1、Designation: E 353 93 (Reapproved 2006)Standard Test Methods forChemical Analysis of Stainless, Heat-Resisting, Maraging,and Other Similar Chromium-Nickel-Iron Alloys1This standard is issued under the fixed designation E 353; the number immediately following the designation indicates the year oforig
2、inal 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.1. Scope1.1 These test methods2cover the chemical analysis ofstainless, he
3、at-resisting, maraging, and other similarchromium-nickel-iron alloys having chemical compositionswithin the following limits:Element Concentration 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 15.00Columbium (Niobium) 0.01 to 4.00Copper 0.01
4、 to 5.00Lead 0.001 to 0.50Manganese 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 1.0
5、0Zirconium 0.001 to 0.201.2 The test methods in this standard are contained in thesections indicated below:SectionsAluminum, Total, by the 8-Quinolinol Gravimetric Method (0.20 to7.00 %)119Aluminum, Total, by the 8-Quinolinol Photometric Method (0.003 to0.20 %)71Carbon, Total, by the CombustionTherm
6、al Conductivity Method2aCarbon, Total, by the Combustion Gravimetric Method (0.05 to1.50 %)98Chromium by the Atomic Absorption Method (0.006 to 1.00 %) 202SectionsChromium by the Peroxydisulfate OxidationTitration Method (0.10to 35.00 %)212Chromium by the Peroxydisulfate-Oxidation Titrimetric Method
7、2bCobalt by the Ion-ExchangePotentiometric Titration Method (2 to15. %)53Cobalt by the Nitroso-R-Salt Photometric Method (0.01 to 5.0 %) 61Copper by the Neocuproine Photometric Method (0.01 to 5.00) %) 109Copper by the Sulfide Precipitation-Electrodeposition GravimetricMethod (0.01 to 5.00 %)82Lead
8、by the Ion-ExchangeAtomic Absorption Method (0.001 to0.50 %)127Manganese by the Periodate Photometric Method (0.01 to 5.00 %) 8Molybdenum by the Ion Exchange8-Hydroxyquinoline GravimetricMethod242Molybdenum by the Photometric Method (0.01 to 1.50 %) 190Nickel by the Dimethylglyoxime Gravimetric Meth
9、od (0.1 to 48.0 %) 172Phosphorus by the Alkalimetric Method (0.02 to 0.35 %) 164Phosphorus by the Molybdenum Blue Photometric Method (0.002 to0.35 %)18Silicon by the Gravimetric Method (0.05 to 4.00 %) 46Sulfur by the Gravimetric Method2cSulfur by the Combustion-Iodate Titration Method (0.005 to 0.5
10、 %) 37Sulfur by the Chromatographic Gravimetric Method2bTin by the Solvent ExtractionAtomic Absorption Method (0.002 to0.10 %)180Tin by the Sulfide-Iodometric Titration Method (0.01 to 0.05 %) 90Titanium, Total, by the Diantipyrylmethane SpectrophotometricMethod (0.01 to 0.35 %)231Vanadium by the At
11、omic Absorption Method (0.006 to 0.15 %) 2211.3 Test methods for the determination of several elementsnot included in this standard can be found in Test Methods E30and Test Methods E 1019.1.4 Some of the concentration ranges given in 1.1 are toobroad to be covered by a single test method and therefo
12、re thisstandard contains multiple test methods for 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 ass
13、tandard. 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 appro-priate safety and health practices and determine
14、 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 Subcommittee E01.01 on Iron, Steel, and Ferroalloys.Curre
15、nt edition approved June 1, 2006. Published June 2006. Originallyapproved in 1968. Last previous edition approved in 2000 as E 353 93 (2000)e1.2These test methods represent revisions of methods covered by ASTM MethodsE30andE38which appear in this publication.1Copyright ASTM International, 100 Barr H
16、arbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.statements are given in Section 5 and in special “Warning”paragraphs throughout these test methods.2. Referenced Documents2.1 ASTM Standards:3D 1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in T
17、est Data toDetermine Conformance with SpecificationsE30 Test Methods for Chemical Analysis of Steel, CastIron, Open-Hearth Iron, and Wrought Iron4E50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE60 Practice for Analysis of
18、Metals, Ores, and RelatedMaterials by Molecular Absorption SpectrometryE 173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Analysis of Metals4E 350 Test Methods for ChemicalAnalysis of Carbon Steel,Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, andWrought IronE 351 T
19、est Methods for Chemical Analysis of Cast IronAll TypesE 352 Test Methods for Chemical Analysis of Tool Steelsand Other Similar Medium- and High-Alloy SteelsE 354 Test Methods for Chemical Analysis of High-Temperature, Electrical, Magnetic, and Other Similar Iron,Nickel, and Cobalt AlloysE 380 Pract
20、ice for Use of the International System of Units(SI)4E 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 of M
21、etals and MetalBearing Ores by Flame Atomic Absorption Spectropho-tometry5E 1806 Practice for Sampling Steel and Iron for Determi-nation of Chemical Composition2.2 Other Document:ISO 5725 Precision of Test MethodsDetermination ofRepeatability and Reproducibility for Inter-LaboratoryTests63. Signific
22、ance and Use3.1 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 A1 on Steel, Stainless Steel, and Related A
23、lloys. It isassumed 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 described in G
24、uide E 882.4. Apparatus, Reagents, and Instrumental Practices4.1 ApparatusSpecialized apparatus requirements arelisted in the “Apparatus” Section in each method. In somecases reference may be made to Practices E50.4.2 Reagents:4.2.1 Purity of ReagentsUnless otherwise indicated, allreagents used in t
25、hese test methods shall conform to the“Reagent Grade” Specifications of the American ChemicalSociety.7Other 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, as
26、 indicated in the section on “Precisionand Bias.”4.2.2 Purity of Water Unless 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 prescribed in thesetest methods shall conform to Practice
27、 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 For procedures for sampling the material, referenceshall be made to Practice E 1806.7. Interlaboratory Studies and Rounding CalculatedValues7.1 These t
28、est 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 in 3.4 to 3.6 of Practice E29.MANGANESE BY THE META PERIODATEPHOTOMETRIC METHOD8. Scope8.1 This method covers the determination of manganese inconcentra
29、tions from 0.01 to 5.00 %.9. Summary of 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 with perchloric acid3For referenced A
30、STM standards, 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.4Withdrawn.5Withdrawn.6Available from American National Standards Institute (A
31、NSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.7“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 N
32、ostrand Co., Inc., New York, NY, and the “United StatesPharmacopeia,” United States Pharmacopeial Convention, Rockville, MD 20852.E 353 93 (2006)2so that the effect of periodate is limited to the oxidation ofmanganese. Photometric measurement is made at approxi-mately 545 nm.10. Concentration Range1
33、0.1 The recommended concentration range is 0.15 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 “narrow-band” instrument. The concentration
34、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.11. Stability of Color11.1 The color is stable for at least 24 h.12. Interferences1
35、2.1 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 colorquality upon treatment with metaperiodate ion, the follow
36、ingprecautions 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 bandwidth of the filter should be less than 30 nm when measured at50 %
37、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 at approximately 526 nm, andthe other at 545 nm. The latter is r
38、ecommended 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 containingmore than 0.5 % tungsten which eliminates the problem bypreventin
39、g 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 dissolve in 20 mL of HNO3by heating.Cool, dilute to volume, and mix. U
40、sing 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. Prepare fresh asneeded.13.3 Potassium Metaperiodate Solution (7.5 g/
41、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 than 90Cfor 20 to 30 min, and cool. Use this water to dilute solut
42、ions 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 of Calibration Curve14.1 Calibration SolutionsUsing pipets, tra
43、nsfer 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 approximately 25 mL ofwater to a 50-mL borosilicate glass volumet
44、ric 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). Cool, dilute to volume with pretreated water, andmix.NOTE 2Immersing the flasks in a boiling water bath is a preferredmeans of heating them for
45、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 centered atapproximately 545 nm. Using the test cell, take the pho
46、tometricreadings 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 photometer to the initial setting,using a light band centered at appro
47、ximately 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 solution.15. Procedure15.1 Test Solution Select and weigh a sam
48、ple 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.15.1.1 To dissolve samples tha
49、t do not require HF, add 8 to10 mL of HCl (1 + 1), and heat.Add HNO3as needed to hastendissolution, and then add 3 to 4 mLin excess. When dissolutionis complete, cool, then add 10 mL of HClO4; evaporate tofumes to oxidize chromium, if present, and to expel HCl.Continue fuming until salts begin to separate. Cool, add 50 mLof water, and digest if necessary to dissolve the salts. Cool andtransfer the solution to either a 100- or 500-ml volumetric flaskas indicated in 6.1. Proceed to 15.2.2.E 353 93 (2006)315.2 For samples whose dissolution is hastened by H
