1、Designation: E350 12Standard Test Methods forChemical Analysis of Carbon Steel, Low-Alloy Steel, SiliconElectrical Steel, Ingot Iron, and Wrought Iron1This standard is issued under the fixed designation E350; the number immediately following the designation indicates the year oforiginal adoption or,
2、 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 Department of Defense.1. Scope1.1
3、 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 Composition Range, %Aluminum 0.001 to 1.50Antimony 0.002 to 0.03Arsenic 0.0005 to 0.10Bismuth 0.00
4、5 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 0.01 to 2.50Molybdenum 0.002 to 1.50Nickel 0.005 to 5.00Nitrogen 0.0005 to 0.04Oxyge
5、n 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 test methods in this standard are contained in thesections indicated as follows:Sec
6、tionsAluminum, Total, by the 8-Quinolinol Gravimetric Method(0.20 % to 1.5 %) 124131Aluminum, Total, by the 8-Quinolinol SpectrophotometricMethod (0.003 % to 0.20 %) 7686Aluminum, Total or Acid-Soluble, by the Atomic AbsorptionSpectrometry Method (0.005 % to 0.20 %) 308317Antimony by the Brilliant G
7、reen SpectrophotometricMethod (0.0002 % to 0.030 %) 142151Bismuth by the Atomic Absorption SpectrometryMethod (0.02 % to 0.25 %) 298307Boron by the Distillation-Curcumin SpectrophotometricMethod (0.0003 % to 0.006 %) 208219Calcium by the Direct-Current Argon Plasma AtomicEmission Spectroscopy Method
8、 (0.0005 % to 0.010 %) 289297Carbon, Total, by the Combustion Gravimetric Method(0.05 % to1.80 %)Discontinued 1995Cerium and Lanthanum by the Direct Current PlasmaAtomic Emission Spectrometry Method(0.003 % to 0.50 % Cerium, 0.001 % to 0.30 % Lanthanum) 249257Chromium by the Atomic Absorption Spectr
9、ometryMethod (0.006 % to 1.00 %) 220229Chromium by the Peroxydisulfate Oxidation-TitrationMethod (0.05 % to 3.99 %) 230238Cobalt by the Nitroso-R Salt SpectrophotometricMethod (0.01 % to 0.30 %) 5362Copper by the Atomic Absorption SpectrometryMethod (0.004 % to 0.5 %) 279288Copper by the Neocuproine
10、 SpectrophotometricMethod (0.005 % to 1.50 %) 114123Lead by the Ion-ExchangeAtomic Absorption SpectrometryMethod (0.001 % to 0.50 %) 132141Manganese by the Atomic Absorption SpectrometryMethod (0.005 % to 2.0 %) 269278Manganese by the Metaperiodate SpectrophotometricMethod (0.01 % to 2.5 %) 9-18Mang
11、anese by the Peroxydisulfate-Arsenite TitrimetricMethod(0.10 % to 2.50 %) 164171Molybdenum by the Thiocyanate SpectrophotometricMethod (0.01 % to 1.50 %) 152163Nickel by the Atomic Absorption SpectrometryMethod (0.003 % to 0.5 %) 318327Nickel by the Dimethylglyoxime GravimetricMethod (0.1 % to 5.00
12、%) 180187Nickel by the Ion-Exchange-Atomic-Absorption SpectrometryMethod (0.005 % to 1.00 %) 1881971These 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, Stee
13、l, and Ferroalloys.Current edition approved Aug. 15, 2012. Published September 2012. Originallyapproved in 1968. Last previous edition approved in 2005 as E350 95 (2005)1.DOI: 10.1520/E0350-12.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United
14、 States.Phosphorus by the Alkalimetric Method(0.02 % to 0.25 %) 172179Phosphorus by the Molybdenum Blue SpectrophotometricMethod (0.003 % to 0.09 %) 19-30Silicon by the Molybdenum Blue SpectrophotometricMethod (0.01 % to 0.06 %) 103113Silicon by the Gravimetric TitrationMethod (0.05 % to 3.5 %) 4652
15、Sulfur by the Combustion-Iodate Titration Method(0.005 % to 0.3 %) 3745Tin by the Sulfide-Iodometric TitrationMethod (0.01 % to 0.1 %) 95102Tin by the Solvent Extraction-Atomic Absorption SpectrometryMethod(0.002 % to 0.10 %) 198207Titanium, Total, by the Diantipyrylmethane SpectrophotometricMethod
16、(0.025 % to 0.30 %) 258268Vanadium by the Atomic Absorption SpectrometryMethod (0.006 % to 0.15 %) 2392481.3 Test methods for the determination of several elementsnot included in this standard can be found in Test MethodsE1019.1.4 Some of the composition ranges given in 1.1 are toobroad to be covere
17、d 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 Scope and Interference sections ofeach test method with the composition of the alloy to beanalyzed.1.5 The values
18、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, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate
19、 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.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE29
20、 Practice for Using Significant Digits in Test Data toDetermine Conformance 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 Spectrophotom
21、etryE135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Analysis of Metals3E319 Practice for the Evaluation of Single-Pan MechanicalBalancesE351 Test Methods for Chemical Analysis of Cast
22、IronAll TypesE352 Test Methods for Chemical Analysis of Tool Steelsand Other Similar Medium- and High-Alloy SteelsE353 Test Methods for Chemical Analysis of Stainless,Heat-Resisting, Maraging, and Other Similar Chromium-Nickel-Iron AlloysE354 Test Methods for Chemical Analysis of High-Temperature, E
23、lectrical, 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,Nitrogen, and Oxygen in Steel, Iron, Nickel, and CobaltAlloys by Various Combustion and Fusi
24、on TechniquesE1024 Guide for Chemical Analysis of Metals and MetalBearing Ores by Flame Atomic Absorption Spectropho-tometry3E1097 Guide for Determination of Various Elements byDirect Current Plasma Atomic Emission SpectrometryE1806 Practice for Sampling Steel and Iron for Determina-tion of Chemical
25、 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-LaboratoryTests3. Terminology3.1 For definitions of terms used in these test
26、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 compositional specifica-tions, particularly those under the jurisdiction of ASTM Com-mitte
27、es A01 on Steel, Stainless 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 laborato
28、ryunder appropriate quality control practices such as thosedescribed in Guide E882.5. Apparatus, Reagents, and Instrumental Practices5.1 ApparatusSpecialized apparatus requirements arelisted in the “Apparatus” Section in each test method.5.2 Reagents:5.2.1 Purity of ReagentsUnless otherwise indicate
29、d, allreagents used in these test methods shall conform to the reagent2For referenced 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
30、 website.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.E350 122grade specifications of the American Chemical Society.5Otherc
31、hemicals may be used, provided it is first ascertained that theyare of sufficiently high purity to permit their use withoutadversely affecting the expected performance of the determi-nation, as indicated in the Precision and Bias section.5.2.2 Purity of WaterUnless otherwise indicated, refer-ences t
32、o water shall be understood to mean reagent water asconforming to Type I or Type II of Specification D1193. TypeIII or IV may be used if they effect no measurable change in theblank or sample.6. Hazards6.1 For precautions to be observed in the use of certainreagents and equipment in these test metho
33、ds, refer to PracticesE50.7. 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 evaluated using PracticeE173 or ISO 5725.8.2 Calculated values shall be rounded to the
34、desired num-ber of places in accordance with the Rounding Method ofPractice E29.MANGANESE BY THE METAPERIODATESPECTROPHOTOMETRIC METHOD9. Scope9.1 This test method covers the determination of manganesein compositions from 0.01 % to 2.5 %.10. Summary of Test Method10.1 Manganous ions are oxidized to
35、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. Spectrophotomet-ric measurement is made at approximately 545 nm.11. Concentration Range11.1 The recommended co
36、ncentration range is from 0.15mg to 0.8 mg of manganese per 50 mL of solution, using a1-cm cell (Note 1) and a spectrophotometer with a band widthof 10 nm or less.NOTE 1This test method has been written for cells having a 1-cmlight path and a “narrow-band” instrument. The concentration rangedepends
37、upon band width and spectral region used as well as cell opticalpath length. 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 24 h.13. Interferences13.1 The eleme
38、nts 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 further change in color qualityupon treatme
39、nt with metaperiodate ion, the following precau-tions must be observed when filter spectrophotometers areused: Select a filter with maximum transmittance between 545nm and 565 nm. The filter must transmit not more than5%ofits maximum at a wavelength shorter than 530 nm. The bandwidth of the filter s
40、hould be less 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 5
41、26 nm, andthe other at 545 nm. The latter is recommended when a“narrow-band” spectrophotometer is used.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 dis
42、solve 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.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. P
43、repare fresh asneeded.14.3 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 1L, and mix.14.4 Water, Pretreated with MetaperiodateAdd 20 mL ofKIO4solution to 1 L of water, mix, heat at not less
44、 than 90 Cfor 20 min to 30 min, and 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. P
45、reparation of Calibration Curve15.1 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 15.3.15.2 Reference Solut
46、ionTransfer approximately 25 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 90 C for 20 min to 30min (Note 2). Cool, dilute to volume with pretreated water, andmix.5Reagent
47、Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC, www.chemistry.org. For suggestions on thetesting of reagents not listed by the American Chemical Society, see the UnitedStates Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention,Inc. (USPC)
48、, Rockville, MD, http:/www.usp.org.E350 123NOTE 2Immersing the flasks in a boiling 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 S
49、olution (15.2) in absorptioncells with a 1-cm light path and using a light band centered atapproximately 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 spectrophotometer to theinitial setting, using a light band centered at approximately 545nm. While maintaining this adjustment, take the spectr
