ASTM D7262-23

Standard Test Methods for Estimating the Permanganate Natural Oxidant Demand of Soil and Aquifer Solids

SIGNIFICANCE AND USE
5.1 Test methods A and B are 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. Test Method C is used to estimate the permanganate total oxidant demand exerted by soil, aquifer solids, chemical contaminants or any other reduced species by determining the quantity of potassium permanganate that is consumed by all components of the bulk aquifer as a function of time. Typically, the measurement of oxidant demand is used to screen potential sites for in situ chemical oxidation (ISCO) with permanganate (Test Methods A and C) and provide information to aid in the design of remediation systems (Test Methods B and C).  
5.2 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.  
5.3 For ISCO injection applications, the PNOD may overestimate the demand exerted due to mass transport related issues. For soil blending applications, the PNOD is a more accurate measure of the demand exerted due to better mass to oxidant contact.
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 D3740 are generally considered capable of competent and objective testing/sampling/inspection/and so forth.
SCOPE
1.1 These test methods cover 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  
Test Method C—Permanganate Total Oxidant Demand  
1.2 These test methods are limited by the reagents employed to a permanganate natural oxidant demand (PNOD) of 40 g KMnO4 per kg soil or aquifer solids after a period of 48 hours (Methods A and C) 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 D6026.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 30-Jun-2023
• ICS: 13.080.01 - Soil quality and pedology in general
• Technical Committee: D18 - Soil and Rock
• Drafting Committee: D18.21 - Groundwater and Vadose Zone Investigations

Relations

• Refers: ASTM D4753-24 - Standard Guide for Evaluating, Selecting, and Specifying Balances and Standard Masses for Use in Soil, Rock, and Construction Materials Testing
• Effective Date: 01-Feb-2024
• Refers: ASTM D3740-23 - Standard Practice for Minimum Requirements for Agencies Engaged in Testing and/or Inspection of Soil and Rock as Used in Engineering Design and Construction
• Effective Date: 01-Nov-2023
• Refers: ASTM D3740-19 - Standard Practice for Minimum Requirements for Agencies Engaged in Testing and/or Inspection of Soil and Rock as Used in Engineering Design and Construction
• Effective Date: 01-Oct-2019
• Refers: ASTM D6286-19 - Standard Guide for Selection of Drilling and Direct Push Methods for Geotechnical and Environmental Subsurface Site Characterization
• Effective Date: 01-Oct-2019
• Refers: ASTM D4753-15 - Standard Guide for Evaluating, Selecting, and Specifying Balances and Standard Masses for Use in Soil, Rock, and Construction Materials Testing
• Effective Date: 01-May-2015
• Refers: ASTM D653-14 - Standard Terminology Relating to Soil, Rock, and Contained Fluids
• Effective Date: 01-Aug-2014
• Refers: ASTM D6286-12 - Standard Guide for Selection of Drilling Methods for Environmental Site Characterization
• Effective Date: 01-Sep-2012
• Refers: ASTM D3740-12a - Standard Practice for Minimum Requirements for Agencies Engaged in Testing and/or Inspection of Soil and Rock as Used in Engineering Design and Construction
• Effective Date: 01-May-2012
• Refers: ASTM D3740-12 - Standard Practice for Minimum Requirements for Agencies Engaged in Testing and/or Inspection of Soil and Rock as Used in Engineering Design and Construction
• Effective Date: 01-Mar-2012
• Refers: ASTM D653-11 - Standard Terminology Relating to Soil, Rock, and Contained Fluids
• Effective Date: 01-Sep-2011
• Refers: ASTM D3740-11 - Standard Practice for Minimum Requirements for Agencies Engaged in Testing and/or Inspection of Soil and Rock as Used in Engineering Design and Construction
• Effective Date: 01-Sep-2011
• Refers: ASTM D3740-10 - Standard Practice for Minimum Requirements for Agencies Engaged in Testing and/or Inspection of Soil and Rock as Used in Engineering Design and Construction
• Effective Date: 01-Mar-2010
• Refers: ASTM D653-09 - Standard Terminology Relating to Soil, Rock, and Contained Fluids
• Effective Date: 01-Jan-2009
• Refers: ASTM D653-08a - Standard Terminology Relating to Soil, Rock, and Contained Fluids
• Effective Date: 01-Dec-2008
• Refers: ASTM D653-08 - Standard Terminology Relating to Soil, Rock, and Contained Fluids
• Effective Date: 01-Nov-2008

Overview

ASTM D7262-23: Standard Test Methods for Estimating the Permanganate Natural Oxidant Demand of Soil and Aquifer Solids provides standardized procedures to estimate the amount of potassium permanganate consumed by organic and inorganic species present in soil and aquifer solids. This standard is critical for evaluating the natural oxidant demand (PNOD) and total oxidant demand (TOD), crucial parameters for assessing the feasibility and design of in situ chemical oxidation (ISCO) remediation strategies using permanganate. The test methods support environmental professionals in site assessment and remediation system design by delivering reproducible measurements of oxidant demand over defined time intervals.

Key Topics

• Permanganate Natural Oxidant Demand (PNOD): Measures the mass of potassium permanganate consumed by soil or aquifer solids as a function of time.
• Test Methods:
  • Test Method A: 48-hour PNOD for soil screening.
  • Test Method B: Kinetics of permanganate consumption for designing remediation efforts.
  • Test Method C: Total oxidant demand considering all bulk components, including contaminants.
• Oxidizable Species: Targets both organic matter and reduced inorganic ions such as ferrous iron and sulfides.
• Use of Potassium Permanganate: Widely used in ISCO processes to treat contaminated or hazardous waste sites.
• Site Screening and ISCO Design: Provides essential data for initial site evaluation and the engineering of remediation systems.
• Reaction Kinetics: Addresses how quickly different species react with permanganate, impacting site treatment planning.
• Limitations: The methods are limited to a PNOD of up to 40 g KMnO4 per kg of soil after specified reaction times.

Applications

• In Situ Chemical Oxidation (ISCO): ASTM D7262 is widely used to assess the viability of permanganate-based ISCO for groundwater and soil remediation projects. It enables practitioners to:
  • Screen sites for natural oxidant demand that might reduce ISCO efficacy.
  • Estimate the dosage of potassium permanganate required for the effective treatment of contaminants.
  • Differentiate between rapid and slow-consuming oxidizable species for tailored ISCO design.
  • Assess both the natural oxidant demand of soil (related to organic/inorganic matter) and the total oxidant demand, including added chemical contaminants.
• Remediation System Design: Accurate assessment of oxidant demand supports the development of cost-effective and efficient site remediation strategies, optimizing oxidant application while minimizing excess use.
• Environmental Site Characterization: The standard is integral in environmental studies, risk assessments, and regulatory compliance for contaminated sites.

Related Standards

When applying ASTM D7262-23, consider the following related ASTM and industry standards for a comprehensive approach:

• ASTM D653: Terminology Relating to Soil, Rock, and Contained Fluids
• ASTM D1193: Specification for Reagent Water, ensuring purity and consistency in testing
• ASTM D3740: Practice for Minimum Requirements for Agencies Engaged in Testing/Inspection of Soil and Rock
• ASTM D6026: Practice for Using Significant Digits and Data Records in Geotechnical Data
• ASTM D6051, D6169, D6282, D6286: Guides for soil and rock sampling and subsurface characterization
• APHA/AWWA/WEF Method 4500-KMnO4: Standard Methods for the Examination of Water and Wastewater
• ANSI/AWWA B603-03: Standard for Permanganates

Practical Value

By following ASTM D7262-23, environmental professionals, laboratories, and site owners gain:

• Reliable Data: Consistent protocols for measuring oxidant demand, supporting regulatory compliance and risk management.
• Improved ISCO Outcomes: Tailored remediation designs based on site-specific oxidant consumption rates.
• Reduced Costs: Avoid over-application of permanganate by understanding the actual oxidant demand of soils and aquifers.
• Enhanced Site Assessment: Early identification of sites best suited for permanganate ISCO, streamlining the remediation decision process.

For technical guidance and official documentation, always refer to the most current edition of ASTM D7262 as published by ASTM International.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D7262 − 23
Standard Test Methods 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* 1.7 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 These test methods cover the estimation of the perman-
ization established in the Decision on Principles for the
ganate natural oxidant demand (PNOD) through the determi-
Development of International Standards, Guides and Recom-
nation of the quantity of potassium permanganate (KMnO )
mendations issued by the World Trade Organization Technical
that organic matter and other naturally occurring oxidizable
Barriers to Trade (TBT) Committee.
species present in soil or aquifer solids will consume under
specified conditions as a function of time. Oxidizable species
2. Referenced Documents
may include organic constituents and oxidizable inorganic
ions, such as ferrous iron and sulfides. The following test 2.1 ASTM Standards:
methods are included: D653 Terminology Relating to Soil, Rock, and Contained
Test Method A—48-hour Permanganate Natural Oxidant Fluids
Demand D1193 Specification for Reagent Water
Test Method B—Permanganate Natural Oxidant Demand D3740 Practice for Minimum Requirements for Agencies
Kinetics Engaged in Testing and/or Inspection of Soil and Rock as
Test Method C—Permanganate Total Oxidant Demand Used in Engineering Design and Construction
D4753 Guide for Evaluating, Selecting, and Specifying Bal-
1.2 These test methods are limited by the reagents employed
ances and Standard Masses for Use in Soil, Rock, and
to a permanganate natural oxidant demand (PNOD) of 40 g
Construction Materials Testing
KMnO per kg soil or aquifer solids after a period of 48 hours
D6026 Practice for Using Significant Digits and Data Re-
(Methods A and C) or two weeks (Method B).
cords in Geotechnical Data
1.3 All observed and calculated values shall conform to the
D6051 Guide for Composite Sampling and Field Subsam-
guidelines for significant digits and rounding established in
pling for Environmental Waste Management Activities
Practice D6026.
D6169 Guide for Selection of Subsurface Soil and Rock
1.4 Units—The values stated in SI units are to be regarded Sampling Devices for Environmental and Geotechnical
as standard. No other units of measurement are included in this Investigations
standard. D6282 Guide for Direct Push Soil Sampling for Environ-
mental Site Characterizations
1.5 This standard does not purport to interpret the results of
D6286 Guide for Selection of Drilling and Direct Push
the data. It is the responsibility of the user of this standard to
Methods for Geotechnical and Environmental Subsurface
interpret the results obtained and to determine the applicability
Site Characterization
of these results prior to use.
2.2 Other Standards:
1.6 This standard does not purport to address all of the
APHA/AWWA/WEF Method 4500—KMnO Standard
safety concerns, if any, associated with its use. It is the
Methods for the Examination of Water and Wastewater,
responsibility of the user of this standard to establish appro-
20th Ed. 1998
priate safety, health, and environmental practices and deter-
ANSI/AWWA B603-03 Standard for Permanganates
mine the applicability of regulatory limitations prior to use.
1 2
These test methods are under the jurisdiction of ASTM Committee D18 on Soil For referenced ASTM standards, visit the ASTM website, www.astm.org, or
and Rock and are the direct responsibility of Subcommittee D18.21 on Groundwater contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
and Vadose Zone Investigations. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved July 1, 2023. Published July 2023. Originally approved the ASTM website.
ɛ1 3
in 2007. Last previous edition approved in 2016 as D7262–10(2016) . DOI: Available from American Water Works Association (AWWA), 6666 W. Quincy
10.1520/D7262-23. Ave., Denver, CO 80235, http://www.awwa.org.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7262 − 23
criteria of Practice D3740 are generally considered capable of competent
3. Terminology
and objective testing/sampling/inspection/and so forth.
3.1 For common definitions of technical terms in this
6. Interferences
standard, refer to Terminology D653.
6.1 Manganese oxides produced as a result of permanganate
3.2 Definitions of Terms Specific to This Standard:
reduction may interfere with the analysis of permanganate
3.2.1 permanganate natural oxidant demand (PNOD )—the
t
(Method 4500-KMnO ).
mass of potassium permanganate consumed per mass of soil or 4
aquifer solids as a function of time.
7. Apparatus
3.2.2 maximum permanganate natural oxidant demand
7.1 Reactor Apparatus—A 250-mL glass vial (borosilicate
(PNOD )—the maximum mass of potassium permanganate
max
glass or equivalent) with an oxidant resistant screw cap is
consumed per mass of soil or aquifer solids over time.
recommended. Zero headspace is not required.
3.2.3 permanganate natural oxidant demand kinetics—the
7.2 Apparatus for Drying Samples—A laboratory oven
rate at which potassium permanganate is consumed by soil or
vented to the outside and capable of delivering sufficient
aquifer solids.
controlled heat to maintain a temperature of 105ºC (610ºC).
4. Summary of Test Methods
7.3 Balance Scales—A balance having a minimum capacity
of 100 g and meeting the requirements of Guide D4753,
4.1 Many organic and reduced inorganic substances present
readable (with no estimation) to 0.1 % of the test mass or
in soil and aquifer solids can be oxidized by permanganate. A
better.
standard potassium permanganate solution is added to a
specific amount of soil or aquifer solids and allowed to react
7.4 Drying Pan—Capable of holding a minimum of 600 g of
for a period of 48 hours (Methods A and C) or two weeks
representative soil.
(Method B). The residual permanganate concentration is mea-
7.5 Spatula.
sured at prescribed sampling times and the difference in
8. Hazards
concentration is used to calculate the PNOD at that time.
t
4.2 Many organic and reduced inorganic substances present 8.1 When performing laboratory analysis and handling
chemicals, safety is a critical component. For this procedure,
in soil and aquifer solids can be oxidized by permanganate.
However, some organic compounds react slowly and may not contact lenses may not be worn. Recommended personal
protective equipment (PPE) for this procedure includes rubber
be completely oxidized within the test period while others may
resist oxidation altogether. gloves, safety glasses or goggles and a lab coat or rubber apron.
8.2 In the event of any chemical spill, refer to the specific
5. Significance and Use
MSDS for a proper clean-up procedure. In the case of solid
5.1 Test methods A and B are used to estimate the perman-
potassium permanganate, sweep the solid into a clean container
ganate natural oxidant demand exerted by the soil or aquifer
and dispose according to state and local regulations. A potas-
solids by determining the quantity of potassium permanganate
sium permanganate spill shall be diluted with water to less than
that is consumed by naturally occurring species as a function of
4 % strength, collected and disposed of in an approved manner.
time. Test Method C is used to estimate the permanganate total
Paper or cloth towels shall not be used to clean any perman-
oxidant demand exerted by soil, aquifer solids, chemical
ganate spill.
contaminants or any other reduced species by determining the
8.3 Excess permanganate solutions can also be neutralized
quantity of potassium permanganate that is consumed by all
by sodium thiosulfate, citric acid, or other reducing agents.
components of the bulk aquifer as a function of time. Typically,
Solution concentrations must be less than 4 % prior to addition
the measurement of oxidant demand is used to screen potential
of any reducing agent. Excess heat can be generated and there
sites for in situ chemical oxidation (ISCO) with permanganate
is a potential for an unwanted reaction.
(Test Methods A and C) and provide information to aid in the
design of remediation systems (Test Methods B and C). 9. Sampling
5.2 While some oxidizable species react relatively quickly 9.1 Collect the sample(s) in accordance with Practices
(that is, days to weeks), others react more slower (weeks to D6051, D6169, D6282, or D6286. A minimum of 600 grams of
months). Consequently, the PNOD is expected to be some soil or aquifer solids is required from each sampling location.
t
fraction of the PNOD .
max
9.2 Samples can be preserved at 4ºC for up to 28 days.
5.3 For ISCO injection applications, the PNOD may over- However, it is the responsibility of the users of the test method
estimate the demand exerted due to mass transport related to ensure the maximum holding time for their samples.
issues. For soil blending applications, the PNOD is a more
accurate measure of the demand exerted due to better mass to
oxidant contact.
NOTE 1—The quality of the result produced by this standard is
Additional references on general laboratory safety and procedures can be found
dependent on the competence of the personnel performing it, and the at: http://www.ceet.niu.edu/labs/safety.html, http://keats.admin.virginia.edu/lsm/
suitability of the equipment and facilities used. Agencies that meet the home.html, and http://www.ehs.iupui.edu/ehs/prog_chemlabsafety.asp.
D7262 − 23
TEST METHOD A—48-HOUR PERMANGANATE NATURAL OXIDANT DEMAND
10. Scope
10.1 The test method is appropriate for the determination of 13.5 Place 100 mL of 20 000 mg/L KMnO stock solution
the 48-hour permanganate natural oxidant demand of soil and in each of the three 250 mL glass vials containing the dried
aquifer solids. The test is designed to be used for site screening sample. Seal each of the vials and invert once to mix the
purposes only. Research has shown that a large percentage of reagents. Store vials at room temperature (20-22°C).
the total permanganate natural oxidant demand can be ex-
13.6 Sample each vial at 48 hours by removing a 1 mL
pressed after a period of 48 hours. Consequently, this test
sample aliquot. A centrifuge or oxidant resistant filter (0.20
method shall not be used to determine the mass of oxidant
μm) shall be used to remove manganese oxides from the
required for the treatment of hazardous waste sites being
sample prior to analysis using Method 4500—KMnO .
considered for ISCO with permanganate.
14. Calculations
11. Summary of Test Method
14.1 PNOD values are expressed in units of mass of
t
11.1 The sample and permanganate solutions are analyzed
potassium permanganate per mass of dry aquifer solids using
for permanganate after a 48-hour reaction period.
the following equation:
V KMnO 2 KMnO
~@ # @ # !
4 0 4 t
12. Reagents and Materials
PNOD 5 (1)
t
m
soil
12.1 Purity of Reagents—Reagent grade chemicals shall be
where:
used.
PNOD = permanganate natural oxidant demand at time
t
12.2 Purity of Water—Reference to water shall be under-
= t (g KMnO /kg soil or aquifer solids),
stood to mean reagent grade water that meets the purity
V = volume of the aqueous phase (L),
specifications of Type I or Type II water according to Specifi-
[KMnO ] = initial potassium permanganate concentration
4 0
cation D1193.
(g/L),
12.3 Potassium Permanganate Stock Solution (20 000 mg/ [KMnO ] = potassium permanganate concentration (g/L) at
4 1
L)—Dissolve 20.0 g of potassium permanganate (KMnO ) in time = t, and
m = mass of dry soil or aquifer solids (kg).
water and dilute to 1 L. Mix the stock solution for a minimum
soil
of two hours to make certain the KMnO crystals have
15. Precision and Bia
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM 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.
´1
Designation: D7262 − 10 (Reapproved 2016) D7262 − 23
Standard Test MethodMethods 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.
ε NOTE—Reapproved with editorial changes in July 2016.
1. Scope*
1.1 This test method coversThese test methods cover the estimation of the permanganate natural oxidant demand (PNOD) through
the determination of the quantity of potassium permanganate (KMnO ) 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
Test Method C—Permanganate Total Oxidant Demand
1.2 This test method isThese test methods are limited by the reagents employed to a permanganate natural oxidant demand
(PNOD) of 6040 g KMnO per kg soil or aquifer solids after a period of 48 hours (Method A) (Methods A and C) 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
D6026.
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 healthsafety, health, and environmental practices and determine
the applicability of regulatory limitations prior to use.
1.7 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
This test method isThese test methods are under the jurisdiction of ASTM Committee D18 on Soil and Rock and isare the direct responsibility of Subcommittee D18.21
on Groundwater and Vadose Zone Investigations.
Current edition approved July 15, 2016July 1, 2023. Published August 2016July 2023. Originally approved in 2007. Last previous edition approved in 20102016 as
ɛ1
D7262D7262–10(2016) –10. DOI: 10.1520/D7262-10R16E01. DOI: 10.1520/D7262-23.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7262 − 23
2. Referenced Documents
2.1 ASTM Standards:
D653 Terminology Relating to Soil, Rock, and Contained Fluids
D1193 Specification for Reagent Water
D3740 Practice for Minimum Requirements for Agencies Engaged in Testing and/or Inspection of Soil and Rock as Used in
Engineering Design and Construction
D4753 Guide for Evaluating, Selecting, and Specifying Balances and Standard Masses for Use in Soil, Rock, and Construction
Materials Testing
D6026 Practice for Using Significant Digits and Data Records in Geotechnical Data
D6051 Guide for Composite Sampling and Field Subsampling for Environmental Waste Management Activities
D6169 Guide for Selection of Subsurface Soil and Rock Sampling Devices for Environmental and Geotechnical Investigations
D6282 Guide for Direct Push Soil Sampling for Environmental Site Characterizations
D6286 Guide for Selection of Drilling and Direct Push Methods for Geotechnical and Environmental Subsurface Site
Characterization
2.2 Other Standards:
APHA/AWWA/WEF Method 4500—KMnO Standard Methods for the Examination of Water and Wastewater, 20th Ed. 1998
ANSI/AWWA B603-03 Standard for Permanganates
3. Terminology
3.1 For common definitions of technical terms in this standard, refer to Terminology D653.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 permanganate natural oxidant demand (PNOD )—the mass of potassium permanganate consumed per mass of soil or aquifer
t
solids as a function of time.
3.2.2 maximum permanganate natural oxidant demand (PNOD )—the maximum mass of potassium permanganate consumed
max
per mass of soil or aquifer solids over time.
3.2.3 permanganate natural oxidant demand kinetics—the rate at which potassium permanganate is consumed by soil or aquifer
solids.
4. Summary of Test MethodMethods
4.1 Many organic and reduced inorganic substances present in soil and aquifer solids can be oxidized by permanganate. A standard
potassium permanganate solution is added to a specific amount of soil or aquifer solids and allowed to react for a period of 48 hours
(Method A) (Methods A and C) or two weeks (Method B). The residual permanganate concentration is measured at prescribed
sampling times and the difference in concentration is used to calculate the PNOD at that time.
t
4.2 Many organic and reduced inorganic substances present in soil and aquifer solids can be oxidized by permanganate. However,
some organic compounds react slowly and may not be completely oxidized within the test period while others may resist oxidation
altogether.
5. Significance and Use
5.1 The test method is Test methods A and B are 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 Test Method C is used to estimate the permanganate total oxidant demand
exerted by soil, aquifer solids, chemical contaminants or any other reduced species by determining the quantity of potassium
permanganate that is consumed by all components of the bulk aquifer as a function of time. Typically, the measurement of oxidant
demand is used to screen potential sites for in situ chemical oxidation (ISCO) with permanganate (Test Method A) and Methods
A and C) and provide information to aid in the design of remediation systems (Test Method B).Methods B and C).
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available from American Water Works Association (AWWA), 6666 W. Quincy Ave., Denver, CO 80235, http://www.awwa.org.
D7262 − 23
5.2 While some oxidizable species react relatively quickly (that is, days to weeks), others react more slower (weeks to months).
Consequently, the PNOD is expected to be some fraction of the PNOD .
t max
5.3 Due For ISCO injection applications, the PNOD may overestimate the demand exerted due to mass transport related issues
at the field-scale it is reasonable to assume that issues. For soil blending applications, the PNOD measured using the test method
t
may overestimate is a more accurate measure of the demand exerted during ISCO applications.due to better mass to oxidant
contact.
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 D3740 are generally considered capable of competent and objective
testing/sampling/inspection/and so forth.
6. Interferences
6.1 Manganese oxides produced as a result of permanganate reduction may interfere with the analysis of permanganate (Method
4500-KMnO ).
7. Apparatus
7.1 Reactor Apparatus—A 250-mL glass vial (borosilicate glass or equivalent) with an oxidant resistant screw cap is
recommended. Zero headspace is not required.
7.2 Apparatus for Drying Samples—A laboratory oven vented to the outside and capable of delivering sufficient controlled heat
to maintain a temperature of 105ºC (610ºC).
7.3 Balance Scales—A balance having a minimum capacity of 100 g and meeting the requirements of Guide D4753, readable
(with no estimation) to 0.1 % of the test mass or better.
7.4 Drying Pan—Capable of holding a minimum of 600 g of representative soil.
7.5 Spatula.
8. Hazards
8.1 When performing laboratory analysis and handling chemicals, safety is a critical component. For this procedure, contact lenses
may not be worn. Recommended personal protective equipment (PPE) for this procedure includes rubber gloves, safety glasses
or goggles and a lab coat or rubber apron.
8.2 In the event of any chemical spill, refer to the specific MSDS for a proper clean-up procedure. In the case of solid potassium
permanganate, sweep the solid into a clean container and dispose according to state and local regulations. A potassium
permanganate spill shouldshall be diluted with water to less than 4 % strength, collected and disposed of in an approved manner.
Paper or cloth towels shouldshall not be used to clean any permanganate spill.
8.3 Excess permanganate solutions can also be neutralized by sodium thiosulfate, citric acid, or other reducing agents. Solution
concentrations must be less than 4 % prior to addition of any reducing agent. Excess heat can be generated and there is a potential
for an unwanted reaction.
9. Sampling
9.1 Collect the sample(s) in accordance with Practices D6051, D6169, D6282, or D6286. A minimum of 600 grams of soil or
aquifer solids is required from each sampling location.
Additional references on general laboratory safety and procedures can be found at: http://www.ceet.niu.edu/labs/safety.html, http://keats.admin.virginia.edu/lsm/
home.html, and http://www.ehs.iupui.edu/ehs/prog_chemlabsafety.asp.
D7262 − 23
9.2 Samples can be preserved at 4ºC for up to 28 days. However, it is the responsibility of the users of the test method to ensure
the maximum holding time for their samples.
TEST METHOD A—48-HOUR PERMANGANATE NATURAL OXIDANT DEMAND
10. Scope
10.1 The test method is appropriate for the determination of the 48-hour permanganate natural oxidant demand of soil and aquifer
solids. The test is designed to be used for site screening purposes only. Research has shown that a large percentage of the total
permanganate natural oxidant demand can be expressed after a period of 48 hours. Consequently, this test method shouldshall not
be used to determine the mass of oxidant required for the treatment of hazardous waste sites being considered for ISCO with
permanganate.
11. Summary of Test Method
11.1 The sample and permanganate solutions are analyzed for permanganate after a 48-hour reaction period.
12. Reagents and Materials
12.1 Purity of Reagents—Reagent grade chemicals shall be used.
12.2 Purity of Water—Reference to water shall be understood to mean reagent grade water that meets the purity specifications of
Type I or Type II water according to Specification D1193.
12.3 Potassium Permanganate Stock Solution (20 000 mg/L)—Dissolve 20.0 g of potassium permanganate (KMnO ) in water and
dilute to 1 L. Mix the stock solution for a minimum of two hours to make certain the KMnO crystals have completely dissolved.
NOTE 2—In place of potassium permanganate, sodium permanganate can be used. However, since the concentration of a commercially available NaMnO
solution may vary, standardization is required. This may be accomplished using ANSI/AWWA B603-03.
13. Procedure
13.1 Dry each sample in the laboratory oven at 105ºC (610ºC) for a period of 24 h.
13.2 Homogenize the dried sample by gently mixing by hand. If large stones or rocks are present they shouldshall be removed
prior to analysis using a No. 10 U.S. standard mesh sieve (2.00 mm).
13.3 Place 100 mL of 20 000 mg/L KMnO stock solution in a 250 mL glass vial for the blank determination.
13.4 Place 50 g of dried sample in each of three 250 mL glass vials (each experiment is run in triplicate).
13.5 Place 100 mL of 20 00
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