1、Designation: D5143 06 (Reapproved 2015)1Standard Test Method forAnalysis of Nitroaromatic and Nitramine Explosive in Soilby High Performance Liquid Chromatography1This standard is issued under the fixed designation D5143; the number immediately following the designation indicates the year oforiginal
2、 adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEReapproved with editorial changes in August 2015.1. Scope*1.1 This test me
3、thod describes a procedure for the labora-tory determination of the concentration 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 (
4、2,4,6-trinitrotoluene), TNB (1,3,5trinitrobenzene), DNB (1,3 dinitrobenzene), 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 D6026.1.2.1 T
5、he procedures used to specify how data are collected/recorded or calculated, in this standard are regarded as theindustry standard. In addition, they are representative of thesignificant digits that generally should be retained. The proce-dures used do not consider material variation, purpose forobt
6、aining the data, special purpose studies, or any consider-ations for the users objectives; and it is common practice toincrease or reduce significant digits of reported data to becommensurate with these considerations. It is beyond the scopeof this standard to consider significant digits used in ana
7、lysismethods for engineering design.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address the safetyconcerns associated with its use. It is the responsibility of theuser of this standa
8、rd to establish appropriate safety and healthpractices and determine the applicability of regulatory limita-tions prior to use.2. Referenced Documents2.1 ASTM Standards:2C670 Practice for Preparing Precision and Bias Statementsfor Test Methods for Construction MaterialsD653 Terminology Relating to S
9、oil, Rock, and ContainedFluidsD3740 Practice for Minimum Requirements for AgenciesEngaged in Testing and/or Inspection of Soil and Rock asUsed in Engineering Design and ConstructionD6026 Practice for Using Significant Digits in GeotechnicalDataE682 Practice for Liquid Chromatography Terms and Rela-t
10、ionships3. Terminology3.1 Definitions:3.1.1 For definitions of common technical terms used in thisstandard, refer to Terminology D653.3.2 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
11、 andreproducible measurements 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 tes
12、t method can be used to determine 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, orstorag
13、e sites.1This test method is under the jurisdiction ofASTM Committee D18 on Soil andRock and is the direct responsibility of Subcommittee D18.06 on Physical-ChemicalInteractions of Soil and Rock.Current edition approved Aug. 15, 2015. Published September 2015. Originallyapproved in 1991. Last previo
14、us edition approved in 2010 as D5143 06(2010)1.DOI: 10.1520/D5143-06R15E01.2For 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
15、 ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15. Apparatus5.1 Liquid Chromatograph, conforming to the descriptionand requirements of Practice E682 and eq
16、uipped 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 forisocratic analysis with flow range capability from 0.1 to 3.0mL/min.5.3 Volumetric Pip
17、ets.5.4 Scintillation Vials.5.5 Plastic B-D Syringe, fitted with a disposable 0.5 mfilter assembly.5.6 Vortex Mixer.5.7 Amber Injector Vials.5.8 Mortar and Pestle.5.9 Rubber Tipped Pestle.5.10 Standard no. 10 (2 mm) sieve.6. Reagents6.1 Unless otherwise stated, it is intended that all reagentsconfor
18、m to the specification of the committee on AnalyticalReagents of the American Chemical Society.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-trinitroben
19、zene),6.5.6 Tetryl, and6.5.7 2,4-DNT and 2,6-DNT.7. Procedure7.1 Sample Preparation:7.1.1 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 throug
20、h a No. 10 sieve to remove thecoarser stones and pebbles. Discard only those particles thatare 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 openi
21、ngsand are collected prior to continuing.7.1.5 Thoroughly mix the collected soil fraction 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.
22、1 Weigh out exactly 2.00 g of soil into a 11.1 mL (6dram) screw top glass vial equipped 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 plac
23、ing the sample in an ultrasonic bath for 18 h.7.2.4 The ultrasonic bath should be maintained 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 Wi
24、th a volumetric pipet, remove a 5.00 mL aliquot ofthe suspension and mix it with a 5.00 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 throug
25、h a 0.5 mfilter usinga3mLdisposable syringe. The first millilitre isdiscarded and the remainder 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
26、a 5 m, reversed-phase LC-18 andLC-CN cartridge column, with a 50/50 methanol/water mobilephase, 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 establ
27、ished byreplicate analysis of a single high range standard. Dilutestandards, controls, and 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 appropr
28、iate for each compound as shown inthe references from the Corps of Engineers. Therefore, cali-bration is accomplished by repeated analysis of a high rangestandard. The mean response (R) for each compound obtainedin the peak height mode is calculated for each analyte. Theresponse factors (RF) are the
29、n obtained by dividing each R bythe known solution concentration (C) for that compound inunits of g/L.RF 5 R/C (1)8.2 The concentrations of analytes in the extracts are ob-tained by dividing the response of each analyte (Ra)bytheappropriate response factor (RFa).Ca5 Ra/RFa(2)3Reagent Chemicals, Amer
30、ican 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 States Pharmacopeiaand National Formulary
31、, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.D5143 06 (2015)128.3 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 the actual mass ofdried soil used (M).Xa5 Ca30.010!/M (3)
32、9. Report9.1 For each soil tested, report the following information:9.1.1 The name of the person performing the test and thedate of the test,9.1.2 The sample identification,9.1.3 The specific analyte,9.1.4 The detection limit, and9.1.5 The concentration of explosive found in g/g of drysoil.10. Preci
33、sion and Bias10.1 Precision:10.1.1 Within-Laboratory PrecisionThe within-laboratorystandard deviations (also called repeatability) for the sevenanalytes were obtained by means of a collaborative test. Thetest results were obtained from seven laboratories conductinganalysis of eight soils in duplicat
34、e. Four of the test soils werefield contaminated soils and four were spiked soils. Thewithin-laboratory standard deviation was obtained from theagreement of duplicates4.Within-laboratory precision estimatesare presented in Table 1. Therefore, the results of two properlyconducted tests by the same op
35、erator 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 1satisfy the 1s and d2s requirements outlined in Practice C670.10.1.2 Between-Laboratory
36、 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 the method described in Footnote 8.5Therefore,the results of two properly conducted
37、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 BiasThe procedure in this test method for measuringthe explosive content of soils has no
38、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 wasobtained from regression analysis of the four spiked soilsanalyzed in duplicate in the
39、collaborative test described above.Results are presented in Table 1.11. Keywords11.1 army; explosives; liquid chromatography; military; soilREFERENCES(1) U.S.Army Corps of Engineers, Cold Regions Research and Engineer-ing Laboratory Report 88-8, Development of an analytical method forthe determinati
40、on of explosive residues in soil, Part II; Additionaldevelopment and ruggedness testing. July, 1988.(2) U.S.Army Corps of Engineers, Cold Regions Research and Engineer-ing Laboratory Report 89-9, Development of an analytical method forthe determination of explosive residues in soil, Part III; Collab
41、orativetest results and final performance evaluation. 1989.(3) U.S.Army Corps of Engineers, Cold Regions Research and Engineer-ing Laboratory Report 85-15, TNT, RDX, and HMX explosives insoils and sediments, analysis techniques and drying losses. October1985.(4) U.S.Army Corps of Engineers, Cold Reg
42、ions Research and Engineer-ing Laboratory Report 85-22, Comparison of extraction techniquesand solvents for explosive residues in soil. November, 1985.4U.S. Army Corps of Engineers, Cold Regions Research and EngineeringLaboratory Report 87-7, Development of an Analytical Method for ExplosiveResidues
43、 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 ofNitroaromatics and Nitramines Residues in SoilAnalyteRetentionTime, MinDetectionLimits,Ag/gBias (Re-covery)B,%PrecisionC, g/gWithin-LabBetween-Lab1s (2ds
44、) 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 (11.3) 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
45、using EPA MDL procedure at the 99 % confidence level.BObtained from the slope of the regression line versus known concentrationscollaborative tests.CObtained from collaborative test results.D5143 06 (2015)13SUMMARY OF CHANGESIn accordance with Committee D18 policy, this section identifies the locati
46、on of changes to this standard sincethe last edition (D5143 06(2010)1) that may impact the use of this standard.(1) Editorial changes were made throughout as part of thefive-year review for this standard.ASTM International takes no position respecting the validity of any patent rights asserted in co
47、nnection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the respo
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49、 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 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 service
