ASTM E248-97

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

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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 09-May-2002
• 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

• Replaced By: ASTM E248-02 - Test Method for Determination of Manganese in Manganese Ores by Pyrophosphate Complexed Permanganate Potentiometric Titrimetry
• Effective Date: 10-May-2002

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: E 248 – 97
Standard Test Method for
Determination of Manganese in Manganese Ores by
Pyrophosphate Complexed Permanganate Potentiometric
Titration
This standard is issued under the fixed designation E 248; 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 (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope followed. Appropriate quality control practices must be fol-
lowed such as those described in Guide E 882.
1.1 This definitive test method covers the determination of
manganese in manganese ore in the range from 15 to 60 %.
5. Interferences
1.2 This standard does not purport to address all of the
5.1 Provision has been made for removal of chromium
safety concerns, if any, associated with its use. It is the
which, under some conditions, is an interfering element.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
6. Apparatus
bility of regulatory limitations prior to use.
6.1 pH Meter equipped with calomel and glass electrodes.
6.2 Potentiometric Titration Apparatus equipped with
2. Referenced Documents
calomel and platinum electrodes. A suitable pH meter may be
2.1 ASTM Standards:
2 used for this purpose.
D 1193 Specification for Reagent Water
6.3 Magnetic Stirrer—Use of a TFE-fluorocarbon covered
E 50 Practices for Apparatus, Reagents, and Safety Precau-
3 stirring bar is recommended.
tions for Chemical Analysis of Metals
E 882 Guide for Accountability and Quality Control in the
7. Reagents
Chemical Analysis of Metals
7.1 Purity of Reagents—Reagent grade chemicals shall be
3. Summary of Test Method used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
3.1 The test sample is decomposed by treatment with
tee on Analytical Reagents of the American Chemical Society,
hydrochloric, nitric, hydrofluoric, and perchloric acids. After
where such specifications are available. Other grades may be
the addition of sodium pyrophosphate and adjustment of the
used, provided it is first ascertained that the reagent is of
acidity, the manganese is determined by oxidation to trivalent
sufficiently high purity to permit its use without lessening the
manganese with a standard solution of potassium permangan-
accuracy of the determination.
ate. The end point is determined potentiometrically.
7.2 Purity of Water—Unless otherwise indicated, references
4. Significance and Use to water shall be understood to mean reagent water conforming
to Specification D 1193.
4.1 This definitive test method is intended to be used as a
7.3 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
referee method for compliance with compositional specifica-
chloric acid (HCl).
tions for manganese content. It is assumed that all who use
7.4 Hydrochloric Acid (1 + 1)—Mix 1 volume of concen-
these procedures will be trained analysts capable of performing
trated HCl (sp gr 1.19) with 1 volume of water.
common laboratory procedures skillfully and safely. It is
7.5 Hydrofluoric Acid (48 %)—Concentrated hydrofluoric
expected that work will be performed in a properly equipped
acid (HF).
laboratory and that proper waste disposal procedures will be
7.6 Hydrogen Peroxide (3 %)—Mix 1 volume of concen-
trated hydrogen peroxide (H O , 30 %) with 9 volumes of
2 2
This test method is under the jurisdiction of ASTM Committee E-1 on
water.
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
lurigical Materials.
Current edition approved April 10, 1997. Published June 1997. Originally “Reagent Chemicals, American Chemical Society Specifications,” Am. Chemi-
published as E 248 – 64 T. Last previous edition E 248 – 95. cal Soc., Washington, DC. For suggestions on the testing of reagents not listed by
Annual Book of ASTM Standards, Vol 11.01. the American Chemical Society, see “Reagent Chemicals and Standards,” by Joseph
Annual Book of ASTM Standards, Vol 03.05. Rosin, D. Van Nostrand Co., Inc., New York, NY, and the “United States
Annual Book of ASTM Standards, Vol 03.06. Pharmacopeia.”
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
E 248
7.7 Nitric Acid (sp gr 1.42)—Concentrated nitric acid 10 mL of HNO , 4 to 5 mL of HF, and 10 mL of HClO and
3 4
(HNO ). heat to affect solution. Evaporate to fumes of HClO . Cool and
3 4
7.8 Perchloric Acid (70 %) (HClO ). rinse down the sides of the beaker. If complete decomposition
7.9 Potassium Permanganate, Standard Solution (0.1 N) has not been effected, add more HCl, HNO , and HF. Evapo-
(Note 1)—The solution may be standardized against oxalate rate to fumes again and fume strongly (Note 2). Withdraw the
solution as described under Reagent No. 13 of Practices E 50. cover slightly and volatilize any chromium present by drop-
wise addition of HCl. When chromyl chloride has been
NOTE 1—The 0.1 normality of the KMnO solution used (3.1606 g/L)
expelled, as evidenced by the disappearance of any orange
is based on the usual valence change of manganese in acid solution from
vapor upon HCl addition, replace the cover and evaporate to a
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) volume of 2 to 3 mL or until the first appearance of salt
The factor 0.0439 mentioned in Section 9, therefore, is based on the
formation on the bottom of the beaker. Cool, add 10 mL of HCl
following calculation: 4/5 3 0.05494 (Mn equivalent of KMnO in7to2
(1 + 1), and 1 mL of H O , and boil for 4 to 5 min.
2 2
valence change).
NOTE 2—In rare instances there may be a small amount of black residue
7.9.1 Preparation—Dissolve 3.2 g of potassium permanga-
at this po
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