Standard Test Method for Screening Fuels in Soils

SIGNIFICANCE AND USE
This test method is a screening procedure for determining the presence of fuels containing aromatic compounds in soils. If the contaminant fuel is available for calibration, the approximate concentration of the fuel in the soil can be calculated. If the fuel type is known, but the contaminant fuel is not available for calibration, an estimate of the contaminant fuel concentration can be calculated using average response factors. If the nature of the contaminant fuel is unknown, a contaminant concentration cannot be calculated, and the test method can only be used only to indicate the presence or absence of fuel contamination.
Fuels containing aromatic compounds, such as diesel fuel and gasoline, as well as other aromatic-containing hydrocarbon materials, such as crude oil, coal oil, and motor oil, can be determined by this test method. The quantitation limit for diesel fuel is about 75 mg/kg. Approximate quantitation limits for other aromatic-containing hydrocarbon materials that can be determined by this screening test method are given in Table 1. Quantitation limits for highly aliphatic materials, such as aviation gasoline and synthetic motor oil, are much higher than those for more aromatic materials, such as coal oil and diesel fuel.
Note 1—The quantitation limits listed in Table 1 are approximate values because in this test method, the quantitation limit can be influenced by the particular fuel type and soil background levels. For information on how the values given in Table 1 were determined, see Appendix X1. Data generated during the development of this screening test method and other information pertaining to this test method can be found in the research reports. (1,2)  
When applying this test method to sites contaminated by diesel fuel, care should be taken in selecting the appropriate response factor from the list given in Table 2, with consideration given to whether or not the fuel contamination is fresh or has undergone weathering/or biodegradatio...
SCOPE
1.1 This test method is a screening procedure for determining the presence of fuels containing aromatic compounds in soils. If the contaminant fuel is available for calibration, the approximate concentration of the fuel in the soil can be calculated. If the contaminant fuel type is known, but the contaminant fuel is not available for calibration, an estimate of the concentration of the fuel in the soil can be determined using average response factors. If the nature of the contaminant fuel is unknown, this screening test method can be used to identify the possible presence of contamination.  
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

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Publication Date
31-Jan-2008
Technical Committee
Current Stage
Ref Project

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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
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
...


This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D5831–02 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
1.1 This test method is a screening procedure for determining the presence of fuels containing aromatic compounds in soils. If
the contaminant fuel is available for calibration, the approximate concentration of the fuel in the soil can be calculated. If the
contaminant fuel type is known, but the contaminant fuel is not available for calibration, an estimate of the concentration of the
fuel in the soil can be determined using average response factors. If the nature of the contaminant fuel is unknown, this screening
test method can be used to identify the possible presence of contamination.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
D 2777 Practice for the Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
E 131 Terminology Relating to Molecular Spectroscopy
E 169 Practices for General Techniques of Ultraviolet-Visible Quantitative Analysis
E 177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E 275 Practice for Describing and Measuring Performance of Ultraviolet, Visible, and Near-Infrared Spectrophotometers
E 691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E 925Practice for the Periodic Calibration of Narrow Band-Pass Spectrophotometers Practice for Monitoring the Calibration
of Ultraviolet-Visible Spectrophotometers whose Spectral Slit Width does not Exceed 2 nm
3. Terminology
3.1 Definitions—For definitions of terms used in this screening test method, refer to Terminology E 131.
4. Summary of Test Method
4.1 Asample of soil is extracted with isopropyl alcohol, and the extract is filtered. The ultraviolet absorbance of the extract is
measured at 254 nm. If the contaminant fuel is available for calibration, the approximate concentration of contamination is
calculated. If the contaminant fuel type is known, but the contaminant fuel is not available for calibration, an estimate of the
contaminant concentration is determined using average response factors. If the nature of the contaminant fuel is not known, the
absorbance value is used to indicate the presence or absence of fuel contamination. Calcium oxide is added to the soil as a
conditioning agent to minimize interferences from humic materials and moisture present in the soil. Particulate interferences are
removed by passing the extract through a filter.
5. Significance and Use
5.1 This screening test method is intended primarily a screening procedure for field use to define the boundaries of soil
contamination.determining the presence of fuels containing aromatic compounds in soils. If the contaminant fuel is available for
calibration, the approximate concentration of the fuel in the soil can be calculated. If the fuel type is known, but the contaminant
fuel is not available for calibration, an estimate of the contaminant fuel concentration can be calculated using average response
This test method is under the jurisdiction of ASTM Committee D34 on Waste Management and is the direct responsibility of Subcommittee D34.01 on Sampling and
Monitoring.
Current edition approved July 10, 2002. Published September 2002. Originally published as D5831–95. Last previous edition D5831–96.
This test method is under the jurisdiction of ASTM Committee D34 on Waste Management and is the direct responsibility of Subcommittee D34.01.05 on Screening
Methods.
Current edition approved Feb. 1, 2008. Published March 2008. Originally approved in 1995. Last previous edition approved in 2003 as D 5831 – 03.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 11.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5831–03 (2008)
factors. If the nature of the contaminant fuel is unknown, a contaminant concentration cannot be calculated, and the test method
can only be used only to indicate the presence or absence of fuel contamination.
5.2 Fuels containing aromatic compounds, such as diesel fuel and gasoline, as well as other aromatic-containing hydrocarbon
materials, such as crude oil, coal oil, and motor oil, can be determined by this test method. The quantitation limit for diesel fuel
is about 75 mg/kg. Approximate quantitation limits for other aromatic-containing hydrocarbon materials that can be determined
by this screening test method are given in Table 1. Quantitation limits for highly aliphatic materials, such as aviation gasoline and
synthetic motor oil, are much higher than those for more aromatic materials, such as coal oil and diesel fuel.
NOTE 1—The quantitation limits listed in Table 1 are approximate values because in this test method, the quantitation limit can be influenced by the
particular fuel type and soil background levels. For information on how the values given in Table 1 were determined, seeAppendix X1. Data generated
during the development of this screening test method and other information pertaining to this test method can be found in the research reports. (1,2)
5.3Extractable material, which scatters or absorbs light at 254 nm, is a potential interference for this screening test method.
5.4This test method may not be applicable to soil located under coniferous trees, because pine tar and turpentine respond as fuel
when tested by this test method, giving high blank absorbance values. See 8.1.2.1 and Note 3 for information on determining if
this test method can be applied to a specific soil located under coniferous trees.
5.3 When applying this test method to sites contaminated by diesel fuel, care should be taken in selecting the appropriate
response factor from the list given in Table 2, with consideration given to whether or not the fuel contamination is fresh or has
undergone weathering/or biodegradation processes. See Appendix X2.
5.4 A factor to consider in using this test method is whether the contamination is a mixture of one or more fuel types. If this
is the case, and a site-specific response factor (seeAppendix X2, Section X2.3) cannot be determined, the response factors for the
individual fuel types in the mixture should be used to estimate contaminant concentrations.
5.5 Certain materials, such as asphalts and asphalt residuals and oils and pitch from trees and other vegetation, which respond
as fuel when tested by the method giving high blank absorbance values, may interfere with use of this test method. See 8.1.2.1
and Note 3 for information on determining if the test method can be applied to a specific soil containing one or more of these types
of materials.
5.6 Extractable material, which scatters or absorbs light at 254 nm, is a potential interference for this screening test method.
6. Apparatus
6.1 Glass Bottles, wide-mouth, 125-mL (4-oz) with polytetrafluoroethylene-lined lids.
6.2 Portable Scale, (for field testing) or laboratory balance, capable of weighing to 0.1 g.
6.3 Portable Stirring Device, (for field testing) or magnetic stir bar and stirrer, which result in motion of the solids during
stirring.
6.4 Syringes, disposable, polyethylene or polypropylene, 10-mL capacity.
6.5 Syringe Filters, disposable, polytetrafluoroethylene, 0.45-µm pore size, 25-mm diameter.
6.6 Spectrometer, set at 254 nm with a 1-cm path length, quartz cell (cuvette).
6.7 Volumetric Flasks and Pipets , for preparing standard solutions.
6.8 Laboratory Balance, capable of weighing to 0.0001 g.
7. Reagents and Materials
7.1 Purity of Reagents—Reagent grade chemicals shall be used in all screening tests. Unless otherwise indicated, it is intended
that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society
Annual Book of ASTM Standards, Vol 03.06.
The boldface numbers given in parentheses refer to a list of references at the end of this test method.
TABLE 1 Approximate Quantitation Limits for Various Fuel Types
in Soils Based on 0.036 AU
Limit of Quantitation (LOQ),
Material
mg/kg
Coal Oil 21
Crude Oil 61
Diesel Fuel 75
Weathered Diesel Fuel 21
Used Motor Oil 162
Weathered Gasoline 170
Unleaded Gasoline 316
Jet Fuel JP-2 378
Motor Oil 533
Aviation Gasoline 1066
Synthetic Motor Oil 1382
D5831–03 (2008)
TABLE 2 Reciprocal Absorptivities at 254 nm for a 1-cm Path
Length Cell
Material 1/Absorptivity, mg/L/AU
Coal Oil 59
Crude Oil 169
Diesel Fuel 209
Weathered Diesel Fuel 58
Used Motor Oil 450
Weathered Gasoline 473
Unleaded Gasoline 877
Jet Fuel JP-2 1050
Motor Oil 1480
Aviation Gasoline 2960
Synthetic Motor Oil 3840
where such specifications are available. Other grades may be used provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of the determination.
7.2 Calcium Oxide Powder, Reagent Grade—Use calcium oxide powder, reagent grade dried at 900°C for 12 h and stored in
a desiccator or tightly sealed glass container prior to use. This is a conditioning agent for removal of interferences caused by the
presence of humic material or moisture, or both, in the sample.
7.3 Isopropyl Alcohol, Reagent Grade—The extraction solvent should have an absorbance value versus air that is less than 0.1.
To maintain purity, the solvent should not be stored for longer than one week in a container having a composition that may leach
UV-absorbing materials.
7.3.1 Transportation of isopropyl alcohol for field testing must comply with current Department of Transportation (DOT)
regulations.
8. Procedure
8.1 Running Blank Analyses:
8.1.1 To ensure that the batch of conditioning agent, syringe, filter cartridge, and so forth, are not contributing to the absorbance
reading, it is recommended that the procedure be performed as specified in 8.3 and 8.4, except using no soil and approximately
5 g of calcium oxide. If the resulting extract has an absorbance value greater than 0.03, the various components should be tested
individually by contacting them with the extraction solvent, and the problem component(s) should be replaced.
8.1.2 In this procedure, the conditioning agent inhibits the extraction of most humic materials, and there is very little, if any,
background from inorganic materials. It is recommended, however, that a blank soil sample be tested as specified in 8.3 and 8.4
by extracting contaminant-free soil of the same type and from the same general area as the site being studied. Approximately 5
gofcalciumoxideshouldbeusedforthisblankextraction.Resultsfromtheblanksoilanalysiscanbeusedtoprovideinformation
on the blank soil absorbance value, the amount of calcium oxide required to dry the soil and inhibit extraction of humic materials,
and the time it takes the soil and calcium oxide to settle after stirring.
8.1.2.1 If the absorbance value of the first soil blank extract is less than 0.05, extraction of the soil samples at the site should
be performed using5gof calcium oxide. If the absorbance value of the first soil blank extract is greater than 0.05, a second blank
sample should be extracted using additional calcium oxide. As stated in 8.1.2, for the first blank sample, approximately5gof
calcium oxide should be used. If a second blank analysis is required, approximately 10 g of calcium oxide should be added to the
soil sample. If the absorbance value of the second blank extract is lower than for the first blank extract, but is still greater than
0.05, a third blank sample should be tested using approximately 15 g of calcium oxide. These steps can be repeated, increasing
the amount of calcium oxide by approximately 5 g each time, until the blank absorbance value is less than 0.05. In this way, the
amount of calcium oxide required to inhibit interferences from humic material and moisture in the soil can be determined. Excess
calcium oxide will not affect the analysis results. If the absorbance of the value of the second blank extract is not decreased by
the addition of 10 g of calcium oxide to the blank sample or if the addition of calcium oxide does not lower the absorbance of
the blank extract to less than 0.05, even with the addition of a large quantity of conditioning agent, and the absorbance of the blank
extract is less than 0.1, the blank absorbance value can be subtracted from the sample absorbance values. If this is done, blank
samples from around the site should be tested to ensure that the blank soil absorbance is constant by 60.02 absorbance units. If
theblankabsorbanceforthesecondblankisnotdecreasedbytheadditionof10gofcalciumoxideandtheabsorbanceoftheblank
extract is greater than 0.1, or if blank, correction is not desired, use of an alternative non-UV-absorbing extraction solvent should
beconsidered.Ifanalternativesolventisused,thestepsdescribedin8.1.1and8.1.2shouldberepeatedusingthedifferentsolvent.
8.1.2.2 Note the time required for the soil and calcium oxide to settle after stirring as determined in 8.1.2 or 8.1.2.1 by
performing the blank soil analysis(es).
Annual Book of ASTM Standards, Vol 14.02.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 and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
D5831–03 (2008)
NOTE 2—An example of a non-UV-absorbing solvent that has been used in place of isopropyl alcohol in this method is n-h
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