ASTM E316-17

Standard Test Method for Determination of Iron in Manganese Ores by Hydrogen Sulfide Reduction-Dichromate Titrimetry

SIGNIFICANCE AND USE
5.1 This test method is intended to be used for compliance with compositional specifications for iron content in manganese ores. 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 iron in manganese ore in the range from 2 % to 20 %.  
Note 1: As used in this test method (except as related to the term relative standard deviation), “percent” or “%” refers to mass fraction (wt/wt) of the form 1g/100g.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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.  
1.4 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: 14-Dec-2017
• ICS: 73.060.20 - Manganese ores
• Technical Committee: E01 - Analytical Chemistry for Metals, Ores, and Related Materials
• Drafting Committee: E01.02 - Ores, Concentrates, and Related Metallurgical Materials

Relations

• Replaces: ASTM E316-11 - Standard Test Method for Determination of Iron in Manganese Ores by Hydrogen Sulfide Reduction-Dichromate Titrimetry
• Effective Date: 15-Dec-2017
• 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) - Standard Guide for Accountability and Quality Control in the Chemical Analysis Laboratory
• Effective Date: 01-Dec-2016
• 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 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 E50-11 - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
• Effective Date: 15-Oct-2011

Overview

ASTM E316-17: Standard Test Method for Determination of Iron in Manganese Ores by Hydrogen Sulfide Reduction-Dichromate Titrimetry provides a reliable, laboratory-based approach for determining the iron content in manganese ores. This test method supports compliance with compositional specifications by offering a standardized titrimetric procedure, enabling consistent and accurate reporting of iron content in the 2% to 20% range. The method is intended for use by skilled analysts in suitably equipped laboratories operating under appropriate safety and environmental controls.

Key Topics

• Measurement Range: Suitable for manganese ores containing iron between 2% and 20% (by mass fraction, wt/wt).
• Test Method Summary:
  • Sample decomposition is performed using hydrochloric, hydrofluoric, and sulfuric acids.
  • Iron is chemically reduced with hydrogen sulfide.
  • Excess hydrogen sulfide is removed by boiling.
  • The amount of iron present is determined by titration with standard potassium dichromate, using sodium diphenylamine sulfonate as the indicator.
• Interferences: Common elements in manganese ore do not interfere with the accuracy of this method.
• Safety and Environmental Considerations:
  • The method involves the use of hazardous reagents (e.g., hydrofluoric acid and hydrogen sulfide). Proper safety, health, and environmental practices are required.
  • Laboratories must follow quality control procedures, such as those found in ASTM E882.

Applications

The ASTM E316-17 standard is crucial for industries and laboratories involved in:

• Mineral and Metallurgical Analysis: Essential for quality control and certification of manganese ore shipments by accurately measuring iron content.
• Mining and Ore Processing: Supports compliance with buyer or regulatory requirements where iron content in manganese ores impacts processing or product specifications.
• Research and Development: Provides a repeatable, standardized method for academic, industrial, or governmental laboratories conducting geochemical or metallurgical studies.
• Quality Assurance: Aids laboratories and facilities in demonstrating adherence to international analysis standards, bolstering market confidence in reported values.

Related Standards

For further reference and laboratory best practices, the following ASTM standards are closely connected to ASTM E316-17:

• ASTM D1193: Specification for Reagent Water – outlines quality requirements for all water used in chemical analyses.
• 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 E882: Guide for Accountability and Quality Control in the Chemical Analysis Laboratory.

Practical Value

Adopting ASTM E316-17 ensures:

• Consistent and Accurate Iron Analysis: Harmonizes laboratory processes and results, facilitating acceptance of data in international trade and regulatory environments.
• Support for Regulatory Compliance: Assists mining and mineral processing companies in meeting composition requirements for manganese ore, supporting operational transparency and efficiency.
• Enhanced Laboratory Quality Control: Fosters implementation of rigorous quality management and traceability in analytical operations.

By following ASTM E316-17, organizations improve their analytical reliability and demonstrate commitment to recognized international standards for iron determination in manganese ores.

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:E316 −17
Standard Test Method for
Determination of Iron in Manganese Ores by Hydrogen
Sulfide Reduction-Dichromate Titrimetry
This standard is issued under the fixed designation E316; 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 E882 Guide for Accountability and Quality Control in the
Chemical Analysis Laboratory
1.1 This test method covers the determination of iron in
manganese ore in the range from2%to20%.
3. Terminology
NOTE 1—As used in this test method (except as related to the term
3.1 Definitions—For definitions of terms used in this test
relative standard deviation), “percent” or “%” refers to mass fraction
method, refer to Terminology E135.
(wt/wt) of the form 1g/100g.
1.2 The values stated in SI units are to be regarded as
4. Summary of Test Method
standard. No other units of measurement are included in this
4.1 The sample is decomposed by treatment with HCl, HF
standard.
and H SO .Any residue is treated for the recovery of insoluble
2 4
1.3 This standard does not purport to address all of the
iron. The iron is reduced with hydrogen sulfide, the insoluble
safety concerns, if any, associated with its use. It is the
sulfides are removed by filtration, and the excess hydrogen
responsibility of the user of this standard to establish appro-
sulfide is expelled by boiling.After cooling, the reduced iron is
priate safety, health, and environmental practices and deter-
titrated with a standard potassium dichromate solution using
mine the applicability of regulatory limitations prior to use.
sodium diphenylamine sulfonate as the indicator.
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard-
5. Significance and Use
ization established in the Decision on Principles for the
5.1 This test method is intended to be used for compliance
Development of International Standards, Guides and Recom-
with compositional specifications for iron content in manga-
mendations issued by the World Trade Organization Technical
nese ores. It is assumed that all who use these procedures will
Barriers to Trade (TBT) Committee.
be trained analysts capable of performing common laboratory
proceduresskillfullyandsafely.Itisexpectedthatworkwillbe
2. Referenced Documents
performed in a properly equipped laboratory and that proper
2.1 ASTM Standards:
waste disposal procedures will be followed. Appropriate qual-
D1193 Specification for Reagent Water
ity control practices must be followed such as those described
E29 Practice for Using Significant Digits in Test Data to
in Guide E882.
Determine Conformance with Specifications
E50 Practices for Apparatus, Reagents, and Safety Consid-
6. Interferences
erations for Chemical Analysis of Metals, Ores, and
6.1 None of the elements normally found in manganese ore
Related Materials
interfere with this test method.
E135 Terminology Relating to Analytical Chemistry for
Metals, Ores, and Related Materials
7. Reagents and Materials
7.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
This test method is under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct all reagents conform to the specifications of the Committee on
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
Analytical Reagents of the American Chemical Society where
lurgical Materials.
such specifications are available. Other grades may be used,
Current edition approved Dec. 15, 2017. Published January 2018. Originally
approved in 1967. Last previous edition approved in 2011 as E316 – 11. DOI:
10.1520/E0316-17.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Reagent Chemicals, American Chemical Society Specifications, American
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Standards volume information, refer to the standard’s Document Summary page on listed by the American Chemical Society, see the United States Pharmacopeia and
the ASTM website. National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E316−17
provided it is first ascertained that the reagent is of sufficiently sample to a 400-mL beaker and reweigh the capped bottle to
high purity to permit its use without lessening the accuracy of the nearest 0.1 mg. The difference between the two masses is
the determination. the mass of the sample.
7.2 Purity of Water—Unless otherwise indicated, references
10.2 Moisten the sample with a few millilitres of water, add
to water shall mean reagent water conforming toType I or II of
15 mL of HCl, cover and heat gently until no further attack is
Specification D1193. Type III or IV may be used if they effect
apparent. Add 5 mL of HNO and warm until the action
no measurable change in the blank or sample.
subsides.Add10dropsto15dropsofHFand15mLofH SO ,
2 4
and heat to copious fumes of SO (do not prolong fuming).
7.3 Ferrous Ammonium Sulfate Solution (approx. 0.10 N)—
Cool, rinse the sides of the beaker with a few millilitres of
Dissolve 40 g of ferrous ammonium sulfate
water, and again heat to fumes of SO . Cool, add 100 mL of
(FeSO (NH ) SO ·6H O)inH SO (1+19).Transfertoa1-L
4 4 2 4 2 2 4
water, and heat to boiling.
flask and dilute to volume with H SO (1 + 19). When the
2 4
sample solution is ready for titration, standardize the
10.3 Filter off any residue through a medium texture paper
FeSO (NH ) SO ·6H O solution against the standard potas-
4 4 2 4 2
into a 400-mLbeaker and wash the paper and residue with hot
siumdichromatesolution(0.1000 N)(7.6)asdescribedin11.1.
water until the iron color is removed from the paper. Reserve
Calculate the millilitres of standard potassium dichromate
the filtrate.
solution equivalent to 1 mL of the FeSO (NH ) SO ·6H O
4 4 2 4 2
10.4 Ignite the paper and residue in a platinum crucible,
solution.
cool, moisten with a few drops of water, and add 3 drops to 4
7.4
...

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: E316 − 11 E316 − 17
Standard Test Method for
Determination of Iron in Manganese Ores by Hydrogen
Sulfide Reduction-Dichromate Titrimetry
This standard is issued under the fixed designation E316; 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 determination of iron in manganese ore in the range from 2 % to 20 %.
NOTE 1—As used in this test method (except as related to the term relative standard deviation), “percent” or “%” refers to mass fraction (wt/wt) of
the form g/100g.1g/100g.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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.
1.4 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
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 sample is decomposed by treatment with hydrochloric, hydrofluoric,HCl, HF and sulfuricH SO acids. . Any residue
2 4
is treated for the recovery of insoluble iron. The iron is reduced with hydrogen sulfide, the insoluble sulfides are removed by
filtration, and the excess hydrogen sulfide is expelled by boiling. After cooling, the reduced iron is titrated with a standard
potassium dichromate solution using sodium diphenylamine sulfonate as the indicator.
5. Significance and Use
5.1 This test method is intended to be used for compliance with compositional specifications for iron content in manganese ores.
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.
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 Sept. 1, 2011Dec. 15, 2017. Published September 2011January 2018. Originally approved in 1967. Last previous edition approved in 20052011
as E316 – 00 (2005). 11. DOI: 10.1520/E0316-11.10.1520/E0316-17.
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
E316 − 17
6. Interferences
6.1 None of the elements normally found in manganese ore interfere with this test method.
7. Reagents and Materials
7.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such
specifications are availableavailable. . Other grades may be used, provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of the determination.
7.2 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.
7.3 Ferrous Ammonium Sulfate Solution (approx. 0.10 N)—Dissolve 40 g of ferrous ammonium sulfate
(FeSO (NH ) SO ·6H O) in sulfuricH SO acid (1 + 19). Transfer to a 1-L flask and dilute to volume with sulfuricH SO acid
4 4 2 4 2 2 4 2 4
(1 + 19). When the sample solution is ready for titration, standardize the FeSO (NH ) SO ·6H O solution against the standard
4 4 2 4 2
potassium dichromate solution (0.1000 N) (7.77.6) as described in 11.1. Calculate the millilitres of standard potassium dichromate
solution equivalent to 1 mL of the FeSO (NH ) SO ·6H O solution.
4 4 2 4 2
7.4 Hydrogen Sulfide—(H S).
7.5 Hydrogen Sulfide Wash Solution.
7.5.1 Saturate H SO (1 + 99) with hydrogen sulfide (HH S).S. Prepare fresh as needed.
2 4 2
7.6 Phosphoric Acid (85 %)—Concentrated phosphoric acid (H PO ).
3 4
7.6 Potassium Dichromate, Standard Solution (0.1000 N)
7.6.1 Dissolve 4.9035 g of Primary Standard Grade potassium dichromate (K Cr O ) in water, transfer to a 1-L volumetric
2 2 47
flask, dilute to volume, and mix.
7.7 Sodium Diphenylamine Sulfonate Indicator Solution (2 g/L).
7.7.1 Dissolve 0.20 g of sodium diphenylamine sulfonate in 100 mL of water. Store in a dark-colored bottle.
7.8 Sodium Pyrosulfate (Na S O ).
2 2 7
8. Hazards
8.1 For precautions to be observed in this method, refer to Practices E50.
8.1.1 Warning—Caution should be used for HF in 10.2.
8.1.2 Warning—Caution should be used for H S in 10.5.
9. Sampling and Sample Preparation
9.1 The test unit shall be collected and prepared to maintain the representative iron content in the lot.
9.2 The laboratory sample shall be pulverized to pass a No. 100 (150-μm)150-um (No. 100) sieve.
9.3 Weigh approximately (within 6 25 mg) an amount of test sample specified as follows:
Content of Iron, % Weight of Sample, g
Content of Iron, % Mass of Sample, g
2 to 10 2.0
10 to 20 1.0
10.
...