ASTM D5831-96(2001)

Designation: D 5831 – 96 (Reapproved 2001)
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 screening test method, refer to Terminology E 131.
1.1 This test method is a screening procedure for determin-
4. Summary of Test Method
ing the presence of fuels containing aromatic compounds in
4.1 A sample of soil is extracted with isopropyl alcohol, and
soils. If the contaminant fuel is available for calibration, the
the extract is filtered. The ultraviolet absorbance of the extract
approximate concentration of the fuel in the soil can be
is measured at 254 nm. If the contaminant fuel is available for
calculated. If the contaminant fuel type is known, but the
calibration, the approximate concentration of contamination is
contaminant fuel is not available for calibration, an estimate of
calculated. If the contaminant fuel type is known, but the
the concentration of the fuel in the soil can be determined using
contaminant fuel is not available for calibration, an estimate of
average response factors. If the nature of the contaminant fuel
the contaminant concentration is determined using average
is unknown, this screening test method can be used to identify
response factors. If the nature of the contaminant fuel is not
the possible presence of contamination.
known, the absorbance value is used to indicate the presence or
1.2 This standard does not purport to address all of the
absence of fuel contamination. Calcium oxide is added to the
safety concerns, if any, associated with its use. It is the
soil as a conditioning agent to minimize interferences from
responsibility of the user of this standard to establish appro-
humic materials and moisture present in the soil. Particulate
priate safety and health practices and determine the applica-
interferences are removed by passing the extract through a
bility of regulatory limitations prior to use.
filter.
2. Referenced Documents
5. Significance and Use
2.1 ASTM Standards:
5.1 This screening test method is intended primarily for
D 2777 Practice for the Determination of Precision and Bias
2 field use to define the boundaries of soil contamination. If the
of Applicable Test Methods of Committee D-19 on Water
contaminant fuel is available for calibration, the approximate
E 131 Terminology Relating to Molecular Spectroscopy
concentration of the fuel in the soil can be calculated. If the
E 169 Practices for General Techniques of Ultraviolet-
fuel type is known, but the contaminant fuel is not available for
Visible Quantitative Analysis
calibration, an estimate of the contaminant fuel concentration
E 177 Practice for Use of the Terms Precision and Bias in
can be calculated using average response factors. If the nature
ASTM Test Methods
of the contaminant fuel is unknown, a contaminant concentra-
E 275 Practice for Describing and Measuring Performance
tion cannot be calculated, and the test method can only be used
of Ultraviolet, Visible, and Near Infrared Spectrophotom-
3 only to indicate the presence or absence of fuel contamination.
eters
5.2 Fuels containing aromatic compounds, such as diesel
E 691 Practice for Conducting an Interlaboratory Study to
4 fuel and gasoline, as well as other aromatic-containing hydro-
Determine the Precision of a Test Method
carbon materials, such as crude oil, coal oil, and motor oil, can
E 925 Practice for the Periodic Calibration of Narrow Band-
3 be determined by this test method. The quantitation limit for
Pass Spectrophotometers
diesel fuel is about 75 mg/kg. Approximate quantitation limits
3. Terminology for other aromatic-containing hydrocarbon materials that can
be determined by this screening test method are given in Table
3.1 Definitions—For definitions of terms used in this
1. Quantitation limits for highly aliphatic materials, such as
aviation gasoline and synthetic motor oil, are much higher than
This test method is under the jurisdiction of ASTM Committee D34 on Waste
those for more aromatic materials, such as coal oil and diesel
Management and is the direct responsibility of Subcommittee D34.02 on Physical
fuel.
and Chemical Characterization.
Current edition approved Oct. 10, 1996. Published December 1996. Originally
NOTE 1—The quantitation limits listed in Table 1 are approximate
published as D 5831 – 95. Last previous edition D 5831 – 95.
values because in this test method, the quantitation limit can be influenced
Annual Book of ASTM Standards, Vol 11.01.
by the particular fuel type and soil background levels. For information on
Annual Book of ASTM Standards, Vol 03.06.
how the values given in Table 1 were determined, see Appendix X1. Data
Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 5831
TABLE 1 Approximate Quantitation Limits for Various Fuel Types
This is a conditioning agent for removal of interferences
in Soils Based on 0.036 AU
caused by the presence of humic material or moisture, or both,
Limit of Quantitation (LOQ),
in the sample.
Material
mg/kg
7.3 Isopropyl Alcohol, Reagent Grade— Transportation of
Coal Oil 21
isopropyl alcohol for field testing must comply with current
Crude Oil 61
Department of Transportation (DOT) regulations.
Diesel Fuel 75
Used Motor Oil 162
Weathered Gasoline 170
8. Procedure
Unleaded Gasoline 316
Jet Fuel JP-2 378
8.1 Preparation of Standard Solutions:
Motor Oil 533
8.1.1 Weigh out 200 mg (weighed to 60.1 mg) of the fuel
Aviation Gasoline 1066
type of interest into a 100-mL volumetric flask and dilute to
Synthetic Motor Oil 1382
volume using isopropyl alcohol. This gives a 2000-mg/L
standard stock solution. Other standard solutions can be
prepared as needed by appropriate dilution of this stock
generated during the development of this screening test method and other
information pertaining to this test method can be found in the research solution. For example, to prepare a 200-mg/L solution of the
report.
fuel type of interest, pipet 5 mL of the stock solution into a
50-mL volumetric flask and dilute to volume using isopropyl
5.3 Extractable material, which scatters or absorbs light at
alcohol. For work in the field, a standard stock solution can be
254 nm, is a potential interference for this screening test
prepared by diluting 25 μL of a fuel standard (density can vary
method.
from; 0.75–0.90 g/mL) to 100 mL with isopropyl alcohol.
6. Apparatus
8.2 Sample Preparation:
8.2.1 Preweigh a 125-mL (4-oz), wide-mouth, glass sample
6.1 Glass Bottles, wide-mouth, 125-mL (4-oz) with
collection bottle having a polytetrafluoroethylene-lined lid.
polytetrafluoroethylene-lined lids.
Record the mass of the empty sample collection bottle to 60.1
6.2 Portable Scale, (for field testing) or laboratory balance,
g.
capable of weighing to 0.1 g.
8.2.2 Add 5 g (weighed to 60.1 g) of soil directly to the
6.3 Portable Stirring Device, (for field testing) or magnetic
preweighed sample collection bottle. Weigh the sample bottle-
stir bar and stirrer, which result in motion of all solids during
plus-sample, and record the mass of the soil sample added to
stirring.
the bottle to 60.1 g.
6.4 Syringe, disposable, plastic, 10-mL capacity.
6.5 Syringe Filters, disposable, 0.45-μm, in 25-mm polytet- 8.2.3 Add approximately5gof calcium oxide, prepared as
rafluoroethylene cartridges. specified in 7.3, to the soil, and stir with a spatula until a
6.6 Spectrometer Set, at 254 nm with a 1-cm path length, uniform dry mixture is obtained. If the soil contains an
quartz cell (cuvette). excessive amount of water (>50 %), add approximately 5 g
6.7 Volumetric Flasks and Pipets, for preparing standard more of calcium oxide.
solutions. 8.3 Sample Extraction and Analysis:
6.8 Laboratory Balance, capable of weighing to 0.0001 g.
8.3.1 Pour 50 mL of isopropyl alcohol into the sample
bottle.
7. Reagents and Materials
8.3.2 Stir the slurry for 3 min using a portable stirring
7.1 Purity of Reagents—Reagent grade chemicals shall be
device or magnetic stir bar and stirrer so that all solids are in
used in all screening tests. Unless otherwise indicated, it is
motion during stirring. A shorter stirring time or hand shaking
intended that all reagents shall conform to the specifications of
may decrease the extraction efficiency.
the Committee on Analytical Reagents of the American Chemi-
8.3.3 Allow the soil slurry to settle briefly, then remove the
cal Society where such specifications are available. Other
lid and draw the supernatant solution into a 10-mL disposable
grades may be used provided it is first ascertained that the
syringe. Attach a filter cartridge to the end of the syringe. Rinse
reagent is of sufficiently high purity to permit its use without
the sample cuvette with filtered extract. Then fill the cuvette
lessening the accuracy of the determination.
with filtered extract for analysis.
7.2 Calcium Oxide Powder, Reagent Grade—Use calcium
8.3.4 Calibration procedures specific to the spectrometer
oxide powder, reagent grade dried at 900°C for 12 h and stored
being used to perform the absorbance measurements must be
in a desiccator or tightly sealed glass container prior to use.
followed. Instrument instructions for spanning from 0 to 1
absorbance unit must be followed. Calibration is to be per-
formed using isopropyl alcohol to zero the instrument, and if a
Schabron, J. F., Niss, N. D., Hart, B. K., and Sorini, S. S., “Remote Chemical
calibration line is to be established, calibration standards
Sensor Development: A New Field Screening Method for Soil Fuel Contamination,”
prepared from the standard stock solution should be used (see
Laramie, WY, WRI-95-R016, 1995.
8.1.1). Calibration using three standards is recommended.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Calibration curves are nonlinear above 1 AU (>90 % of the
listed by the American Chemical Society, see Analar Standards for Laboratory
light absorbed). As a result, readings must be made below this
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
level. In addition, the extract absorbance reading must fall
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. between the absorbance readings of two calibration standards.
D 5831
NOTE 2—For general information on the techniques most often used in
should be performed as specified, except with no soil. If
ultraviolet analysis, see Practice E 169. For additional information on the
significant absorbance is noted, the various components should
performance of ultraviolet spectrophotometers, see Practice E 275. For
be tested individually by contacting them with isopropyl
information on evaluating the performance of an ultraviolet spectropho-
alcohol, and the problem component(s) should be replaced.
tometer to verify its suitability for continued routine use, see Practice
8.3.10 In this procedure, the conditioning agent inhibits the
E 925.
extraction of most humic materials, and there is very little, if
8.3.5 Read and record the absorbance of the extract at 254
any, background from inorganic materials. It is recommended,
nm.
however, that a blank soil sample should be tested by extract-
8.3.6 Determine an approximate or estimated concentration
ing contaminant-free soil of the same type and from the same
of a known fuel type in the filtered extract.
general area as the site being studied. If any absorbance is
8.3.6.1 If the contaminant fuel was used for calibration, an
measured for the blank, the sample values should be corrected
approximate concentration of the fuel in the extract can be
for this procedure.
calculated using a calibration line. Record this approximate
8.3.11 Also, it is recommended that one spike should be run
concentration of the fuel in the extract in milligrams/litre.
for every batch of samples or for every 20 samples, whichever
8.3.6.2 If the contaminant fuel type is known, but the
is most frequent. A soil sample is spiked by adding 5 μL of
contaminant fuel was not used for calibration, an estimated
diesel fuel or 25 μL of gasoline and shaking the bottle for 3
concentration of the fuel type in the extract can be calculated
min. The extraction and analysis then are performed as
by multiplying the absorbance of the extract by the reciprocal
outlined in 8.2.3-8.3.5. Recovery is calculated by comparing
absorptivity for that fuel type (see Table 2 and Eq 1). Record
the absorbance of the extract from the spiked soil at 254 nm
this estimated concentration of the fuel in the extract in
with the absorbance of a solution of 5 μL of diesel fuel or 25
milligrams/litre.
μL of gasoline in 50 mL of isopropyl alcohol. After correction
~Absorbance!3~1/Absorptivity!5 Estimated concentration of the
for any material appearing in the unspiked soil, the recovery
fuel in the filtered extract ~mg/L!
should be within 20 % of the true value.
(1)
9. Record
NOTE 3—Information pertaining to the reciprocal absorptivity values
are listed in Table X1.1 of the appendix.
9.1 Record the following information:
9.1.1 Type of the fuel contaminant,
8.3.7 Convert the approximate or estimated concentration of
9.1.2 Mass of the empty sample collection bottle, g,
fuel in the extract (see 8.3.6.1 or 8.3.6.2) to an approximate or
9.1.3 Mass of the sample bottle-plus-soil sample, g,
estimated concentration of the fuel in the original soil sample
9.1.4 Mass of the soil sample, g,
in milligrams/kilograms by multiplying the concentration of
9.1.5 Volume of isopropyl alcohol (solvent) used in the
the fuel in the extract in milligrams/litre by a factor represent-
extraction, mL,
ing the solvent volume in millilitres-to-sample mass in grams
9.1.6 Solvent for zeroing spectrometer,
ratio used in the extraction, that is, a factor of ten is used for a
9.1.7 Calibration standard solutions and absorbance values
solvent volume-to-soil mass ratio of 50 mL of isopropyl
at 254 nm,
alcohol:5gof soil. If the extract is diluted, the appropriate
9.1.8 One/absorptivity for the fuel type of interest, if the
correction must be made. Record the approximate/estimated
contaminant fuel is not used for calibration,
concentration of the fuel in the soil sample in milligrams/
9.1.9 Absorbance of the soil sample extract at 254 nm,
kilograms.
9.1.10 Approximate/estimated concentration of the fuel in
8.3.8 If the nature of the fuel-type contaminant is unknown,
the filtered extract, mg/L,
the concentration of the contaminant can not be calculated. In
9.1.11 Approximate/estimated
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