1、Designation: E1473 09E1473 16Standard Test Methods forChemical Analysis of Nickel, Cobalt,Cobalt and High-Temperature Alloys1This standard is issued under the fixed designation E1473; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision,
2、 the year of 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 of nickel, cobalt,cobalt and high-temperature alloys ha
3、ving chemicalcompositions 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 0.0
4、01 to 0.05Manganese 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.
5、001 to 0.01Zirconium 0.01 to 2.50Element Composition 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 0.0
6、1 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 0.101 These test methods are under the jurisdiction ofASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and are the direct r
7、esponsibilityof Subcommittee E01.08 on Ni and Co and High Temperature Alloys.Current edition approved June 1, 2009April 1, 2016. Published July 2009May 2016. Originally approved in 1992. Last previous edition approved in 20032009 asE1473 03.E1473 09. DOI: 10.1520/E1473-09.10.1520/E1473-16.This docum
8、ent is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as a
9、ppropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1Silicon 0.01 to 5.00Tantalum 0.005 to 1.00Tin 0.002 to 0.1
10、0Titanium 0.01 to 5.00Tungsten 0.01 to 18.00Vanadium 0.01 to 3.25Zinc 0.001 to 0.01Zirconium 0.01 to 2.501.2 The test methods in this standard are contained in the sections indicated as follows:SectionsAluminum, Total by the 8-Quinolinol Gravimetric Method(0.20 % to 7.00 %)62 to 69Chromium by the At
11、omic Absorption Method(0.018 % to 1.00 %)100 to 109Chromium by the Peroxydisulfate OxidationTitration Method(0.10 % to 33.00 %)110 to 118Cobalt by the Ion-Exchange-Potentiometric Titration Method(2 % to 75 %)34 to 41Cobalt by the Nitroso-R-Salt Photometric Method(0.10 % to 5.0 %)42 to 51Copper by Ne
12、ocuproine Photometric Method(0.010 % to 10.00 %)52 to 61Iron by the Silver Reduction Titrimetric Method(1.0 % to 50.0 %)127 to 134Manganese by the Metaperiodate Photometric Method(0.05 % to2.00 %)8 to 17Molybdenum by the Ion Exchange8-HydroxyquinolineGravimetric Method (1.5 % to 30 %)119 to 126Molyb
13、denum by the Photometric Method(0.01 % to 1.50 %)88 to 99Nickel by the Dimethylglyoxime Gravimetric Method(0.1 % to 84.0 %)70 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 %) 27 to 33Sulfur by the Combustion-Io
14、date Titration Method(0.006 % to 0.1 %)218 to 26Tantalum by the Ion ExchangePyrogallol SpectrophotometricMethod (0.03 % to 1.0 %)143 to 151Tin by the Solvent Extraction-Atomic Absorption Method(0.002 % to 0.10 %)78 to 87Aluminum, Total by the 8-Quinolinol Gravimetric Method(0.20 % to 7.00 %)53 to 60
15、Chromium by the Atomic Absorption Method(0.018 % to 1.00 %)91 to 100Chromium by the Peroxydisulfate OxidationTitration Method(0.10 % to 33.00 %)101 to 109Cobalt by the Ion-Exchange-Potentiometric Titration Method(2 % to 75 %)25 to 32Cobalt by the Nitroso-R-Salt Spectrophotometric Method(0.10 % to 5.
16、0 %)33 to 42Copper by Neocuproine Spectrophotometric Method(0.010 % to 10.00 %)43 to 52Iron by the Silver Reduction Titrimetric Method(1.0 % to 50.0 %)118 to 125Manganese by the Metaperiodate Spectrophotometric Method(0.05 % to 2.00 %)8 to 17Molybdenum by the Ion Exchange8-HydroxyquinolineGravimetri
17、c Method (1.5 % to 30 %)110 to 117Molybdenum by the Spectrophotometric Method(0.01 % to 1.50 %)79 to 90Nickel by the Dimethylglyoxime Gravimetric Method(0.1 % to 84.0 %)61 to 68Niobium by the Ion ExchangeCupferron Gravimetric Method(0.5 % to 6.0 %)126 to 133Silicon by the Gravimetric Method (0.05 %
18、to 5.00 %) 18 to 24Tantalum by the Ion ExchangePyrogallol SpectrophotometricMethod (0.03 % to 1.0 %)134 to 142Tin by the Solvent Extraction-Atomic Absorption Method(0.002 % to 0.10 %)69 to 78These test methods were extracted from Test Methods E354 and the references to Test Methods E350, E351, E352,
19、 and E353 contained therein.E1473 1621.3 Methods for the determination of several elements not included in these test methods can be found in Other test methodsapplicable to the analysis of nickel alloys that may be used in lieu of or in addition to this method are Test Methods E30E1019,E76E1834, E1
20、835and, E1019E1917, E1938, E2465, E2594, E2823.1.4 Some of the concentrationcomposition ranges given in 1.1 are too broad to be covered by a single method, and therefore,these test methods contain multiple methods for some elements. The user must select the proper test method by matching theinformat
21、ion given in the scope and interference sections of each test method with the composition of the alloy to be analyzed.1.5 The values stated in SI units are to be regarded as standard. In some cases, exceptions allowed in Practice E380 are alsoused.1.6 This standard does not purport to address all of
22、 the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. Specific hazard statements are given in Section 7 and in 13.4, 29.11
23、5.1.1, 15.1.2, 21.2, 22.5, 66.357.3,123.5114.5, 124.14115.4, 139.4130.4, 139.5130.5, 147.5138.5, and 147.6138.6.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data to Determine Conformance with SpecificationsE30 Test
24、Methods for Chemical Analysis of Steel, Cast Iron, Open-Hearth Iron, and Wrought Iron (Withdrawn 1995)4E50 Practices forApparatus, Reagents, and Safety Considerations for ChemicalAnalysis of Metals, Ores, and Related MaterialsE60 Practice for Analysis of Metals, Ores, and Related Materials by Spectr
25、ophotometryE76 Test Methods for Chemical Analysis of Nickel-Copper Alloys (Withdrawn 2003)4E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related MaterialsE173 Practice for Conducting Interlaboratory Studies of Methods for Chemical Analysis of Metals (Withdrawn 1998)3E350 Te
26、st Methods for Chemical Analysis of Carbon Steel, Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, and WroughtIronE351 Test Methods for Chemical Analysis of Cast IronAll TypesE352 Test Methods for Chemical Analysis of Tool Steels and Other Similar Medium- and High-Alloy SteelsE353 Test Methods
27、 for Chemical Analysis of Stainless, Heat-Resisting, Maraging, and Other Similar Chromium-Nickel-IronAlloysE354 Test Methods for Chemical Analysis of High-Temperature, Electrical, Magnetic, and Other Similar Iron, Nickel, andCobalt AlloysE380 Practice for Use of the International System of Units (SI
28、) (the Modernized Metric System) (Withdrawn 1997)4E882 Guide for Accountability and Quality Control in the Chemical Analysis LaboratoryE1019 Test Methods for Determination of Carbon, Sulfur, Nitrogen, and Oxygen in Steel, Iron, Nickel, and Cobalt Alloys byVarious Combustion and Fusion TechniquesE160
29、1 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical MethodE1834 Test Method for Analysis of Nickel Alloys by Graphite Furnace Atomic Absorption SpectrometryE1835 Test Method for Analysis of Nickel Alloys by Flame Atomic Absorption SpectrometryE1917 Test Me
30、thod for Determination of Phosphorus in Nickel, Ferronickel, and Nickel Alloys by PhosphovanadomolybdateSpectrophotometryE1938 Test Method for Determination of Titanium in Nickel Alloys by Diantipyrylmethane SpectrophotometryE2465 Test Method for Analysis of Ni-Base Alloys by Wavelength Dispersive X
31、-Ray Fluorescence SpectrometryE2594 Test Method forAnalysis of NickelAlloys by Inductively Coupled PlasmaAtomic Emission Spectrometry (Performance-Based Method)E2823 Test Method for Analysis of Nickel Alloys by Inductively Coupled Plasma Mass Spectrometry (Performance-BasedMethod)2.2 Other Document:
32、ISO 5725 Precision of Test MethodsDetermination of Repeatability and Reproducibility for Inter-Laboratory Tests43. Terminology3.1 DefinitionsFor definitions of terms used in these test methods, refer to Terminology E135.3.1 For definitions of terms used in these test methods, refer to Terminology E1
33、35.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this historical standard is
34、 referenced on www.astm.org.4 Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.E1473 1634. Significance and Use4.1 These test methods for the chemical analysis of metals and alloys are primarily intended as referee methods
35、 to test suchmaterials for compliance with compositional specifications, particularly those under the jurisdiction ofASTM Committee B02B02on Nonferrous Metals and Alloys. It is assumed that all who use these test methods will be trained analysts capable of performingcommon laboratory procedures skil
36、lfully and safely. It is expected that work will be performed in a properly equipped laboratoryunder appropriate quality control practices such as those described in Guide E882.5. Apparatus, Reagents, and Instrumental Practice5.1 ApparatusSpecialized apparatus requirements are listed in theApparatus
37、“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, all reagents used in these test methods shall conform to the specificationsof the Committee on Analytical Reagents of the American Chemical S
38、ociety where such specifications are available.5 Otherchemicals may be used, provided it is first ascertained that they are of sufficiently high purity to permit their use without adverselyaffecting the expected performance of the determination, as indicated in the Precision and Bias sections.5.2.2
39、Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water as defined byType conforming to Type I or II of Specification D1193. Type III or IV may be used if they effect no measurable change in theblank or sample.5.3 PhotometricSpectrophotometric Practic
40、ePhotometricSpectrophotometric practice prescribed in these test methods shallconform to Practice E60.6. Interlaboratory Studies and Rounding Calculated Values6.1 These test methods have been evaluated using in accordance with Practice E173 (withdrawn 1997) or ISO 5725. TheReproducibility R2 of Prac
41、tice E173 corresponds to the Reproducibility Index R of Practice E1601. The Repeatability R1 ofPractice E173 corresponds to the Repeatability Index r of Practice E1601.6.2 Round calculated values to the desired number of places as directed in 3.4 to 3.6 of Rounding of test results obtained usingthis
42、 Test Method shall be performed in accordance with Practice E29. , Rounding Method, unless an alternative rounding methodis specified by the customer or applicable material specification.7. Hazards7.1 For precautions to be observed in the use of certain reagents and equipment in these test methods,
43、refer to Practices E50.MANGANESE BY THE METAPERIODATE PHOTOMETRICSPECTROPHOTOMETRIC METHOD8. Scope8.1 This test method covers the determination of manganese in concentrations from 0.05 % to 2.00 %.9. Summary of Test Method9.1 Manganous ions are oxidized to permanganate ions by treatment with perioda
44、te. Tungsten when present at concentrationsinamounts greater than 0.5 % is kept in solution with phosphoric acid (HH3PO4) Solutions of the samples are fumed withperchloricHClO4 acid so that the effect of periodate is limited to the oxidation of manganese. PhotometricSpectrophotometricmeasurements ar
45、e made at 545 nm.10. Concentration Range10.1 The recommended concentration range is from 0.15 mg to 0.8 mg of manganese per 50 mL of solution, using a 1-cm cell(Note 1) and a spectrophotometer with a band width of 10 nm or less.NOTE 1This test method has been written for cells having a 1-cm light pa
46、th and a “narrow-band” instrument. The concentration range depends uponband width and spectral region used as well as cell optical path length. Cells having other dimensions may be used, provided suitable adjustments canbe made in the amounts of sample and reagents used.11. Stability of Color11.1 Th
47、e color is stable for at least 24 h.5 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC, www.chemistry.org. For suggestions on the testing ofreagents not listed by theAmerican Chemical Society, see the United States Pharmacopeia and National Formu
48、lary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD, http:/www.usp.org.E1473 16412. Interferences12.1 PerchloricHClO4 acid treatment, which is used in the procedure, yields solutions which can be highly colored due to thepresence of hexavalent chromium (Cr(VI)Cr(VI) ions.Although these io
49、ns and other colored ions in the sample solution undergono further change in color quality upon treatment with metaperiodate ion, the following precautions must be observed when filterphotometersspectrophotometers are used: Select a filter with maximum transmittance between 545 nm and 565 nm. The filter musttransmit not more than 5 % of its maximum at a wavelength shorter than 530 nm. The band width of the filter should be less than30 nm when measured at 50 % of its maximum transmittance. Similar restrictions apply with respect to the wavelength regionempl
