ASTM D5143-06(2010)e1

Standard Test Method for Analysis of Nitroaromatic and Nitramine Explosive in Soil by High Performance Liquid Chromatography

SIGNIFICANCE AND USE
This test method can be used to make reliable and reproducible measurements in soil in the range from the detection level to the percent levels of each of seven explosive compounds.
This test method does not attempt to quantify the reactivity or mobility of the explosive content, only the concentration of these compounds in the soil.
This test method can be used to determine the extent of contamination resulting from the use, misuse, or spillage of explosive compounds. It is useful to determine the effectiveness of clean-up actions at disposal sites, and to determine the environmental impact at explosives disposal, manufacturing, or storage sites.
SCOPE
1.1 This test method describes a procedure for the laboratory determination of the concentration of nitroaromatic and nitramine explosives in soil. The explosives involved in this test 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 trinitrobenzene), 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 the guidelines for significant digits and rounding established in Practice D6026  
1.2.1 The method used to specify how data are collected, calculated, or recorded in this standard is not directly related to the accuracy to which the data can be applied in design of other uses, or both. How one applies the results obtained using this standard is beyond its scope. (See Practice D3740)
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address the safety concerns associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 30-Sep-2010
• ICS: 71.100.30 - Explosives. Pyrotechnics and fireworks
• Technical Committee: D18 - Soil and Rock
• Drafting Committee: D18.06 - Physical-Chemical Interactions of Soil and Rock

Relations

• Replaces: ASTM D5143-06 - Standard Test Method for Analysis of Nitroaromatic and Nitramine Explosive in Soil by High Performance Liquid Chromatography
• Effective Date: 01-Oct-2010

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
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Designation: D5143 − 06(Reapproved 2010)
Standard Test Method for
Analysis of Nitroaromatic and Nitramine Explosive in Soil
by High Performance Liquid Chromatography
This standard is issued under the fixed designation D5143; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Added reference to Practice D3740 and revised the units statement in 1.3 editorially October 2010.
1. Scope for Test Methods for Construction Materials
D653 Terminology Relating to Soil, Rock, and Contained
1.1 This test method describes a procedure for the labora-
Fluids
tory determination of the concentration of nitroaromatic and
D3740 Practice for Minimum Requirements for Agencies
nitramine explosives in soil. The explosives involved in this
Engaged in Testing and/or Inspection of Soil and Rock as
testmethodareasfollows:HMX(octahydro-1,3,5,7-tetranitro-
Used in Engineering Design and Construction
1,3,5,7-tetrazocine), RDX (hexahydro-1,3,5-trinitrol-1,3,5-
D6026 Practice for Using Significant Digits in Geotechnical
triazine), TNT (2,4,6-trinitrotoluene), TNB (1,3,5
Data
trinitrobenzene), DNB (1,3 dinitrobenzene), tetryl (methyl-2,
E682 Practice for Liquid Chromatography Terms and Rela-
4,6-trinitrophenylnitramine), and 2,4-DNT (2,4-
tionships
dinitrotoluene).
1.2 All observed and calculated values shall conform to the
3. Terminology
guidelines for significant digits and rounding established in
3.1 Definitions:
Practice D6026
3.1.1 Refer to Terms and Symbols D653 for the definitions
1.2.1 The method used to specify how data are collected,
of standard terms relating to soil and rock.
calculated, or recorded in this standard is not directly related to
3.2 Definitions of Terms Specific to This Standard:
theaccuracytowhichthedatacanbeappliedindesignofother
3.2.1 HPLC—high power liquid chromatography.
uses, or both. How one applies the results obtained using this
standard is beyond its scope. (See Practice D3740)
4. Significance and Use
1.3 The values stated in SI units are to be regarded as
4.1 This test method can be used to make reliable and
standard. No other units of measurement are included in this
reproducible measurements in soil in the range from the
standard.
detection level to the percent levels of each of seven explosive
1.4 This standard does not purport to address the safety
compounds.
concerns associated with its use. It is the responsibility of the
user of this standard to establish appropriate safety and health 4.2 This test method does not attempt to quantify the
practices and determine the applicability of regulatory limita-
reactivity or mobility of the explosive content, only the
tions prior to use. concentration of these compounds in the soil.
4.3 This test method can be used to determine the extent of
2. Referenced Documents
contamination resulting from the use, misuse, or spillage of
2.1 ASTM Standards:
explosive compounds. It is useful to determine the effective-
C670 Practice for Preparing Precision and Bias Statements
ness of clean-up actions at disposal sites, and to determine the
environmentalimpactatexplosivesdisposal,manufacturing,or
storage sites.
ThistestmethodisunderthejurisdictionofASTMCommitteeD18onSoiland
RockandisthedirectresponsibilityofSubcommitteeD18.06onPhysical-Chemical
Interactions of Soil and Rock.
5. Apparatus
Current edition approved Oct. 1, 2010. Published December 2010. Originally
5.1 Liquid Chromatograph, conforming to the description
approved in 1991. Last previous edition approved in 2006 as D5143 – 06. DOI:
10.1520/D5143-06R10E01.
and requirements of Practice E682 and equipped with two 25
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
cmby4.6mmreversed-phaseHPLCcolumns(oneLC-18,one
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
LC-CN); a fixed 254 nm UV detector; an integrator and a 100
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. µL sample loop injector.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D5143 − 06 (2010)
5.2 Solvent Delivery Module, should be reliable enough for 7.2.1 Weigh out exactly 2.00 g of soil into a 11.1 mL (6
isocratic analysis with flow range capability from 0.1 to 3.0 dram) screw top glass vial equipped with a TFE-fluorocarbon-
mL/min. lined cap.
7.2.2 With a volumetric pipette, introduce 10.0 mL of
5.3 Volumetric Pipets.
acetonitrile to the soil, and screw on the closures tightly.
5.4 Scintillation Vials.
7.2.3 Place the vials on a vortex mixer for 1 min followed
by placing the sample in an ultrasonic bath for 18 h.
5.5 Plastic B-D Syringe, fitted with a disposable 0.5 µm
filter assembly. 7.2.4 The ultrasonic bath should be maintained near ambi-
ent temperature to minimize loss of tetryl due to thermal
5.6 Vortex Mixer.
degradation. Remove the samples from the bath and allow
5.7 Amber Injector Vials.
them to stand for a minimum of 15 min to allow the larger
particles to settle.
5.8 Mortar and Pestle.
7.2.5 With a volumetric pipet, remove a 5.00 mL aliquot of
5.9 Rubber Tipped Pestle.
the suspension and mix it with a 5.00 mL of 5 g/L aqueous
CaCl in a glass scintillation vial. Shake the vials and allow to
6. Reagents 2
stand for 15 min.
6.1 Unless otherwise stated, it is intended that all reagents
7.2.6 Filter about 5 mL of the clarified sample into a clean
conform to the specification of the committee on Analytical
scintillation vial by forcing the supernatant through a 0.5 µm
Reagents of the American Chemical Society.
filter usinga3mL disposable syringe. The first millilitre is
discarded and the remainder saved for analysis. Place the
6.2 HPLC Grade Methanol.
filtered sample in an amber injection vial for analysis.
6.3 HPLC Grade Acetonitrile.
7.3 Liquid Chromatographic Analysis:
6.4 ASTM Type I Water.
7.3.1 Accomplish the liquid chromatograph separations iso-
6.5 Reference Standards of the following:
cratically by the use of a 5 µm, reversed-phase LC-18 and
6.5.1 HMX,
LC-CN cartridge column, with a 50/50 methanol/water mobile
6.5.2 RDX,
phase, at a flow of 1.5 mL/min. The LC-CN cartridge column
6.5.3 TNT,
is used for confirmation of the analytical results.
6.5.4 DNB (1,3-dinitrobenzene),
7.3.2 Make quantifications at the 254 nm wavelength.
6.5.5 TNB (1,3,5-trinitrobenzene),
7.3.3 Base quantitation on response factors established by
6.5.6 Tetryl, and
replicate analysis of a single high range standard. Dilute
6.5.7 2,4-DNT and 2,6-DNT.
standards, controls, and blanks 1:1 with aqueous CaCl prior to
analysis.
7. Procedure
7.3.4 Theelutiontimeforthetotalassayislessthan15min.
7.1 Sample Preparation:
8. Calculation
7.1.1 Air dry the soil to a constant mass out of direct
8.1 Experience indicates that a linear calibration curve with
sunlight at normal ambient humidity and 20 to 25 °C (room
zero intercept is appropriate for each compound. Therefore,
temperature).
calibration is accomplished by repeated analysis of a high
7.1.2 Disaggregate the soil using a rubber t
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