1、Designation: E 1473 03Standard 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 (e) 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 chemicalcompos
3、itions 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 0.01Zirconiu
5、m 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 to7.00 %)262 to 69Chromium by the Atomic Absorption Method (0.018 to 1.00 %)2100 to 109Chromium by the Peroxydisulfate OxidationT
6、itration Method(0.10 to 33.00 %)2110to118Cobalt by the Ion-Exchange-Potentiometric Titration Method (2 to75 %)234 to 41Cobalt by the Nitroso-R-Salt Photometric Method (0.10 to5.0 %)242 to 51Copper by Neocuproine Photometric Method (0.010 to 10.00 %)252 to 61Iron by the Silver Reduction Titrimetric M
7、ethod (1.0 to 50.0 %)2127 to 134Manganese by the Metaperiodate Photometric Method (0.05 to2.00 %)28to17Molybdenum by the Ion Exchange8-Hydroxyquinoline Gravi-metric Method (1.5 to 30 %)2119to126Molybdenum by the Photometric Method (0.01 to 1.50 %)288 to 99Nickel by the Dimethylglyoxime Gravimetric M
8、ethod (0.1 to84.0 %)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 to0.1 %)218 to 26Tantalum by the Ion ExchangePyrogallol SpectrophotometricMe
9、thod (0.03 to 1.0%) 143 to 151Tin by the Solvent Extraction-Atomic Absorption Method (0.002to 0.10 %)278 to 871.3 Methods for the determination of several elements notincluded in these test methods can be found in Test MethodsE 30, E 76, and E 1019.1.4 Some of the concentration ranges given in 1.1 a
10、re 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 composition of the alloy to beanal
11、yzed.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 of this standard to est
12、ablish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific hazardstatements are given in Section 7 and in special caution andwarning paragraphs throughout these test methods.2. Referenced Documents2.1 ASTM Standards:3D 1193 Speci
13、fication for Reagent Water1These test methods are under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Material and are the directresponsibility of Subcommittee E01.08 on Ni and Co and High-TemperatureAlloys.Current edition approved December 1, 2003. Publ
14、ished January 2004. Originallyapproved in 1992. Last previous edition approved in 1998 as E 1473 94a (1998).2These test methods were extracted from Test Methods E 354 and the referencesto Test Methods E 350, E 351, E 352, and E 353 contained therein.3For referenced ASTM standards, visit the ASTM web
15、site, 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United Sta
16、tes.E29 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 IronE50 Practices for Apparatus, Reagents, and Safety Precau-tions for Chemical Analysis of MetalsE59 Practic
17、e for Sampling Steel and Iron for Determinationof Chemical CompositionE60 Practice for Photometric and SpectrophotometricMethods for Chemical Analysis of MetalsE76 Test Methods for ChemicalAnalysis of Nickel-CopperAlloysE 173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Ana
18、lysis of MetalsE 350 Test Methods for ChemicalAnalysis of Carbon Steel,Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, andWrought IronE 351 Test Methods for Chemical Analysis of Cast IronAll TypesE 352 Test Methods for Chemical Analysis of Tool Steelsand Other Similar Medium- and High-Alloy S
19、teelsE 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-Temperature, Electrical, Magnetic, and Other Similar Iron,Nickel, and Cobalt AlloysE 380 Practice for Use of the Internat
20、ional System of Units(SI) (the Modernized Metric System)E 882 Guide for Accountability and Quality Control in theChemical Analysis LaboratoryE 1019 Test Methods for Determination of Carbon, Sulfur,Nitrogen, and Oxygen in Steel and in Iron, Nickel, andCobalt AlloysE 1024 Guide for Chemical Analysis o
21、f Metals and MetalBearing Ores by Flame Atomic Absorption Spectropho-tometryE 1097 Guide for Direct Current Plasma Emission Spec-trometry Analysis2.2 Other Document:ISO 5725 Precision of Test MethodsDetermination ofRepeatability and Reproducibility for Inter-LaboratoryTests43. Significance and Use3.
22、1 These test methods for the chemical 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 B-2 on Nonferrous Metals andAlloys. It is assumed thatall
23、 who use these test methods will 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 882.4. Apparatus, Rea
24、gents, and Instrumental Practice4.1 ApparatusSpecialized apparatus requirements arelisted in the Apparatus section in each test method. In somecases, reference may be made to Practices E50.4.2 Reagents:4.2.1 Purity of ReagentsUnless otherwise indicated, allreagents used in these test methods shall c
25、onform to thespecifications of the Committee on Analytical Reagents of theAmerican Chemical Society where such specifications areav-ailable.5Other chemicals may be used, provided it is firstascertained that they are of sufficiently high purity to permittheir use without adversely affecting the expec
26、ted performanceof the determination, as indicated in the Precision and Biassection.4.2.2 Purity of WaterUnless otherwise indicated, refer-ences to water shall be understood to mean reagent water asdefined by Type II of Specification D 1193.4.3 Photometric PracticePhotometric practice prescribedin th
27、ese test methods shall conform to Practice E60.5. Sampling5.1 For procedures for sampling the material, referenceshall be made to Method E59.6. Interlaboratory Studies and Rounding CalculatedValues6.1 These test methods have been evaluated using PracticeE 173 or ISO 5725.6.2 Round calculated values
28、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 certainreagents and equipment in these test methods, refer to PracticesE50.MANGANESE BY THE METAPERIODATEPHOTOMETRIC METHOD8. Scope8.1 This test method covers the deter
29、mination of manganesein concentrations from 0.05 to 2.00 %.9. Summary of Test Method9.1 Manganous ions are oxidized to permanganate ions bytreatment with periodate. Tungsten when present at concentra-tions greater than 0.5 % is kept in solution with phosphoricacid. Solutions of the samples are fumed
30、 with perchloric acidso that the effect of periodate is limited to the oxidation ofmanganese. Photometric measurements are made at 545 nm.4Available from American National Standards Institute, 11 West 42nd St., 13thFloor, New York, NY 10036.5Reagent Chemicals, American Chemical Society Specification
31、s, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmaceutical Convention, I
32、nc. (USPC), Rockville,MD.E147303210. Concentration Range10.1 The recommended concentration range is from 0.15 to0.8 mg of manganese per 50 mL of solution, using a 1-cm cell(Note 1) and a spectrophotometer with a band width of 10 nmor less.NOTE 1This test method has been written for cells having a 1-
33、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 suitableadjustments can be made in the amounts of sample and reagents used.11. Stability of Col
34、or11.1 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 Cr (VI) ions.Although these ions and other coloredions in the sample solution undergo no further change in
35、 colorquality upon treatment with metaperiodate ion, the followingprecautions must be observed when filter photometers are used:Select a filter with maximum transmittance between 545 and565 nm. The filter must transmit not more than 5 % of itsmaximum at a wavelength shorter than 530 nm. The bandwidt
36、h of the filter should be less than 30 nm when measured at50 % of its maximum transmittance. Similar restrictions applywith respect to the wavelength region employed when other“wide-band” instruments are used.12.2 The spectral transmittance curve of permanganate ionsexhibits two useful minima, one a
37、t 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 producing a turbidity in the final solution. Aspecial procedure is provided for use with samples containingmo
38、re 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 0.4000 g of assayed, high-purity manganese (purity: 99.99 % minimum), to a 500-mLvolumetric flask and dissolv
39、e 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 MixtureCautiously, whilestirring, add 100 mL of HNO3and 400 mL of H3PO4to 400mL of water. Cool, dilute to 1 L, and mix. Prepa
40、re 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 mL of H3PO4, cool, dilute to 1 L,and mix.13.4 Water, Pretreated with MetaperiodateAdd 20 mL ofKIO4solution to 1 L of water, mix, heat at not less tha
41、n 90Cfor 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 reducing agents in the untreated water. CautionAvoidthe use of this water for other purposes.14. Preparation
42、of Calibration Curve14.1 Calibration SolutionsUsing pipets, transfer 5, 10,15, 20, and 25 mL of manganese standard solution (1mL = 0.032 mg Mn) to 50-mL borosilicate glass volumetricflasks, and, if necessary, dilute to approximately 25 mL.Proceed as directed in 14.3.14.2 Reference SolutionTransfer a
43、pproximately 25 mL ofwater to a 50-mL borosilicate glass volumetric flask. Proceedas directed in 14.314.3 Color DevelopmentAdd 10 mL of KIO4solution,and heat the solutions at not less than 90C for 20 to 30 min(Note 2). Cool, dilute to volume with pretreated water, andmix.NOTE 2Immersing the flasks i
44、n 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 correc-tion using the Reference Solution (14.2) in absorption cellswith a 1-cm light path and using a light band cen
45、tered atapproximately 545 nm. Using the test cell, take the photometricreadings of the calibration solutions versus the referencesolution (14.2)14.4.2 Single-Cell PhotometerTransfer a suitable portionof the reference solution (14.2) to an absorption cell with a1-cm light path and adjust the photomet
46、er 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 Calibration CurvePlot the net photometric readingsof the calibration solutions against milligrams of manganeseper 50 mL of s
47、olution.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 0.5 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.
48、1.1 To dissolve samples that do not require HF, add 8to 10 mL of HCl (1 + 1), and heat. Add HNO3as needed tohasten dissolution, and then add 3 to 4 mL in excess. Whendissolution is complete, cool, then add 10 mL of HClO4;evaporate to fumes to oxidize chromium, if present, and toexpel HCl. Continue f
49、uming 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 to 15.1.3.15.1.1.2 For samples whose dissolution is hastened by HF,add 8 to 10 mL of HCl (1 + 1), and heat.Add HNO3and a fewdrops of HF as needed to hasten dissolution, and then add 3 toE14730334mLofHNO3. When dissolution is complete, cool, then add10 mL of HClO4, evaporate to fumes to oxidize chromium, ifpresent, and to expel HCl. Continue fuming until salts begin toseparate. Cool, ad
