ASTM E2575 - 08 Standard Test Method for Determination of Oxygen in Copper and Copper Alloys (Withdrawn 2017).pdf

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1、Designation: E2575 08Standard Test Method forDetermination of Oxygen in Copper and Copper Alloys1This standard is issued under the fixed designation E2575; 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 This test method covers the determination of oxygen incopper and copper alloys in concentrations from 0.0005 to0.04 %.1.2 This standa

3、rd does not purport to 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.2. Referenced Documents2.1 AST

4、M Standards:2E50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE882 Guide for Accountability and Quality Control in theChemical Analysis

5、LaboratoryE1019 Test Methods for Determination of Carbon, Sulfur,Nitrogen, and Oxygen in Steel, Iron, Nickel, and CobaltAlloys by Various Combustion and Fusion TechniquesE1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodIEEE/ASTM SI 10 Standard

6、for Use of the InternationalSystem of Units (SI): The Modern Metric System2.2 Material Certificates:BCR No. 18 Oxygen in Phosphorus-Deoxidized Copper3BCR No. 22 Oxygen in ETP Copper3BCR No. 58 Oxygen in Continuous Cast Copper Rod3NCS NS 41004 Oxygen in Pure Copper4NIST SRM 885 Refined Copper53. Term

7、inology3.1 DefinitionsFor definitions of terms used in this testmethod, refer to Terminology E135.4. Summary of Test Method4.1 This test method is intended for use with commerciallyavailable inert gas fusion determinators.4.2 The test specimen is fused in a graphite crucible undera flowing inert gas

8、 stream (argon (Ar), helium (He), or nitrogen(N2) at a temperature sufficient to release oxygen. Oxygenfrom the specimen combines with carbon from the crucible toform carbon monoxide (CO). The detector output is convertedto the mass fraction of oxygen in the specimen using apreviously establish cali

9、bration. Depending on the instrumentdesign, CO is oxidized to carbon dioxide (CO2) or left as COand swept by the inert gas stream into an infrared detector.4.3 In a typical instrument based on infrared detection theevolved gases are swept into an infrared cell through whichinfrared energy is transmi

10、tted. The CO in the gas streamabsorbs some of the transmitted infrared energy and thedecrease in the energy reaching the detector is processed anddisplayed directly as percent oxygen. Some instruments oxi-dize the CO to CO2, which is subsequently measured by aninfrared cell designed to measure CO2.5

11、. Significance and Use5.1 This test method is primarily intended as a referee testfor compliance with compositional specifications. It is assumedthat all who use this test method will be trained analysts,capable of performing common laboratory procedures skill-fully and safely. It is expected that w

12、ork will be performed ina properly equipped laboratory.6. Interferences6.1 The elements usually present in copper and its alloys donot interfere.1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and is the directresponsib

13、ility of Subcommittee E01.05 on Cu, Pb, Zn, Cd, Sn, Be, their Alloys, andRelated Metals.Current edition approved March 1, 2008. Published April 2008. DOI: 10.1520/E2575-08.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For An

14、nual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from European Commission, Joint Research Centre, Institute forReference Materials and Measurements, Retieseweg 111, B-2440 Geel, Belgium,http:/irmm.jrc.ec.europa.eu/.4Available f

15、rom Central Iron and Steel Research Institute (CISRI), No. 76Xueyan Nanlu, Haidian District, Beijing, China 100081, http:/ from National Institute of Standards and Technology (NIST), 100Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http:/www.nist.gov.Copyright ASTM International, 100 Barr Harb

16、or Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesNOTICE: This standard has either been superseded and replaced by a new version or withdrawn.Contact ASTM International (www.astm.org) for the latest information17. Apparatus7.1 InstrumentFusion and measurement apparatus con-sistin

17、g of an electrode furnace, provision for scrubbing impu-rities from analytical gas stream, infrared measurement system,and auxiliary gas purification systems. (See Note 1.)NOTE 1The apparatus and analysis systems have been previouslydescribed in Test Method E1019. Several models of commercial oxygen

18、determinators are available and presently in use by industry. Each has itsown unique design characteristics and operational requirements. Consultthe instrument manufacturers manual for operational details.7.2 Graphite CruciblesThe crucibles must be made ofhigh-purity graphite as recommended by the i

19、nstrument manu-facturer and be of the dimensions recommended by theinstrument manufacturer.7.3 TweezersApproximately 6 in. (152 mm), used duringthe sample preparation process.7.4 BalanceMeasurement apparatus with capacity up to10 g capable of weighing 60.1 mg accurately or as specifiedby the instrum

20、ent manufacturer.8. Reagents and Materials8.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such spec

21、ifications are available.6Other grades may beused, provided it is first ascertained that the reagent is ofsufficient high purity to permit its use without lessening theaccuracy of the determination.8.2 Graphite Powder/Carbon BlackHigh-purity graphitepowder or carbon black specified by the instrument

22、 manufac-turer.8.3 Inert GasUse the purity and type (Ar, He, or N2)specified by the instrument manufacturer.8.4 Magnesium Perchlorate (Mg(ClO4)2)AnhydrousUsed as a moisture trap. Use purity specified by the instrumentmanufacturer.8.5 Rare Earth/Copper OxideReagent used in some in-struments to oxidiz

23、e CO to CO2. Use purity specified by theinstrument manufacturer.8.6 Sodium Hydroxide Impregnated ClayUsed to absorbCO2in the inert gas stream. Use purity specified by theinstrument manufacturer.8.7 MethanolUsed in sample preparation, see Section 10.8.8 Copper Pickle SolutionPrepare a fresh solution

24、ofequal parts of concentrated nitric acid (HNO3), concentratedacetic acid (CH3OOH), and concentrated phosphoric acid(H3PO4). Used in sample preparation, see Section 10.9. Hazards9.1 For hazards to be observed in the use of certain reagentsin this test method refer to Practice E50.9.2 Use care when h

25、andling hot crucibles and operatingfurnaces to avoid injury by either burn or electrical shock.10. Sampling and Sample Preparation10.1 Use only solid samples to minimize the potential forerrors due to surface oxidation. Samples must be of the propersize to permit free introduction into the sample-lo

26、ading deviceof the instrument. Sample weight range should be 0.5 to 2.0 g.Refer to instrument manufacturers recommendations.10.2 Cut the sample to an appropriate size using a siliconcarbide, water-cooled cut-off wheel or by other means that willavoid overheating. Avoid oxide cutting or abrading mate

27、rials.10.3 Etch sample with concentrated hydrochloric acid (HCl)at 20C for 3 minutes.10.4 Etch sample in a mixture of equal parts of concentratedHNO3, concentrated CH3COOH, and concentrated H3PO4at70C for one minute.10.5 Rinse sample in three (3) successive distilled waterrinses.10.6 Rinse sample in

28、 three (3) successive methanol rinses.10.7 Dry in a stream of hot air (hair drier).10.8 Do not touch sample with fingers during and followingthe final stages of cleaning. Store the prepared sample in adesiccator. If samples are not analyzed within four hours ofpreparation, repeat 10.3-10.7 prior to

29、analysis. (See Note 2.)NOTE 2Careful adherence to the sample preparation proceduredescribed above is critical to obtaining accurate and precise results. Theuse of small and irregular shaped samples requires a diligent effort toensure that all surface contamination has been removed.11. Preparation of

30、 Apparatus11.1 Assemble the apparatus as recommended by the manu-facturer. Make the required power, gas, and water connections.Turn on the instrument and allow sufficient warm up time tostabilize the system.11.2 Change the chemical reagents and filters as required.Test the furnace and the analyzer t

31、o insure the absence of leaks.Make a minimum of two determinations using a sample asdirected in Section 13 to condition the instrument beforeattempting to calibrate the system or to determine the value ofthe blank.11.3 Calibrate balance as recommended by the manufac-turer using internal or external

32、weights traceable to the SI (seeIEEE /ASTM SI 10).12. Calibration12.1 Calibration Reference Materials (see Note 3)Useonly copper or copper alloy reference materials. Select fourreference materials containing approximately 0.0005, 0.01,0.03, and 0.04 % oxygen and designate them as Calibrants A,B, C,

33、and D respectively.6Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC, www.chemistry.org. For suggestions on thetesting of reagents not listed by the American Chemical Society, see the UnitedStates Pharmacopeia and National Formulary, U.S. Pharmaco

34、peial Convention,Inc. (USPC), Rockville, MD, http:/www.usp.org.E2575 082NOTE 3The oxygen content of the materials selected must fall withinthe scope stated by the standard test method, and within the analyticalrange of the determinator.12.2 Measurement System ConditioningUsing a copperalloy referenc

35、e material, or Calibrant C (see Note 4), proceedas directed in Section 13. Repeat until the absence of drift isindicated. Continue running a series of samples until the lastfour readings have a maximum range of 0.001 % oxygen.NOTE 4Due to availability and cost issues associated with manycertified re

36、ference materials, it is acceptable to use more readily availableand less expensive samples with known oxygen content of sufficienthomogeneity to condition the measurement system. In some cases thesecopper alloy samples may be plated to prevent oxidation during storage.In this case they can be used

37、without additional surface treatment.12.3 Determination of Blank ReadingProceed as directedin Section 13 with a graphite crucible containing graphitepowder or carbon black (see Note 5) and analyze the graphitecrucible with the sample omitted. Use a fresh crucible eachtime. Determine the average blan

38、k of at least three individualruns and enter this value into the appropriate mechanism of theinstrument. Refer to the instrument manufacturers instructionsfor proper blanking procedures.NOTE 5The addition of graphite powder or carbon black (0.05 to 0.5 gdepending on crucible size and style) is desig

39、ned to optimize furnaceperformance and facilitate the release of oxygen from the test sample.Refer to the instrument manufacturers instructions for recommendedgraphite powder additions.12.4 Calibration Procedure:12.4.1 Prepare a minimum of four appropriate size speci-mens of Calibrant C as directed

40、in Section 10.12.4.2 Run a series of at least four samples of Calibrant C.Adjust the instrument calibration to provide a reading within60.0005 % of the known value for the Calibrant using theaverage of the last four readings. Refer to the manufacturersinstructions. Follow the calibration procedure r

41、ecommendedby the manufacturer using Calibrant C to determine thecalibration slope. Weigh specimens to the nearest 1 mg. Thiscopper oxygen reference material should have oxygen contentgreater than or approximately equal to the unknown sampleswithin the scope of this test method (0.0005 and 0.04 %). T

42、reateach specimen as directed in Section 13.12.4.3 Confirm the calibration by analyzing an additionalspecimen of Calibrant C after the calibration procedure iscompleted. The value should agree with the assigned value forCalibrant C within a range of 6ts (95 % confidence level),where s is the standar

43、d deviation of the determinations ofCalibrant C and t is the students variable. If not, repeat thecalibration procedure.12.4.4 Prepare a minimum of four appropriate size speci-mens of Calibrant D as directed in Section 10.12.4.5 Treat each specimen as directed in Section 13, beforeproceeding to the

44、next one.12.4.6 Record the results and compare them to the assignedvalue for Calibrant D. The average of the results should agreewith the assigned value for Calibrant D within a range of6t (s2+(U/2)2)0.5, where s is the standard deviation of thedeterminations of Calibrant D and U is the expanded unc

45、er-tainty (95 % confidence level) of the assigned value forCalibrant D (see Note 6). If not, refer to the instrumentmanufacturers instructions for checking linearity of the sys-tem.NOTE 6The certificate of analysis may provide the value for theexpansion factor for U. If it does, substitute that valu

46、e for 2 in thedenominator of the term U/2. It is possible that the certificate will give anuncertainty estimate that is not expanded. In that case, the value in thedenominator should be 1.12.4.7 Analyze Calibrants A and B following the sameconvention as Calibrants C and D in 12.4.1-12.4.6.13. Proced

47、ure13.1 Assemble apparatus, calibrate, set the blank, and testthe performance as directed in Section 12.13.2 Prepare an appropriate sized specimen, prepared asdirected in Section 10, weighed to the nearest 1 mg, andtransfer to the instrument sample-loading device. Refer toinstrument manufacturers in

48、structions regarding entry ofsample mass.13.3 Place the crucible with carbon black or graphitepowder into the determinator per the instrument manufactur-ers instructions and start the crucible outgas cycle (see Note7).13.4 After the outgas cycle, transfer the sample to thecrucible and start the anal

49、ysis cycle (see Note 7).NOTE 7For some instruments this procedure is automatic.13.5 Some instrument manufacturers recommend drift cor-rection of the apparatus to accommodate for variances that maychange calibration. Please refer to the manufacturers instruc-tions with regards to these procedures.NOTE 8The user may drift correct the calibration per the instrumentmanufacturers instructions utilizing an in-house or commercially avail-able reference material; provided that it is sufficiently homogeneous andstable