1、Designation: E353 14Standard Test Methods forChemical Analysis of Stainless, Heat-Resisting, Maraging,and Other Similar Chromium-Nickel-Iron Alloys1This standard is issued under the fixed designation E353; the number immediately following the designation indicates the year oforiginal adoption or, in
2、 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.1. Scope1.1 These test methods cover the chemical analysis ofstainless, heat-resisting, maragin
3、g, and other similarchromium-nickel-iron alloys having chemical compositionswithin the following limits:Element Composition Range, %Aluminum 0.002 to 5.50Boron 0.001 to 0.20Carbon 0.01 to 1.50Chromium 0.01 to 35.00Cobalt 0.01 to 15.00Niobium 0.01 to 4.00Copper 0.01 to 5.00Lead 0.001 to 0.50Manganese
4、 0.01 to 20.00Molybdenum 0.01 to 7.00Nickel 0.01 to 48.00Nitrogen 0.001 to 0.50Phosphorus 0.002 to 0.35Selenium 0.01 to 0.50Silicon 0.01 to 4.00Sulfur 0.002 to 0.50Tantalum 0.01 to 0.80Tin 0.001 to 0.05Titanium 0.01 to 4.50Tungsten 0.01 to 4.50Vanadium 0.005 to 1.00Zirconium 0.001 to 0.201.2 The tes
5、t methods in this standard are contained in thesections indicated below:SectionsAluminum, Total, by the 8-QuinolinolGravimetric Method (0.20 % to7.00 %)119Aluminum, Total, by the 8-QuinolinolSpectrophotometric Method (0.003 %to 0.20 %)71Carbon, Total, by theCombustionThermal ConductivityMethodDiscon
6、tinuedCarbon, Total, by the CombustionGravimetric Method (0.05 % to1.50 %)DiscontinuedChromium by the Atomic AbsorptionMethod (0.006 % to 1.00 %)202SectionsChromium by the PeroxydisulfateOxidationTitration Method (0.10 %to 35.00 %)212Chromium by the Peroxydisulfate-Oxidation Titrimetric MethodDiscon
7、tinuedCobalt by the Ion-ExchangePotentiometric TitrationMethod(2%to15%)53Cobalt by the Nitroso-R-SaltSpectrophotometric Method (0.01 %to 5.0 %)61Copper by the NeocuproineSpectrophotometric Method (0.01 %to 5.00) %)109Copper by the Sulfide Precipitation-Electrodeposition Gravimetric Method(0.01 % to
8、5.00 %)82Lead by the Ion-Exchange-AtomicAbsorption Method (0.001 % to0.50 %)127Manganese by the PeriodateSpectrophotometric Method (0.01 %to 5.00 %)8Molybdenum by the Ion Exchange8-Hydroxyquinoline Gravimetric Method242Molybdenum by the SpectrophotometricMethod (0.01 % to 1.50 %)190Nickel by the Dim
9、ethylglyoximeGravimetric Method (0.1 % to 48.0 %)172Phosphorus by the Alkalimetric Method(0.02 % to 0.35 %)164Phosphorus by the Molybdenum BlueSpectrophotometric Method (0.002 %to 0.35 %)18Silicon by the Gravimetric Method (0.05%to4.00%)46Sulfur by the Gravimetric Method DiscontinuedSulfur by the Co
10、mbustion-IodateTitration Method (0.005 % to 0.5 %)DiscontinuedSulfur by the ChromatographicGravimetric MethodDiscontinuedTin by the Solvent ExtractionAtomicAbsorption Method (0.002 % to0.10 %)180Tin by the Sulfide-Iodometric TitrationMethod (0.01 % to 0.05 %)90Titanium, Total, by theDiantipyrylmetha
11、neSpectrophotometric Method (0.01 %to 0.35 %)231Vanadium by the Atomic AbsorptionMethod (0.006 % to 0.15 %)2211.3 Test methods for the determination of carbon and sulfurnot included in this standard can be found in Test MethodsE1019.1These test methods are under the jurisdiction of ASTM Committee E0
12、1 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 E353 93 (20
13、06).DOI: 10.1520/E0353-14.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States11.4 Some of the composition ranges given in 1.1 are toobroad to be covered by a single test method and therefore thisstandard contains multiple test methods for
14、 some elements.The user must select the proper test method by matching theinformation given in the Scope and Interference sections ofeach method 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 addr
15、ess all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish 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
16、 special “Warning”paragraphs throughout these test methods.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE50 Practices for Apparatus, Reagents, and Safety Consid-eratio
17、ns 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, and Related MaterialsE173 Practice for Conducting Interlaboratory Studies ofMethods for
18、 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 Cast IronAllTypesE352 Test Methods for ChemicalAnalysis of Tool Steels andOther Similar
19、 Medium- and High-Alloy SteelsE354 Test Methods for Chemical Analysis of High-Temperature, Electrical, Magnetic, and Other Similar Iron,Nickel, and Cobalt AlloysE882 Guide for Accountability and Quality Control in theChemical Analysis LaboratoryE1019 Test Methods for Determination of Carbon, Sulfur,
20、Nitrogen, and Oxygen in Steel, Iron, Nickel, and CobaltAlloys by Various Combustion and Fusion TechniquesE1024 Guide for Chemical Analysis of Metals and MetalBearing Ores by Flame Atomic Absorption Spectropho-tometry (Withdrawn 2004)3E1601 Practice for Conducting an Interlaboratory Study toEvaluate
21、the Performance of an Analytical MethodE1806 Practice for Sampling Steel and Iron for Determina-tion of Chemical Composition2.2 Other Document:ISO 5725 Precision of Test MethodsDetermination ofRepeatability and Reproducibility for Inter-LaboratoryTests43. Terminology3.1 For definitions of terms used
22、 in these test methods, referto Terminology E135.4. 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 ofAS
23、TM Committee A1 on Steel, Stainless Steel, and RelatedAlloys. It is assumed that all who use these test methods willbe trained analysts capable of performing common laboratoryprocedures skillfully and safely. It is expected that work will beperformed in a properly equipped laboratory under appropria
24、tequality control practices such as those described in GuideE882.5. Apparatus, Reagents, and Instrumental Practices5.1 ApparatusSpecialized apparatus requirements arelisted in the “Apparatus” Section in each method.5.2 Reagents:5.2.1 Purity of ReagentsUnless otherwise indicated, allreagents used in
25、these test methods shall conform to the“Reagent Grade” Specifications of the American ChemicalSociety.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 determination, a
26、s indicated in the Precision and Biassection.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.
27、3 Spectrophotometric 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 PracticesE50.2For referenced ASTM standards, visit the ASTM websit
28、e, 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 American Natio
29、nal Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, www.ansi.org.5“Reagent Chemicals, American Chemical Society Specifications,” AmericanChemical Society, Washington, DC. For suggestions on the testing of Reagents notlisted by the American Chemical Society, see the United S
30、tates Pharmacopeia andNational Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.E353 1427. Sampling7.1 For procedures for sampling the material, referenceshall be made to Practice E1806.8. Interlaboratory Studies and Rounding CalculatedValues8.1 These test methods have been evalu
31、ated in accordancewith Practice E173 (withdrawn 1997) or ISO 5725. Thereproducibility R2 of Practice E173 corresponds to the repro-ducibility index R of Practice E1601. The repeatability R1 ofPractice E173 corresponds to the repeatability index r ofPractice E1601.8.2 Calculated values shall be round
32、ed to the desired num-ber of places in accordance with the rounding method ofPractice E29.MANGANESE BY THE META PERIODATESPECTROPHOTOMETRIC METHOD9. Scope9.1 This method covers the determination of manganese incompositions from 0.01 % to 5.00 %.10. Summary of Method10.1 Manganous ions are oxidized t
33、o permanganate ions bytreatment with periodate. Tungsten when present at composi-tions greater than 0.5 % is kept in solution with H3PO4.Solutions of the samples are fumed with HClO4so that theeffect of periodate is limited to the oxidation of manganese.Spectrophotometric measurement is made at appr
34、oximately545 nm.11. Composition Range11.1 The recommended composition range is 0.15 mg to 0.8mg of manganese per 50 mL of solution, using a 1-cm cell (seeNote 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 “narr
35、ow-band” instrument. The composition 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
36、 for at least 24 h.13. Interferences13.1 HClO4treatment, 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 metap
37、eriodate ion, 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
38、 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.13.2 The spectral transmittance curve of permanganate ionsexhibits two useful minima, one at approximately 526 nm, andthe
39、 other at 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 e
40、liminates 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.C
41、ool, dilute 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 mL of HNO3and 400 mL of H3PO4to 400mL of water. Cool, dilute to 1 L, and mix. Prepare fresh asneeded.14.3 Potassi
42、um Metaperiodate 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
43、cool. Use this 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
44、Calibration 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
45、 mL ofwater 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 boilin
46、g water bath 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 c
47、entered atE353 143approximately 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 p
48、ath and adjust the 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
49、 the calibration curve.16. Procedure16.1 Test Solution Select and weigh a sample in accor-dance with the following:Manganese, %SampleWeight, gTolerance inSampleWeight, mgDilution,mLAliquotVolume, mL0.01 to 0.5 0.80 0.5 100 200.45 to 1.0 0.35 0.3 100 200.85 to 2.0 0.80 0.5 500 201.95 to 5.0 0.80 0.5 500 10Transfer it to a 300-mL Erlenmeyer flask.16.1.1 To dissolve samples that do not require HF, add 8 mLto 10 mL of HCl (1 + 1), and heat. Add HNO3as needed tohasten dissolution, and then add 3 mLto 4 mLin excess. Whendissolution is complete, cool, then add
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