ASTM E465-00
(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
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.
General Information
Relations
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation:E465–00
Standard Test Methods for
Determination of Manganese (IV) in Manganese Ores by
Redox Titration
This standard is issued under the fixed designation E 465; 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.
1. Scope tent in manganese ores. It is assumed that all who use these
procedures will be trained analysts capable of performing
1.1 These test methods cover the determination of manga-
common laboratory procedures skillfully and safely. It is
nese dioxide in amounts commonly found in manganese ore.
expected that work will be performed in a properly equipped
The determination measures the amount of manganese (IV)
laboratory and that proper waste disposal procedures will be
present in the sample.The result may be expressed as available
followed. Appropriate quality control practices shall be fol-
oxygen or as manganese dioxide. The following test methods
lowed, such as those described in Guide E 882.
are included and may be used interchangeably:
Sections
5. Interferences
Test Method A (Ferrous Ammonium Sulfate) 9-13
5.1 The elements ordinarily present in manganese ores do
Test Method B (Periodate (Sodium Oxalate) 14-18
not interfere in either test method.
1.2 This standard does not purport to address all of the
6. Reagents and Materials
safety concerns, if any, associated with its use. It is the
6.1 Purity of Reagents—Reagent grade chemicals shall be
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- used in all tests. Unless otherwise indicated, it is intended that
all reagents conform to the specifications of the Committee on
bility of regulatory limitations prior to use.
Analytical Reagents of the American Chemical Society where
2. Referenced Documents
such specifications are available. Other grades may be used,
2.1 ASTM Standards: provided it is first ascertained that the reagent is of sufficient
D 1193 Specification for Reagent Water high purity to permit its use without lessening the accuracy of
E 50 Practices for Apparatus, Reagents, and Safety Precau- the determination.
tions for Chemical Analysis of Metals 6.2 Purity of Water—Unless otherwise indicated, references
E 135 Terminology Relating to Analytical Chemistry for to water shall be understood to mean reagent water as defined
Metals, Ores, and Related Materials by Type I of Specification D 1193.
E 882 Guide for Accountability and Quality Control in the
4 7. Hazards
Chemical Analysis Laboratory
7.1 Forprecautionstobeobservedinthesemethods,referto
3. Terminology
Practice E 50.
3.1 Definitions—For definitions of terms used in this test
8. Sampling and Sample Preparation
method, refer to Terminology E 135.
8.1 The sample shall pass a No. 100 (150-µm) sieve.
4. Significance and Use
TEST METHOD A—FERROUS AMMONIUM
4.1 This test method is intended to be used for compliance
SULFATE METHOD
with compositional specifications for manganese dioxide con-
9. Summary of Test Method
9.1 The test sample is dissolved in an excess of ferrous
These test methods are under the jurisdiction of ASTM Committee E01 on
ammonium sulfate solution. The manganese dioxide reacts
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
lurgical Materials.
Current edition approved Nov. 10, 2000. Published January 2001. Originally Reagent Chemicals, American Chemical Society Specifications, American
published as E 465 – 72 T. Last previous edition E 465 – 95a. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Annual Book of ASTM Standards, Vol 11.01. listed by the American Chemical Society, see “Reagent Chemicals and Standards,”
Annual Book of ASTM Standards, Vol 03.05. by Joseph Rosin, D. Nostrand Co., Inc., New York, NY, and the “United States
Annual Book of ASTM Standards, Vol 03.06. Pharmacopeia.”
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E465
with an equivalent amount of ferrous iron. The excess ferrous
B = millilitres of standard K Cr O solution required to
2 2 7
iron is titrated with standard potassium dichromate solution
titrate the excess of ferrous ammonium sulfate in the
using sodium diphenylamine sulfonate as an indicator.
sample solution,
C = the normality of standard K Cr O solution, and
2 2 7
10. Reagents and Materials D = grams of test sample used.
10.1 Ferrous Ammonium Sulfate Solution (45 g/L)—
13. Precision and Bias
Dissolve 45 g of ferrous ammonium sulfate
13.1 Precision—Table 1 indicates the precision of the test
[Fe(NH ) (SO ) ·6H O] in 1 Lof sulfuric acid (H SO , 1 + 7).
4 2 4 2 2 2 4
method between laboratories.
10.2 Potassium Dichromate, Standard Solution (0.1 N)
13.2 Bias—Noinformationonthebiasofthistestmethodis
10.2.1 Dissolve 4.9035 g of Primary Standard Grade potas-
known. Accepted reference materials may have not been
sium dichromate (K Cr O ) in water, transfer to a 1-L volu-
2 2 7
included in the materials used in the interlaboratory study.
metric flask, dilute to volume, and mix.
Users of the method are encouraged to employ accepted
10.3 Sodium Diphenylamine Sulfonate Indicator Solution (2
reference materials, if available, and to judge the bias of the
g/L)
method from the difference between the accepted value for the
10.3.1 Dissolve 0.20 g of sodium diphenylamine sulfonate
manganese dioxide content and the mean value from interlabo-
in 100 mL of water. Store in a dark-colored bottle.
ratory testing of the reference material.
TEST METHOD B—SODIUM OXALATE METHOD
11. Procedure
11.1 Transfer approximately 0.4 g of test sample to a small,
14. Summary of Test Method
dry weighing bottle and place in a drying oven. Dry at 120°C
14.1 The test sample is dissolved in sulfuric acid in the
for 1 h, cap the bottle, and cool to room temperature in a
presence of sodium oxalate. The manganese dioxide reacts
desiccator. Momentarily release the cap to equalize the pres-
with an equivalent amount of oxalate. The excess sodium
sure and weigh the capped bottle to the nearest 0.1 mg. Repeat
oxalate is titrated with a standard solution of potassium
the drying and weighing until there is no further weight loss.
permanganate.
Transfer the test sample to a dry 300-mLErlenmeyer flask and
reweigh the capped bottle to the nearest 0.1 mg.The difference
15. Reagents and Materials
is the weight of the test sample.
15.1 1,10 Phenanthroline Indicator Solution (0.025 M)
11.2 Add 50.0 mL of the ferrous ammonium sulfate solu-
15.1.1 Dissolve 1.485 g of 1,10-phenanthroline monony-
tion, plus an additional 10.0 mL for each 0.1 g of MnO
drate and 0.695 g of ferrousulfate (Fe SO ·7 H O) in 50
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.