ASTM E463-09
(Test Method)Standard Test Method for Determination of Silica in Fluorspar by Silico-Molybdate Visible Spectrometry
Standard Test Method for Determination of Silica in Fluorspar by 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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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: E463 − 09
StandardTest Method for
Determination of Silica in Fluorspar by Silico-Molybdate
1
Visible Spectrometry
This standard is issued under the fixed designation E463; 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 photometrically after extraction of the silico-molybdate com-
plex with normal butyl alcohol. Photometric measurement of
1.1 This test method covers the determination of silica in
the extract is made at 400 nm.
fluorspar in concentrations from 0.5 % to 10 %.
1.2 The values stated in SI units are to be regarded as
5. Significance and Use
standard. No other units of measurement are included in this
5.1 This test method is intended as a referee method for
standard.
compliance with compositional specifications for impurity
1.3 This standard does not purport to address all of the
content. It is assumed that all who use this procedure will be
safety concerns, if any, associated with its use. It is the
trained analysts capable of performing common laboratory
responsibility of the user of this standard to establish appro-
practices skillfully and safely. It is expected that work will be
priate safety and health practices and determine the applica-
performed in a properly equipped laboratory and that proper
bility of regulatory limitations prior to use.
wastedisposalprocedureswillbefollowed.Followappropriate
2. Referenced Documents
quality control practices such as those described in Guide
2
E882.
2.1 ASTM Standards:
D1193 Specification for Reagent Water
6. Interferences
E50 Practices for Apparatus, Reagents, and Safety Consid-
erations for Chemical Analysis of Metals, Ores, and
6.1 The elements ordinarily present in commercial fluor-
Related Materials
spars do not interfere in this test method.
E135 Terminology Relating to Analytical Chemistry for
Metals, Ores, and Related Materials
7. Reagents and Materials
E276 TestMethodforParticleSizeorScreenAnalysisatNo.
7.1 Purity of Reagents—Reagent grade chemicals shall be
4 (4.75-mm) Sieve and Finer for Metal-Bearing Ores and
used in all tests. Unless otherwise indicated, it is intended that
Related Materials
all reagents conform to the specifications of the Committee on
E882 Guide for Accountability and Quality Control in the
Analytical Reagents of the American Chemical Society where
Chemical Analysis Laboratory
3
such specifications are available. Other grades may be used,
3. Terminology provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
3.1 Definitions—For definitions of terms used in this test
the determination.
method, refer to Terminology E135.
7.2 Purity of Water—Unless otherwise indicated, references
4. Summary of Test Method
to water shall be understood to mean reagent water as defined
4.1 The sample is fused with anhydrous sodium borate and
by Type I of Specification D1193.
the melt is dissolved in dilute HCl. Silica is determined
7.3 Ammonium Molybdate Solution (100 g/L)—Dissolve
100 g of ammonium-heptamolybdate [(NH ) Mo O ·4H O]
1 4 6 7 24 2
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.
Current edition approved May 1, 2009. Published June 2009. Originally
3
approved in 1972. Last previous edition approved in 2008 as E463 – 08. DOI: Reagent Chemicals, American Chemical Society Specifications , American
10.1520/E0463-09. Chemical Society, Washington, DC, http://www.chemistry.org. For suggestions on
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or the testing of reagents not listed by the American Chemical Society, see Annual
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., http://
Standards volume information, refer to the standard’s Document Summary page on uk.vwr.com, and the United States Pharmacopeia and National Formulary, U.S.
the ASTM website. Pharmacopeial Convention, Inc. (USPC), Rockville, MD, http://www.usp.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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E463 − 09
7.4 Silica (SiO )—Heat pure silicic acid in a platinum flux settles on the crucible cover (Note 3). Transfer the cooled
2
crucible to expel combined water by gradually increasing crucible to
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:E463–08 Designation:E463–09
Standard Test Method for
AnalysisDetermination of Silica in Fluorspar by Silico-
1
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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method covers the determination of silica in fluorspar in concentrations from 0.5 % to 10 %.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D 1193 Specification for Reagent Water
E50 Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related
Materials
E 135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E 276 TestMethodforParticleSizeorScreenAnalysisatNo.4(4.75-mm)SieveandFinerforMetal-BearingOresandRelated
Materials
E 882 Guide for Accountability and Quality Control in the Chemical Analysis Laboratory
3. Terminology
3.1 Definitions—For definitions of terms used in this test method, refer to Terminology E 135.
4. Summary of Test Method
4.1 The sample is fused with anhydrous sodium borate and the melt is dissolved in dilute HCl. Silica is determined
photometrically after extraction of the silico-molybdate complex with normal butyl alcohol. Photometric measurement of the
extract is made at 400 nm.
5. Significance and Use
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 E 882.
6. Interferences
6.1 The elements ordinarily present in commercial fluorspars do not interfere in this test method.
7. Reagents and Materials
7.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such
1
This test method is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and is the direct responsibility of
Subcommittee E01.02 on Ores, Concentrates, and Related Metallurgical Materials.
Current edition approved Dec. 15, 2008.May 1, 2009. Published JanuaryJune 2009. Originally approved in 1972. Last previous edition approved in 20032008 as
E 463 – 038.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
E463–09
3
specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity
to permit its use without lessening the accuracy of the determination.
7.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by
Type I of Specification D 1193.
7.3 Ammonium Molybdate Solution (100 g/L)—Dissolve 100 g of ammonium-heptamolybdate [(NH ) Mo O ·4H O] in
4 6 7 24 2
500 mL of water, dilute to 1 L, and mix.
7.4 Silica (SiO )—Heat pure silicic acid in a platinum crucible to expel combined water by gradually increasing temperature
2
to 1050 °C. Maintain at 1050 °C for at least 5 min. Cool to room temperature in a desiccator.
7.5 Sodium Borate (Na B O )—Anhydrous powder, low-silica content.
2 4 7
NOTE 1—If low silica sodium borate is not available, pr
...
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