ASTM E815-11
(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
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 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.
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Designation: E815 − 11
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 4 (4.75-mm) Sieve and Finer for Metal-Bearing Ores and
Related Materials
1.1 This test method covers the determination of calcium
E882Guide for Accountability and Quality Control in the
fluorideinacid-gradefluorsparandothertypesoffluorsparthat
Chemical Analysis Laboratory
can be rendered soluble by the procedure described in the test
E1601Practice for Conducting an Interlaboratory Study to
method.
Evaluate the Performance of an Analytical Method
1.2 The values stated in SI units are to be regarded as
E1763Guide for Interpretation and Use of Results from
standard. No other units of measurement are included in this
Interlaboratory Testing of Chemical Analysis Methods
standard.
1.3 This test method has been evaluated in accordance with 3. Terminology
Practice E1601 and Guide E1763. Unless otherwise noted in
3.1 Definitions—For definitions of terms used in this test
the precision and bias section, the lower limit in the scope of
method, refer to Terminology E135.
each method specifies the lowest analyte content that may be
analyzed with acceptable error (defined as a nominal 5 % risk
4. Summary of Test Method
of obtaining a 50 % or larger relative difference in results on
4.1 The sample is decomposed by digesting with nitric and
the same test sample in two laboratories).
perchloric acids and the fluorine is expelled by fuming. The
1.4 This standard does not purport to address all of the
residue is dissolved in dilute hydrochloric acid, the solution
safety concerns, if any, associated with its use. It is the
made alkaline, and the calcium titrated with standard EDTA
responsibility of the user of this standard to establish appro-
solution. Calcium present as carbonate is determined in a
priate safety and health practices and determine the applica-
separate sample with EDTA solution, after extracting the
bility of regulatory limitations prior to use.
former with dilute acetic acid. A correction for calcium
fluoride, solubilized by dilute acetic acid digestion, is applied,
2. Referenced Documents
bydeterminingthefluorideintheaceticacidextractbyfluoride
2
2.1 ASTM Standards:
ion-selective electrode. The CaF content is then calculated.
2
D1193Specification for Reagent Water
E50Practices for Apparatus, Reagents, and Safety Consid-
5. Significance and Use
erations for Chemical Analysis of Metals, Ores, and
5.1 Fluorsparisusedasafluxinsteelmaking,glassindustry,
Related Materials
and manufacture of hydrofluoric acid.
E135Terminology Relating to Analytical Chemistry for
5.2 This test method is intended to be used for compliance
Metals, Ores, and Related Materials
with compositional specifications for calcium fluoride content.
E276TestMethodforParticleSizeorScreenAnalysisatNo.
It is assumed that all who use these procedures will be trained
analysts capable of performing common laboratory procedures
skillfullyandsafely.Itisexpectedthatworkwillbeperformed
1
This test method is under the jurisdiction of ASTM Committee E01 on
in a properly equipped laboratory and that proper waste
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
disposal procedures will be followed. Appropriate quality
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
lurgical Materials.
control practices must be followed such as those described in
Current edition approved Sept. 1, 2011. Published September 2011. Originally
Guide E882.
approved in 1981. Last previous edition approved in 2004 as E815 – 04. DOI:
10.1520/E0815-11.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 6. Interferences
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.1 None of the elements normally found in fluorspar
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. interfere with this test method.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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E815 − 11
7. Apparatus 1 L in a volumetric flask. Store in a stoppered polyethylene
−
3 bottle.This solution has a concentration of 1 mL=0.10 mg F
7.1 Fluoride Ion-Selective Electrode.
and is stable for 6 months.
7.2 Magnetic Stirrer and TFE-Fluorocarbon-Coated Spin
8.11 Triethanolamine Solution (1+1) —Mix 50 mL of
Bar.
triethanolamine (NC
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:E815–04 Designation:E815–11
Standard Test Method for
Determination of Calcium Fluoride in Fluorspar by
1
Complexometric TitrationTitrimetry
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
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
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
E50 PracticesforApparatus,Reagents,andSafetyConsiderationsforChemicalAnalysisofMetals,Ores,andRelatedMaterials
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E276 TestMethodforParticleSizeorScreenAnalysisatNo.4(4.75-mm)SieveandFinerforMetal-BearingOresandRelated
Materials
E882 Guide forAccountability and Quality Control in the ChemicalAnalysis LaboratoryGuide forAccountability 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
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 Thesampleisdecomposedbydigestingwithnitricandperchloricacidsandthefluorineisexpelledbyfuming.Theresidue
isdissolvedindilutehydrochloricacid,thesolutionmadealkaline,andthecalciumtitratedwithstandardEDTAsolution.Calcium
present as carbonate is determined in a separate sample with EDTA solution, after extracting the former with dilute acetic acid.
Acorrection for calcium fluoride, solubilized by dilute acetic acid digestion, is 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, glass industry, and manufacture of hydrofluoric acid.
5.2 This test method is intended to be used for compliance with compositional specifications for calcium fluoride content. It is
1
This test method is under the jurisdiction ofASTM Committee E01 onAnalytical 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 May 1, 2004. Published June 2004. Originally approved in 1981. Last previous edition approved in 1999 as E815–99. DOI: 10.1520/E0815-04.
Current edition approved Sept. 1, 2011. Published September 2011. Originally approved in 1981. Last previous edition approved in 2004 as E815 – 04. DOI:
10.1520/E0815-11.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@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 ----------------------
E815–11
assumedthatallwhousetheseprocedureswillbetrainedanalystscapableofperformingcommonlaboratoryproceduresskillfully
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
...
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