ASTM E815-17
(Test Method)Standard Test Method for Determination of Calcium Fluoride in Fluorspar by Complexometric Titrimetry
Standard Test Method for Determination of Calcium Fluoride in Fluorspar by Complexometric Titrimetry
SIGNIFICANCE AND USE
5.1 Fluorspar is used as a flux in the steelmaking and glass industry, and in the manufacture of HF.
5.2 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 E882.
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 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 test method has been evaluated in accordance with Practice E1601 and Guide E1763. Unless otherwise noted in the precision and bias section, the lower limit in the scope of each method specifies the lowest analyte content that may be analyzed with acceptable error (defined as a nominal 5 % risk of obtaining a 50 % or larger relative difference in results on the same test sample in two laboratories).
1.4 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.
1.5 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.
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Designation: E815 − 17
Standard Test Method for
Determination of Calcium Fluoride in Fluorspar by
1
Complexometric Titrimetry
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 Determine Conformance with Specifications
E50Practices for Apparatus, Reagents, and Safety Consid-
1.1 This test method covers the determination of calcium
erations for Chemical Analysis of Metals, Ores, and
fluorideinacid-gradefluorsparandothertypesoffluorsparthat
Related Materials
can be rendered soluble by the procedure described in the test
E135Terminology Relating to Analytical Chemistry for
method.
Metals, Ores, and Related Materials
1.2 The values stated in SI units are to be regarded as
E276TestMethodforParticleSizeorScreenAnalysisatNo.
standard. No other units of measurement are included in this
4 (4.75-mm) Sieve and Finer for Metal-Bearing Ores and
standard.
Related Materials
E882Guide for Accountability and Quality Control in the
1.3 This test method has been evaluated in accordance with
Practice E1601 and Guide E1763. Unless otherwise noted in Chemical Analysis Laboratory
E1601Practice for Conducting an Interlaboratory Study to
the precision and bias section, the lower limit in the scope of
each method specifies the lowest analyte content that may be Evaluate the Performance of an Analytical Method
E1763Guide for Interpretation and Use of Results from
analyzed with acceptable error (defined as a nominal 5 % risk
of obtaining a 50 % or larger relative difference in results on Interlaboratory Testing of Chemical Analysis Methods
3
(Withdrawn 2015)
the same test sample in two laboratories).
1.4 This standard does not purport to address all of the
3. Terminology
safety concerns, if any, associated with its use. It is the
3.1 Definitions—For definitions of terms used in this test
responsibility of the user of this standard to establish appro-
method, refer to Terminology E135.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4. Summary of Test Method
1.5 This international standard was developed in accor-
4.1 ThesampleisdecomposedbydigestingwithHNO and
dance with internationally recognized principles on standard-
3
HCLO and the fluorine is expelled by fuming. The residue is
ization established in the Decision on Principles for the
4
dissolved in dilute HCL, the solution made alkaline, and the
Development of International Standards, Guides and Recom-
calciumtitratedwithstandardEDTAsolution.Calciumpresent
mendations issued by the World Trade Organization Technical
as carbonate is determined in a separate sample with EDTA
Barriers to Trade (TBT) Committee.
solution, after extracting the former with dilute acetic acid. A
2. Referenced Documents
correctionforcalciumfluoride,solubilizedbydiluteaceticacid
2
digestion, is applied by determining the fluoride in the acetic
2.1 ASTM Standards:
acid extract by fluoride ion-selective electrode. The CaF
D1193Specification for Reagent Water 2
content is then calculated.
E29Practice for Using Significant Digits in Test Data to
5. Significance and Use
1
This test method is under the jurisdiction of ASTM Committee E01 on
5.1 Fluorspar is used as a flux in the steelmaking and glass
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
industry, and in the manufacture of HF.
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
lurgical Materials.
5.2 This test method is intended to be used for compliance
CurrenteditionapprovedMay1,2017.PublishedJuly2017.Originallyapproved
with compositional specifications for calcium fluoride content.
in1981.Lastpreviouseditionapprovedin2011asE815–11.DOI:10.1520/E0815-
It is assumed that all who use these procedures will be trained
17.
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 The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
E815 − 17
analysts capable of performing common laboratory procedures 8.8 Potassium Hydroxide Solution A—Dissolve 225 g of
skillfullyandsafely.Itisexpectedthatworkwillbeperformed KOH in water and dilute to 1 L with water. Store in a plastic
in a properly equipped laborato
...
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: E815 − 11 E815 − 17
Standard Test Method for
Determination of Calcium Fluoride in Fluorspar by
1
Complexometric Titrimetry
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. 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 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 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 test method has been evaluated in accordance with Practice E1601 and Guide E1763. Unless otherwise noted in the
precision and bias section, the lower limit in the scope of each method specifies the lowest analyte content that may be analyzed
with acceptable error (defined as a nominal 5 % risk of obtaining a 50 % or larger relative difference in results on the same test
sample in two laboratories).
1.4 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.
1.5 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E50 Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E276 Test Method for Particle Size or Screen Analysis at No. 4 (4.75-mm) Sieve and Finer for Metal-Bearing Ores and Related
Materials
E882 Guide for Accountability and Quality Control in the Chemical Analysis Laboratory
E1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method
E1763 Guide for Interpretation and Use of Results from Interlaboratory Testing of Chemical Analysis Methods (Withdrawn
3
2015)
3. Terminology
3.1 Definitions—For definitions of terms used in this test method, refer to Terminology E135.
4. Summary of Test Method
4.1 The sample is decomposed by digesting with nitricHNO and perchloricHCLO acids and the fluorine is expelled by fuming.
3 4
The residue is dissolved in dilute hydrochloric acid, HCL, the solution made alkaline, and the calcium titrated with standard EDTA
solution. Calcium present as carbonate is determined in a separate sample with EDTA solution, after extracting the former with
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 Sept. 1, 2011May 1, 2017. Published September 2011July 2017. Originally approved in 1981. Last previous edition approved in 20042011 as
E815 – 04.11. DOI: 10.1520/E0815-11.10.1520/E0815-17.
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 Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
The last approved version of this historical standard is referenced on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
E815 − 17
dilute acetic acid. A correction for calcium fluoride, solubilized by dilute acetic acid digestion, is applied,applied by determining
the fluoride in the acetic acid extract by fluoride ion-selective electrode. The CaF content is then calculated.
2
5. Significance and Use
5.1 Fluorspar is used as a flux in steelmaking, the steelmaking and glass industry, and in the manuf
...
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