1、Designation: D 5143 06Standard Test Method forAnalysis of Nitroaromatic and Nitramine Explosive in Soilby High Performance Liquid Chromatography1This standard is issued under the fixed designation D 5143; the number immediately following the designation indicates the year oforiginal adoption or, in
2、the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method describes a procedure for the labora-tory determination of the co
3、ncentration of nitroaromatic andnitramine explosives in soil. The explosives involved in thistest method are as follows: HMX (octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine), RDX (hexahydro-1,3,5-trinitrol-1,3,5-triazine), TNT (2,4,6-trinitrotoluene), TNB (1,3,5 trinitroben-zene), DNB (1,3 dinitro
4、benzene), tetryl (methyl-2,4,6-trinitrophenylnitramine), and 2,4-DNT (2,4-dinitrotoluene).1.2 All observed and calculated values shall conform to theguidelines for significant digits and rounding established inPractice D 60261.2.1 The method used to specify how data are collected,calculated, or reco
5、rded in this standard is not directly related tothe accuracy to which the data can be applied in design of otheruses, or both. How one applies the results obtained using thisstandard is beyond its scope.1.3 The values stated in SI units are to be regarded as thestandard.1.4 This standard does not pu
6、rport to address the safetyconcerns associated with its use. It is the responsibility of theuser of this standard to establish appropriate safety and healthpractices and determine the applicability of regulatory limita-tions prior to use.2. Referenced Documents2.1 ASTM Standards:2C 670 Practice for
7、Preparing Precision and Bias Statementsfor Test Methods for Construction MaterialsD 653 Terminology Relating to Soil, Rock, and ContainedFluidsD 6026 Practice for Using Significant Digits in Geotechni-cal DataE 682 Practice for Liquid Chromatography Terms and Re-lationships3. Terminology3.1 Definiti
8、ons:3.1.1 Refer to Terms and Symbols D 653 for the definitionsof standard terms relating to soil and rock.3.2 Definitions of Terms Specific to This Standard:3.2.1 HPLChigh power liquid chromatography.4. Significance and Use4.1 This test method can be used to make reliable andreproducible measurement
9、s in soil in the range from thedetection level to the percent levels of each of seven explosivecompounds.4.2 This test method does not attempt to quantify thereactivity or mobility of the explosive content, only theconcentration of these compounds in the soil.4.3 This test method can be used to dete
10、rmine the extent ofcontamination resulting from the use, misuse, or spillage ofexplosive compounds. It is useful to determine the effective-ness of clean-up actions at disposal sites, and to determine theenvironmental impact at explosives disposal, manufacturing, orstorage sites.5. Apparatus5.1 Liqu
11、id Chromatograph, conforming to the descriptionand requirements of Practice E 682 and equipped with two 25cm by 4.6 mm reversed-phase HPLC columns (one LC-18, oneLC-CN); a fixed 254 nm UV detector; an integrator and a 100L sample loop injector.5.2 Solvent Delivery Module, should be reliable enough f
12、orisocratic analysis with flow range capability from 0.1 to 3.0mL/min.5.3 Volumetric Pipets.5.4 Scintillation Vials.5.5 Plastic B-D Syringe, fitted with a disposable 0.5 mfilter assembly.5.6 Vortex Mixer.1This test method is under the jurisdiction ofASTM Committee D18 on Soil andRock and is the dire
13、ct responsibility of Subcommittee D18.06 on Physical-ChemicalInteractions of Soil and Rock.Current edition approved Nov. 1, 2006. Published December 2006. Originallyapproved in 1991. Last previous edition approved in 1998 as D 514391(2004)e1.2For referenced ASTM standards, visit the ASTM website, ww
14、w.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.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive,
15、 PO Box C700, West Conshohocken, PA 19428-2959, United States.5.7 Amber Injector Vials.5.8 Mortar and Pestle.5.9 Rubber Tipped Pestle.6. Reagents6.1 Unless otherwise stated, it is intended that all reagentsconform to the specification of the committee on AnalyticalReagents of the American Chemical S
16、ociety.36.2 HPLC Grade Methanol.6.3 HPLC Grade Acetonitrile.6.4 ASTM Type I Water.6.5 Reference Standards of the following:6.5.1 HMX,6.5.2 RDX,6.5.3 TNT,6.5.4 DNB (1,3-dinitrobenzene),6.5.5 TNB (1,3,5-trinitrobenzene),6.5.6 Tetryl, and6.5.7 2,4-DNT and 2,6-DNT.7. Procedure7.1 Sample Preparation:7.1.
17、1 Air dry the soil to a constant mass out of directsunlight at normal ambient humidity and 20 to 25C (roomtemperature).7.1.2 Disaggregate the soil using a rubber tipped pestle andmortar, and sieve the soil through a No. 10 sieve to remove thecoarser stones and pebbles. Discard only those particles t
18、hatare not passable through the No. 10 sieve.7.1.3 Grind the soil using a pestle and mortar.7.1.4 Sieve the soil through a 30 mesh sieve. Ensure that allof the particles are ground to pass through the sieve openingsand are collected prior to continuing.7.1.5 Thoroughly mix the collected soil fractio
19、n and draw a2.00 gm sample for each test replicate.7.1.6 Thoroughly clean the sieves, pestles, and mortars withlaboratory soap and water followed by an isopropanol rinsebetween samples.7.2 Extraction of Soil:7.2.1 Weigh out exactly 2.00 g of soil into a 11.1 mL (6dram) screw top glass vial equipped
20、with a TFE-fluorocarbon-lined cap.7.2.2 With a volumetric pipette, introduce 10.0 mL ofacetonitrile to the soil, and screw on the closures tightly.7.2.3 Place the vials on a vortex mixer for 1 min followedby placing the sample in an ultrasonic bath for 18 h.7.2.4 The ultrasonic bath should be mainta
21、ined near ambi-ent temperature to minimize loss of tetryl due to thermaldegradation. Remove the samples from the bath and allowthem to stand for a minimum of 15 min to allow the largerparticles to settle.7.2.5 With a volumetric pipet, remove a 5.00 mL aliquot ofthe suspension and mix it with a 5.00
22、mL of 5 g/L aqueousCaCl2in a glass scintillation vial. Shake the vials and allow tostand for 15 min.7.2.6 Filter about 5 mL of the clarified sample into a cleanscintillation vial by forcing the supernatant through a 0.5 mfilter usinga3mLdisposable syringe. The first millilitre isdiscarded and the re
23、mainder saved for analysis. Place thefiltered sample in an amber injection vial for analysis.7.3 Liquid Chromatographic Analysis:7.3.1 Accomplish the liquid chromatograph separations iso-cratically by the use of a 5 m, reversed-phase LC-18 andLC-CN cartridge column, with a 50/50 methanol/water mobil
24、ephase, at a flow of 1.5 mL/min. The LC-CN cartridge columnis used for confirmation of the analytical results.7.3.2 Make quantifications at the 254 nm wavelength.7.3.3 Base quantitation on response factors established byreplicate analysis of a single high range standard. Dilutestandards, controls, a
25、nd blanks 1:1 with aqueous CaCl2prior toanalysis.7.3.4 The elution time for the total assay is less than 15 min.8. Calculation8.1 Experience indicates that a linear calibration curve withzero intercept is appropriate for each compound. Therefore,calibration is accomplished by repeated analysis of a
26、highrange standard. The mean response (R) for each compoundobtained in the peak height mode is calculated for each analyte.The response factors ( RF) are then obtained by dividing eachR by the known solution concentration (C) for that compoundin units of g/L.RF 5 R/C (1)8.2 The concentrations of ana
27、lytes in the extracts are ob-tained by dividing the response of each analyte ( Ra)bytheappropriate response factor ( RFa).Ca5 Ra/RFa(2)8.3 The concentration in soil (Xa), on a g/g basis, is thenobtained by multiplying the solution concentration by the totalvolume of extract (0.010 L) and dividing by
28、 the actual mass ofdried soil used (M).Xa5 Ca3 0.010!/M (3)9. Report9.1 For each soil tested, report the following information:9.1.1 The sample identification,9.1.2 The specific analyte,9.1.3 The detection limit, and9.1.4 The concentration of explosive found in g/g of drysoil.10. Precision and Bias1
29、0.1 Precision:10.1.1 Within-Laboratory PrecisionThe within-laboratory standard deviations (also called repeatability) for theseven analytes were obtained by means of a collaborative test.The test results were obtained from seven laboratories conduct-ing analysis of eight soils in duplicate. Four of
30、the test soils3Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United St
31、ates Pharmacopeiaand National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.D5143062were field contaminated soils and four were spiked soils. Thewithin-laboratory standard deviation was obtained from theagreement of duplicates4.Within-laboratory precision estimatesare presente
32、d in Table 1. Therefore, the results of two properlyconducted tests by the same operator with the same equipmenton duplicate samples should not be considered suspect unlessthey differ by more than the values presented in the within lab,2ds column of Table 1 (See Footnote 7).4The data in Table 1satis
33、fy the 1s and d2s requirements outlined in Practice C 670.10.1.2 Between-Laboratory PrecisionThe between-laboratory precision (also called reproducibility) was obtainedfrom the results of a seven-laboratory collaborative test. Thebetween-laboratory precision estimates (see Table 1) wereobtained by t
34、he method described in Footnote 8.5Therefore,the results of two properly conducted tests by different opera-tors with the different equipment on duplicate samples shouldnot be considered suspect unless they differ by more than thevalues presented in the between lab, 2ds column of Table 1.10.2 BiasTh
35、e procedure in this test method for measuringthe explosive content of soils has no bias because the value ofthe explosive residue content is only defined in terms of the testmethod. However, to aid the user of this standard in determin-ing bias relative to other methods, the percent recovery wasobta
36、ined from regression analysis of the four spiked soilsanalyzed in duplicate in the collaborative test described above.Results are presented in Table 1.11. Keywords11.1 Army; explosives; liquid chromatography; military;soil.References(1) 0.2 U.S. Army Corps of Engineers, Cold Regions Researchand Engi
37、neering Laboratory Report 88-8, Development ofan analytical method for the determination of explosiveresidues in soil, Part II; Additional development and rugged-ness testing. July, 1988.(2) 0.3 U.S. Army Corps of Engineers, Cold Regions Researchand Engineering Laboratory Report 89-9, Development of
38、an analytical method for the determination of explosiveresidues in soil, Part III; Collaborative test results and finalperformance evaluation. 1989.(3) 0.4 U.S. Army Corps of Engineers, Cold Regions Researchand Engineering Laboratory Report 85-15, TNT, RDX, andHMX explosives in soils and sediments,
39、analysis techniquesand drying losses. October 1985.(4) 0.5 U.S. Army Corps of Engineers, Cold Regions Researchand Engineering Laboratory Report 85-22, Comparison ofextraction techniques and solvents for explosive residues insoil. November, 1985.SUMMARY OF CHANGESIn accordance with Committee D18 poli
40、cy, this section identifies the location of changes to this standard sincethe last edition (91(2004)e1) that may impact the use of this standard.(1) Standard statements for significant digits was added to theScope Section.(2) Added Practice D 6026 to Section 2.1.(3) Added Summary of Changes Section.
41、4U.S. Army Corps of Engineers, Cold Regions Research and EngineeringLaboratory Report 87-7, Development of an Analytical Method for ExplosiveResidues in Soil, June 1987.5Youden, W. J. and Steiner, E. H. Statistical Manual of the AOAC, 1978.TABLE 1 Performance Data for Method for Determination ofNitr
42、oaromatics and Nitramines Residues in SoilAnalyteRetentionTime, MinDetectionLimits,Ag/gBias (Re-covery)B,%PrecisionC, g/gWithin-LabBetween-Lab1s (2ds) 1s (2ds)HMX 2.4 1.27 95.4 3.7 (10.5) 5.7 (16.1)RDX 3.7 0.74 96.8 2.3 (6.5) 4.3 (12.2)TNB 5.1 0.29 92.0 4.4 (12.4) 6.8 (19.2)DNB 6.2 0.11 93.0 4.0 (11
43、.3) 6.9 (19.5)Tetryl 6.9 0.12 74.7 17.9 (50.6) 30.7 (86.8)TNT 8.4 0.08 96.8 3.5 (9.9) 4.7 (13.3)2,4-DNT 10.1 0.03 96.0 3.4 (9.6) 4.4 (12.4)AObtained using EPA MDL procedure at the 99 % confidence level.BObtained from the slope of the regression line versus known concentrationscollaborative tests.COb
44、tained from collaborative test results.D5143063ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights,
45、and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revi
46、sion of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you
47、shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D5143064
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