ASTM E53-2002 Standard Test Method for Determination of Copper in Unalloyed Copper by Gravimetry《用重量分析法测定非合金铜中铜含量的标准试验方法》.pdf
《ASTM E53-2002 Standard Test Method for Determination of Copper in Unalloyed Copper by Gravimetry《用重量分析法测定非合金铜中铜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 E53-2002 Standard Test Method for Determination of Copper in Unalloyed Copper by Gravimetry《用重量分析法测定非合金铜中铜含量的标准试验方法》.pdf(4页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: E 53 02Standard Test Method forDetermination of Copper in Unalloyed Copper byGravimetry1This standard is issued under the fixed designation E 53; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, the year of last revisio
2、n. A number in parentheses indicates the year of last reapproval. A superscriptepsilon (e) 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 chemical analysis of
3、 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 address all of
4、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 Section 9 and 8.4.2
5、. Referenced Documents2.1 ASTM Standards:E29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications2E50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE 121 Test Methods for Chemical Ana
6、lysis of Copper-Tellurium Alloys3E 135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related Materials3E 173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Analysis of Metals3E 255 Practice for Sampling Copper and Copper Alloys forthe Determination of Chem
7、ical Composition3E 1024 Guide for Chemical Analysis of Metals and MetalBearing Ores by Flame Atomic Absorption Spectropho-tometry4E 1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical Method43. Terminology3.1 DefinitionsFor definitions of terms used in t
8、his testmethod, refer to Terminology E 135.4. 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 isdetermined by atomic absorption spectroscopy.5. Significance an
9、d 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 laboratoryprocedures skillfully and safely. It is expected that
10、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 codeposit. If interfering amounts are present,proceed in accord
11、ance with Test Methods E 121.7. Apparatus7.1 Electrodes for Electroanalysis:7.1.1 ElectrodesPlatinum electrodes of the stationary typeare recommended as described in 7.1.2 and 7.1.3, but strictadherence to the exact size and shape of the electrodes is notmandatory. When agitation of the electrolyte
12、is permissible inorder to decrease the time of deposition, one of the types ofrotating forms of electrodes, generally available, may beemployed. The surface of the platinum electrodes should besmooth, clean, and bright to promote uniform deposition andgood adherence. Sandblasting is not recommended.
13、1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores and Related Materials and is the directresponsibility of Subcommittee E01.05 on Cu, Pb, Zn, Cd, Sn, Be, their Alloys andRelated Metals.Current edition approved Dec. 10, 2002. Published June 2003
14、. Originallyapproved in 1946. Last previous edition approved in 1998 as E 53 98.2Annual Book of ASTM Standards, Vol 14.02.3Annual Book of ASTM Standards, Vol 03.05.4Annual Book of ASTM Standards, Vol 03.06.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428
15、-2959, United States.7.1.2 CathodesPlatinum cathodes may be formed eitherfrom plain or perforated sheets or from wire gauze, and may beeither open or closed cylinders. Gauze cathodes are recom-mended, and shall be made preferably from 50-mesh gauzewoven from wire approximately 0.21 mm (0.0085 in.) i
16、ndiameter. The cathode should be stiffened by doubling thegauze for about 3 mm at the top and the bottom of the cylinderor by reinforcing the gauze at the top and bottom with aplatinum band or ring. The cylinder should be approximately30 mm in diameter and 50 mm in height. The stem should bemade fro
17、m a platinum alloy wire such as platinum-iridium,platinum-rhodium, or platinum-ruthenium, having a diameterof approximately 1.30 mm. It should be flattened and weldedthe entire length of the gauze. The overall height of the cathodeshould be approximately 130 mm. A cathode of these dimen-sions will h
18、ave a surface area of 135 cm2exclusive of the stem.7.1.3 AnodesPlatinum anodes may be of the spiral typewhen anodic deposits are not being determined, or if thedeposits are small (as in the electrolytic determination of leadwhen it is present in the amounts not over 0.2 %). When usedin analyses wher
19、e both cathodic and anodic plates are to bedetermined, the anodes should be of wire gauze. Spiral anodesshould be made from 1.00-mm or larger platinum wire formedinto a spiral of seven turns having a height of approximately 50mm and a diameter of 12 mm, the overall height beingapproximately 130 mm.
20、A spiral anode of this description willhave a surface area of 9 cm2. Platinum gauze anodes should bemade of the same material and of the same general design asplatinum gauze cathodes. The anode cylinder should be ap-proximately 12 mm in diameter and 50 mm in height and theoverall height of the anode
21、 should be approximately 130 mm.A gauze anode of these dimensions will have a surface area of54 cm2. Both areas are exclusive of the stem.7.2 Atomic Absorption Spectrophotometer:7.2.1 Determine that the atomic absorption spectrophotom-eter is suitable for use as described in Guide E 1024. Thevariabi
22、lity for the highest calibration solution should notexceed 1 %.7.2.2 Operating Parameters:Wavelength 3275 Bandpass About 2 Gas mixture Air-acetyleneFlame type Lean7.2.3 Instrument ResponseAdequate instrument responseis obtained if the difference between the readings of the twohighest of five equally
23、 spaced calibration solutions is sufficientto permit an estimation equivalent to one twentieth of thedifference.7.2.4 Curve LinearityThe upper limit of the useableportion of a calibration curve is normally set such that thedifference between the readings of the two highest of fiveequally spaced cali
24、bration 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 otherwisestated.8. Reagents8.1 Copper, Standard Solution A (1 mL = 1.0 mg Cu)Transfer 1.000 g of ele
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