1、Designation: E 1473 09Standard Test Methods forChemical Analysis of Nickel, Cobalt, and High-TemperatureAlloys1This standard is issued under the fixed designation E 1473; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、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 These test methods describe the chemical analysis ofnickel, cobalt, and high-temperature alloys having chemicalcomposi
3、tions within the following limits:Element Concentration Range, %Aluminum 0.005 to 7.00Beryllium 0.001 to 0.05Boron 0.001 to 1.00Calcium 0.002 to 0.05Carbon 0.001 to 1.10Chromium 0.10 to 33.00Cobalt 0.10 to 75.00Copper 0.01 to 35.00Iron 0.01 to 50.00Lead 0.001 to 0.01Magnesium 0.001 to 0.05Manganese
4、0.01 to 3.0Molybdenum 0.01 to 30.0Niobium (Columbium) 0.01 to 6.0Nickel 0.10 to 98.0Nitrogen 0.001 to 0.20Phosphorus 0.002 to 0.08Sulfur 0.002 to 0.10Silicon 0.01 to 5.00Tantalum 0.005 to 1.00Tin 0.002 to 0.10Titanium 0.01 to 5.00Tungsten 0.01 to 18.00Vanadium 0.01 to 3.25Zinc 0.001 to 0.01Zirconium
5、 0.01 to 2.501.2 The test methods in this standard are contained in thesections indicated as follows:SectionsAluminum, Total by the 8-Quinolinol Gravimetric Method(0.20 % to 7.00 %)262 to 69Chromium by the Atomic Absorption Method(0.018 % to 1.00 %)2100 to 109Chromium by the Peroxydisulfate Oxidatio
6、nTitration Method(0.10 % to 33.00 %)2110 to 118Cobalt by the Ion-Exchange-Potentiometric Titration Method(2%to75%)234 to 41Cobalt by the Nitroso-R-Salt Photometric Method(0.10 % to 5.0 %)242 to 51Copper by Neocuproine Photometric Method (0.010 % to10.00 %)252 to 61Iron by the Silver Reduction Titrim
7、etric Method(1.0 % to 50.0 %)2127 to 134Manganese by the Metaperiodate Photometric Method (0.05 % to2.00 %)28 to 17Molybdenum by the Ion Exchange8-HydroxyquinolineGravimetric Method (1.5 % to 30 %)2119 to 126Molybdenum by the Photometric Method(0.01 % to 1.50 %)288 to 99Nickel by the Dimethylglyoxim
8、e Gravimetric Method(0.1 % to 84.0 %)270 to 77Niobium by the Ion ExchangeCupferron Gravimetric Method(0.5 % to 6.0 %)135 to 142Silicon by the Gravimetric Method (0.05 % to 5.00 %)227 to 33Sulfur by the Combustion-Iodate Titration Method(0.006 % to 0.1 %)218 to 26Tantalum by the Ion ExchangePyrogallo
9、l SpectrophotometricMethod (0.03 % to 1.0 %)143 to 151Tin by the Solvent Extraction-Atomic Absorption Method(0.002 % to 0.10 %)278 to 871.3 Methods for the determination of several elements notincluded in these test methods can be found in Test MethodsE30, E76, and E 1019.1.4 Some of the concentrati
10、on ranges given in 1.1 are toobroad to be covered by a single method, and therefore, thesetest methods contain multiple methods for some elements. Theuser must select the proper test method by matching theinformation given in the scope and interference sections ofeach test method with the compositio
11、n of the alloy to beanalyzed.1.5 The values stated in SI units are to be regarded asstandard. In some cases, exceptions allowed in Practice E 380are also used.1.6 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user
12、 of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific hazard1These test methods are under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and are
13、the directresponsibility of Subcommittee E01.08 on Ni and Co and High TemperatureAlloys.Current edition approved June 1, 2009. Published July 2009. Originally approvedin 1992. Last previous edition approved in 2003 as E 1473 03.2These test methods were extracted from Test Methods E 354 and the refer
14、encesto Test Methods E 350, E 351, E 352, and E 353 contained therein.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.statements are given in Section 7 and in 13.4, 29.1, 66.3, 123.5,124.14, 139.4, 139.5, 147.5, and 147.6.2. Referenc
15、ed Documents2.1 ASTM Standards:3D 1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE30 Test Methods for Chemical Analysis of Steel, CastIron, Open-Hearth Iron, and Wrought Iron4E50 Practices for Apparatus, Reagents,
16、 and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE60 Practice for Analysis of Metals, Ores, and RelatedMaterials by Molecular Absorption SpectrometryE76 Test Methods for ChemicalAnalysis of Nickel-CopperAlloys4E 135 Terminology Relating to Analytical Chemistry f
17、orMetals, Ores, and Related MaterialsE 173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Analysis of Metals4E 350 Test Methods for ChemicalAnalysis of Carbon Steel,Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, andWrought IronE 351 Test Methods for Chemical Analysis
18、of Cast IronAll TypesE 352 Test Methods for Chemical Analysis of Tool Steelsand Other Similar Medium- and High-Alloy SteelsE 353 Test Methods for Chemical Analysis of Stainless,Heat-Resisting, Maraging, and Other Similar Chromium-Nickel-Iron AlloysE 354 Test Methods for Chemical Analysis of High-Tem
19、perature, Electrical, Magnetic, and Other Similar Iron,Nickel, and Cobalt AlloysE 380 Practice for Use of the International System of Units(SI) (the Modernized Metric System)4E 882 Guide for Accountability and Quality Control in theChemical Analysis LaboratoryE 1019 Test Methods for Determination of
20、 Carbon, Sulfur,Nitrogen, and Oxygen in Steel, Iron, Nickel, and CobaltAlloys by Various Combustion and Fusion Techniques3. Terminology3.1 Definitions: DefinitionsFor definitions of terms usedin these test methods, refer to Terminology E 135.4. Significance and Use4.1 These test methods for the chem
21、ical analysis of metalsand alloys are primarily intended as referee methods to testsuch materials for compliance with compositional specifica-tions, particularly those under the jurisdiction of ASTM Com-mittee B02 on Nonferrous Metals andAlloys. It is assumed thatall who use these test methods will
22、be trained analysts capableof performing common laboratory procedures skillfully andsafely. It is expected that work will be performed in a properlyequipped laboratory under appropriate quality control practicessuch as those described in Guide E 882.5. Apparatus, Reagents, and Instrumental Practice5
23、.1 ApparatusSpecialized apparatus requirements arelisted in the Apparatus section in each test method. In somecases, reference may be made to Practices E50.5.2 Reagents:5.2.1 Purity of ReagentsUnless otherwise indicated, allreagents used in these test methods shall conform to thespecifications of th
24、e Committee on Analytical Reagents of theAmerican Chemical Society where such specifications areavailable.5Other chemicals may be used, provided it is firstascertained that they are of sufficiently high purity to permittheir use without adversely affecting the expected performanceof the determinatio
25、n, as indicated in the Precision and Biassections.5.2.2 Purity of WaterUnless otherwise indicated, refer-ences to water shall be understood to mean reagent water asdefined by Type II of Specification D 1193.5.3 Photometric PracticePhotometric practice prescribedin these test methods shall conform to
26、 Practice E60.6. Interlaboratory Studies and Rounding CalculatedValues6.1 These test methods have been evaluated using PracticeE 173.6.2 Round calculated values to the desired number of placesas directed in 3.4 to 3.6 of Practice E29.7. Hazards7.1 For precautions to be observed in the use of certain
27、reagents and equipment in these test methods, refer to PracticesE50.MANGANESE BY THE METAPERIODATEPHOTOMETRIC METHOD8. Scope8.1 This test method covers the determination of manganesein concentrations from 0.05 % to 2.00 %.9. Summary of Test Method9.1 Manganous ions are oxidized to permanganate ions
28、bytreatment with periodate. Tungsten when present at concentra-tions greater than 0.5 % is kept in solution with phosphoricacid (H3PO4). Solutions of the samples are fumed withperchloric acid so that the effect of periodate is limited to theoxidation of manganese. Photometric measurements are madeat
29、 545 nm.3For 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.4Withdrawn. The last approved version of this histori
30、cal standard is referencedon www.astm.org.5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC, http:/pubs.acs.org/reagents/index.html. Forsuggestions on the testing of reagents not listed by the American Chemical Society,see the United States Pharma
31、copeia and National Formulary, U.S. PharmacopeialConvention, Inc. (USPC), Rockville, MD, http:/www.usp.org.E147309210. Concentration Range10.1 The recommended concentration range is from0.15 mg to 0.8 mg of manganese per 50 mL of solution, usinga 1-cm cell (Note 1) and a spectrophotometer with a ban
32、dwidth of 10 nm or less.NOTE 1This test method has been written for cells having a 1-cmlight path and a “narrow-band” instrument. The concentration rangedepends upon band width and spectral region used as well as cell opticalpath length. Cells having other dimensions may be used, provided suitablead
33、justments can be made in the amounts of sample and reagents used.11. Stability of Color11.1 The color is stable for at least 24 h.12. Interferences12.1 Perchloric acid treatment, which is used in the proce-dure, yields solutions which can be highly colored due to thepresence of hexavalent chromium (
34、Cr(VI) ions. Althoughthese ions and other colored ions in the sample solutionundergo no further change in color quality upon treatment withmetaperiodate ion, the following precautions must be observedwhen filter photometers are used: Select a filter with maximumtransmittance between 545 nm and 565 n
35、m. The filter musttransmit not more than 5 % of its maximum at a wavelengthshorter than 530 nm. The band width of the filter should be lessthan 30 nm when measured at 50 % of its maximum transmit-tance. Similar restrictions apply with respect to the wavelengthregion employed when other “wide-band” i
36、nstruments areused.12.2 The spectral transmittance curve of permanganate ionsexhibits two useful minima, one at approximately 526 nm, andthe other at 545 nm. The latter is recommended when a“narrow-band” spectrophotometer is used.12.3 Tungsten, when present in amounts of more than 0.5 %interferes by
37、 producing a turbidity in the final solution. Aspecial procedure is provided for use with samples containingmore than 0.5 % tungsten which eliminates the problem bypreventing the precipitation of the tungsten.13. Reagents13.1 Manganese, Standard Solution (1 mL = 0.032 mgMn)Transfer the equivalent of
38、 0.4000 g of assayed, high-purity manganese (purity 99.99 % minimum), to a 500-mLvolumetric flask and dissolve in 20 mL of HNO3by heating.Cool, dilute to volume, and mix. Using a pipet, transfer 20 mLto a 500-mL volumetric flask, dilute to volume, and mix.13.2 Nitric-Phosphoric Acid MixtureCautiousl
39、y, whilestirring, add 100 mL of HNO3and 400 mL of H3PO4to400 mL of water. Cool, dilute to 1 L, and mix. Prepare fresh asneeded.13.3 Potassium Metaperiodate Solution (7.5 g/L)Dissolve 7.5 g of potassium metaperiodate (KIO4) in 200 mLof hot HNO3(1 + 1), add 400 mLof H3PO4, cool, dilute to 1 L,and mix.
40、13.4 Water, Pretreated with MetaperiodateAdd 20 mL ofKIO4solution to 1 L of water, mix, heat at not less than 90 Cfor 20 to 30 min, and cool. Use this water to dilute solutions tovolume that have been treated with KIO4solution to oxidizemanganese, and thus avoid reduction of permanganate ions byany
41、reducing agents in the untreated water. (WarningAvoidthe use of this water for other purposes.)14. Preparation of Calibration Curve14.1 Calibration SolutionsUsing pipets, transfer (5, 10,15, 20, and 25) mL of manganese standard solution(1 mL = 0.032 mg Mn) to 50-mLborosilicate glass volumetricflasks
42、, and, if necessary, dilute to approximately 25 mL.Proceed as directed in 14.3.14.2 Reference SolutionTransfer approximately 25 mL ofwater to a 50-mL borosilicate glass volumetric flask. Proceedas directed in 14.3.14.3 Color DevelopmentAdd 10 mL of KIO4solution,and heat the solutions at not less tha
43、n 90 C for 20 to 30 min(Note 2). Cool, dilute to volume with pretreated water, andmix.NOTE 2Immersing the flasks in a boiling water bath is a preferredmeans of heating them for the specified period to ensure complete colordevelopment.14.4 Photometry:14.4.1 Multiple-Cell PhotometerMeasure the cell co
44、rrec-tion using the Reference Solution (14.2) in absorption cellswith a 1-cm light path and using a light band centered atapproximately 545 nm. Using the test cell, take the photomet-ric readings of the calibration solutions versus the referencesolution (14.2).14.4.2 Single-Cell PhotometerTransfer a
45、 suitable portionof the reference solution (14.2) to an absorption cell with a1-cm light path and adjust the photometer to the initial setting,using a light band centered at approximately 545 nm. Whilemaintaining this adjustment, take the photometric readings ofthe calibration solutions.14.5 Calibra
46、tion CurvePlot the net photometric readingsof the calibration solutions against milligrams of manganeseper 50 mL of solution.15. Procedure15.1 Test SolutionsSelect and weigh a sample in accor-dance with the following:Manganese,%SampleWeight, gTolerance inSampleWeight, mgDilution,mL0.01 to 0.5 0.80 0
47、.5 1000.45 to 1.0 0.35 0.3 1000.85 to 2.0 0.80 0.5 50015.1.1 For Samples Containing Not More Than 0.5 %Tungsten:15.1.1.1 To dissolve samples that do not require HF, add8 mL to 10 mL of HCl (1 + 1), and heat. Add HNO3as neededto hasten dissolution, and then add 3 mL to 4 mL in excess.When dissolution
48、 is complete, cool, then add 10 mL of HClO4;evaporate to fumes to oxidize chromium, if present, and toexpel HCl. Continue fuming until salts begin to separate. Cool,add 50 mL of water, and digest if necessary to dissolve thesalts. Cool and transfer the solution to a 100-mL volumetricflask. Proceed t
49、o 15.1.3.15.1.1.2 For samples whose dissolution is hastened by HF,add 8 mL to 10 mL of HCl (1 + 1), and heat. Add HNO3and afew drops of HF as needed to hasten dissolution, and then addE14730933 mL to 4 mL of HNO3. When dissolution is complete, cool,then add 10 mL of HClO4, evaporate to fumes to oxidizechromium, if present, and to expel HCl. Continue fuming untilsalts begin to separate. Cool, add 50 mL of water, digest ifnecessary to dissolve the salts, cool, and transfer the solution toeither a 100-mL or 500-mL volumetric flask as indicated in15.1. Proce
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