedfor longer than one week in a container having a compositionthat may leach UV-absorbing materials.7.3.1 Transportation of isopropyl alcohol for field testingmust comply with current Department of Transportation (DOT)regulatio
29、ns.8. Procedure8.1 Running Blank Analyses:8.1.1 To ensure that the batch of conditioning agent, sy-ringe, filter cartridge, and so forth, are not contributing to theabsorbance reading, it is recommended that the procedure beperformed as specified in 8.3 and 8.4, except using no soil and3The boldface
30、 numbers given in parentheses refer to a list of references at theend of this test method.4Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standar
31、ds for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.TABLE 1 Approximate Quantitation Limits for Various Fuel Typesin Soils Based on 0.036 AUMaterialLimit of Quantitation (LOQ),mg
32、/kgCoal Oil 21Crude Oil 61Diesel Fuel 75Weathered Diesel Fuel 21Used Motor Oil 162Weathered Gasoline 170Unleaded Gasoline 316Jet Fuel JP-2 378Motor Oil 533Aviation Gasoline 1066Synthetic Motor Oil 1382TABLE 2 Reciprocal Absorptivities at 254 nm for a 1-cm PathLength CellMaterial 1/Absorptivity, mg/L
33、/AUCoal Oil 59Crude Oil 169Diesel Fuel 209Weathered Diesel Fuel 58Used Motor Oil 450Weathered Gasoline 473Unleaded Gasoline 877Jet Fuel JP-2 1050Motor Oil 1480Aviation Gasoline 2960Synthetic Motor Oil 3840D5831032approximately5gofcalcium oxide. If the resulting extract hasan absorbance value greater
34、 than 0.03, the various componentsshould be tested individually by contacting them with theextraction solvent, and the problem component(s) should bereplaced.8.1.2 In this procedure, the conditioning agent inhibits theextraction of most humic materials, and there is very little, ifany, background fr
35、om inorganic materials. It is recommended,however, that a blank soil sample be tested as specified in 8.3and 8.4 by extracting contaminant-free soil of the same typeand from the same general area as the site being studied.Approximately5gofcalcium oxide should be used for thisblank extraction. Result
36、s from the blank soil analysis can beused to provide information on the blank soil absorbance value,the amount of calcium oxide required to dry the soil and inhibitextraction of humic materials, and the time it takes the soil andcalcium oxide to settle after stirring.8.1.2.1 If the absorbance value
37、of the first soil blank extractis less than 0.05, extraction of the soil samples at the siteshould be performed using5gofcalcium oxide. If theabsorbance value of the first soil blank extract is greater than0.05, a second blank sample should be extracted using addi-tional calcium oxide. As stated in
38、8.1.2, for the first blanksample, approximately5gofcalcium oxide should be used. Ifa second blank analysis is required, approximately 10 g ofcalcium oxide should be added to the soil sample. If theabsorbance value of the second blank extract is lower than forthe first blank extract, but is still gre
39、ater than 0.05, a third blanksample should be tested using approximately 15 g of calciumoxide. These steps can be repeated, increasing the amount ofcalcium oxide by approximately 5 g each time, until the blankabsorbance value is less than 0.05. In this way, the amount ofcalcium oxide required to inh
40、ibit interferences from humicmaterial and moisture in the soil can be determined. Excesscalcium oxide will not affect the analysis results. If theabsorbance of the value of the second blank extract is notdecreased by the addition of 10 g of calcium oxide to the blanksample or if the addition of calc
41、ium oxide does not lower theabsorbance of the blank extract to less than 0.05, even with theaddition of a large quantity of conditioning agent, and theabsorbance of the blank extract is less than 0.1, the blankabsorbance value can be subtracted from the sample absor-bance values. If this is done, bl
42、ank samples from around thesite should be tested to ensure that the blank soil absorbance isconstant by 60.02 absorbance units. If the blank absorbancefor the second blank is not decreased by the addition of 10 g ofcalcium oxide and the absorbance of the blank extract is greaterthan 0.1, or if blank
43、, correction is not desired, use of analternative non-UV-absorbing extraction solvent should beconsidered. If an alternative solvent is used, the steps describedin 8.1.1 and 8.1.2 should be repeated using the differentsolvent.8.1.2.2 Note the time required for the soil and calcium oxideto settle aft
44、er stirring as determined in 8.1.2 or 8.1.2.1 byperforming the blank soil analysis(es).NOTE 2An example of a non-UV-absorbing solvent that has beenused in place of isopropyl alcohol in this method is n-heptane. Informationon use of this solvent can be found in the research report. (2)NOTE 3In testin
45、g soil suspected of containing asphalt materials or oilsor pitch from trees or other vegetation, it is recommended that if the blankabsorbance value cannot be lowered to less than 0.05 by the addition ofcalcium oxide, the blank absorbance value should be subtracted from thesample absorbance values.
46、However, as stated in 8.1.2.1, this should onlybe done if the blank absorbance is less than 0.1. If the blank absorbanceis greater than 0.1, the method should not be used to test the soil.8.1.3 Also, it is recommended that one spike should be runfor every batch of samples or for every 20 samples, wh
47、icheveris most frequent. A soil sample is spiked by adding 5 L ofdiesel fuel or 25 L of gasoline and shaking the bottle for 3min. The extraction and analysis then are performed asoutlined in 8.3.3-8.4.5. Recovery is calculated by comparingthe absorbance of the extract from the spiked soil at 254 nmw
48、ith the absorbance of a solution of 5 L of diesel fuel or 25L of gasoline in 50 mL of isopropyl alcohol. After correctionfor any material appearing in the unspiked soil, the recoveryshould be within 20 % of the true value.8.2 Preparation of Standard Solutions:8.2.1 Weigh out 200 mg (weighed to 60.1
49、mg) of the fueltype of interest into a 100-mL volumetric flask and dilute tovolume using isopropyl alcohol. This gives a 2000-mg/Lstandard stock solution. Other standard solutions can beprepared as needed by appropriate dilution of this stocksolution. For example, to prepare a 200-mg/L solution of thefuel type of interest, pipet 5 mL of the stock solution into a50-mL volumetric flask and dilute to volume using isopropylalcohol. For work in the field, a standard stock solution can beprepared by diluting 25 L of a fuel standard (density can varyfrom ;0.750.90 g/mL) to 100
