ASTM D5143-91(2004)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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.
Designation:D5143–91 (Reapproved 2004)
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. Terminology
1.1 This test method describes a procedure for the labora- 3.1 Definitions:
tory determination of the concentration of nitroaromatic and 3.1.1 Refer to Terms and Symbols D 653 for the definitions
nitramine explosives in soil. The explosives involved in this of standard terms relating to soil and rock.
testmethodareasfollows:HMX(octahydro-1,3,5,7-tetranitro- 3.2 Definitions of Terms Specific to This Standard:
1,3,5,7-tetrazocine), RDX (hexahydro-1,3,5-trinitrol-1,3,5- 3.2.1 HPLC—high power liquid chromatography.
triazine), TNT (2,4,6-trinitrotoluene), TNB (1,3,5 trinitroben-
4. Significance and Use
zene), DNB (1,3 dinitrobenzene), tetryl (methyl-2,4,6-
4.1 This test method can be used to make reliable and
trinitrophenylnitramine), and 2,4-DNT (2,4-dinitrotoluene).
1.2 The values stated in SI units are to be regarded as the reproducible measurements in soil in the range from the
detection level to the percent levels of each of seven explosive
standard.
1.3 This standard does not purport to address the safety compounds.
4.2 This test method does not attempt to quantify the
concerns associated with its use. It is the responsibility of the
user of this standard to establish appropriate safety and health reactivity or mobility of the explosive content, only the
concentration of these compounds in the soil.
practices and determine the applicability of regulatory limita-
tions prior to use. 4.3 This test method can be used to determine the extent of
contamination resulting from the use, misuse, or spillage of
2. Referenced Documents
explosive compounds. It is useful to determine the effective-
2.1 ASTM Standards: ness of clean-up actions at disposal sites, and to determine the
C 670 Practice for Preparing Precision Statements for Test environmental impact at explosives dispoal, manufacturing, or
Methods for Construction Materials storage sites.
D 653 Terminology Relating to Soil, Rock, and Contained
5. Apparatus
Fluids
E 682 Practice for Liquid Chromatography Terms and Re- 5.1 Liquid Chromatograph, conforming to the description
and requirements of Practice E 682 and equipped with two 25
lationships
cmby4.6mmreversed-phaseHPLCcolumns(oneLC-18,one
LC-CN); a fixed 254 nm UV detector; an integrator and a 100
µL sample loop injector.
This method is under the jurisdiction of ASTM Committee D18 on Soil and
5.2 Solvent Delivery Module, should be reliable enough for
Rock and is the direct responsibility of Subcommittee D18.06 on Physico-Chemical
isocratic analysis with flow range capability from 0.1 to 3.0
Properties of Soils and Rocks.
mL/min.
Current edition approved July 1, 2004. Published September 2004. Originally
approved in 1990. Last previous editionn approved in 1998 as D 5143–91(1998).
5.3 Volumetric Pipets.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.4 Scintillation Vials.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
5.5 Plastic B-D Syringe, fitted with a disposable 0.5 µm
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. filter assembly.
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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.
D5143–91 (2004)
5.6 Vortex Mixer. 7.2.5 With a volumetric pipet, remove a 5.00 mL aliquot of
5.7 Amber Injector Vials. the suspension and mix it with a 5.00 mL of 5 g/L aqueous
5.8 Mortar and Pestle. CaCl in a glass scintillation vial. Shake the vials and allow to
5.9 Rubber Tipped Pestle. stand for 15 min.
7.2.6 Filter about 5 mL of the clarified sample into a clean
6. Reagents
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.
7.3.2 Make quantifications at the 254 nm wavelength.
6.5.3 TNT,
6.5.4 DNB (1,3-dinitrobenzene), 7.3.3 Base quantitation on response factors established by
replicate analysis of a single high range standard. Dilute
6.5.5 TNB (1,3,5-trinitrobenzene),
6.5.6 Tetryl, and standards, controls, and blanks 1:1 with aqueous CaCl prior to
analysis.
6.5.7 2,4-DNT and 2,6-DNT.
7.3.4 Theelutiontimeforthetotalassayislessthan15min.
7. Procedure
8. Calculation
7.1 Sample Preparation:
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 tipped pestle and
range standard. The mean response (R) for each compound
mortar, and sieve the soil through a No. 10 sieve to remove the
obtainedinthepeakheightmodeiscalculatedforeachanalyte.
coarser stones and pebbles. Discard only those particles that
The response factors ( RF) are then obtained by dividing each
are not passable through the No. 10 sieve.
R by the known solution concentration (C) for that compound
7.1.3 Grind the soil using a pestle and mortar.
in units of µg/L.
7.1.4 Sieve the soil through a 30 mesh sieve. Ensure that all
RF 5 R/C (1)
of the particles are ground to pass through the sieve openings
8.2 The concentrations of analytes in the extracts are ob-
and are collected prior to continuing.
tained by dividing the response of each analyte ( R)bythe
a
7.1.5 Thoroughly mix the collected soil fraction and draw a
appropriate response factor ( RF ).
a
2.00 gm sample for each test replicat
...