1、Designation: E 351 93 (Reapproved 2006)Standard Test Methods forChemical Analysis of Cast IronAll Types1This standard is issued under the fixed designation E 351; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last rev
2、ision. 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 Department of Defense.1. Scope1.1 These test methods2cover the chemical analys
3、is of pigiron, gray cast iron (including alloy and austenitic), white castiron, malleable cast iron, and ductile (nodular3) iron havingchemical compositions within the following limits:Element Concentration Range, %Aluminum40.003 to 0.50Antimony 0.005 to 0.03Arsenic40.02 to 0.10Bismuth40.001 to 0.03
4、Boron40.001 to 0.10Cadmium40.001 to 0.005Carbon 1.25 to 4.50Cerium40.005 to 0.05Chromium 0.01 to 30.00Cobalt40.01 to 4.50Copper 0.03 to 7.50Lead40.001 to 0.15Magnesium 0.002 to 0.10Manganese 0.06 to 2.50Molybdenum 0.01 to 5.00Nickel 0.01 to 36.00Phosphorus 0.01 to 0.90Selenium40.001 to 0.06Silicon 0
5、.10 to 6.0Sulfur 0.005 to 0.25Tellurium40.001 to 0.35Tin40.001 to 0.35Titanium40.001 to 0.20Tungsten40.001 to 0.20Vanadium40.005 to 0.50Zinc40.005 to 0.201.2 The test methods in this standard are contained in thesections indicated below:SectionsCarbon, Graphitic, by the Direct Combustion Gravimetric
6、 Method (1to 3 %) 108Carbon, Total by the Combustion Gravimetric Method (1.25 to4.50 %) 97Cerium and Lanthanum by the D-C Plasma Optical EmissionMethod (Ce: 0.003 to 0.5 %; La: 0.001 to 0.30 %) 237Chromium by the Atomic Absorption Method (0.006 to 1.00 %) 208Chromium by the Peroxydisulfate Oxidation
7、Titration Method(0.006 to 1.00 %) 218Chromium by the Peroxydisulfate-Oxidation Titrimetric Method (0.05to 30.0 %)4aCobalt by the Ion-ExchangePotentiometric Titration Method (2.0 to4.5 %) 53Cobalt by the Nitroso-R-Salt Photometric Method (0.01 to 4.50 %) 61Copper by the Neocuproine Photometric Method
8、 (0.03 to 7.5 %) 116Copper by the Sulfide Precipitation-Electrodeposition GravimetricMethod (0.03 to 7.5 %) 81Lead by the Ion-ExchangeAtomic Absorption Method (0.001 to0.15 %) 126Magnesium by the Atomic Absorption Method (0.002 to 0.10 %) 71Manganese by the Periodate Photometric Method (0.10 to 2.00
9、 %) 8Manganese by the Peroxydisulfate-Arsenite Titrimetric Method (0.10to 3.5 %) 152Molybdenum by the Ion Exchange8-Hydroxyquinoline GravimetricMethod 257Molybdenum by the Photometric Method (0.01 to 1.5 %) 196Nickel by the Dimethylglyoxime Gravimetric Method (0.1 to36.00 %) 168Nickel by the Ion Exc
10、hange-Atomic Absorption Method (0.005 to1.00 %) 176Phosphorus by the Alkalimetric Method (0.02 to 0.90 %) 160Phosphorus by the Molybdenum Blue Photometric Method (0.02 to0.90 %) 18Silicon by the Gravimetric Method (0.1 to 6.0 %) 46Sulfur by the Gravimetric Method 30Sulfur by the Combustion-Iodate Ti
11、tration Method (0.005 to 0.25 %) 37Sulfur by the Chromatographic Gravimetric Method4bTin by the Solvent Extraction-Atomic Absorption Method (0.002 to0.10 %) 186Tin by the Sulfide-Iodometric Titration Method (0.01 to 0.35 %) 89Titanium, Total, by the Diantipyrylmethane SpectrophotometricMethod (0.006
12、 to 0.35 %) 246Vanadium by the Atomic Absorption Method (0.006 to 0.15 %) 2271.3 Procedures for the determination of several elements notincluded in these test methods can be found in Test MethodsE30and Test Methods E 1019.1.4 Some of the concentration ranges given in 1.1 are toobroad to be covered
13、by a single method and therefore thisstandard contains multiple methods for some elements. The1These 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
14、 Ferroalloys.Current edition approved June 1, 2006. Published June 2006. Originallyapproved in 1968. Last previous edition approved in 2000 as E 351 93 (2000)e1.2These test methods represent revisions of methods covered by Test MethodsE30, which appear in this publication. Typical alloy specificatio
15、n numbers for thiscategory are listed in the Appendix.3As typified by compositions listed in Cast Metals Handbook, 1957, pp.196197.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.user must select the proper method by matching the inf
16、orma-tion given in the Scope and Interference 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. In some cases, exceptions allowed in Practice E 380are also used.1.6 This standard does not purport to address all of
17、 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 5 and in special “
18、Warning”paragraphs throughout these Methods.2. Referenced Documents2.1 ASTM Standards:4D 1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE30 Test Methods for Chemical Analysis of Steel, CastIron, Open-Hearth Iron,
19、and Wrought Iron.5E50 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 SpectrometryE 173 Practice for Conducting Interlaboratory Studies ofM
20、ethods for Chemical Analysis of Metals5E 350 Test Methods for ChemicalAnalysis of Carbon Steel,Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, andWrought IronE 352 Test Methods for Chemical Analysis of Tool Steelsand Other Similar Medium- and High-Alloy SteelsE 353 Test Methods for Chemical A
21、nalysis of Stainless,Heat-Resisting, Maraging, and Other Similar Chromium-Nickel-Iron AlloysE 380 Practice for Use of the International System of Units(SI) (Modernized Metric System)5E 882 Guide for Accountability and Quality Control in theChemical Analysis LaboratoryE 1019 Test Methods for Determin
22、ation of Carbon, Sulfur,Nitrogen, and Oxygen in Steel and in Iron, Nickel, andCobalt AlloysE 1024 Guide for Chemical Analysis of Metals and MetalBearing Ores by Flame Atomic Absorption Spectropho-tometry6E 1806 Practice for Sampling Steel and Iron for Determi-nation of Chemical Composition2.2 Other
23、Document:ISO 5725 Precision of Test MethodsDetermination ofRepeatability and Reproducibility for Inter-LaboratoryTests73. Significance 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 compo
24、sitional specifica-tions, particularly those under the jurisdiction of ASTM Com-mittee A04 on Iron Castings. It is assumed that all who usethese test methods will be trained analysts capable of perform-ing common laboratory procedures skillfully and safely. It isexpected that work will be performed
25、in a properly equippedlaboratory under appropriate quality control practices such asthose described in Guide E 882.4. Apparatus, Reagents, and Instrumental Practices4.1 ApparatusSpecialized apparatus requirements arelisted in the Apparatus section in each method. In some casesreference may be made t
26、o Practices E50.4.2 Reagents:4.2.1 Purity of ReagentsUnless otherwise indicated, allreagents used in these test methods shall conform to theReagent Grade Specifications of the American Chemical Soci-ety.8Other chemicals may be used, provided it is first ascer-tained that they are of sufficiently hig
27、h purity to permit theiruse without adversely affecting the expected performance ofthe determination, as indicated in the section on “Precision andBias.”4.2.2 Purity of WaterUnless otherwise indicated, refer-ences to water shall be understood to mean reagent water asdefined by Type II of Specificati
28、on 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 For procedures for sampling the materia
29、l, 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 in 3.4 to 3.6 of Practice E29.4For refer
30、enced ASTM 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.5Withdrawn.6Withdrawn.7Available from American National Standards Insti
31、tute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.8Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH
32、Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.E 351 93 (2006)2MANGANESE BY THE METAPERIODATEPHOTOMETRIC METHOD8. Scope8.1 This test method covers the determination of manganesein concentrations from 0.10
33、to 2.00 %.9. Summary of Method9.1 Manganous ions are oxidized to permanganate ions byreaction with metaperiodate ions. Solutions of the samples arefumed with perchloric acid so that the effect of metaperiodateion is limited to the oxidation of manganese. Photometricmeasurement is made at approximate
34、ly 545 nm.10. 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 band width of 10 nmor less.NOTE 1This method has been written for cells having a 1-cm lightpath and a narrow-band in
35、strument. 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.11. Stability of Color11.1 The color is stable for at l
36、east 24 h.12. Interferences12.1 The elements ordinarily present do not interfere. Per-chloric acid treatment, which is used in the procedure, yieldssolutions which can be highly colored due to the presence of Cr(VI) ions. Although these ions and other colored ions in thesample solution undergo no fu
37、rther change in color qualityupon treatment with metaperiodate ion, the following precau-tions must be observed when filter photometers are used: Selecta filter with maximum transmittance between 545 and 565 nm.The filter must transmit not more than 5 % of its maximum ata wavelength shorter than 530
38、 nm. The band width of the filtershould be less than 30 nm when measured at 50 % of itsmaximum transmittance. Similar restrictions apply with re-spect to the wavelength region employed when other wide-band instruments are used.12.2 The spectral transmittance curve of permanganate ionsexhibits two us
39、eful minima, one at approximately 526 nm, andthe other at 545 nm. The latter is recommended when anarrow-band spectrophotometer is used.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
40、 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 MixtureCautiously, whilestirring, add 100 mL of HNO3and 400 mL of H3PO4to 400mL of water
41、. 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 MetaperiodateAdd 20 mL ofKIO4solution to 1
42、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 untreated water. WarningAvoidthe use of this wate
43、r 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 approximately 25 mL.Proceed as directed in 1
44、4.3.14.2 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). Cool, dilute to volume with pretreated wate
45、r, 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 Solution (14.2) in absorption cellswith a 1-cm
46、 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 Solution (14.2) to an absorption cell with a
47、1-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 readingsof the calibration solutions agains
48、t milligrams of manganeseper 50 mL of solution.15. Procedure15.1 Test Solution:15.1.1 Select and weigh a sample in accordance with thefollowing:E 351 93 (2006)3Maganese,%SampleWeight, gTolerance inSample Weight,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 500Tran
49、sfer it to a 300-mL Erlenmeyer flask.15.1.2 To dissolve samples that do not require HF, add 8 to10 mLof 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 volumetricflask as indicated in 15.1.1. Proceed to 15.1.4.15
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