ASTM E463-03
(Test Method)Standard Test Method for Silica in Fluorspar by the Silico-Molybdate Visible Spectrometry
Standard Test Method for Silica in Fluorspar by the Silico-Molybdate Visible Spectrometry
SIGNIFICANCE AND USE
This test method is intended as a referee method for compliance with compositional specifications for impurity content. It is assumed that all who use this procedure will be trained analysts capable of performing common laboratory practices 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. Follow appropriate quality control practices such as those described in Guide E 882.
SCOPE
1.1 This test method covers the determination of silica in fluorspar in concentrations from 0.5 to 10 %.
1.2 This standard does not purport to address all of the safety problems, 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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Standards Content (Sample)
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Designation:E463–03
Standard Test Method for
Silica in Fluorspar by the Silico-Molybdate Visible
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Spectrometry
This standard is issued under the fixed designation E 463; 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 molybdate complex with normal butyl alcohol. Photometric
measurement of the extract is made at 400 nm.
1.1 This test method covers the determination of silica in
fluorspar in concentrations from 0.5 to 10 %.
5. Significance and Use
1.2 This standard does not purport to address all of the
5.1 This test method is intended as a referee method for
safety problems, if any, associated with its use. It is the
compliance with compositional specifications for impurity
responsibility of the user of this standard to establish appro-
content. It is assumed that all who use this procedure will be
priate safety and health practices and determine the applica-
trained analysts capable of performing common laboratory
bility of regulatory limitations prior to use.
practices skillfully and safely. It is expected that work will be
2. Referenced Documents performed in a properly equipped laboratory and that proper
2 wastedisposalprocedureswillbefollowed.Followappropriate
2.1 ASTM Standards:
quality control practices such as those described in Guide
D 1193 Specification for Reagent Water
E 882.
E50 Practices for Apparatus, Reagents, and Safety Precau-
tions for Chemical Analysis of Metals
6. Interferences
E 135 Terminology Relating to Analytical Chemistry for
6.1 The elements ordinarily present in commercial fluor-
Metals, Ores and Related Materials
spars do not interfere in this test method.
E 276 Test Method for Particle Size or Screen Analysis at
No. 4 (4.75-mm) Sieve and Finer for Metal-Bearing Ores
7. Reagents and Materials
and Related Materials
7.1 Purity of Reagents—Reagent grade chemicals shall be
E 882 Guide for Accountability and Quality Control in the
used in all tests. Unless otherwise indicated, it is intended that
Chemical Analysis Laboratory
all reagents conform to the specifications of the Committee on
3. Terminology Analytical Reagents of the American Chemical Society where
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such specifications are available. Other grades may be used,
3.1 Definitions—For definitions of terms used in this test
provided it is first ascertained that the reagent is of sufficiently
method, refer to Terminology E 135.
high purity to permit its use without lessening the accuracy of
4. Summary of Test Method the determination.
7.2 Purity of Water—Unless otherwise indicated, references
4.1 The sample is fused with anhydrous sodium borate and
to water shall be understood to mean reagent water as defined
the melt is dissolved in dilute hydrochloric acid. Silica is
by Type I of Specification D 1193.
determined photometrically after extraction of the silico-
7.3 Ammonium Molybdate Solution (100 g/L)—Dissolve
100 g of ammonium-heptamolybdate [(NH ) Mo O ·4H O]
4 6 7 24 2
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This test method is under the jurisdiction of ASTM Committee E01 on
in 500 mL of water, dilute to 1 L, and mix.
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
lurgical Materials.
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Current edition approved June 10, 2003. Published October 2003. Originally Reagent Chemicals, American Chemical Society Specifications, American
approved in 1972. Last previous edition approved in 1998 as E 463 – 72 (1998). Chemical Society, Washington, DC. For suggestions on the testing of reagents not
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Annual Standards for Laboratory
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
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E463–03
problems. This prevents damage to the beaker.
7.4 Silica (SiO )—Heat pure silicic acid in a platinum
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crucible to expel combined water by gradually increasing
10.8 Placethebeakeronasteambathandswirloccasionally
temperature to 1050°C. Maintain at 1050°C for at least 5 min.
until the melt is completely dissolved (Note 4). Cool, remove
Cool to room temperature in a desiccator.
and rinse the platinum crucible and c
...
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