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ASTM E815-04

(Test Method)

Standard Test Method for Determination of Calcium Fluoride in Fluorspar by Complexometric Titration

Standard Test Method for Determination of Calcium Fluoride in Fluorspar by Complexometric Titration

SIGNIFICANCE AND USE
Fluorspar is used as a flux in steelmaking, glass industry, and manufacture of hydrofluoric acid.
This test method is intended to be used for compliance with compositional specifications for calcium fluoride content. 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 must be followed such as those described in Guide E 882.
SCOPE
1.1 This test method covers the determination of calcium fluoride in acid-grade fluorspar and other types of fluorspar that can be rendered soluble by the procedure described in the test method.
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

Status
Historical
Publication Date
30-Apr-2004
ICS
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

Replaces
ASTM E815-99 - Standard Test Method for Determination of Calcium Fluoride in Fluorspar by Complexometric Titration
Effective Date
01-May-2004
Replaced By
ASTM E815-11 - Standard Test Method for Determination of Calcium Fluoride in Fluorspar by Complexometric Titrimetry
Effective Date
01-Sep-2011

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ASTM E815-04 - Standard Test Method for Determination of Calcium Fluoride in Fluorspar by Complexometric TitrationASTM E815-04 - Standard Test Method for Determination of Calcium Fluoride in Fluorspar by Complexometric Titration
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ASTM E815-04 - Standard Test Method for Determination of Calcium Fluoride in Fluorspar by Complexometric Titration
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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:E815–04
Standard Test Method for
Determination of Calcium Fluoride in Fluorspar by
1
Complexometric Titration
This standard is issued under the fixed designation E815; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope residue is dissolved in dilute hydrochloric acid, the solution
made alkaline, and the calcium titrated with standard EDTA
1.1 This test method covers the determination of calcium
solution. Calcium present as carbonate is determined in a
fluorideinacid-gradefluorsparandothertypesoffluorsparthat
separate sample with EDTA solution, after extracting the
can be rendered soluble by the procedure described in the test
former with dilute acetic acid. A correction for calcium
method.
fluoride, solubilized by dilute acetic acid digestion, is applied,
1.2 This standard does not purport to address all of the
bydeterminingthefluorideintheaceticacidextractbyfluoride
safety concerns, if any, associated with its use. It is the
ion-selective electrode. The CaF content is then calculated.
responsibility of the user of this standard to establish appro- 2
priate safety and health practices and determine the applica-
5. Significance and Use
bility of regulatory limitations prior to use.
5.1 Fluorsparisusedasafluxinsteelmaking,glassindustry,
2. Referenced Documents and manufacture of hydrofluoric acid.
2
5.2 This test method is intended to be used for compliance
2.1 ASTM Standards:
with compositional specifications for calcium fluoride content.
D1193 Specification for Reagent Water
It is assumed that all who use these procedures will be trained
E50 Practices for Apparatus, Reagents, and Safety Consid-
analysts capable of performing common laboratory procedures
erations for Chemical Analysis of Metals, Ores, and
skillfullyandsafely.Itisexpectedthatworkwillbeperformed
Related Materials
in a properly equipped laboratory and that proper waste
E135 Terminology Relating to Analytical Chemistry for
disposal procedures will be followed. Appropriate quality
Metals, Ores, and Related Materials
control practices must be followed such as those described in
E276 Test Method for Particle Size or Screen Analysis at
Guide E882.
No. 4 (4.75-mm) Sieve and Finer for Metal-Bearing Ores
and Related Materials
6. Interferences
E882 Guide for Accountability and Quality Control in the
6.1 None of the elements normally found in fluorspar
Chemical Analysis Laboratory
interfere with this test method.
3. Terminology
7. Apparatus
3.1 Definitions—For definitions of terms used in this test
3
7.1 Fluoride Ion-Selective Electrode.
method, refer to Terminology E135.
7.2 Magnetic Stirrer and TFE-Fluorocarbon-Coated Spin
4. Summary of Test Method Bar.
7.3 pH Meter with High Impedance—Suitable for ion-
4.1 The sample is decomposed by digesting with nitric and
selective electrode.
perchloric acids and the fluorine is expelled by fuming. The
7.4 Polyethylene Beakers, 100-mL.
4
7.5 Single Junction Ag/AgCl Reference Electrode.
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
8. Reagents and Materials
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
lurgical Materials. 8.1 Purity of Reagents—Reagent grade chemicals shall be
Current edition approved May 1, 2004. Published June 2004. Originally
used in all tests. Unless otherwise indicated, it is intended that
approved in 1981. Last previous edition approved in 1999 as E815–99. DOI:
all reagents conform to the specifications of the Committee on
10.1520/E0815-04.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Orion model 94-91 has been found suitable for this purpose.
4
the ASTM website. Orion model 90-01-00 has been found suitable for this purpose.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
E815–04
Analytical Reagents of theAmerican Chemical Society where (8.7) and warm. Cool, transfer to a 1-Lvolumetric flask, dilute
5
such specifications are available. Other grades may be used, to volume with water, and mix. This solution has a concentra-
provided it is first ascertained that the reagent is of sufficient tion of 1 mL=1.0000 mg of calcium.
high purity to permit its use without lessening the accuracy of
11.1.1 Titration—
the determination.
11.1.1.1 Transfer a 50.00
...

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