ASTM E478-08(2017) Standard Test Methods for Chemical Analysis of Copper Alloys.pdf

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1、Designation: E478 08 (Reapproved 2017)Standard Test Methods forChemical Analysis of Copper Alloys1This standard is issued under the fixed designation E478; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision.

2、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 These test methods cover the chemical analysis ofcopper alloys having chemical ranges within the followinglimits:2Element Composition

3、, %Aluminum 12.0 maxAntimony 1.0 maxArsenic 1.0 maxCadmium 1.5 maxCobalt 1.0 maxCopper 40.0 minIron 6.0 maxLead 27.0 maxManganese 6.0 maxNickel 50.0 maxPhosphorus 1.0 maxSilicon 5.0 maxSulfur 0.1 maxTin 20.0 maxZinc 50.0 max1.2 The test methods appear in the following order:SectionsAluminum by the C

4、arbamate Extraction-Ethyl-enedinitrilotetraacetate Titrimetric TestMethod 2 % to 12 % 7178Copper by the Combined ElectrodepositionGravimetric and Oxalyldihydrazide Spectro-photometric Test Method 50 %, minimum 1018Iron by the 1,10-Phenanthroline Spectrophoto-metric Test Method 0.003 % to 1.25 % 1928

5、Lead by Atomic Absorption Spectrometry0.002%to15% 90 100Lead by the Ethylenedinitrilotetraacetic Acid(EDTA) Titrimetric Test Method 2.0 % to30.0 % 2936Nickel by the Dimethylglyoxime ExtractionSprectophotometric Test Method 0.03 % to5.0 % 3746Nickel by the Dimethylglyoxime GravimetricTest Method 4 %

6、to 50 % 5562Silver in Silver-Bearing Copper by Atomic Ab-sorption Spectrometry 0.01 % to 0.12 % 101 112Tin by the Iodotimetric Titration Test Method0.5 % to 20 % 6370Tin by the Phenylfluorone SpectrophotometricTest Method 0.01 % to 1.0 % 113 123Zinc by Atomic Absorption Spectrometry 0.2 %to 2 % 7989

7、Zinc by the Ethylenedinitrilotetraacetic Acid(EDTA) Titrimetric Test Method 2 % to 40 % 47541.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns, if any, ass

8、ociated 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.1.5 This international standard was developed in accor-dance with internationally recognized princi

9、ples on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:3E29 Practice for Using Significan

10、t Digits in Test Data toDetermine Conformance with SpecificationsE50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE60 Practice for Analysis of Metals, Ores, and RelatedMaterials by SpectrophotometryE135 Terminology Relating

11、to Analytical Chemistry forMetals, Ores, and Related MaterialsE173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Analysis of Metals (Withdrawn1998)4E255 Practice for Sampling Copper and Copper Alloys forthe Determination of Chemical CompositionE1601 Practice for Conducting a

12、n Interlaboratory Study to1These test methods are under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and are the directresponsibility of Subcommittee E01.05 on Cu, Pb, Zn, Cd, Sn, Be, Precious Metals,their Alloys, and Related Metals.Current ed

13、ition approved Jan. 15, 2017. Published March 2017. Originallyapproved in 1973. Last previous edition approved in 2008 as E478 08. DOI:10.1520/E0478-08R17.2The actual limits of application of each test method are presented in 1.2.3For referenced ASTM standards, visit the ASTM website, www.astm.org,

14、orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.4The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International, 100 Barr Harbor D

15、rive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations

16、issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1Evaluate the Performance of an Analytical Method3. Terminology3.1 For definitions of terms used in these test methods, referto Terminology E135.4. Significance and Use4.1 These test methods for the chemical analysis

17、of metalsand alloys are primarily intended as referee methods to testsuch materials for compliance with composition specifications.It is assumed that all who use these methods will be trainedanalysts capable of performing common laboratory proceduresskillfully and safely. It is expected that work wi

18、ll be performedin a properly equipped laboratory.5. Apparatus, Reagents, and Spectrophotometric Practice5.1 Apparatus, standard solutions, and other reagents re-quired for each determination are listed in separate sectionspreceding the procedure. Spectrophotometers shall conform tothe requirements p

19、rescribed in Practice E60.5.2 Spectrophotometric practice prescribed in these testmethods shall conform to Practice E60.6. Hazards6.1 Specific hazard statements are given in 33.7, 51.13, and107.1.6.2 For other precautions to be observed in the use of certainreagents in these test methods, refer to P

20、ractices E50.7. Sampling7.1 For procedures for sampling the material, refer toPractice E255. However, this practice does not supersede anysampling requirements specified in a specific ASTM materialspecification.8. Rounding Calculated Values8.1 Calculated values shall be rounded to the desired num-be

21、r of places as directed in Practice E29.9. Interlaboratory Studies9.1 These test methods were evaluated in accordance withPractice E173 unless otherwise noted in the precision section.Practice E173 has been replaced by Practice E1601. TheReproducibility R2corresponds to the Reproducibility Index Rof

22、 Practice E1601. The Repeatability R1of Practice E173corresponds to the Repeatability Index r of Practice E1601.COPPER BY THE COMBINEDELECTRODEPOSITION GRAVIMETRIC ANDOXALYLDIHYDRAZIDE SPECTROPHOTOMETRICTEST METHOD10. Scope10.1 This test method covers the determination of copper incompositions great

23、er than 50 %.10.2 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization Techni

24、calBarriers to Trade (TBT) Committee.11. Summary of Test Method11.1 After dissolution of the sample in HNO3and HF, theoxides of nitrogen are reduced with hydrogen peroxide, and thecopper deposited electrolytically. Loss of platinum from theanode is minimized by the addition of lead. The copperoxalyl

25、dihydrazide complex is formed with the copper remain-ing in the electrolyte. Photometric measurement is made atapproximately 540 nm.12. Interferences12.1 The elements ordinarily present do not interfere if theirconcentrations are under the maximum limits shown in 1.1.13. Apparatus13.1 Polytetrafluor

26、oethylene or Polypropylene Beakers,250-mL capacity.13.2 Polytetrafluoroethylene or Polypropylene Split Covers.13.3 Electrodes for ElectroanalysisRecommended sta-tionary type platinum electrodes are described in 13.3.1 and13.3.2. The surface of the platinum electrode should besmooth, clean, and brigh

27、t to promote uniform deposition andgood adherence. Deviations from the exact size and shape areallowable. In instances where it is desirable to decrease thetime of deposition and agitation of the electrolyte ispermissible, a generally available rotating type of electrodemay be employed. Cleaning of

28、the electrode by sandblasting isnot recommended.13.3.1 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 an

29、d bottom of gauze cathodesshould be reinforced 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

30、, or platinum-ruthenium, having a diameter of approximately 1.3 mm. Itshould be flattened and welded the entire length of the gauze.The overall height of the cathode should be approximately130 mm. A cathode of these dimensions will have a surfacearea of 135 cm2exclusive of the stem.13.3.2 AnodesPlat

31、inum anodes may be a spiral type whenanodic deposits are not being determined, or if the deposits aresmall (as in the electrolytic determination of lead when it ispresent in compositions below 0.2 %). Spiral anodes should bemade from 1.0 mm or larger platinum wire formed into a spiralof seven turns

32、having a height of approximately 50 mm and adiameter of 12 mm with an overall height of approximately130 mm.Aspiral anode of these dimensions will have a surfacearea of 9 cm2. When both cathode and anode plates are to bedetermined, the anode should be made of the same material anddesign as the elect

33、rode described in 13.3.1. The anode cylinderE478 08 (2017)2should be approximately 12 mm in diameter and 50 mm inheight and the overall height of the anode should be approxi-mately 130 mm. A gauze anode of these dimensions will havea surface area of 54 cm2exclusive of the stem.13.3.3 Gauze cathodes

34、are recommended where rapid elec-trolysis is used.14. Reagents14.1 Ammonium Chloride Solution (0.02 g L)Dissolve0.02 g of ammonium chloride (NH4Cl) in water and dilute to1L.14.2 Hydrogen Peroxide (3 %)Dilute 100 mL of 30 %hydrogen peroxide to 1 L.14.3 Lead Nitrate Solution (10 g L) Dissolve 10.0 g o

35、flead nitrate (Pb(NO3)2) in water and dilute to 1 L.15. Procedure15.1 Transfer a 2.000-g sample, weighed to the nearest0.1 mg, to a 250-mL polytetrafluoroethylene or polypropylenebeaker, add 2 mL of HF, and 30 mL of HNO3(1 + 1). Coverwith a cover glass and allow to stand for a few minutes until ther

36、eaction has nearly ceased. Warm but do not heat over 80 C.When dissolution is complete, add 25 mL of 3 % H2O2and3 mL of Pb(NO3)2solution. Rinse the cover glass and dilute toapproximately 150 mL with NH4Cl solution.15.2 With the electrolyzing current off, position the anodeand the accurately weighed

37、cathode in the solution so that thegauze is completely immersed. Cover the beaker with a splitplastic cover.15.3 Start the electrolysis and increase the voltage until theammeter indicates a current which is equivalent to about1.0 A dm2and electrolyze overnight. Alternatively electrolyzeat a current

38、density of 4 A dm2for 1.5 h. (The more rapidprocedure requires the use of gauze electrodes).15.4 Slowly withdraw the electrodes (or lower the beaker)with the current still flowing, and rinse with a stream of waterfrom a wash bottle. Quickly remove the cathode, rinse it inwater, and then dip into two

39、 successive baths of ethanol ormethanol. Dry in an oven at 110 C for 3 min to 5 min.15.5 Return the voltage to zero and turn off the switch.Reserve the electrolyte.15.6 Allow the electrode to cool to room temperature andweigh.16. Calculation16.1 Calculate the percentage of copper as follows:Copper,

40、% 5 A1B!/C# 3100 (1)where:A = deposited copper, g,B = copper in the electrolyte as calculated in 17.10,g,andC = sample used, g.17. Spectrophotometric Determination of the ResidualCopper in the Electrolyte17.1 InterferencesThe elements ordinarily present do notinterfere if their composition is under

41、the maximum limitsshown in 1.1.17.2 Concentration RangeThe recommended concentra-tion is from 0.0025 mg to 0.07 mg of copper per 50 mL ofsolution, using a 2-cm cell.NOTE 1This procedure has been written for cells having a 2-cm lightpath. Cells having other dimensions may be used, provided suitablead

42、justments can be made in the amounts of sample and reagents used.17.3 Stability of ColorThe color fully develops in 20 minand is stable for 1 h.17.4 Reagents:17.4.1 Acetaldehyde Solution (40 %)Dilute 400 mL ofacetaldehyde to 1 L with water.17.4.2 Boric Acid Solution (50 gL)Dissolve 50 g of boricacid

43、 (H3BO3) in hot water, cool, and dilute to 1 L.17.4.3 Citric Acid Solution (200 gL)Dissolve 200 g ofcitric acid in water and dilute to 1 L.17.4.4 Copper, Standard Solution A (1 mL = 1.0 mg Cu)Transfer a 1.000-g sample of electrolytic copper (purity:99.9 % minimum) to a 250-mL beaker and add 10 mL of

44、HNO3(1 + 1). Evaporate nearly to dryness. Add 5 mL of waterto dissolve the residue. Transfer to a 1-L volumetric flask,dilute to volume, and mix.17.4.5 Copper, Standard Solution B (1 mL = 0.010 mgCu)Using a pipet, transfer 10 mL of Copper Solution A(1 mL = 1.0 mg Cu) to a 1-Lvolumetric flask, dilute

45、 to volume,and mix.17.4.6 Oxalyldihydrazide Solution (2.5 g/L)Dissolve 2.5 gof oxalyldihydrazide in warm water and dilute to 1 L.17.5 Preparation of Calibration Curve:17.5.1 Calibration Solutions:17.5.1.1 Transfer 25 mL of boric acid solution to a 250-mLvolumetric flask and then add a solution conta

46、ining 150 mL ofwater, 2 mL of HF, and 30 mL of HNO3(1 + 1). Dilute tovolume and mix.17.5.1.2 Transfer 10 mL of this solution to each of four50-mL volumetric flasks. Using pipets, transfer (1, 3, 5, and7) mL of Copper Solution B (1 mL = 0.010 mg Cu) to theflasks. Proceed as directed in 17.5.3.17.5.2

47、Reference SolutionAdd 10 mL of boric acid solu-tion prepared as directed in 17.5.1.1 to a 50-mL volumetricflask and proceed as directed in 17.5.3.17.5.3 Color DevelopmentAdd in order, and with mixingafter each addition, 5 mL of citric acid solution, 6 mL ofNH4OH, 10 mL of acetaldehyde solution, and

48、10 mL of ox-alyldihydrazide solution. Cool, dilute to volume, and mix.Allow to stand for 30 min and proceed as directed in 17.5.4.17.5.4 Spectrophotometry:17.5.4.1 Multiple-Cell SpectrophotometerMeasure thecell correction using absorption cells with a 2-cm light path anda light band centered at appr

49、oximately 540 nm. Using the testcell, take the spectrophotometric readings of the calibrationsolutions.E478 08 (2017)317.5.4.2 Single-Cell SpectrophotometerTransfer a suit-able portion of the reference solution to an absorption cell witha 2-cm light path and adjust the spectrophotometer to the initialsetting using a light band centered at approximately 540 nm.While maintaining this adjustment, take the spectrophotomet-ric readings of the calibration solutions.17.5.5 Calibration CurvePlot the net s