ASTM D5831-03(2008)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D5831–03 (Reapproved 2008)
Standard Test Method for
Screening Fuels in Soils
This standard is issued under the fixed designation D 5831; 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 is a screening procedure for determin- 3.1 Definitions—For definitions of terms used in this
ing the presence of fuels containing aromatic compounds in screening test method, refer to Terminology E 131.
soils. If the contaminant fuel is available for calibration, the
4. Summary of Test Method
approximate concentration of the fuel in the soil can be
calculated. If the contaminant fuel type is known, but the 4.1 Asample of soil is extracted with isopropyl alcohol, and
the extract is filtered. The ultraviolet absorbance of the extract
contaminant fuel is not available for calibration, an estimate of
theconcentrationofthefuelinthesoilcanbedeterminedusing is measured at 254 nm. If the contaminant fuel is available for
calibration, the approximate concentration of contamination is
average response factors. If the nature of the contaminant fuel
is unknown, this screening test method can be used to identify calculated. If the contaminant fuel type is known, but the
contaminant fuel is not available for calibration, an estimate of
the possible presence of contamination.
1.2 This standard does not purport to address all of the the contaminant concentration is determined using average
response factors. If the nature of the contaminant fuel is not
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- known,theabsorbancevalueisusedtoindicatethepresenceor
absence of fuel contamination. Calcium oxide is added to the
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. soil as a conditioning agent to minimize interferences from
humic materials and moisture present in the soil. Particulate
2. Referenced Documents
interferences are removed by passing the extract through a
2.1 ASTM Standards: filter.
D 2777 Practice for Determination of Precision and Bias of
5. Significance and Use
Applicable Test Methods of Committee D19 on Water
E 131 Terminology Relating to Molecular Spectroscopy 5.1 This test method is a screening procedure for determin-
ing the presence of fuels containing aromatic compounds in
E 169 Practices for General Techniques of Ultraviolet-
Visible Quantitative Analysis soils. If the contaminant fuel is available for calibration, the
approximate concentration of the fuel in the soil can be
E 177 Practice for Use of the Terms Precision and Bias in
ASTM Test Methods calculated. If the fuel type is known, but the contaminant fuel
is not available for calibration, an estimate of the contaminant
E 275 Practice for Describing and Measuring Performance
of Ultraviolet, Visible, and Near-Infrared Spectrophotom- fuel concentration can be calculated using average response
factors. If the nature of the contaminant fuel is unknown, a
eters
E 691 Practice for Conducting an Interlaboratory Study to contaminant concentration cannot be calculated, and the test
method can only be used only to indicate the presence or
Determine the Precision of a Test Method
E 925 Practice for Monitoring the Calibration of absence of fuel contamination.
5.2 Fuels containing aromatic compounds, such as diesel
Ultraviolet-Visible Spectrophotometers whose Spectral
Slit Width does not Exceed 2 nm fuel and gasoline, as well as other aromatic-containing hydro-
carbon materials, such as crude oil, coal oil, and motor oil, can
be determined by this test method. The quantitation limit for
This test method is under the jurisdiction of ASTM Committee D34 on Waste
diesel fuel is about 75 mg/kg.Approximate quantitation limits
Management and is the direct responsibility of Subcommittee D34.01.05 on
for other aromatic-containing hydrocarbon materials that can
Screening Methods.
be determined by this screening test method are given in Table
Current edition approved Feb. 1, 2008. Published March 2008. Originally
approved in 1995. Last previous edition approved in 2003 as D 5831 – 03.
1. Quantitation limits for highly aliphatic materials, such as
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
aviationgasolineandsyntheticmotoroil,aremuchhigherthan
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
those for more aromatic materials, such as coal oil and diesel
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. fuel.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5831–03 (2008)
TABLE 1 Approximate Quantitation Limits for Various Fuel Types TABLE 2 Reciprocal Absorptivities at 254 nm for a 1-cm Path
in Soils Based on 0.036 AU Length Cell
Limit of Quantitation (LOQ), Material 1/Absorptivity, mg/L/AU
Material
mg/kg
Coal Oil 59
Coal Oil 21 Crude Oil 169
Crude Oil 61 Diesel Fuel 209
Diesel Fuel 75 Weathered Diesel Fuel 58
Weathered Diesel Fuel 21 Used Motor Oil 450
Used Motor Oil 162 Weathered Gasoline 473
Weathered Gasoline 170 Unleaded Gasoline 877
Unleaded Gasoline 316 Jet Fuel JP-2 1050
Jet Fuel JP-2 378 Motor Oil 1480
Motor Oil 533 Aviation Gasoline 2960
Aviation Gasoline 1066 Synthetic Motor Oil 3840
Synthetic Motor Oil 1382
6.5 Syringe Filters, disposable, polytetrafluoroethylene,
0.45-µm pore size, 25-mm diameter.
NOTE 1—The quantitation limits listed in Table 1 are approximate
values because in this test method, the quantitation limit can be influenced
6.6 Spectrometer, set at 254 nm with a 1-cm path length,
by the particular fuel type and soil background levels. For information on
quartz cell (cuvette).
how the values given in Table 1 were determined, seeAppendix X1. Data
6.7 Volumetric Flasks and Pipets, for preparing standard
generated during the development of this screening test method and other
solutions.
information pertaining to this test method can be found in the research
6.8 Laboratory Balance, capable of weighing to 0.0001 g.
reports. (1,2)
5.3 Whenapplyingthistestmethodtositescontaminatedby
7. Reagents and Materials
diesel fuel, care should be taken in selecting the appropriate
7.1 Purity of Reagents—Reagent grade chemicals shall be
response factor from the list given in Table 2, with consider-
used in all screening tests. Unless otherwise indicated, it is
ation given to whether or not the fuel contamination is fresh or
intended that all reagents shall conform to the specifications of
has undergone weathering/or biodegradation processes. See
theCommitteeonAnalyticalReagentsoftheAmericanChemi-
Appendix X2.
cal Society where such specifications are available. Other
5.4 Afactor to consider in using this test method is whether
grades may be used provided it is first ascertained that the
thecontaminationisamixtureofoneormorefueltypes.Ifthis
reagent is of sufficiently high purity to permit its use without
is the case, and a site-specific response factor (see Appendix
lessening the accuracy of the determination.
X2, Section X2.3) cannot be determined, the response factors
7.2 Calcium Oxide Powder, Reagent Grade—Use calcium
for the individual fuel types in the mixture should be used to
oxide powder, reagent grade dried at 900°C for 12 h and stored
estimate contaminant concentrations.
in a desiccator or tightly sealed glass container prior to use.
5.5 Certain materials, such as asphalts and asphalt residuals
This is a conditioning agent for removal of interferences
and oils and pitch from trees and other vegetation, which
caused by the presence of humic material or moisture, or both,
respond as fuel when tested by the method giving high blank
in the sample.
absorbance values, may interfere with use of this test method.
7.3 Isopropyl Alcohol, Reagent Grade—The extraction sol-
See 8.1.2.1 and Note 3 for information on determining if the
vent should have an absorbance value versus air that is less
test method can be applied to a specific soil containing one or
than 0.1. To maintain purity, the solvent should not be stored
more of these types of materials.
for longer than one week in a container having a composition
5.6 Extractable material, which scatters or absorbs light at
that may leach UV-absorbing materials.
254 nm, is a potential interference for this screening test
7.3.1 Transportation of isopropyl alcohol for field testing
method.
mustcomplywithcurrentDepartmentofTransportation(DOT)
regulations.
6. Apparatus
6.1 Glass Bottles, wide-mouth, 125-mL (4-oz) with
8. Procedure
polytetrafluoroethylene-lined lids.
8.1 Running Blank Analyses:
6.2 Portable Scale, (for field testing) or laboratory balance,
8.1.1 To ensure that the batch of conditioning agent, sy-
capable of weighing to 0.1 g.
ringe, filter cartridge, and so forth, are not contributing to the
6.3 Portable Stirring Device, (for field testing) or magnetic
absorbance reading, it is recommended that the procedure be
stir bar and stirrer, which result in motion of the solids during
performed as specified in 8.3 and 8.4, except using no soil and
stirring.
6.4 Syringes, disposable, polyethylene or polypropylene,
10-mL capacity.
Reagent Chemicals, American Chemical Society Specifications , American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
The boldface numbers given in parentheses refer to a list of references at the and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
end of this test method. MD.
D5831–03 (2008)
NOTE 3—Intestingsoilsuspectedofcontainingasphaltmaterialsoroils
approximately5gof calcium oxide. If the resulting extract has
or pitch from trees or other vegetation, it is recommended that if the blank
an absorbance value greater than 0.03, the various components
absorbance value cannot be lowered to less than 0.05 by the addition of
should be tested individually by contacting them with the
calcium oxide, the blank absorbance value should be subtracted from the
extraction solvent, and the problem component(s) should be
sample absorbance values. However, as stated in 8.1.2.1, this should only
replaced.
be done if the blank absorbance is less than 0.1. If the blank absorbance
is greater than 0.1, the method should not be used to test the soil.
8.1.2 In this procedure, the conditioning agent inhibits the
extraction of most humic materials, and there is very little, if
8.1.3 Also, it is recommended that one spike should be run
any, background from inorganic materials. It is recommended,
for every batch of samples or for every 20 samples, whichever
however, that a blank soil sample be tested as specified in 8.3
is most frequent. A soil sample is spiked by adding 5 µL of
and 8.4 by extracting contaminant-free soil of the same type
diesel fuel or 25 µL of gasoline and shaking the bottle for 3
and from the same general area as the site being studied.
min. The extraction and analysis then are performed as
Approximately5gof calcium oxide should be used for this
outlined in 8.3.3-8.4.5. Recovery is calculated by comparing
blank extraction. Results from the blank soil analysis can be
the absorbance of the extract from the spiked soil at 254 nm
usedtoprovideinformationontheblanksoilabsorbancevalue,
with the absorbance of a solution of 5 µL of diesel fuel or 25
theamountofcalciumoxiderequiredtodrythesoilandinhibit
µL of gasoline in 50 mL of isopropyl alcohol.After correction
extraction of humic materials, and the time it takes the soil and
for any material appearing in the unspiked soil, the recovery
calcium oxide to settle after stirring.
should be within 20 % of the true value.
8.1.2.1 If the absorbance value of the first soil blank extract
8.2 Preparation of Standard Solutions:
is less than 0.05, extraction of the soil samples at the site
8.2.1 Weigh out 200 mg (weighed to 60.1 mg) of the fuel
should be performed using5gof calcium oxide. If the
type of interest into a 100-mL volumetric flask and dilute to
absorbance value of the first soil blank extract is greater than
volume using isopropyl alcohol. This gives a 2000-mg/L
0.05, a second blank sample should be extracted using addi-
standard stock solution. Other standard solutions can be
tional calcium oxide. As stated in 8.1.2, for the first blank
prepared as needed by appropriate dilution of this stock
sample, approximately5gof calcium oxide should be used. If
solution. For example, to prepare a 200-mg/L solution of the
a second blank analysis is required, approximately 10 g of
fuel type of interest, pipet 5 mL of the stock solution into a
calcium oxide should be added to the soil sample. If the
50-mL volumetric flask and dilute to volume using isopropyl
absorbance value of the second blank extract is lower than for
alcohol. For work in the field, a standard stock solution can be
thefirstblankextract,butisstillgreaterthan0.05,athirdblank
prepared by diluting 25 µLof a fuel standard (density can vary
sample should be tested using approximately 15 g of calcium
from ;0.75–0.90 g/mL) to 100 mL with isopropyl alcohol.
oxide. These steps can be repeated, increasing the amount of
8.3 Sample Preparation:
calcium oxide by approximately 5 g each time, until the blank
8.3.1 Preweigh a 125-mL (4-oz), wide-mouth, glass sample
absorbance value is less than 0.05. In this way, the amount of
collection bottle having a polytetrafluoroethylene-lined lid.
calcium oxide required to inhibit interferences from humic
Record the mass of the empty sample collection bottle to 60.1
material and moisture in the soil can be determined. Excess
g.
calcium oxide will not affect the analysis results. If the
8.3.2 Add 5 g (weighed to 60.1 g) of soil directly to the
absorbance of the value of the second blank extract is not
preweighed sample collection bottle. Weigh the sample bottle-
decreased by the addition of 10 g of calcium oxide to the blank
plus-sample, and record the mass of the soil sample added to
sample or if the addition of calcium oxide does not lower the
the bottle to 60.1 g.
absorbance of the blank extract to less than 0.05, even with the
8.3.3 Add the appropriate amount of calcium oxide as
addition of a large quantity of conditioning agent, and the
determined in 8.1.2.1 to the soil. The calcium oxide should be
absorbance of the b
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