ASTM D7262-07
(Test Method)Standard Test Method for Estimating the Permanganate Natural Oxidant Demand of Soil and Aquifer Solids
Standard Test Method for Estimating the Permanganate Natural Oxidant Demand of Soil and Aquifer Solids
SIGNIFICANCE AND USE
The test method is used to estimate the permanganate natural oxidant demand exerted by the soil or aquifer solids by determining the quantity of potassium permanganate that is consumed by naturally occurring species as a function of time. Typically the measurement of PNOD is used to screen potential sites for in situ chemical oxidation (ISCO) with permanganate (Test Method A) and provide information to aid in the design of remediation systems (Test Method B).
While some oxidizable species react relatively quickly (that is, days to weeks), others react more slower (weeks to months). Consequently, the PNODt is expected to be some fraction of the PNODmax.
Due to mass transport related issues at the field-scale it is reasonable to assume that the PNODt measured using the test method may overestimate the demand exerted during ISCO applications.
Note 1—The quality of the result produced by this standard is dependent on the competence of the personnel performing it, and the suitability of the equipment and facilities used. Agencies that meet the criteria of Practice D 3740 are generally considered capable of competent and objective testing/sampling/inspection/and so forth.
SCOPE
1.1 This test method covers the estimation of the permanganate natural oxidant demand (PNOD) through the determination of the quantity of potassium permanganate (KMnO4) that organic matter and other naturally occurring oxidizable species present in soil or aquifer solids will consume under specified conditions as a function of time. Oxidizable species may include organic constituents and oxidizable inorganic ions, such as ferrous iron and sulfides. The following test methods are included:Test Method A-48-hour Permanganate Natural Oxidant Demand Test Method B-Permanganate Natural Oxidant Demand Kinetics
1.2 This test method is limited by the reagents employed to a permanganate natural oxidant demand (PNOD) of 60 g KMnO4 per kg soil or aquifer solids after a period of 48 hours (Method A) or two weeks (Method B).
1.3 All observed and calculated values shall conform to the guidelines for significant digits and rounding established in Practice D 6026.
1.4 Units - The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to interpret the results of the data. It is the responsibility of the user of this standard to interpret the results obtained and to determine the applicability of these results prior to use.
1.6 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.
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Designation:D7262–07
Standard Test Method for
Estimating the Permanganate Natural Oxidant Demand of
Soil and Aquifer Solids
This standard is issued under the fixed designation D7262; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 This test method covers the estimation of the perman- 2.1 ASTM Standards:
ganate natural oxidant demand (PNOD) through the determi- D1193 Specification for Reagent Water
nation of the quantity of potassium permanganate (KMnO ) D3740 Practice for Minimum Requirements for Agencies
that organic matter and other naturally occurring oxidizable Engaged in Testing and/or Inspection of Soil and Rock as
species present in soil or aquifer solids will consume under Used in Engineering Design and Construction
specified conditions as a function of time. Oxidizable species D4753 Guide for Evaluating, Selecting, and Specifying
may include organic constituents and oxidizable inorganic Balances and Standard Masses for Use in Soil, Rock, and
ions, such as ferrous iron and sulfides. The following test Construction Materials Testing
methods are included: D6026 PracticeforUsingSignificantDigitsinGeotechnical
Test Method A—48-hour Permanganate Natural Oxidant Data
Demand D6051 Guide for Composite Sampling and Field Subsam-
Test Method B—Permanganate Natural Oxidant Demand pling for Environmental Waste Management Activities
Kinetics D6169 Guide for Selection of Soil and Rock Sampling
1.2 This test method is limited by the reagents employed to Devices Used With Drill Rigs for Environmental Investi-
a permanganate natural oxidant demand (PNOD) of 60 g gations
KMnO4 per kg soil or aquifer solids after a period of 48 hours D6282 Guide for Direct Push Soil Sampling for Environ-
(Method A) or two weeks (Method B). mental Site Characterizations
1.3 All observed and calculated values shall conform to the D6286 Guide for Selection of Drilling Methods for Envi-
guidelines for significant digits and rounding established in ronmental Site Characterization
Practice D6026. 2.2 Other Standards:
1.4 Units—The values stated in SI units are to be regarded Method 4500—KMnO Standard Methods for the Exami-
as standard. No other units of measurement are included in this nation of Water and Wastewater, 20th Ed. 1998
standard. ANSI/AWWA B603-03. Standard for Permanganates
1.5 This standard does not purport to interpret the results of
3. Terminology
the data. It is the responsibility of the user of this standard to
interpret the results obtained and to determine the applicability 3.1 Definitions of Terms Specific to This Standard:
3.1.1 permanganate natural oxidant demand (PNOD)—the
of these results prior to use.
t
1.6 This standard does not purport to address all of the mass of potassium permanganate consumed per mass of soil or
aquifer solids as a function of time.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 3.1.2 maximum permanganate natural oxidant demand
(PNOD )—the maximum mass of potassium permanganate
priate safety and health practices and determine the applica-
max
bility of regulatory limitations prior to use. consumed per mass of soil or aquifer solids over time.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
ThistestmethodisunderthejurisdictionofASTMCommitteeD18onSoiland contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Rock and is the direct responsibility of Subcommittee D18.21 on GroundWater and Standards volume information, refer to the standard’s Document Summary page on
Vadose Zone Investigations. the ASTM website.
Current edition approved June 15, 2007. PublishedAugust 2007. DOI: 10.1520/ Available fromAmerican Water WorksAssociation (AWWA), 6666 W. Quincy
D7262-07. Ave., Denver, CO 80235, http://www.awwa.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D7262–07
3.1.3 permanganate natural oxidant demand kinetics—the 7. Apparatus
rate at which potassium permanganate is consumed by soil or
7.1 Reactor Apparatus—A 250-mL glass vial (Pyrex or
aquifer solids.
equivalent) with an oxidant resistant screw cap is recom-
mended. Zero headspace is not required.
4. Summary of Test Method
7.2 Apparatus for Drying Samples—A laboratory oven
4.1 Many organic and reduced inorganic substances present
capable of delivering sufficient controlled heat to maintain a
in soil and aquifer solids can be oxidized by permanganate. A
temperature of 105ºC.
standard potassium permanganate solution is added to a
7.3 Balance Scales—Abalance having a minimum capacity
specific amount of soil or aquifer solids and allowed to react
of 100g and meeting the requirements of Guide D4753,
for a period of 48 hours (MethodA) or two weeks (Method B).
readable (with no estimation) to 0.1 % of the test mass or
The residual permanganate concentration is measured at pre-
better.
scribed sampling times and the difference in concentration is
used to calculate the PNOD at that time.
t
8. Hazards
4.2 Many organic and reduced inorganic substances present
in soil and aquifer solids can be oxidized by permanganate. 8.1 When performing laboratory analysis and handling
chemicals, safety is a critical component. For this procedure,
However, some organic compounds react slowly and may not
be completely oxidized within the test period while others may contact lenses may not be worn. Recommended personal
protective equipment (PPE) for this procedure includes rubber
resist oxidation altogether.
gloves,safetyglassesorgogglesandalabcoatorrubberapron.
5. Significance and Use
8.2 In the event of any chemical spill, refer to the specific
5.1 The test method is used to estimate the permanganate
MSDS for a proper clean-up procedure. In the case of solid
natural oxidant demand exerted by the soil or aquifer solids by
potassiumpermanganate,sweepthesolidintoacleancontainer
determining the quantity of potassium permanganate that is
and dispose according to state and local regulations. A potas-
consumed by naturally occurring species as a function of time.
sium permanganate spill should be diluted with water to less
TypicallythemeasurementofPNODisusedtoscreenpotential
than 4 % strength, collected and disposed of in an approved
sites for in situ chemical oxidation (ISCO) with permanganate
manner. Paper or cloth towels should not be used to clean any
(Test Method A) and provide information to aid in the design
permanganate spill.
of remediation systems (Test Method B).
8.3 Excess permanganate solutions can also be neutralized
5.2 While some oxidizable species react relatively quickly
by sodium thiosulfate, citric acid, or other reducing agents.
(that is, days to weeks), others react more slower (weeks to
Solution concentrations must be less than 4 % prior to addition
months). Consequently, the PNOD is expected to be some
t
of any reducing agent. Excess heat can be generated and there
fraction of the PNOD .
max is a potential for an unwanted reaction.
5.3 Due to mass transport related issues at the field-scale it
isreasonabletoassumethatthePNOD measuredusingthetest
t
9. Sampling
method may overestimate the demand exerted during ISCO
9.1 Collect the sample(s) in accordance with Practices
applications.
D6051,D6169,D6282,orD6286.Aminimumof600gramsof
NOTE 1—The quality of the result produced by this standard is
soil or aquifer solids is required from each sampling location.
dependent on the competence of the personnel performing it, and the
9.2 Samples can be preserved at 4ºC for up to 28 days.
suitability of the equipment and facilities used. Agencies that meet the
However, it is the responsibility of the users of the test method
criteria of Practice D3740 are generally considered capable of competent
to ensure the maximum holding time for their samples.
and objective testing/sampling/inspection/and so forth.
6. Interferences
6.1 Manganese oxides produced as a result of permanganate
Additional references on general laboratory safety and procedures can be found
reduction may interfere with the analysis of permanganate
at: http://www.ceet.niu.edu/labs/safety.html, http://keats.admin.virginia.edu/lsm/
(Method 4500-KMnO ). home.html, and http://www.ehs.iupui.edu/ehs/prog_chemlabsafety.asp.
D7262–07
TEST METHOD A—48-HOUR PERMANGANATE NATURAL OXIDANT DEMAND
10. Scope 13.5 Place 100 ml of 20 000 mg/l KMnO4 stock solution in
each of the three 250 ml glass vials containing the dried
10.1 The test method is appropriate for the determination of
sample. Seal each of the vials and invert once to mix the
the 48-hour permanganate natural oxidant demand of soil and
reagents. Store vials at room temperature (20–22°C).
aquifer solids.The test is designed to be used for site screening
13.6 Sample each vial at 48 hours by removinga1ml
purposes only. Research has shown that a large percentage of
sample aliquot. A centrifuge or oxidant resistant filter (20 µm)
the total permanganate natural oxidant demand can be ex-
should be used to remove manganese oxides from the sample
pressed after a period of 48 hours. Consequently, this test
prior to analysis using Meth
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