ASTM E248-20

Standard Test Method for Determination of Manganese in Manganese Ores by Pyrophosphate Complexed Permanganate Potentiometric Titrimetry

SIGNIFICANCE AND USE
5.1 This test method is intended to be used as a referee method for compliance with compositional specifications for manganese content. It is assumed that all who use these procedures will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that work will be performed in a properly equipped laboratory and that proper waste disposal procedures will be followed. Appropriate quality control practices must be followed such as those described in Guide E882.
SCOPE
1.1 This test method covers the determination of manganese in manganese ore in the range from 15 % to 60 %.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.3 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-2020
• ICS: 73.060.20 - Manganese ores
• ICS: 77.040.30 - Chemical analysis of metals
• Technical Committee: E01 - Analytical Chemistry for Metals, Ores, and Related Materials
• Drafting Committee: E01.02 - Ores, Concentrates, and Related Metallurgical Materials

Relations

• Refers: ASTM E135-20 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 01-Jan-2020
• Refers: ASTM E135-19 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-May-2019
• Refers: ASTM E50-17 - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
• Effective Date: 01-Sep-2017
• Refers: ASTM E882-10(2016)e1 - Standard Guide for Accountability and Quality Control in the Chemical Analysis Laboratory
• Effective Date: 01-Dec-2016
• Refers: ASTM E882-10(2016) - Standard Guide for Accountability and Quality Control in the Chemical Analysis Laboratory
• Effective Date: 01-Dec-2016
• Refers: ASTM E50-11(2016) - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
• Effective Date: 01-Aug-2016
• Refers: ASTM E135-16 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-May-2016
• Refers: ASTM E135-15a - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 01-Jul-2015
• Refers: ASTM E135-15 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-May-2015
• Refers: ASTM E135-14b - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-Aug-2014
• Refers: ASTM E135-14a - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 01-Apr-2014
• Refers: ASTM E135-14 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-Feb-2014
• Refers: ASTM E135-13a - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 01-Dec-2013
• Refers: ASTM E691-13 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-May-2013
• Refers: ASTM E691-11 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Nov-2011

Overview

ASTM E248-20, titled "Standard Test Method for Determination of Manganese in Manganese Ores by Pyrophosphate Complexed Permanganate Potentiometric Titrimetry," is an internationally recognized method developed by ASTM International. This standard specifies a precise referee test method for quantifying manganese content within manganese ores, covering a range from 15% to 60% manganese. It is primarily intended for use in laboratories to ensure compliance with compositional specifications and is applicable in both industry and research contexts where accurate manganese quantification is required.

Key Topics

• Test Method Scope
  • Determination of manganese in manganese ores from 15% to 60% concentration.
  • Utilizes pyrophosphate complexed permanganate potentiometric titrimetry for accurate results.
• Significance
  • Serves as a referee method for validating manganese content to meet regulatory and quality standards.
  • Intended for skilled laboratory analysts using proper quality control practices, as outlined in ASTM Guide E882.
• Sample Preparation and Safety
  • Requires all users to adhere to established safety, health, and environmental procedures.
  • Assumes work is conducted in a properly equipped laboratory following appropriate waste disposal.
• Instrumentation and Reagents
  • Requires potentiometric titration apparatus, pH meter with calomel and glass electrodes, and use of reagent-grade chemicals.
  • Potassium permanganate and sodium pyrophosphate are central to the analytical process.
• Quality Control
  • Accuracy and precision must be maintained by following recommended laboratory protocols and reference materials.

Applications

This standard test method has wide-ranging applications in the mining, metallurgy, and materials quality assurance industries:

• Ore Quality Assessment
  • Used by mining companies and mineral processors to verify manganese ore quality for trading, processing, and export.
• Compliance Testing
  • Serves as an authoritative method for regulatory compliance with local and international composition standards for manganese content.
• Research and Development
  • Supports laboratory research requiring high-precision manganese quantification in geological samples and metallurgical research.
• Quality Assurance
  • Applied as a referee method in dispute resolution or in validating the results from routine or alternative manganese analysis techniques.

Related Standards

Several ASTM standards complement or are referenced by ASTM E248-20, enhancing its robustness and supporting best laboratory practices:

• ASTM D1193: Specification for Reagent Water - Ensures the purity required for accurate chemical analysis.
• ASTM E29: Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications.
• ASTM E50: Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials.
• ASTM E135: Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials.
• ASTM E691: Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method.
• ASTM E882: Guide for Accountability and Quality Control in the Chemical Analysis Laboratory.

Conclusion

ASTM E248-20 is an essential standard for laboratories and industries engaged in the determination of manganese in manganese ores. By providing a consistent and accurate method for potentiometric titrimetric analysis, it supports quality control, compliance, and research activities. Consistent use of this standardized test method assists organizations in meeting rigorous industry and regulatory requirements for manganese ore composition, thereby assuring product quality and integrity throughout the supply chain.

Keywords: ASTM E248-20, manganese ore analysis, potentiometric titrimetry, manganese content determination, pyrophosphate complexed permanganate, quality control, compositional compliance, metallurgical testing.

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: E248 − 20
Standard Test Method for
Determination of Manganese in Manganese Ores by
Pyrophosphate Complexed Permanganate Potentiometric
Titrimetry
This standard is issued under the fixed designation E248; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Terminology
3.1 Definitions—For definitions of terms used in this test
1.1 Thistestmethodcoversthedeterminationofmanganese
method, refer to Terminology E135.
in manganese ore in the range from 15% to 60%.
1.2 This standard does not purport to address all of the
4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
4.1 The test sample is decomposed by treatment with HCl,
responsibility of the user of this standard to establish appro-
HNO ,HF,andHClO .Aftertheadditionofsodiumpyrophos-
3 4
priate safety, health, and environmental practices and deter-
phate (Na P O ·10H O) and adjustment of the acidity, the
4 2 7 2
mine the applicability of regulatory limitations prior to use.
manganese is determined by oxidation to trivalent manganese
1.3 This international standard was developed in accor-
withastandardsolutionofpotassiumpermanganate(KMnO ).
dance with internationally recognized principles on standard-
The end point is determined potentiometrically.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
5. Significance and Use
mendations issued by the World Trade Organization Technical
5.1 This test method is intended to be used as a referee
Barriers to Trade (TBT) Committee.
method for compliance with compositional specifications for
manganese content. It is assumed that all who use these
2. Referenced Documents
procedures will be trained analysts capable of performing
2.1 ASTM Standards:
common laboratory procedures skillfully and safely. It is
D1193Specification for Reagent Water
expected that work will be performed in a properly equipped
E29Practice for Using Significant Digits in Test Data to
laboratory and that proper waste disposal procedures will be
Determine Conformance with Specifications
followed. Appropriate quality control practices must be fol-
E50Practices for Apparatus, Reagents, and Safety Consid-
lowed such as those described in Guide E882.
erations for Chemical Analysis of Metals, Ores, and
6. Interferences
Related Materials
E135Terminology Relating to Analytical Chemistry for
6.1 Provision has been made for removal of chromium,
Metals, Ores, and Related Materials
which, under some conditions, is an interfering element.
E691Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method 7. Apparatus
E882Guide for Accountability and Quality Control in the
7.1 pH Meter equipped with calomel and glass electrodes.
Chemical Analysis Laboratory
7.2 Potentiometric Titration Apparatus equipped with calo-
mel and platinum electrodes.Asuitable pH meter may be used
for this purpose.
This test method is under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct 7.3 Magnetic Stirrer—Use of a TFE-fluorocarbon covered
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
stirring bar is recommended.
lurgical Materials.
CurrenteditionapprovedJuly1,2020.PublishedJuly2021.Originallyapproved
8. Reagents
in 1964. Last previous edition approved in 2012 as E248–12. DOI: 10.1520/
E0248-20.
8.1 Purity of Reagents—Reagent grade chemicals shall be
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
used in all tests. Unless otherwise indicated, it is intended that
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
all reagents shall conform to the specifications of the Commit-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. tee onAnalytical Reagents of theAmerican Chemical Society,
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E248 − 20
where such specifications are available. Other grades may be 9. Hazards
used, provided it is first ascertained that the reagent is of
9.1 For precautions to be observed in this method, refer to
sufficiently high purity to permit its use without lessening the
Practice E50.
accuracy of the determination.
8.2 Purity of Water—Unless otherwise indicated, references 10. Sample Preparation
to water mean reagent water conforming to Type I or II of
10.1 The laboratory sample shall be pulverized, if
Specification D1193. Type III or IV may be used if they effect
necessary, so that 100% passes a 150-µm (No. 100) sieve.
no measurable change in the blank or sample.
11. Procedure
8.3 Hydrogen Peroxide (3 %)—Mix 1 volume of concen-
trated hydrogen peroxide (H O , 30%) with 9 volumes of
2 2
11.1 Transfer approximately 0.40 g (or 0.30 g if the man-
water.
ganese content exceeds 50%) of the prepared sample to a
small weighing bottle. Place into a drying oven and dry at
8.4 Potassium Permanganate (KMnO ), Standard Solution
120°C for 1 h. Cap the bottle and cool to room temperature in
(0.1N)
a desiccator. Loosen the stopper momentarily and weigh the
NOTE 1—The 0.1 normality of the KMnO solution used (3.1606 g/L)
cappedbottleandtestsampletothenearest0.1mg.Drythetest
is based on the usual valence change of manganese in acid solution from
sample for an additional 30 min. Cap the bottle, cool in a
7 to 2. In this test method, the manganese in the sample is oxidized from
desiccator, and reweigh. Repeat the drying and weighing until
Mn(II) to Mn(III) while the KMnO is reduced from Mn(VII) to Mn(III).
The factor 0.0439 used in Section 12, therefore, is based on the following
constant mass is obtained. Transfer the sample to a 600-mL
calculation: 4/5 × 0.05494 (Mn equivalent of KMnO in 7 to 2 valence
beaker and reweigh the capped bottle to the nearest 0.1 mg.
change).
The difference between the last two weighings is the mass of
8.4.1 Preparation—Dissolve 3.2 g of potassium perman-
the sample.
ganate (KMnO ) in 1 L of water. Let stand in the dark for
11.2 To the 600-mL beaker add 10 mL of HCl, 10 mL of
2weeks. Filter, without washing, through a Gooch crucible or
HNO , 4 mLto 5 mLof HF, and 10 mLof HClO and heat to
3 4
a fine porosity fritted-glass crucible.Avoid contact with rubber
affect solutio
...

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.
Designation: E248 − 12 E248 − 20
Standard Test Method for
Determination of Manganese in Manganese Ores by
Pyrophosphate Complexed Permanganate Potentiometric
Titrimetry
This standard is issued under the fixed designation E248; 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 definitive test method covers the determination of manganese in manganese ore in the range from 15 % to 60 %.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.3 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.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E50 Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E882 Guide for Accountability and Quality Control in the Chemical Analysis Laboratory
3. Terminology
3.1 Definitions—For definitions of terms used in this test method, refer to Terminology E135.
4. Summary of Test Method
4.1 The test sample is decomposed by treatment with HCL,HCl, HNO , HF, and HClO . After the addition of sodium
3 4
pyrophosphate (Na P O ·10H O) and adjustment of the acidity, the manganese is determined by oxidation to trivalent manganese
4 2 7 2
with a standard solution of potassium permanganate. permanganate (KMnO ). The end point is determined potentiometrically.
This test method is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and is the direct responsibility of
Subcommittee E01.02 on Ores, Concentrates, and Related Metallurgical Materials.
Current edition approved June 1, 2012July 1, 2020. Published July 2012July 2021. Originally approved in 1964. Last previous edition approved in 20072012 as
E248 – 07.E248 – 12. DOI: 10.1520/E0248-12.10.1520/E0248-20.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E248 − 20
5. Significance and Use
5.1 This definitive test method is intended to be used as a referee method for compliance with compositional specifications for
manganese content. It is assumed that all who use these procedures will be trained analysts capable of performing common
laboratory procedures skillfully and safely. It is expected that work will be performed in a properly equipped laboratory and that
proper waste disposal procedures will be followed. Appropriate quality control practices must be followed such as those described
in Guide E882.
6. Interferences
6.1 Provision has been made for removal of chromium, which, under some conditions, is an interfering element.
7. Apparatus
7.1 pH Meter equipped with calomel and glass electrodes.
7.2 Potentiometric Titration Apparatus equipped with calomel and platinum electrodes. A suitable pH meter may be used for this
purpose.
7.3 Magnetic Stirrer—Use of a TFE-fluorocarbon covered stirring bar is recommended.
8. Reagents
8.1 Purity of Reagents—Reagent grade chemicals shall be used in all 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, 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.
8.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to
Type I or II of Specification D1193. Type III or IV may be used if they effect no measurable change in the blank or sample.
8.3 Hydrogen Peroxide (3 %)—Mix 1 volume of concentrated hydrogen peroxide (H O , 30 %) with 9 volumes of water.
2 2
8.4 Potassium Permanganate, Permanganate (KMnO ), Standard Solution (0.1 N) (0.1N)
NOTE 1—The 0.1 normality of the KMnO solution used (3.1606 g/L) is based on the usual valence change of manganese in acid solution from 7 to 2.
In this test method, the manganese in the sample is oxidized from Mn(II) to Mn(III) while the KMnO is reduced from Mn(VII) to Mn(III)Mn(III). The
factor 0.0439 used in Section 12, therefore, is based on the following calculation: 4/5 × 0.05494 (Mn equivalent of KMnO in 7 to 2 valence change).
8.4.1 Preparation—Dissolve 3.2 g of potassium permanganate (KMnO ) in 1 L of water. Let stand in the dark for 2 weeks.
2 weeks. Filter, without washing, through a Gooch crucible or a fine porosity fritted-glass crucible. Avoid contact with rubber or
other organic material. Store in a dark-colored glass-stoppered bottle.
8.4.2 Standardization—Dry a portion of the National Institute of Standards and Technology (NIST) NIST standard sample, or
equivalent, of sodium oxalate at 105 °C. Transfer 0.3000 g of the sodium oxalate (Na C O ) to a 600-mL beaker. Add 250 mL
2 2 4
of H SO (5 + 95), previously boiled for 10 min to 15 min and then cooled to 27 °C 6 3 °C, and stir until the oxalate has dissolved.
2 4
Add 39 mL to 40 mL of the KMnO solution (8.4.1), at a rate of 25 mL/min to 35 mL/min, while stirring slowly. Let stand until
the pink color disappears (about 45 s). Heat to 55 °C to 60 °C and complete the titration by adding KMnO solution (8.4.1), until
a faint pink color persists for 30 s. Add the last 0.5 mL to 1 mL dropwise, allowing each drop to become decolorized before adding
the next drop. To determine the blank: Titrate 250 mL of H SO (5 + 95), treated as above, with KMnO solution (8.4.1) to a faint
2 4 4
pink color. The blank correction is usually equivalent to 0.03 × 0.05 mL.mL to 0.05 mL.
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC, www.chemistry.org. For suggestions on the testing of
reagents not listed by the American Chemical Society, see the United States Pharmacopeia and National Formulary, www.uspnf.com, U.S. Pharmacopeial Convention, INC
(USPC), Rockville, MD.
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