ASTM E815-2017a red 9375 Standard Test Method for Determination of Calcium Fluoride in Fluorspar by EDTA Complexometric Titrimetry《用EDTA络合滴定法测定氟石中氟化钙含量的标准试验方法》.pdf
《ASTM E815-2017a red 9375 Standard Test Method for Determination of Calcium Fluoride in Fluorspar by EDTA Complexometric Titrimetry《用EDTA络合滴定法测定氟石中氟化钙含量的标准试验方法》.pdf》由会员分享,可在线阅读,更多相关《ASTM E815-2017a red 9375 Standard Test Method for Determination of Calcium Fluoride in Fluorspar by EDTA Complexometric Titrimetry《用EDTA络合滴定法测定氟石中氟化钙含量的标准试验方法》.pdf(5页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: E815 17E815 17aStandard Test Method forDetermination of Calcium Fluoride in Fluorspar by EDTAComplexometric Titrimetry1This standard is issued under the fixed designation E815; the number immediately following the designation indicates the year oforiginal adoption or, in the case of rev
2、ision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of calcium fluoride in acid-grade fluorspar and other typ
3、es of fluorspar that canbe 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
4、E1763. Unless otherwise noted in theprecision and bias section, the lower limit in the scope of each method specifies the lowest analyte content that may be analyzedwith acceptable error (defined as a nominal 5 % risk of obtaining a 50 % or larger relative difference in results on the same testsampl
5、e 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 responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of r
6、egulatory limitations prior to use.1.5 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Or
7、ganization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data to Determine Conformance with SpecificationsE50 Practices forApparatus, Reagents, and Safety Considerations fo
8、r ChemicalAnalysis of Metals, Ores, and Related MaterialsE135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related MaterialsE276 Test Method for Particle Size or ScreenAnalysis at No. 4 (4.75-mm) Sieve and Finer for Metal-Bearing Ores and RelatedMaterialsE882 Guide for Accounta
9、bility and Quality Control in the Chemical Analysis LaboratoryE1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical MethodE1763 Guide for Interpretation and Use of Results from Interlaboratory Testing of Chemical Analysis Methods (Withdrawn2015)33. Termi
10、nology3.1 DefinitionsFor definitions of terms used in this test method, refer to Terminology E135.4. Summary of Test Method4.1 The sample is decomposed by digesting with HNO3 and HCLOHClO4 and the fluorine is expelled by fuming. The residueis dissolved in dilute HCL,HCl, the solution made alkaline,
11、and the calcium titrated with standard EDTAsolution. Calcium presentas carbonate is determined in a separate sample with EDTAsolution, after extracting the former with dilute acetic acid.Acorrection1 This test method is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals,
12、 Ores, and Related Materials and is the direct responsibility ofSubcommittee E01.02 on Ores, Concentrates, and Related Metallurgical Materials.Current edition approved May 1, 2017Sept. 15, 2017. Published July 2017October 2017. Originally approved in 1981. Last previous edition approved in 20112017
13、as E815 11.17. DOI: 10.1520/E0815-17.10.1520/E0815-17A.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The
14、last approved version of this historical standard is referenced on www.astm.org.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. Becauseit may not be technically possible to adequa
15、tely depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocke
16、n, PA 19428-2959. United States1for calcium fluoride, solubilized by dilute acetic acid digestion, is applied by determining the fluoride in the acetic acid extract byfluoride ion-selective electrode. The CaF2 content is then calculated.5. Significance and Use5.1 Fluorspar is used as a flux in the s
17、teelmaking and glass industry,industries, 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 isassumed that all who use these procedures will be trained analysts capable of performing common labor
18、atory procedures skillfullyand safely. It is expected that work will be performed in a properly equipped laboratory and that proper waste disposal procedureswill be followed. Appropriate quality control practices must be followed such as those described in Guide E882.6. Interferences6.1 None of the
19、elements normally found in fluorspar interfereinterferes with this test method.7. Apparatus7.1 Fluoride Ion-Selective Electrode.47.2 Magnetic Stirrer and TFE-Fluorocarbon-Coated Spin Bar.7.3 pH Meter with High ImpedanceSuitable for ion-selective electrode.7.4 Polyethylene Beakers, 100-mL.7.5 Single
20、Junction Ag/AgCl Reference Electrode.58. Reagents and Materials8.1 Purity of ReagentsReagent grade Reagent-grade chemicals shall be used in all tests. Unless otherwise indicated, it isintended that all reagents conform to the specifications of the Committee onAnalytical Reagents of theAmerican Chemi
21、cal Societywhere such specifications are available.6 Other grades may be used, provided it is first ascertained that the reagent is of sufficienthigh purity to permit its use without lessening the accuracy of the determination.8.2 Purity of WaterUnless otherwise indicated, references to water shall
22、be understood to mean reagent water conforming toType I or II of Specification D1193. Type III or IV may be used if they effect no measurable change in the blank or sample.8.3 Acetic Acid Solution (1 + 10)Mix 1 volume of glacial acetic acid (CH3COOH) with 10 volumes of water.8.4 Calcium Carbonate, h
23、igh purity (minimum 99.95 % CaCO3).8.5 Ethylenediaminetetraacetic Acid Disodium Salt (EDTA)-Na2C10H14O8N22H2O Solution (0.025 mol/L)Dissolve 9.3062g of EDTA in water, transfer to a 1-L volumetric flask, dilute to volume, and mix.8.6 Hydroxynaphthol Blue Indicator Grind 0.2 g of the salt with 50 g so
24、dium chloride (NaCl).8.7 Potassium Acetate BufferDilute 283 mL of glacial acetic acid (CH3COOH) to 1200 mL with water. While cooling andstirring, add KOH solution B (8.9) to adjust the pH to 5.0 (approximately 350 mL of KOH solution B are required).8.8 Potassium Hydroxide Solution ADissolve 225 g of
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