ASTM E465-00(2005)
(Test Method)Standard Test Methods for Determination of Manganese (IV) in Manganese Ores by Redox Titration
Standard Test Methods for Determination of Manganese (IV) in Manganese Ores by Redox Titration
SIGNIFICANCE AND USE
This test method is intended to be used for compliance with compositional specifications for manganese dioxide 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 shall be followed, such as those described in Guide E 882.
SCOPE
1.1 These test methods cover the determination of manganese dioxide in amounts commonly found in manganese ore. The determination measures the amount of manganese (IV) present in the sample. The result may be expressed as available oxygen or as manganese dioxide. The following test methods are included and may be used interchangeably: SectionsTest Method A (Ferrous Ammonium Sulfate)9-13Test Method B (Periodate (Sodium Oxalate)14-18
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.
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Designation:E465–00(Reapproved2005)
Standard Test Methods for
Determination of Manganese (IV) in Manganese Ores by
Redox Titration
This standard is issued under the fixed designation E465; 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 3. Terminology
1.1 These test methods cover the determination of manga- 3.1 Definitions—For definitions of terms used in this test
nese dioxide in amounts commonly found in manganese ore. method, refer to Terminology E135.
The determination measures the amount of manganese (IV)
4. Significance and Use
present in the sample.The result may be expressed as available
oxygen or as manganese dioxide. The following test methods 4.1 This test method is intended to be used for compliance
with compositional specifications for manganese dioxide con-
are included and may be used interchangeably:
tent in manganese ores. It is assumed that all who use these
Sections
procedures will be trained analysts capable of performing
Test Method A (Ferrous Ammonium Sulfate) 9-13
common laboratory procedures skillfully and safely. It is
Test Method B (Periodate (Sodium Oxalate) 14-18
expected that work will be performed in a properly equipped
1.2 The values stated in SI units are to be regarded as
laboratory and that proper waste disposal procedures will be
standard. No other units of measurement are included in this
followed. Appropriate quality control practices shall be fol-
standard.
lowed, such as those described in Guide E882.
1.3 This standard does not purport to address all of the
5. Interferences
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5.1 The elements ordinarily present in manganese ores do
priate safety and health practices and determine the applica-
not interfere in either test method.
bility of regulatory limitations prior to use.
6. Reagents and Materials
2. Referenced Documents
6.1 Purity of Reagents—Reagent grade chemicals shall be
2.1 ASTM Standards:
used in all tests. Unless otherwise indicated, it is intended that
D1193 Specification for Reagent Water
all reagents conform to the specifications of the Committee on
E50 Practices for Apparatus, Reagents, and Safety Consid-
Analytical Reagents of the American Chemical Society where
erations for Chemical Analysis of Metals, Ores, and
such specifications are available. Other grades may be used,
Related Materials
provided it is first ascertained that the reagent is of sufficient
E135 Terminology Relating to Analytical Chemistry for
high purity to permit its use without lessening the accuracy of
Metals, Ores, and Related Materials
the determination.
E882 Guide for Accountability and Quality Control in the
6.2 Purity of Water—Unless otherwise indicated, references
Chemical Analysis Laboratory
to water shall be understood to mean reagent water as defined
by Type I of Specification D1193.
These test methods are under the jurisdiction of ASTM Committee E01 on
7. Hazards
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
7.1 Forprecautionstobeobservedinthesemethods,referto
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
lurgical Materials.
Practice E50.
Current edition approved Oct. 1, 2005. Published October 2005. Originally
approved in 1972. Last previous edition approved in 2000 as E465 – 00. DOI:
10.1520/E0465-00R05. Reagent Chemicals, American Chemical Society Specifications, American
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Chemical Society, Washington, DC. For suggestions on the testing of reagents not
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM listed by the American Chemical Society, see “Reagent Chemicals and Standards,”
Standards volume information, refer to the standard’s Document Summary page on by Joseph Rosin, D. Nostrand Co., Inc., New York, NY, and the “United States
the ASTM website. Pharmacopeia.”
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E465–00 (2005)
8. Sampling and Sample Preparation 12. Calculation
12.1 Calculate the percentage of manganese dioxide as
8.1 The sample shall pass a No. 100 (150-µm) sieve.
follows:
TEST METHOD A—FERROUS AMMONIUM
Manganese dioxide, % 5 [~A 2 B! 3 C 3 4.3465]/D (1)
SULFATE METHOD
where:
A = millilitres of standard K Cr O solution used to estab-
2 2 7
9. Summary of Test Method
lish the correlation in 11.6,
9.1 The test sample is dissolved in an excess of ferrous
B = millilitres of standard K Cr O solution required to
2 2 7
ammonium sulfate solution. The manganese dioxide reacts
titrate the excess of ferrous ammonium sulfate in the
with an equivalent amount of ferrous iron. The excess ferrous
sample solution,
iron is titrated with standard potassium dichromate solution
C = the normality of standard K Cr O solution, and
2 2 7
using sodium diphenylamine sulfonate as an indicator.
D = grams of test sample used.
13. Precision and Bias
10. Reagents and Materials
13.1 Precision—Table 1 indicates the precision of the test
10.1 Ferrous Ammonium Sulfate Solution (45 g/L)—
method between laboratories.
Dissolve 45 g of ferrous ammonium sulfate
13.2 Bias—Noinformationonthebiasofthistestmethodis
[Fe(NH ) (SO ) ·6H O] in 1 Lof sulfuric acid (H SO , 1 + 7).
4 2 4 2 2 2 4
known. Accepted reference materials may have not been
10.2 Potassium Dichromate, Standard Solution (0.1 N)
included in the materials used in the interlaboratory study.
10.2.1 Dissolve 4.9035 g of Primary Standard Grade potas-
Users of the method are encouraged to employ accepted
sium dichromate (K Cr O ) in water, transfer to a 1-L volu-
2 2 7
reference materials, if available, and to judge the bias of the
metric flask, dilute to volume, and mix.
method from the difference between the accepted value for the
10.3 Sodium Diphenylamine Sulfonate Indicator Solution (2
manganese dioxide content and the mean value from interlabo-
g/L)
ratory testing of the reference material.
10.3.1 Dissolve 0.20 g of sodium diphenylamine sulfonate
in 100 mL of water. Store in a dark-colored bottle.
TEST METHOD B—SODIUM OXALATE METHOD
14. Summary of Test Method
11. Procedure
14.1 The test sample is dissolved in sulfuric acid in the
11.1 Transfer approximately 0.4 g of test sample to a small,
presence of sodium oxalate. The manganese dioxide reacts
dry weighing bottle and place in a drying oven. Dry at 120°C
with an equivalent amount of oxalate. The excess sodium
for 1 h, cap the bottle, and cool to room temperature in a
oxalate is titrated with a standard solution of potassium
desiccator. Momentarily release the cap to equalize the pres-
permanganate.
sure and weigh the capped bottle to the nearest 0.1 mg. Repeat
the drying and weighing until there is no further weight loss.
15. Reagents and Materials
Transfer the test sample to a dry 300-mLErlenme
...
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