ASTM D5143-90(1998)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D5143–90 (Reapproved 1998)
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 D 5143; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3.1.1 Refer to Terms and Symbols D 653 for the definitions
of standard terms relating to soil and rock.
1.1 This test method describes a procedure for the labora-
3.2 Definitions of Terms Specific to This Standard:
tory determination of the concentration of nitroaromatic and
3.2.1 HPLC—high power liquid chromatography.
nitramine explosives in soil. The explosives involved in this
testmethodareasfollows:HMX(octahydro-1,3,5,7-tetranitro-
4. Significance and Use
1,3,5,7-tetrazocine), RDX (hexahydro-1,3,5-trinitrol-1,3,5-
4.1 This test method can be used to make reliable and
triazine), TNT (2,4,6-trinitrotoluene), TNB (1,3,5 trinitroben-
reproducible measurements in soil in the range from the
zene), DNB (1,3 dinitrobenzene), tetryl (methyl-2,4,6-
detection level to the percent levels of each of seven explosive
trinitrophenylnitramine), and 2,4-DNT (2,4-dinitrotoluene).
compounds.
1.2 The values stated in SI units are to be regarded as the
4.2 This test method does not attempt to quantify the
standard.
reactivity or mobility of the explosive content, only the
1.3 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
2. Referenced Documents environmental impact at explosives dispoal, manufacturing, or
storage sites.
2.1 ASTM Standards:
C 670 Practice for Preparing Precision Statements for Test
5. Apparatus
Methods for Construction Materials
5.1 Liquid Chromatograph, conforming to the description
D 653 Terminology Relating to Soil, Rock, and Contained
3 and requirements of Practice E 682 and equipped with two 25
Fluids
cm by 4.6 mm reversed-phase HPLC columns (one LC-18, one
E 11 Specification for Wire Cloth Sieves for Testing Pur-
4 LC-CN); a fixed 254 nm UV detector; an integrator and a 100
poses
µL sample loop injector.
E 682 Practice for Liquid Chromatography Terms and Re-
5 5.2 Solvent Delivery Module, should be reliable enough for
lationships
isocratic analysis with flow range capability from 0.1 to 3.0
3. Terminology mL/min.
5.3 Volumetric Pipets.
3.1 Definitions:
5.4 Scintillation Vials.
5.5 Plastic B-D Syringe, fitted with a disposable 0.5 µm
This method is under the jurisdiction of ASTM Committee D-18 on Soil and filter assembly.
Rock and is the direct responsibility of Subcommittee D18.06 on Physico-Chemical
5.6 Vortex Mixer.
Properties of Soils and Rocks.
5.7 Amber Injector Vials.
Current edition approved Nov. 30, 1990. Published January 1990.
5.8 Mortar and Pestle.
Annual Book of ASTM Standards, Vol 04.02.
Annual Book of ASTM Standards, Vol 04.08.
5.9 Rubber Tipped Pestle.
Annual Book of ASTM Standards, Vol 14.02.
Annual Book of ASTM Standards, Vol 14.01.
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D5143–90 (1998)
6. Reagents 7.2.6 Filter about 5 mL of the clarified sample into a clean
scintillation vial by forcing the supernatant through a 0.5 µm
6.1 Unless otherwise stated, it is intended that all reagents
filter usinga3mL disposable syringe. The first millilitre is
conform to the specification of the committee on Analytical
discarded and the remainder saved for analysis. Place the
Reagents of the American Chemical Society.
filtered sample in an amber injection vial for analysis.
6.2 HPLC Grade Methanol.
7.3 Liquid Chromatographic Analysis:
6.3 HPLC Grade Acetonitrile.
7.3.1 Accomplish the liquid chromatograph separations iso-
6.4 ASTM Type I Water.
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 Experience indicates that a linear calibration curve with
temperature).
zero intercept is appropriate for each compound. Therefore,
7.1.2 Disaggregate the soil using a rubber tipped pestle and
calibration is accomplished by repeated analysis of a high
mortar, and sieve the soil through a No. 10 sieve to remove the
range standard. The mean response (R) for each compound
coarser stones and pebbles. Discard only those particles that
obtainedinthepeakheightmodeiscalculatedforeachanalyte.
are not passable through the No. 10 sieve.
The response factors ( RF) are then obtained by dividing each
7.1.3 Grind the soil using a pestle and mortar.
R by the known solution concentration (C) for that compound
7.1.4 Sieve the soil through a 30 mesh sieve. Ensure that all
in units of µg/L.
of the particles are ground to pass through the sieve openings
RF 5 R/C (1)
and are collected prior to continuing.
7.1.5 Thoroughly mix the collected soil fraction and draw a
8.2 The concentrations of analytes in the extracts are ob-
2.00 gm sample for each test replicate.
tained by dividing the response of each analyte ( R)bythe
a
7.1.6 Thoroughly clean the sieves, pestles, and mortars with
appropriate response factor ( RF ).
a
laboratory soap and water followed by an isopropanol rinse
C 5 R /RF (2)
a a a
between samples.
8.3 The concentration in soil (X ), on aµ g/g basis, is then
a
7.2 Extraction of Soil:
o
...