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ASTM E815-99

(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

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
09-Nov-1999
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

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Replaced By
ASTM E815-04 - Standard Test Method for Determination of Calcium Fluoride in Fluorspar by Complexometric Titration
Effective Date
01-May-2004

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ASTM E815-99 - Standard Test Method for Determination of Calcium Fluoride in Fluorspar by Complexometric TitrationASTM E815-99 - Standard Test Method for Determination of Calcium Fluoride in Fluorspar by Complexometric Titration
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ASTM E815-99 - 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: E 815 – 99
Standard Test Method for
Determination of Calcium Fluoride in Fluorspar by
1
Complexometric Titration
This standard is issued under the fixed designation E 815; 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 4. Significance and Use
1.1 This test method covers the determination of calcium 4.1 Fluorspar is used as a flux in steelmaking, glass industry,
fluoride in acid-grade fluorspar and other types of fluorspar that and manufacture of hydrofluoric acid.
can be rendered soluble by the procedure described in the test 4.2 This test method is intended to be used for compliance
method. with compositional specifications for calcium fluoride content.
1.2 This standard does not purport to address all of the It is assumed that all who use these procedures will be trained
safety concerns, if any, associated with its use. It is the analysts capable of performing common laboratory procedures
responsibility of the user of this standard to establish appro- skillfully and safely. It is expected that work will be performed
priate safety and health practices and determine the applica- in a properly equipped laboratory and that proper waste
bility of regulatory limitations prior to use. disposal procedures will be followed. Appropriate quality
control practices must be followed such as those described in
2. Referenced Documents
Guide E 882.
2.1 ASTM Standards:
2
5. Interferences
D 1193 Specification for Reagent Water
E 50 Practices for Apparatus, Reagents, and Safety Precau- 5.1 None of the elements normally found in fluorspar
3
tions for Chemical Analysis of Metals interfere with this test method.
E 276 Test Methods for Particle Size or Screen Analysis at
6. Apparatus
No. 4 (4.75-mm) Sieve and Finer for Metal-Bearing Ores
3 5
and Related Materials 6.1 Fluoride Ion-Selective Electrode.
E 882 Guide for Accountability and Quality Control in the 6.2 Magnetic Stirrer and TFE-Fluorocarbon-Coated Spin
4
Bar.
Chemical Analysis Laboratory
6.3 pH Meter with High Impedance—Suitable for ion-
3. Summary of Test Method
selective electrode.
3.1 The sample is decomposed by digesting with nitric and 6.4 Polyethylene Beakers, 100-mL.
6
perchloric acids and the fluorine is expelled by fuming. The 6.5 Single Junction Ag/AgCl Reference Electrode.
residue is dissolved in dilute hydrochloric acid, the solution
7. Reagents and Materials
made alkaline, and the calcium titrated with standard EDTA
7.1 Purity of Reagents—Reagent grade chemicals shall be
solution. Calcium present as carbonate is determined in a
separate sample with EDTA solution, after extracting the used in all tests. Unless otherwise indicated, it is intended that
all reagents conform to the specifications of the Committee on
former with dilute acetic acid. A correction for calcium
fluoride, solubilized by dilute acetic acid digestion, is applied, Analytical Reagents of the American Chemical Society where
7
such specifications are available. Other grades may be used,
by determining the fluoride in the acetic acid extract by fluoride
ion-selective electrode. The CaF content is then calculated.
2
1
This test method is under the jurisdiction of ASTM Committee E-1 on
5
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct Orion model 94-91 has been found suitable for this purpose.
6
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal- Orion model 90-01-00 has been found suitable for this purpose.
7
lurgical Materials. Reagent Chemicals, American Chemical Society Specifications, American
Current edition approved Nov. 10, 1999. Published January 2000. Originally Chemical Society, Washington, DC. For suggestions on the testing of reagents not
published as E 815 – 81. Last previous edition E 815 – 94. listed by the American Chemical Society, see Analar Standards for Laboratory
2
Annual Book of ASTM Standards, Vol 11.01. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
3
Annual Book of ASTM Standards, Vol 03.05. and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
4
Annual Book of ASTM Standards, Vol 03.06. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
E 815
provided it is first ascertained that the reagent is of sufficient 9.1.1.2 Add 0.2 g of hydroxynaphthol blue indicator and
high purity to permit its use without lessening the accuracy of titrate immediately with 0.025 M EDTA solution ( 7.5). At the
the determination. equivalen
...

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