ASTM D5143-06(2015)e1

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D5143 − 06 (Reapproved 2015)
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—Reapproved with editorial changes in August 2015.
1. Scope* 2. Referenced Documents
2.1 ASTM Standards:
1.1 This test method describes a procedure for the labora-
C670 Practice for Preparing Precision and Bias Statements
tory determination of the concentration of nitroaromatic and
for Test Methods for Construction Materials
nitramine explosives in soil. The explosives involved in this
D653 Terminology Relating to Soil, Rock, and Contained
test method are as follows: HMX (octahydro-1,3,5,7-tetranitro-
Fluids
1,3,5,7-tetrazocine), RDX (hexahydro-1,3,5-trinitrol-1,3,5-
D3740 Practice for Minimum Requirements for Agencies
triazine), TNT (2,4,6-trinitrotoluene), TNB (1,3,5
Engaged in Testing and/or Inspection of Soil and Rock as
trinitrobenzene), DNB (1,3 dinitrobenzene), tetryl (methyl-2,
Used in Engineering Design and Construction
4,6-trinitrophenylnitramine), and 2,4-DNT (2,4-
D6026 Practice for Using Significant Digits in Geotechnical
dinitrotoluene).
Data
1.2 All observed and calculated values shall conform to the
E682 Practice for Liquid Chromatography Terms and Rela-
guidelines for significant digits and rounding established in
tionships
Practice D6026.
1.2.1 The procedures used to specify how data are collected/ 3. Terminology
recorded or calculated, in this standard are regarded as the
3.1 Definitions:
industry standard. In addition, they are representative of the
3.1.1 For definitions of common technical terms used in this
significant digits that generally should be retained. The proce-
standard, refer to Terminology D653.
dures used do not consider material variation, purpose for
3.2 Definitions of Terms Specific to This Standard:
obtaining the data, special purpose studies, or any consider-
3.2.1 HPLC—high power liquid chromatography.
ations for the user’s objectives; and it is common practice to
increase or reduce significant digits of reported data to be
4. Significance and Use
commensurate with these considerations. It is beyond the scope
4.1 This test method can be used to make reliable and
of this standard to consider significant digits used in analysis
reproducible measurements in soil in the range from the
methods for engineering design.
detection level to the percent levels of each of seven explosive
1.3 The values stated in SI units are to be regarded as
compounds.
standard. No other units of measurement are included in this
4.2 This test method does not attempt to quantify the
standard.
reactivity or mobility of the explosive content, only the
1.4 This standard does not purport to address the safety concentration of these compounds in the soil.
concerns associated with its use. It is the responsibility of the
4.3 This test method can be used to determine the extent of
user of this standard to establish appropriate safety and health
contamination resulting from the use, misuse, or spillage of
practices and determine the applicability of regulatory limita-
explosive compounds. It is useful to determine the effective-
tions prior to use.
ness of clean-up actions at disposal sites, and to determine the
environmental impact at explosives disposal, manufacturing, or
storage sites.
This test method is under the jurisdiction of ASTM Committee D18 on Soil and
Rock and is the direct responsibility of Subcommittee D18.06 on Physical-Chemical
Interactions of Soil and Rock. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Aug. 15, 2015. Published September 2015. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
ɛ1
approved in 1991. Last previous edition approved in 2010 as D5143 – 06(2010) . Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D5143-06R15E01. the ASTM website.
*A Summary of Changes section appears at the end of this standard
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D5143 − 06 (2015)
5. Apparatus 7.1.5 Thoroughly mix the collected soil fraction and draw a
2.00 gm sample for each test replicate.
5.1 Liquid Chromatograph, conforming to the description
7.1.6 Thoroughly clean the sieves, pestles, and mortars with
and requirements of Practice E682 and equipped with two 25
laboratory soap and water followed by an isopropanol rinse
cm by 4.6 mm reversed-phase HPLC columns (one LC-18, one
between samples.
LC-CN); a fixed 254 nm UV detector; an integrator and a 100
µL sample loop injector.
7.2 Extraction of Soil:
7.2.1 Weigh out exactly 2.00 g of soil into a 11.1 mL (6
5.2 Solvent Delivery Module, should be reliable enough for
isocratic analysis with flow range capability from 0.1 to 3.0 dram) screw top glass vial equipped with a TFE-fluorocarbon-
lined cap.
mL/min.
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
5.5 Plastic B-D Syringe, fitted with a disposable 0.5 µm
by placing the sample in an ultrasonic bath for 18 h.
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
5.8 Mortar and Pestle.
particles to settle.
5.9 Rubber Tipped Pestle. 7.2.5 With a volumetric pipet, remove a 5.00 mL aliquot of
the suspension and mix it with a 5.00 mL of 5 g/L aqueous
5.10 Standard no. 10 (2 mm) sieve.
CaCl in a glass scintillation vial. Shake the vials and allow to
6. Reagents stand for 15 min.
7.2.6 Filter about 5 mL of the clarified sample into a clean
6.1 Unless otherwise stated, it is intended that all reagents
scintillation vial by forcing the supernatant through a 0.5 µm
conform to the specification of the committee on Analytical
filter using a 3 mL disposable syringe. The first millilitre is
Reagents of the American Chemical Society.
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-
cratically by the use of a 5 µm, reversed-phase LC-18 and
6.5 Reference Standards of the following:
LC-CN cartridge column, with a 50/50 methanol/water mobile
6.5.1 HMX,
phase, at a flow of 1.5 mL/min. The LC-CN cartridge column
6.5.2 RDX,
is used for confirmation of the analytical results.
6.5.3 TNT,
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 The elution time for the total assay is less than 15 min.
7.1 Sample Preparation:
7.1.1 Air dry the soil to a constant mass out of direct
8. Calculation
sunlight at normal ambient humidity and 20 to 25°C (room
8.1 Exper
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