ASTM E53-2007(2013) 6875 Standard Test Method for Determination of Copper in Unalloyed Copper by Gravimetry《采用重量测定法测定非合金铜中铜的标准试验方法》.pdf
《ASTM E53-2007(2013) 6875 Standard Test Method for Determination of Copper in Unalloyed Copper by Gravimetry《采用重量测定法测定非合金铜中铜的标准试验方法》.pdf》由会员分享,可在线阅读,更多相关《ASTM E53-2007(2013) 6875 Standard Test Method for Determination of Copper in Unalloyed Copper by Gravimetry《采用重量测定法测定非合金铜中铜的标准试验方法》.pdf(4页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: E53 07 (Reapproved 2013)Standard Test Method forDetermination of Copper in Unalloyed Copper byGravimetry1This standard is issued under the fixed designation E53; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, the year
2、 of last revision. A number in parentheses indicates the year of last reapproval. A superscriptepsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test method covers the chemi
3、cal analysis of copperhaving minimum purity of 99.75 % to 99.95 %.1.2 This test method covers the electrolytic determination ofcopper in chemical, electrolytic, and fire refined copper. In thismethod silver is deposited with the copper, and is reported ascopper.1.3 This standard does not purport to
4、address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific precau-tionary statements are given in 8.4
5、and Section 9.2. Referenced Documents2.1 ASTM Standards:2E29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE121 Test Methods fo
6、r Chemical Analysis of Copper-Tellurium Alloys (Withdrawn 2010)3E135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Analysis of Metals (Withdrawn1998)3E255 Practice for Sampling Copper and
7、 Copper Alloys forthe Determination of Chemical CompositionE1024 Guide for Chemical Analysis of Metals and MetalBearing Ores by Flame Atomic Absorption Spectropho-tometry (Withdrawn 2004)3E1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical Method3. Term
8、inology3.1 DefinitionsFor definitions of terms used in this testmethod, refer to Terminology E135.4. Summary of Test Method4.1 The sample is dissolved in an acid mixture and thecopper is electrolytically deposited and weighed on a taredplatinum cathode. Copper remaining in the electrolyte isdetermin
9、ed by atomic absorption spectroscopy.5. Significance and Use5.1 This test method for the chemical analysis of copper isprimarily intended to test for compliance with compositionalspecifications. It is assumed that all who use this method willbe trained analysts capable of performing common laborator
10、yprocedures skillfully and safely. It is expected that work will beperformed in a properly equipped laboratory.6. Interferences6.1 Elements normally present in refined copper with aminimum purity of 99.85 % do not interfere.6.2 Approximately one-half of any selenium or telluriumpresent will co-depos
11、it. If interfering amounts are present,proceed in accordance with Test Methods E121.7. Apparatus7.1 Electrodes for Electroanalysis:7.1.1 ElectrodesRecommended stationary type platinumelectrodes are described in 7.1.2 and 7.1.3. The surface of theplatinum electrodes should be smooth, clean, and brigh
12、t topromote uniform deposition and good adherence. Deviationsfrom the exact size and shape are allowable. In instances whereit is desirable to decrease the time of deposition and agitation1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and R
13、elated Materials and is the directresponsibility of Subcommittee E01.05 on Cu, Pb, Zn, Cd, Sn, Be, Precious Metals,their Alloys, and Related Metals.Current edition approved Oct. 1, 2013. Published October 2013. Originallyapproved in 1946. Last previous edition approved in 2007 as E53 07. DOI:10.1520
14、/E0053-07R13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical st
15、andard is referenced onwww.astm.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1of the electrolyte is permissible, a generally available, rotatingtype of electrode may be employed. Cleaning of the electrodeby sandblasting is not r
16、ecommended.7.1.2 CathodesPlatinum cathodes may be either open orclosed cylinders formed from sheets that are plain orperforated, or from gauze. Gauze cathodes are recommended;preferably from 50-mesh gauze woven from approximately0.21 mm diameter wire. The top and bottom of gauze cathodesshould be re
17、inforced by doubling the gauze about 3 mm ontoitself, or by the use of platinum bands or rings. The cylindershould be approximately 30 mm in diameter and 50 mm inheight. The stem should be made from a platinum alloy wiresuch as platinum-iridium, platinum-rhodium, or platinum-ruthenium, having a diam
18、eter of approximately 1.3 mm. Itshould be flattened and welded the entire length of the gauze.The overall height of the cathode should be approximately 130mm. A cathode of these dimensions will have a surface area of135 cm2exclusive of the stem.7.1.3 AnodesPlatinum anodes may be a spiral type whenan
19、odic deposits are not being determined, or if the deposits aresmall (as in the electrolytic determination of lead when it ispresent in concentrations below 0.2 %). Spiral anodes shouldbe made from 1.0-mm or larger platinum wire formed into aspiral of seven turns having a height of approximately 50 m
20、mand a diameter of 12 mm with an overall height of approxi-mately 130 mm. A spiral anode of these dimensions will havea surface area of 9 cm2. When both cathode and anode platesare to be determined, the anodes should be made of the samematerial and design as the electrode described in 7.1.2. Theanod
21、e cylinder should be approximately 12 mm in diameterand 50 mm in height and the overall height of the anode shouldbe approximately 130 mm. A gauze anode of these dimensionswill have a surface area of 54 cm2exclusive of the stem.7.2 Atomic Absorption Spectrometer:7.2.1 Determine that the atomic absor
22、ption spectrometer issuitable for use as described in Guide E1024. The variabilityfor the highest calibration solution should not exceed 1 %.7.2.2 Operating Parameters:Wavelength 327.5 nmBandpass About 0.2 nmGas mixture Air-acetyleneFlame type Lean7.2.3 Instrument ResponseAdequate instrument respons
23、eis obtained if the difference between the readings of the twohighest of five equally spaced calibration solutions is sufficientto permit an estimation equivalent to one twentieth of thedifference.7.2.4 Curve LinearityThe upper limit of the usable por-tion of a calibration curve is normally set such
24、 that thedifference between the readings of the two highest of fiveequally spaced calibration solutions is more than 0.7 times thedifference between the lowest of the calibration solutions.Absorbance values are used in this calculation.7.3 Glassware, shall be borosilicate glass unless otherwisestate
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