1、Designation: E354 14Standard Test Methods forChemical Analysis of High-Temperature, Electrical,Magnetic, and Other Similar Iron, Nickel, and Cobalt Alloys1This standard is issued under the fixed designation E354; the number immediately following the designation indicates the year oforiginal adoption
2、 or, in the case of revision, 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.This standard has been approved for use by agencies of the U.S. Department of Defense.1.
3、 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:ElementCompositionRange, %Aluminum 0.005 to 18.00Beryllium 0.001 to 0.05Boron 0.001 to 1.00Calci
4、um 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 0.08Silicon 0.01 to 5.00S
5、ulfur 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 % to7.00 %)100Carbon
6、, Total, by the Combustion-Thermal Conductivity Method DiscontinuedCarbon, Total, by the Combustion Gravimetric Method (0.05 % to1.10 %)DiscontinuedChromium by the Atomic Absorption Method (0.006 % to 1.00 %) 165Chromium by the Peroxydisulfate OxidationTitration Method(0.10 % to 33.00 %)175Chromium
7、by the Peroxydisulfate-Oxidation Titrimetric Method DiscontinuedCobalt by the Ion-Exchange-Potentiometric Titration Method (2 % to75 %)53Cobalt by the Nitroso-R-Salt Spectrophotometric Method (0.10 % to5.0 %)61Copper by Neocuproine Spectrophotometric Method (0.01 % to10.00 %)90Copper by the Sulfide
8、Precipitation-Electrodeposition GravimetricMethod (0.01 % to 10.00 %)71Iron by the Silver ReductionTitrimetric Method (1.0 % to 50.0 %) 192Manganese by the Periodate Spectrophotometric Method (0.05 % to2.00 %)9Molybdenum by the Ion Exchange8-Hydroxyquinoline Gravi-metric Method (1.5 % to 30 %)184Mol
9、ybdenum by the Spectrophotometric Method (0.01 % to 1.50 %) 153Nickel by the Dimethylglyoxime Gravimetric Method (0.1 % to84.0 %)135Phosphorus by the Molybdenum Blue Spectrophotometric Method(0.002 % to 0.08 %)19Silicon by the Gravimetric Method (0.05 % to 5.00 %) 46Sulfur by the Gravimetric Method
10、DiscontinuedSulfur by the Combustion-Iodate Titration Method (0.005 % to0.1 %)DiscontinuedSulfur by the Chromatographic Gravimetric MethodTin by the Solvent ExtractionAtomic Absorption Method (0.002 %to 0.10 %)1431.3 Methods for the determination of carbon and sulfur notincluded in this standard can
11、 be found in Test Methods E1019.1.4 Some of the composition ranges given in 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
12、 sections of eachmethod with the composition of the alloy to be analyzed.1.5 The values stated in SI units are to be regarded asstandard.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 e
13、stablish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific hazardsstatements are given in Section 6 and in special “Warning”paragraphs throughout these test methods.1These test methods are under the jurisdiction of ASTM Committ
14、ee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and are the directresponsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.Current edition approved Sept. 15, 2014. Published November 2014. Originallyapproved in 1968. Last previous edition approved in 2006 as E354 9
15、3 (2006).DOI: 10.1520/E0354-14.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States12. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data toDetermine Conforma
16、nce with SpecificationsE50 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 SpectrophotometryE135 Terminology Relating to Analytical Chemistry forMetals, Ores, a
17、nd Related MaterialsE173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Analysis of Metals (Withdrawn1998)3E350 Test Methods for Chemical Analysis of Carbon Steel,Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, andWrought IronE351 Test Methods for ChemicalAnalysis of C
18、ast IronAllTypesE352 Test Methods for ChemicalAnalysis of Tool Steels andOther Similar Medium- and High-Alloy SteelsE353 Test Methods for Chemical Analysis of Stainless,Heat-Resisting, Maraging, and Other Similar Chromium-Nickel-Iron AlloysE882 Guide for Accountability and Quality Control in theChem
19、ical Analysis 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 MethodE1806 Pract
20、ice for Sampling Steel and Iron for Determina-tion of Chemical Composition2.2 Other Document:ISO 5725 Precision of Test MethodsDetermination of Re-peatability and Reproducibility for Inter-Laboratory Tests43. Terminology3.1 For definitions of terms used in these test methods, referto Terminology E13
21、5.4. Significance and Use4.1 These test methods for the chemical analysis of metalsand alloys are primarily intended as referee methods to testsuch materials for compliance with compositionalspecifications, particularly those under the jurisdiction of theASTM Committee on Steel, Stainless Steel and
22、RelatedAlloys.It is assumed that all who use these test methods will be trainedanalysts capable of performing common laboratory proceduresskillfully and safely. It is expected that work will be performedin a properly equipped laboratory under appropriate qualitycontrol practices such as those descri
23、bed in Guide E882.5. Apparatus, Reagents, and Instrumental Practice5.1 ApparatusSpecialized apparatus requirements arelisted in the “Apparatus” Section in each method.5.2 Reagents:5.2.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended th
24、atall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available. Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening th
25、e accuracy ofthe determination.5.2.2 Purity of WaterUnless otherwise indicated, refer-ences to water shall be understood to mean reagent water asconforming to Type I or Type II of Specification D1193. TypeIII or IVmay be used if they effect no measurable change in theblank or sample.5.3 Spectrophoto
26、metric PracticeSpectrophotometricpractice prescribed in these test methods shall conform toPractice E60.6. Hazards6.1 For precautions to be observed in the use of certainreagents and equipment in these methods, refer to PracticesE50.7. Sampling7.1 For procedures for sampling the material, references
27、hall be made to Practice E1806.8. Interlaboratory Studies and Rounding CalculatedValues8.1 These test methods have been evaluated in accordancewith Practice E173 (withdrawn 1997) or ISO 5725. TheReproducibility R2 of Practice E173 corresponds to the Re-producibility Index R of Practice E1601. The Re
28、peatability R1of Practice E173 corresponds to the Repeatability Index r ofPractice E16018.2 Calculated values shall be rounded to the desired num-ber of places in accordance with the Rounding Method ofPractice E29.MANGANESE BY THE METAPERIODATESPECTROPHOTOMETRIC METHOD9. Scope9.1 This method covers
29、the determination of manganese incompositions from 0.05 % to 2.00 %.10. Summary of Method10.1 Manganous ions are oxidized to permanganate ions bytreatment with periodate. Tungsten when present at composi-tions greater than 0.5 % is kept in solution with H3PO4.2For referenced ASTM standards, visit th
30、e 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.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from A
31、merican National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.E354 142Solutions of the samples are fumed with HClO4so that theeffect of periodate is limited to the oxidation of manganese.Spectrophotometric measurements are made at approximately545 nm.1
32、1. Concentration Range11.1 The recommended concentration range is 0.15 mg 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 method has been written for cells having a 1-cm lightpath and a “narrow-band” instrume
33、nt. The concentration range dependsupon band width and spectral region used as well as cell optical pathlength. Cells having other dimensions may be used, provided suitableadjustments can be made in the amounts of sample and reagents used.12. Stability of Color12.1 The color is stable for at least 2
34、4 h.13. Interferences13.1 HClO4acid treatment, which is used in the procedure,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 colorquality upon treatment with metaperiodate i
35、on, the followingprecautions must be observed when filter spectrophotometersare used: Select a filter with maximum transmittance between545 nm and 565 nm.The filter must transmit not more than 5 %of its maximum at a wavelength shorter than 530 nm. The bandwidth of the filter should be less than 30 n
36、m when measured at50 % of its maximum transmittance. Similar restrictions applywith respect to the wavelength region employed when other“wide-band” instruments are used.13.2 The spectral transmittance curve of permanganate ionsexhibits two useful minima, one at approximately 526 nm, andthe other at
37、545 nm. The latter is recommended when a“narrow-band” spectrophotometer is used.13.3 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 containingmore than 0.5 % tungsten which eliminates
38、the problem bypreventing the precipitation of the tungsten.14. Reagents14.1 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 dissolve in 20 mL of HNO3by heating.Cool, dilut
39、e to volume, and mix. Using a pipet, transfer 20 mLto a 500-mL volumetric flask, dilute to volume, and mix.14.2 Nitric-Phosphoric Acid MixtureCautiously, whilestirring, add 100 mLof HNO3and 400 mLof H3PO4to 400 mLof water. Cool, dilute to 1 L, and mix. Prepare fresh as needed.14.3 Potassium Metaperi
40、odate Solution (7.5 g/L)Dissolve7.5 g of potassium metaperiodate (KIO4) in 200 mL of hotHNO3(1 + 1), add 400 mL of H3PO4, cool, dilute to 1 L, andmix.14.4 Water, Pretreated with MetaperiodateAdd 20 mL ofKIO4solution to 1 L of water, mix, heat at not less than 90Cfor 20 min to 30 min, and cool. Use t
41、his water to dilutesolutions to volume that have been treated with KIO4solutionto oxidize manganese, and thus avoid reduction of permangan-ate ions by any reducing agents in the untreated water.CautionAvoid the use of this water for other purposes.15. Preparation of Calibration Curve15.1 Calibration
42、 SolutionsUsing pipets, transfer 5 mL, 10mL, 15 mL, 20 mL, and 25 mLof manganese standard solution(1 mL = 0.032 mg Mn) to 50-mL borosilicate glass volumetricflasks, and, if necessary, dilute to approximately 25 mL.Proceed as directed in 15.3.15.2 Reference SolutionTransfer approximately 25 mL ofwate
43、r to a 50-mL borosilicate glass volumetric flask. Proceedas directed in 15.3.15.3 Color DevelopmentAdd 10 mL of KIO4solution,and heat the solutions at not less than 90C for 20 min to 30min (Note 2). Cool, dilute to volume with pretreated water, andmix.NOTE 2Immersing the flasks in a boiling water ba
44、th is a preferredmeans of heating them for the specified period to ensure complete colordevelopment.15.4 Spectrophotometry:15.4.1 Multiple-Cell SpectrophotometerMeasure the cellcorrection using the Reference Solution (15.2) in absorptioncells with a 1-cm light path and using a light band centered at
45、approximately 545 nm. Using the test cell, take the spectro-photometric readings of the calibration solutions versus theReference Solution (15.2)15.4.2 Single-Cell SpectrophotometerTransfer a suitableportion of the Reference Solution (15.2) to an absorption cellwith a 1-cm light path and adjust the
46、spectrophotometer to theinitial setting, using a light band centered at approximately 545nm. While maintaining this adjustment, take the spectrophoto-metric readings of the calibration solutions.15.5 Calibration CurveFollow the instrument manufac-turers instructions for generating the calibration cu
47、rve.16. Procedure16.1 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 50016.1.1 For Samples Containing Not More Than 0.5 %Tungsten:16.1.1.1
48、To dissolve samples that do not require HF, add 8mL 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 is complete, cool, then add 10 mL of HClO4;evaporate to fumes to oxidize chromium, if present, and toexpel HCl. Continue
49、 fuming until salts begin to separate. Cool,E354 143add 50 mL of water, and digest if necessary to dissolve thesalts. Cool and transfer the solution to a 100-mL volumetricflask. Proceed to 16.1.3.16.1.1.2 For samples whose dissolution is hastened by HF,add 8 mL to 10 mL of HCl (1 + 1), and heat. Add HNO3anda few drops of HF as needed to hasten dissolution, and then add3mLto4mLofHNO3. When dissolution is complete, cool,then add 10 mL or HClO4, evaporate to fumes to oxidizechromium, if present, and to expel HCl. Continue fuming untilsalts begin to separate
