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ASTM E463-98

(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

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.

General Information

Status
Historical
Publication Date
09-May-1998
ICS
73.060.40 - Aluminium ores
73.080 - Non-metalliferous minerals
Technical Committee
E01 - Analytical Chemistry for Metals, Ores, and Related Materials
Drafting Committee
E01.02 - Ores, Concentrates, and Related Metallurgical Materials
Current Stage
Ref Project

Relations

Replaced By
ASTM E463-03 - Standard Test Method for Silica in Fluorspar by the Silico-Molybdate Visible Spectrometry
Effective Date
10-Jun-2003

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ASTM E463-98 - Standard Test Method for Silica in Fluorspar by the Silico-Molybdate Visible SpectrometryASTM E463-98 - Standard Test Method for Silica in Fluorspar by the Silico-Molybdate Visible Spectrometry
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ASTM E463-98 - Standard Test Method for Silica in Fluorspar by the Silico-Molybdate Visible Spectrometry
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: E 463 – 98
Standard Test Method for
Silica in Fluorspar by the Silico-Molybdate Visible
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 5. Concentration Range
1.1 This test method covers the determination of silica in 5.1 The recommended concentration range is from 0.2 to
fluorspar in concentrations from 0.5 to 10 %. 2.0 mg of silica per 100 mL of solution, using a 1-cm cell.
1.2 This standard does not purport to address all of the
NOTE 1—Cells having other dimensions may be used, provided suitable
safety problems, if any, associated with its use. It is the
adjustments can be made in the amounts of sample and reagent used.
responsibility of the user of this standard to establish appro-
6. Stability of Color
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
6.1 After the addition of the ammonium molybdate, color is
fully developed within 10 min and is stable after extraction
2. Referenced Documents
with butyl alcohol.
2.1 ASTM Standards:
E 50 Practices for Apparatus, Reagents, and Safety Precau- 7. Interferences
tions for Chemical Analysis of Metals
7.1 The elements ordinarily present in commercial fluor-
E 276 Test Method for Particle Size or Screen Analysis at
spars do not interfere in this test method.
No. 4 (4.75-mm) Sieve and Finer for Metal-Bearing Ores
8. Reagents
and Related Materials
E 882 Guide for Accountability and Quality Control in the
8.1 Purity and Concentration of Reagents—The purity and
Chemical Analysis Laboratory
concentration of the common chemical reagents used shall
conform to Practices E 50. Special apparatus and reagents are
3. Summary of Test Method
located in separate sections preceding the procedure.
3.1 The sample is fused with anhydrous sodium borate and
8.2 Ammonium Molybdate Solution (100 g/L)—Dissolve
the melt is dissolved in dilute hydrochloric acid. Silica is
100 g of ammonium-heptamolybdate [(NH ) Mo O ·4H O]
4 6 7 24 2
determined photometrically after extraction of the silico-
in 500 mL of water, dilute to 1 L, and mix.
molybdate complex with normal butyl alcohol. Photometric
8.3 Silica (SiO )—Heat pure silicic acid in a platinum
measurement of the extract is made at 400 nm.
crucible to expel combined water by gradually increasing
temperature to 1050°C. Maintain at 1050°C for at least 5 min.
4. Significance and Use
Cool to room temperature in a desiccator.
4.1 This test method is intended as a referee method for
8.4 Sodium Borate (Na B O )—Anhydrous powder, low-
2 4 7
compliance with compositional specifications for impurity
silica content.
content. It is assumed that all who use this procedure will be
NOTE 2—If low silica sodium borate is not available, prepare the
trained analysts capable of performing common laboratory
reagent as follows: Transfer 247 g of boric acid to a large platinum dish.
practices skillfully and safely. It is expected that work will be
Expel water by gradually increasing the temperature to about 1000°C.
performed in a properly equipped laboratory and that proper
When effervescence ceases, gradually introduce 106 g of sodium carbon-
waste disposal procedures will be followed. Follow appropriate
ate into the molten mass. Maintain at a temperature of about 1000°C until
quality control practices such as those described in Guide
a clear melt is obtained.
E 882.
9. Sample Preparation
9.1 The analytical sample shall be pulverized, if necessary,
This test method is under the jurisdiction of ASTM Committee E-1 on
to pass a No. 100 (150-μm) sieve (see Test Method E 276). Dry
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
at 105 to 110°C for a minimum of 1 h.
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
lurgical Materials.
10. Procedure
Current edition approved Jan. 15, 1993. Published March 1993. Originally
published as E463 – 72. Last previous edition E463 – 72 (1998).
10.1 Transfer7gofNa B O to each of six 25-mL platinum
2 4 7
Annual Book of ASTM Standards, Vol 03.05.
3 crucibles. Form a cavity in the center of the flux.
Annual Book of ASTM Standards, Vol 03.06.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
E 463
10.2 Into Crucibles 1 and 2 weigh 0.100 to1gofthe dry separatory funnel, shake for 30 s, allow the phases to separate,
sample. Choose sample weights to provide from 5 to 10 mg of and discard the acid layer. Repeat the washing twice more.
SiO . 10.14 Transfer the butyl alcohol phase to a dry 100-mL
10.3 Into Crucibles 3 and 4 weigh 10.0 mg of SiO reagent. volumetric flask. Wash the separatory funnel twice with 1 or
10.4 Crucibles 5 and 6 serve as blanks. 2-mL portions of butyl alcohol, and add the washings to the
10.5 Mix the contents of the crucibles with a platinum or volumetric flask. Add 1 mL of ethyl alcohol, dilute to volume
polyethylene rod. Transfer adhering particles to the crucible. with butyl alcohol, and mix.
10.6 Cover the crucible and heat gently until moisture is
11. Photometry
expelled. Increase the temperature until complete fusion re-
11.1 Adjust the photometer to the initial setting using water
sults.
as
...

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5.1 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 E882.
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1.4 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the standard.  
1.5 Unless the order specifies the applicable “M” specification designation, the material shall be furnished to the inch units.  
1.6 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.

  • Technical specification
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    English language
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  • Technical specification
    5 pages
    English language
    sale 15% off