ASTM D7262-10(2016)e1

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

SIGNIFICANCE AND USE
5.1 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).  
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 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 D3740 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 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 health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 14-Jul-2016
• 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

Standards Content (Sample)

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
´1
Designation: D7262 − 10 (Reapproved 2016)
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.
ε NOTE—Reapproved with editorial changes in July 2016.
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- D653 Terminology Relating to Soil, Rock, and Contained
nation of the quantity of potassium permanganate (KMnO ) Fluids
that organic matter and other naturally occurring oxidizable D1193 Specification for Reagent Water
species present in soil or aquifer solids will consume under D3740 Practice for Minimum Requirements for Agencies
specified conditions as a function of time. Oxidizable species Engaged in Testing and/or Inspection of Soil and Rock as
may include organic constituents and oxidizable inorganic Used in Engineering Design and Construction
ions, such as ferrous iron and sulfides. The following test D4753 Guide for Evaluating, Selecting, and Specifying Bal-
methods are included: ances and Standard Masses for Use in Soil, Rock, and
Test Method A—48-hour Permanganate Natural Oxidant Construction Materials Testing
Demand D6026 Practice for Using Significant Digits in Geotechnical
Test Method B—Permanganate Natural Oxidant Demand Data
Kinetics D6051 Guide for Composite Sampling and Field Subsam-
pling for Environmental Waste Management Activities
1.2 This test method is limited by the reagents employed to
D6169 Guide for Selection of Soil and Rock Sampling
a permanganate natural oxidant demand (PNOD) of 60 g
Devices Used With Drill Rigs for Environmental Investi-
KMnO per kg soil or aquifer solids after a period of 48 hours
gations
(Method A) or two weeks (Method B).
D6282 Guide for Direct Push Soil Sampling for Environ-
1.3 All observed and calculated values shall conform to the
mental Site Characterizations
guidelines for significant digits and rounding established in
D6286 Guide for Selection of Drilling Methods for Environ-
Practice D6026.
mental Site Characterization
1.4 Units—The values stated in SI units are to be regarded 2.2 Other Standards:
as standard. No other units of measurement are included in this Method 4500—KMnO Standard Methods for the Examina-
standard. tion of Water and Wastewater, 20th Ed. 1998
ANSI/AWWA B603-03 Standard for Permanganates
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
3. Terminology
interpret the results obtained and to determine the applicability
3.1 For common definitions of technical terms in this
of these results prior to use.
standard, refer to Terminology D653.
1.6 This standard does not purport to address all of the
3.2 Definitions of Terms Specific to This Standard:
safety concerns, if any, associated with its use. It is the
3.2.1 permanganate natural oxidant demand (PNOD )—the
responsibility of the user of this standard to establish appro- t
mass of potassium permanganate consumed per mass of soil or
priate safety and health practices and determine the applica-
aquifer solids as a function of time.
bility of regulatory limitations prior to use.
1 2
This test method is under the jurisdiction of ASTM Committee D18 on Soil and For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Rock and is the direct responsibility of Subcommittee D18.21 on Groundwater and contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Vadose Zone Investigations. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved July 15, 2016. Published August 2016. Originally the ASTM website.
approved in 2007. Last previous edition approved in 2010 as D7262–10. DOI: Available from American Water Works Association (AWWA), 6666 W. Quincy
10.1520/D7262-10R16E01. 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
´1
D7262 − 10 (2016)
3.2.2 maximum permanganate natural oxidant demand 7. Apparatus
(PNOD )—the maximum mass of potassium permanganate
max
7.1 Reactor Apparatus—A 250-mL glass vial (borosilicate
consumed per mass of soil or aquifer solids over time.
glass or equivalent) with an oxidant resistant screw cap is
3.2.3 permanganate natural oxidant demand kinetics—the
recommended. Zero headspace is not required.
rate at which potassium permanganate is consumed by soil or
7.2 Apparatus for Drying Samples—A laboratory oven ca-
aquifer solids.
pable of delivering sufficient controlled heat to maintain a
4. Summary of Test Method temperature of 105ºC (610ºC).
4.1 Many organic and reduced inorganic substances present 7.3 Balance Scales—A balance having a minimum capacity
in soil and aquifer solids can be oxidized by permanganate. A
of 100 g and meeting the requirements of Guide D4753,
standard potassium permanganate solution is added to a
readable (with no estimation) to 0.1 % of the test mass or
specific amount of soil or aquifer solids and allowed to react
better.
for a period of 48 hours (Method A) or two weeks (Method B).
The residual permanganate concentration is measured at pre- 8. Hazards
scribed sampling times and the difference in concentration is
8.1 When performing laboratory analysis and handling
used to calculate the PNOD at that time.
t
chemicals, safety is a critical component. For this procedure,
4.2 Many organic and reduced inorganic substances present
contact lenses may not be worn. Recommended personal
in soil and aquifer solids can be oxidized by permanganate.
protective equipment (PPE) for this procedure includes rubber
However, some organic compounds react slowly and may not
gloves, safety glasses or goggles and a lab coat or rubber apron.
be completely oxidized within the test period while others may
8.2 In the event of any chemical spill, refer to the specific
resist oxidation altogether.
MSDS for a proper clean-up procedure. In the case of solid
potassium permanganate, sweep the solid into a clean container
5. Significance and Use
and dispose according to state and local regulations. A potas-
5.1 The test method is used to estimate the permanganate
sium permanganate spill should be diluted with water to less
natural oxidant demand exerted by the soil or aquifer solids by
than 4 % strength, collected and disposed of in an approved
determining the quantity of potassium permanganate that is
manner. Paper or cloth towels should not be used to clean any
consumed by naturally occurring species as a function of time.
permanganate spill.
Typically the measurement of PNOD is used to screen potential
sites for in situ chemical oxidation (ISCO) with permanganate 8.3 Excess permanganate solutions can also be neutralized
(Test Method A) and provide information to aid in the design by sodium thiosulfate, citric acid, or other reducing agents.
of remediation systems (Test Method B). Solution concentrations must be less than 4 % prior to addition
of any reducing agent. Excess heat can be generated and there
5.2 While some oxidizable species react relatively quickly
is a potential for an unwanted reaction.
(that is, days to weeks), others react more slower (weeks to
months). Consequently, the PNOD is expected to be some
t
9. Sampling
fraction of the PNOD .
max
9.1 Collect the sample(s) in accordance with Practices
5.3 Due to mass transport related issues at the field-scale it
D6051, D6169, D6282, or D6286. A minimum of 600 grams of
is reasonable to assume that the PNOD measured using the test
t
soil or aquifer solids is required from each sampling location.
method may overestimate the demand exerted during ISCO
applications.
9.2 Samples can be preserved at 4ºC for up to 28 days.
NOTE 1—The quality of the result produced by this standard is
However, it is the responsibility of the users of the test method
dependent on the competence of the personnel performing it, and the
to ensure the maximum holding time for their samples.
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
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.
TEST METHOD A—48-HOUR PERMANGANATE NATURAL OXIDANT DEMAND
10. Scope
10.1 The test method is appropriate for the determination of the total permanganate natural oxidant demand can be ex-
the 48-hour permanganate natural oxidant demand of soil and
pressed after a period of 48 hours. Consequently, this test
aquifer solids. The test is designed to be used for site screening
method should not be used to determine the mass of oxidant
purposes only. Research has shown that a large percentage of
´1
D7262 − 10 (2016)
required for the treatment of hazardous waste sites being 13.6 Sample each vial at 48 hours by removing a 1 mL
considered for ISCO with permanganate. sample aliquot. A centrifuge or oxidant resistant filter (20 µm)
should be used to remove manganese oxides from the sample
11. Summary of Test Method
prior to analysis using Method 4500—KMnO .
11.1 The sample and permanganate solutions are analyzed
for permanganate after a 48-hour reaction period.
...

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 D7262 − 10 (Reapproved 2016)
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*
1.1 This test method covers 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
1.2 This test method is limited by the reagents employed to a permanganate natural oxidant demand (PNOD) of 60 g
KMnO4KMnO 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
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 health practices and determine the applicability of regulatory
limitations prior to use.
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 in Geotechnical Data
D6051 Guide for Composite Sampling and Field Subsampling for Environmental Waste Management Activities
D6169 Guide for Selection of Soil and Rock Sampling Devices Used With Drill Rigs for Environmental Investigations
D6282 Guide for Direct Push Soil Sampling for Environmental Site Characterizations
D6286 Guide for Selection of Drilling Methods for Environmental Site Characterization
2.2 Other Standards:
Method 4500—KMnO Standard Methods for the Examination of Water and Wastewater, 20th Ed. 1998
ANSI/AWWA B603-03 Standard for Permanganates
This test method is under the jurisdiction of ASTM Committee D18 on Soil and Rock and is the direct responsibility of Subcommittee D18.21 on Groundwater and Vadose
Zone Investigations.
Current edition approved July 1, 2010July 15, 2016. Published August 2010August 2016. Originally approved in 2007. Last previous edition approved in 20072010 as
D7262–07.–10. DOI: 10.1520/D7262-10.10.1520/D7262-10R16E01.
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.
*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
´1
D7262 − 10 (2016)
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
t
aquifer solids as a function of time.
3.2.2 maximum permanganate natural oxidant demand (PNOD ) —)—the maximum mass of potassium permanganate
max
consumed 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 Method
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) 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 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).
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 to mass transport related issues at the field-scale it is reasonable to assume that the PNOD measured using the test
t
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 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 (Pyrex (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 capable of delivering sufficient controlled heat to maintain a temperature
of 105 ºC (6 10 ºC).105ºC (610ºC).
7.3 Balance Scales—A balance having a minimum capacity of 100g 100 g and meeting the requirements of Guide D4753,
readable (with no estimation) to 0.1 % of the test mass or better.
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 should be diluted with water to less than 4 % strength, collected and disposed of in an approved manner. Paper
or cloth towels should not be used to clean any permanganate spill.
´1
D7262 − 10 (2016)
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.
9.2 Samples can be preserved at 4 ºC 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.
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.
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 should 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 o
...