1、Designation: E 350 95 (Reapproved 2005)e1Standard Test Methods forChemical Analysis of Carbon Steel, Low-Alloy Steel, SiliconElectrical Steel, Ingot Iron, and Wrought Iron1This standard is issued under the fixed designation E 350; the number immediately following the designation indicates the year o
2、foriginal 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 Department
3、 of Defense.e1NOTEEditorial changes were made throughout in June 2007.1. Scope1.1 These test methods cover the chemical analysis ofcarbon steels, low-alloy steels, silicon electrical steels, ingotiron, and wrought iron having chemical compositions withinthe following limits:Element Concentration Ran
4、ge, %Aluminum 0.001 to 1.50Antimony 0.002 to 0.03Arsenic 0.0005 to 0.10Bismuth 0.005 to 0.50Boron 0.0005 to 0.02Calcium 0.0005 to 0.01Cerium 0.005 to 0.50Chromium 0.005 to 3.99Cobalt 0.01 to 0.30Columbium (Niobium) 0.002 to 0.20Copper 0.005 to 1.50Lanthanum 0.001 to 0.30Lead 0.001 to 0.50Manganese 0
5、.01 to 2.50Molybdenum 0.002 to 1.50Nickel 0.005 to 5.00Nitrogen 0.0005 to 0.04Oxygen 0.0001 to 0.03Phosphorus 0.001 to 0.25Selenium 0.001 to 0.50Silicon 0.001 to 5.00Sulfur 0.001 to 0.60Tin 0.002 to 0.10Titanium 0.002 to 0.60Tungsten 0.005 to 0.10Vanadium 0.005 to 0.50Zirconium 0.005 to 0.151.2 The
6、test methods in this standard are contained in thesections indicated as follows:SectionsAluminum, Total, by the 8-Quinolinol Gravimetric Method (0.20to 1.5 %) 124131Aluminum, Total, by the 8-Quinolinol Photometric Method (0.003to 0.20 %) 7686Aluminum, Total or Acid-Soluble, by the Atomic AbsorptionM
7、ethod (0.005 to 0.20 %) 308317Antimony by the Brilliant Green Photometric Method (0.0002 to0.030 %) 142151Bismuth by the Atomic Absorption Method (0.02 to 0.25 %) 298307Boron by the Distillation-Curcumin Photometric Method (0.0003to 0.006 %) 208219Calcium by the Direct-Current Argon Plasma Optical E
8、missionSpectroscopy Method (0.0005 to 0.010 %) 289297Carbon, Total, by the Combustion Gravimetric Method (0.05 to1.80 %)Discontinued 1995Cerium and Lanthanum by the D-C Plasma Optical EmissionMethod (0.003 to 0.50 % Cerium, 0.001 to 0.30 % Lanthanum) 249257Chromium by the Atomic Absorption Method (0
9、.006 to 1.00 %) 220229Chromium by the Peroxydisulfate Oxidation-Titration Method(0.05 to 3.99 %) 230238Cobalt by the Nitroso-R Salt Photometric Method (0.01 to0.30 %) 5362Copper by the Atomic Absorption Method (0.004 to 0.5 %) 279288Copper by the Neocuproine Photometric Method (0.005 to1.50 %) 11412
10、3Lead by the Ion-ExchangeAtomic Absorption Method (0.001 to0.50 %) 132141Manganese by the Atomic Absorption Method (0.005 to 2.0 %) 269278Manganese by the Metaperiodate Photometric Method (0.01 to2.5 %) 8-17Manganese by the Peroxydisulfate-Arsenite Titrimetric Method(0.10 to 2.50 %) 164171Molybdenum
11、 by the Thiocyanate Photometric Method (0.01 to1.50 %) 152163Nickel by the Atomic Absorption Method (0.003 to 0.5 %) 318327Nickel by the Dimethylglyoxime Gravimetric Method (0.1 to5.00 %) 180187Nickel by the Ion-Exchange-AtomicAbsorption Method (0.005to 1.00 %) 188197Phosphorus by the Alkalimetric M
12、ethod (0.02 to 0.25 %) 172179Phosphorus by the Molybdenum Blue Photometric Method (0.003to 0.09 %) 18-29Silicon by the Molybdenum Blue Photometric Method (0.01 to0.06 %) 103113Silicon by the Gravimetric Titration Method (0.01 to 3.5 %) 4652Sulfur by the Combustion-Iodate Titration Method (0.005 to0.
13、3 %) 3745Tin by the Sulfide-Iodometric Titration Method (0.01 to 0.1 %) 95102Tin by the Solvent Extraction-Atomic Absorption Method (0.002to 0.10 %) 198207Titanium, Total, by the Diantipyrylmethane SpectrophotometricMethod (0.025 to 0.30 %) 258268Vanadium by the Atomic Absorption Method (0.006 to 0.
14、15 %) 2392481These 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.Current edition approved May 1, 2005. Published May 2005. Originallya
15、pproved in 1968. Last previous edition approved in 2000 as E 350 95 (2000)e1.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.1.3 Test methods for the determination of several elementsnot included in this standard can be found in Test
16、 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 therefore thisstandard contains multiple test methods for some elements.The user must select the proper test method by matching theinformation given in the Sco
17、pe and Interference sections ofeach test method with the composition of the alloy to beanalyzed.1.5 The values stated in SI units are to be regarded asstandard. In some cases, exceptions allowed in IEEE/ASTM SI10 are also used.1.6 This standard does not purport to address all of thesafety concerns,
18、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 “Warning”paragraphs th
19、roughout 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 Methods for Chemical Analysis of Steel, CastIron, Open-Hearth Iron, and Wrought Iron
20、3E50 Practices for Apparatus, Reagents, and Safety Consid-erations for ChemicalAnalysis of Metals, Ores and RelatedMaterialsE 60 Practice for Analysis of Metals, Ores, and RelatedMaterials by Molecular Absorption SpectrometryE 173 Practice for Conducting Interlaboratory Studies ofMethods for Chemica
21、l Analysis of Metals3E 319 Practice for the Evaluation of Single-Pan MechanicalBalancesE 351 Test Methods for Chemical Analysis of Cast IronAll TypesE 352 Test Methods for Chemical Analysis of Tool Steelsand Other Similar Medium- and High-Alloy SteelsE 353 Test Methods for Chemical Analysis of Stain
22、less,Heat-Resisting, Maraging, and Other Similar Chromium-Nickel-Iron AlloysE 354 Test Methods for Chemical Analysis of High-Temperature, Electrical, Magnetic, and Other Similar Iron,Nickel, and Cobalt AlloysE 882 Guide for Accountability and Quality Control in theChemical Analysis LaboratoryE 1019
23、Test Methods for Determination of Carbon, Sulfur,Nitrogen, and Oxygen in Steel and in Iron, Nickel, andCobalt AlloysE 1024 Guide for Chemical Analysis of Metals and Metal-Bearing Ores by Flame Atomic Absorption Spectropho-tometryE 1097 Guide for Direct Current Plasma Emission Spec-trometry AnalysisE
24、 1806 Practice for Sampling Steel and Iron for Determi-nation of Chemical CompositionIEEE/ASTM SI 10 Standard for Use of the InternationalSystem of Units (SI): The Modern Metric System2.2 ISO Standard:4ISO 5725 Precision of Test MethodsDetermination ofRepeatability and Reproducibility for Inter-Labo
25、ratoryTests3. 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 compositional specifica-tions, particularly those under the jurisdiction of ASTM Com-mittees A01 on Steel, Stainl
26、ess Steel, and Related Alloys andA04 on Iron Castings. It is assumed that all who use these testmethods will be trained analysts capable of performing com-mon laboratory procedures skillfully and safely. It is expectedthat work will be performed in a properly equipped laboratoryunder appropriate qua
27、lity control practices such as thosedescribed in Guide E 882.4. Apparatus, Reagents, and Instrumental Practices4.1 ApparatusSpecialized apparatus requirements arelisted in the “Apparatus” Section in each test method. In somecases reference may be made to Practices E50.4.2 Reagents:4.2.1 Purity of Re
28、agentsUnless otherwise indicated, allreagents used in these test methods shall conform to the reagentgrade specifications of the American Chemical Society.5Otherchemicals may be used, provided it is first ascertained that theyare of sufficiently high purity to permit their use withoutadversely affec
29、ting the expected performance of the determi-nation, as indicated in the Precision and Bias section.4.2.2 Purity of WaterUnless otherwise indicated, refer-ences to water shall be understood to mean reagent water asdefined by Type II of Specification D 1193.5. Hazards5.1 For precautions to be observe
30、d in the use of certainreagents and equipment in these test methods, refer to PracticesE50.6. Sampling6.1 For procedures for sampling the material, referenceshall be made to Practice E 1806.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at servi
31、ceastm.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, 11 West 42nd St., 13thFloor, New York, NY 10036.5Reagent Chemicals, American Chemical Society Specificati
32、ons , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention,
33、 Inc. (USPC), Rockville,MD.E 350 95 (2005)e127. 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 in accordance with the Rounding Method ofPractice E2
34、9.MANGANESE BY THE METAPERIODATEPHOTOMETRIC METHOD8. Scope8.1 This test method covers the determination of manganesein concentrations from 0.01 to 2.5 %.9. Summary of Test Method9.1 Manganous ions are oxidized to permanganate ions byreaction with metaperiodate ions. Solutions of the samples arefumed
35、 with perchloric acid so that the effect of metaperiodateion is limited to the oxidation of manganese. Photometricmeasurement is made at approximately 545 nm.10. Concentration Range10.1 The recommended concentration range is from 0.15 to0.8 mg of manganese per 50 mL of solution, using a 1-cm cell(No
36、te 1) and a spectrophotometer with a band width of 10 nmor less.NOTE 1This test method has been written for cells having a 1-cmlight path and a “narrow-band” instrument. The concentration rangedepends upon band width and spectral region used as well as cell opticalpath length. Cells having other dim
37、ensions 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. Interferences12.1 The elements ordinarily present do not interfere. Per-chloric acid treatment, which is used in the procedure
38、, 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 further change in color qualityupon treatment with metaperiodate ion, the following precau-tions must be observed when filter photometers are
39、used: Selecta filter with maximum transmittance between 545 and 565 nm.The filter must transmit not more than5%ofitsmaximum ata wavelength shorter than 530 nm. The band width of the filtershould be less than 30 nm when measured at 50 % of itsmaximum transmittance. Similar restrictions apply with re-
40、spect 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 recommended when a“narrow-band” spectrophotometer is used.13. R
41、eagents13.1 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. Using a pipet, transfer 20 mLto a 500-mL v
42、olumetric flask, dilute to volume, and mix.13.2 Nitric-Phosphoric Acid Mixture Cautiously, 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/L)Dissolve 7.5 g of potassium metaperiod
43、ate (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 solutions tovolume that have been treated with
44、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, transfer 5, 10,15, 20, and 25 mL of manganese
45、 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 volumetric flask. Proceedas directed in 14.3.14.
46、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 the specified period to ensure complete c
47、olordevelopment.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 photometricreadings of the calibration solut
48、ions 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 approximately 545 nm. Whilemaintaining this ad
49、justment, 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:15.1.1 Select and weigh a sample in accordance with thefollowing:E 350 95 (2005)e13Manganese,%SampleWeight,gTolerance inSample Weight,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 2.5 0.80 0.5 500 10Transfer the sample to a 100
