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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

Relations

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
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:
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
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
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.
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
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.
This test method is under the jurisdiction of ASTM Committee E-1 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct Orion model 94-91 has been found suitable for this purpose.
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal- Orion model 90-01-00 has been found suitable for this purpose.
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
Annual Book of ASTM Standards, Vol 11.01. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 03.05. and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
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.
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. equivalence point, the color changes from pink to blue.
Determine the calcium equivalent of the EDTA solution as
7.2 Purity of Water—Unless otherwise indicated, references
follows:
to water shall be understood to mean reagent water as defined
by Type I of Specification D 1193.
1 mL of EDTA solution 5 ~50.0/V! 5 C mg of calcium (1)
7.3 Acetic Acid Solution (1 + 10)—Mix 1 volume of glacial
where:
acetic acid (CH COOH) with 10 volumes of water.
V 5 millilitres of EDTA used.
7.4 Calcium Carbonate, high purity (minimum 99.95 %
NOTE 1—If a sample with a known CaF content is available, the
CaCO ).
standardization with CaCO can be omitted. The “standard” CaF sample
3 2
7.5 Ethylenediaminetetraacetic Acid Disodium Salt
should then be carried through all steps of the procedure.
(EDTA)-—Na C H O N ·2H O Solution (0.025 mol/L)—
10 14 8 2 2
9.2 Calibration—Transfer 10 mL of acetic acid (1 + 10)
Dissolve 9.3062 g of EDTA in water, transfer to a 1-L
(7.3) into a series of seven 100-mL polyethylene beakers and
volumetric flask, dilute to volume, and mix.
add 20 mL of potassium acetate buffer (7.9) (Note 2). Add
7.6 Hydrochloric Acid (2 + 98)—Mix 2 volumes of concen-
standard fluoride solution (7.12) and water according to the
trated hydrochloric acid (HCl) with 98 volumes of water.
following:
7.7 Hydrochloric Acid (1 + 10)—Mix 1 volume of concen-
−
Test Standard F mL Solution mg Water, mL
trated hydrochloric acid (HCl) with 10 volumes of water.
1 005
2 0.5 0.05 4.5
7.8 Hydroxynaphthol Blue Indicator— Grind 0.2 g of the
3 1.0 0.10 4.0
salt with 50 g sodium chloride (NaCl).
4 2.0 0.20 3.0
5 3.0 0.30 2.0
7.9 Potassium Acetate Buffer—Dilute 283 mL of glacial
6 4.0 0.40 1.0
acetic acid (CH COOH) to 1200 mL with water. While cooling
7 5.0 0.50 0
and stirring, add 50 % (W/V) potassium hydroxide solution
Stir the solution, immerse the electrodes (6.1 and 6.5) and
(KOH) to adjust the pH to 5.0 (approximately 350 mL of KOH
wait for 3 to 5 min for potential to reach equilibrium. Record
solution are required).
the potential in millivolts. Plot millivolts (linear scale) versus
7.10 Potassium Hydroxide Solution (22.5 %) (W/V)—
−
F concentration in milligrams (log scale) on a semilog paper.
Dissolve 225 g of potassium hydroxide (KOH) in water and
dilute to 1 L with water. Store in a plastic bottle.
NOTE 2—Potential measurements in calibration standards and sample
should be carried out concurrently.
7.11 Potassium Hydroxide Solution (50 %) (W/V)—
Dissolve 500 g of potassium hydroxide (KOH) in water and
10. Procedure
dilute to 1 L. Store in a plastic bottle.
10.1 Determination of Total Calcium:
7.
...

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