1、Designation: E 354 93 (Reapproved 2006)Standard Test Methods forChemical Analysis of High-Temperature, Electrical,Magnetic, and Other Similar Iron, Nickel, and Cobalt Alloys1This standard is issued under the fixed designation E 354; the number immediately following the designation indicates the year
2、 oforiginal adoption or, in the case of revision, the year of 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.This standard has been approved for use by agencies of the Departme
3、nt of Defense.1. Scope1.1 These test methods cover the chemical analysis ofhigh-temperature, electrical, magnetic, and other similar iron,nickel, and cobalt alloys having chemical compositions withinthe following limits:ElementConcentrationRange, %Aluminum 0.005 to 18.00Beryllium 0.001 to 0.05Boron
4、0.001 to 1.00Calcium 0.002 to 0.05Carbon 0.001 to 1.10Chromium 0.10 to 33.00Cobalt 0.10 to 75.00Columbium (Niobium) 0.01 to 6.0Copper 0.01 to 10.00Iron 0.01 to 85.00Magnesium 0.001 to 0.05Manganese 0.01 to 3.0Molybdenum 0.01 to 30.0Nickel 0.10 to 84.0Nitrogen 0.001 to 0.20Phosphorus 0.002 to 0.08Sil
5、icon 0.01 to 5.00Sulfur 0.002 to 0.10Tantalum 0.005 to 10.0Titanium 0.01 to 5.00Tungsten 0.01 to 18.00Vanadium 0.01 to 3.25Zirconium 0.01 to 2.501.2 The test methods in this standard are contained in thesections indicated below:SectionsAluminum, Total, by the 8-Quinolinol Gravimetric Method (0.20 to
6、7.00 %)100Carbon,Total, by the Combustion-Thermal Conductivity Method1aCarbon, Total, by the Combustion Gravimetric Method (0.05 to1.10 %)79Chromium by the Atomic Absorption Method (0.006 to 1.00 %) 165Chromium by the Peroxydisulfate OxidationTitration Method(0.10 to 33.00 %)175Chromium by the Perox
7、ydisulfate-Oxidation Titrimetric Method1bCobalt by the Ion-Exchange-Potentiometric Titration Method (2 to75 %)53Cobalt by the Nitroso-R-Salt Photometric Method (0.10 to 5.0 %) 61Copper by Neocuproine Photometric Method (0.01 to 10.00 %) 90Copper by the Sulfide Precipitation-Electrodeposition Gravime
8、tricMethod (0.01 to 10.00 %)71Iron by the Silver ReductionTitrimetric Method (1.0 to 50.0 %) 192Manganese by the Periodate Photometric Method (0.05 to 2.00 %) 8Molybdenum by the Ion Exchange8-Hydroxyquinoline Gravi-metric Method (1.5 to 30 %)184Molybdenum by the Photometric Method (0.01 to 1.50 %) 1
9、53Nickel by the Dimethylglyoxime Gravimetric Method (0.1 to84.0 %)135Phosphorus by the Molybdenum Blue Photometric Method (0.002to 0.08 %)18Silicon by the Gravimetric Method (0.05 to 5.00 %) 46Sulfur by the Gravimetric Method1 cSulfur by the Combustion-Iodate Titration Method (0.005 to0.1 %)37Sulfur
10、 by the Chromatographic Gravimetric Method1bTin by the Solvent ExtractionAtomic Absorption Method (0.002to 0.10 %)1431.3 Methods for the determination of several elements notincluded in this standard can be found in Test Methods E30and Test Methods E 1019.1.4 Some of the concentration ranges given i
11、n 1.1 are toobroad to be covered by a single method and therefore thisstandard contains multiple methods for some elements. Theuser must select the proper method by matching the informa-tion given in the Scope and Interference sections of eachmethod with the composition of the alloy to be analyzed.1
12、.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 establish
13、 appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific hazards1These test methods are under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores and Related Materials and are the directresponsibility of Su
14、bcommittee E01.01 on Iron, Steel, and Ferroalloys.Current edition approved June 1, 2006. Published June 2006. Originallyapproved in 1968. Last previous edition approved in 2000 as E 354 93 (2000)e1.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, U
15、nited States.statements are given in Section 5 and in special “Warning”paragraphs throughout these test methods.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE30 Test
16、Methods for Chemical Analysis of Steel, CastIron, Open-Hearth Iron, and Wrought Iron3E50 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 Molecular Absorption Sp
17、ectrometryE 173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Analysis 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 T
18、est 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 380 Practice for Use of the International System of Units(SI) (the Modernized
19、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 1806 Practice for Sampling Steel and Iron for Determi-nation of Chemical Com
20、position2.2 Other Document:ISO 5725 Precision of Test MethodsDetermination ofRepeatability and Reproducibility for Inter-LaboratoryTests43. Significance and Use3.1 These test methods for the chemical analysis of metalsand alloys are primarily intended as referee methods to testsuch materials for com
21、pliance with compositional specifica-tions, particularly those under the jurisdiction of ASTM Com-mittee on Steel, Stainless Steel and Related Alloys. It isassumed that all who use these test methods will be trainedanalysts capable of performing common laboratory proceduresskillfully and safely. It
22、is expected that work will be performedin a properly equipped laboratory under appropriate qualitycontrol practices such as those described in Guide E 882.4. Apparatus, Reagents, and Instrumental Practice4.1 ApparatusSpecialized apparatus requirements arelisted in the “Apparatus” Section in each met
23、hod. 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 conform to the“Reagent Grade” Specifications of the American ChemicalSociety.5Other chemicals may be used, provided it is firstascert
24、ained that they are of sufficiently high purity to permittheir use without adversely affecting the expected performanceof the determination, as indicated in the section on “Precisionand Bias.”4.2.2 Purity of WaterUnless otherwise indicated, refer-ences to water shall be understood to mean reagent wa
25、ter asdefined by Type II of Specification D 1193.4.3 Photometric PracticePhotometric practice prescribedin these test methods shall conform to Practice E60.5. Hazards5.1 For precautions to be observed in the use of certainreagents and equipment in these methods, refer to PracticesE50.6. Sampling6.1
26、For procedures for sampling the material, referenceshall be made to Practice E 1806.7. Interlaboratory Studies and Rounding CalculatedValues7.1 These test methods have been evaluated using PracticeE 173 or ISO 5725.7.2 Calculated values shall be rounded to the desired num-ber of places as directed i
27、n 3.4 to 3.6 of Practice E29.MANGANESE BY THE METAPERIODATEPHOTOMETRIC METHOD8. Scope8.1 This method covers the determination of manganese inconcentrations from 0.05 to 2.00 percent.9. Summary of Method9.1 Manganous ions are oxidized to permanganate ions bytreatment with periodate. Tungsten when pre
28、sent at concentra-tions greater than 0.5 % is kept in solution with phosphoricacid. Solutions of the samples are fumed with perchloric acidso that the effect of periodate is limited to the oxidation ofmanganese. Photometric measurements are made at approxi-mately 545 nm.2For referenced ASTM standard
29、s, 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.3Withdrawn.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4t
30、h Floor, New York, NY 10036.5“Reagent Chemicals, American Chemical Society Specifications,” Am. Chemi-cal Soc., Washington, DC. For suggestions on the testing of Reagents not listed bytheAmerican Chemical Society, see “Reagent Chemicals and Standards,” by JosephRosin, D. Van Nostrand Co., Inc., New
31、York, NY, and the “United StatesPharmacopeia.” United States Pharmacopeial Convention, Rockville, MD 20852.E 354 93 (2006)210. Concentration Range10.1 The recommended concentration range is 0.15 to 0.8mg of manganese per 50 mL of solution, using a 1-cm cell(Note 1) and a spectrophotometer with a ban
32、d width of 10 nmor less.NOTE 1This method has been written for cells having a 1-cm lightpath and a “narrow-band” instrument. The concentration range dependsupon band width and spectral region used as well as cell optical pathlength. Cells having other dimensions may be used, provided suitableadjustm
33、ents 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 Cr (VI) ions.Although thes
34、e ions and other coloredions in the sample solution undergo no further change in 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 n
35、ot more than 5 % of itsmaximum at a wavelength shorter than 530 nm. The bandwidth 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 sp
36、ectral 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 producing a turbidity in the
37、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 0.4000 g of assayed, high-pur
38、ity 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 Mixture Cautiously, whilestirring, add 100 mL
39、 of HNO3and 400 mL of H3PO4to 400mL 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 mL of H3PO4, cool, dilute to 1 L,and mix.13.4 Water, Pretreated with
40、 MetaperiodateAdd 20 mL ofKIO4solution to 1 L of water, mix, heat at not less than 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 untre
41、ated water. CautionAvoidthe 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 (1mL = 0.032 mg Mn) to 50-mL borosilicate glass volumetricflasks, and, if necessary, dilute to
42、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 than 90C for 20 to 30 min(Note 2).
43、 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 correc-tion using the Reference So
44、lution (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 photometricreadings of the calibration solutions versus the ReferenceSolution (14.2)14.4.2 Single-Cell PhotometerTransfer a suitable portionof the Reference S
45、olution (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 Calibration CurvePlot the net photometric
46、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:E 354 93 (2006)3Manganese,%SampleWeight, gTolerance inSampleWeight, mgDilution,mL0.01 to 0.5 0.80 0.5 1000.45 to 1.0 0
47、.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, 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 ad
48、d 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 to 15.1.3.15.1.1.2 For sampl
49、es whose dissolution is hastened by HF,and 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 to4mLofHNO3. When dissolution is complete, cool, then add10 mL or HClO4, evaporate to fumes to oxidize chromium, ifpresent, and to expel HCl. Continue fuming until salts begin toseparate. Cool, add 50 mL of water, digest if necessary todissolve the salts, cool, and transfer the solution to either a 100-or 500-mL volumetric flask as indicated in 15.1.5. Proceed to15.1.3.15.1.2 For Samples Containing More T
