1、Designation: E352 93 (Reapproved 2006)E352 13Standard Test Methods forChemical Analysis of Tool Steels and Other Similar Medium-and High-Alloy Steels1This standard is issued under the fixed designation E352; 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.1. Scope1.1 These test methods cover the chemical analysis of tool steels and other similar m
3、edium- and high-alloy steels havingchemical compositions within the following limits:Element Concentration Range, %Element Composition Range, %Aluminum 0.005 to 1.5Boron 0.001 to 0.10Carbon 0.03 to 2.50Chromium 0.10 to 14.0Cobalt 0.10 to 14.0Copper 0.01 to 2.0Lead 0.001 to 0.01Manganese 0.10 to 15.0
4、0Molybdenum 0.01 to 10.00Nickel 0.02 to 4.00Nitrogen 0.001 to 0.20Phosphorus 0.002 to 0.05Silicon 0.10 to 2.50Sulfur 0.002 to 0.40Tungsten 0.01 to 21.00Vanadium 0.02 to 5.501.2 The test methods in this standard are contained in the sections indicated below:SectionsCarbon, Total, by the CombustionThe
5、rmalConductivity Method2aCarbon, Total, by the Combustion GravimetricalMethod (0.05 to 2.50 %) 78Chromium by the Atomic Absorption Method (0.006 to 1.00 %) 174Chromium by the PeroxydisulfateOxidationTitration Method (0.10 to 14.00 %) 184Chromium by the Peroxydisulfate-OxidationTitrimetric Method 2 b
6、Cobalt by the Ion-ExchangePotentiometricTitration Method (2 to 14 %) 52Cobalt by the Nitroso-R-SaltPhotometricMethod (0.10 to 5.0 %) 60Copper by the NeocuproinePhotometric Method (0.01 to 2.00 %) 89Copper by the Sulfide Precipitation-Electrodeposition Gravimetric Method (0.01 to 2.0 %) 70Lead by the
7、 Ion-ExchangeAtomicAbsorptionMethod (0.001 to 0.001 %) 99Nickel by the DimethylglyoximeGravimetricMethod (0.1 to 4.0 %) 1441 These test methods are under the jurisdiction of the ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and are the directresponsibility of Sub
8、committee E01.01 on Iron, Steel, and Ferroalloys.Current edition approved June 1, 2006Feb. 1, 2013. Published June 2006May 2013. Originally approved in 1968. Last previous edition approved in 20002006 as E352 93(2000)(2006).1. DOI: 10.1520/E0352-93R06.10.1520/E0352-13.This document is not an ASTM st
9、andard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all ca
10、ses only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1SectionsManganese by the PeriodatePhotometricMethod (0.10 to 5.00 %) 8Molybdenu
11、m by the Ion Exchange8-Hydro-xyquinoline Gravimetric Method 203Molybdenum by the Photometric Method (0.01 to 1.50 %) 162Phosphorus by the Alkalimetric Method (0.01 to 0.05 %) 136Phosphorus by the Molybdenum BluePhoto-metric Method (0.002 to 0.05 %) 18Silicon by the Gravimetric Method (0.10 to 2.50 %
12、) 45Sulfur by the Gravimetric Method2cSulfur by the Combustion-IodateTitrationMethod (0.005 to 0.4 %) 36Sulfur by the Chromatographic GravimetricMethod 2bTin by the Solvent ExtractionAtomicAbsorp-tion Method (0.002 to 0.10 %) 152Vanadium by the AtomicAbsorption Method (0.006 to 0.15 %) 193SectionsCa
13、rbon, Total, by the CombustionThermal Conductivity MethodDiscontinued 1986Carbon, Total, by the Combustion GravimetricalMethodDiscontinuedChromium by the Atomic Absorption Method (0.006 % to 1.00 %) 174Chromium by the PeroxydisulfateOxidationTitrationMethod (0.10 % to 14.00 %) 184Chromium by the Per
14、oxydisulfate-OxidationTitrimetric MethodDiscontinued 1980Cobalt by the Ion-ExchangePotentiometric Titration Method (2 % to 14 %) 52Cobalt by the Nitroso-R-SaltSpectrophotometric Method (0.10 % to 5.0 %) 60Copper by the NeocuproineSpectrophotometric Method (0.01 % to 2.00 %) 89Copper by the Sulfide P
15、recipitation-Electrodeposition Gravimetric Method (0.01 % to 2.0 %) 70Lead by the Ion-ExchangeAtomicAbsorptionMethod (0.001 % to 0.01 %) 99Nickel by the DimethylglyoximeGravimetricMethod (0.1 % to 4.0 %) 144Manganese by the PeriodateSpectrophotometric Method (0.10 % to 5.00 %) 8Molybdenum by the Ion
16、 Exchange8-Hydroxyquinoline Gravimetric Method 203Molybdenum by the Spectrophotometric Method (0.01 % to 1.50 %) 162Phosphorus by the Alkalimetric Method (0.01 % to 0.05 %) 136Phosphorus by the Molybdenum BlueSpectrophotometric Method (0.002 % to 0.05 %) 18Silicon by the Gravimetric Method (0.10 % t
17、o 2.50 %) 45Sulfur by the GravimetricMethodDiscontinued 1988Sulfur by the Combustion-IodateTitrationMethodDiscontinuedSulfur by the ChromatographicGravimetric MethodDiscontinued 1980Tin by the Solvent ExtractionAtomicAbsorption Method (0.002 % to 0.10 %) 152Vanadium by the AtomicAbsorption Method (0
18、.006 % to 0.15 %) 1931.3 Test methods for the determination of several elements carbon and sulfur not included in this standard can be found in TestMethods E30 and Test Methods E1019.E352 1321.4 Some of the concentrationcomposition ranges given in 1.1 are too broad to be covered by a single test met
19、hod and thereforethis standard 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 of each test method with the composition of the alloy to be analyzed.1.5 The values stated in SI units
20、are to be regarded as standard. In some cases, exceptions allowed in Practice E380 are alsoused.1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health p
21、ractices and determine the applicability of regulatorylimitations prior to use. Specific hazards statements are given in Section 56 and in special “Warning” paragraphs throughout thesetest methods.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE29 Practice for Using
22、Significant Digits in Test Data to Determine Conformance with SpecificationsE30 Test Methods for Chemical Analysis of Steel, Cast Iron, Open-Hearth Iron, and Wrought Iron (Withdrawn 1995)4E50 Practices forApparatus, Reagents, and Safety Considerations for ChemicalAnalysis of Metals, Ores, and Relate
23、d MaterialsE60 Practice for Analysis of Metals, Ores, and Related Materials by SpectrophotometryE135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related MaterialsE173 Practice for Conducting Interlaboratory Studies of Methods for Chemical Analysis of Metals (Withdrawn 1998)3E3
24、50 Test Methods for Chemical Analysis of Carbon Steel, Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, and WroughtIronE351 Test Methods for Chemical Analysis of Cast IronAll TypesE353 Test Methods for Chemical Analysis of Stainless, Heat-Resisting, Maraging, and Other Similar Chromium-Nickel-
25、IronAlloysE380 Practice for Use of the International System of Units (SI) (the Modernized Metric System) (Withdrawn 1997)4E882 Guide for Accountability and Quality Control in the Chemical Analysis LaboratoryE1019 Test Methods for Determination of Carbon, Sulfur, Nitrogen, and Oxygen in Steel, Iron,
26、Nickel, and Cobalt Alloys byVarious Combustion and Fusion TechniquesE1024 Guide for Chemical Analysis of Metals and Metal Bearing Ores by Flame Atomic Absorption Spectrophotometry(Withdrawn 2004)3E1806 Practice for Sampling Steel and Iron for Determination of Chemical Composition2.2 Other Document:4
27、ISO 5725 Precision of Test MethodsDetermination of Repeatability and Reproducibility for Inter-Laboratory Tests3. Terminology3.1 For definitions of terms used in these test methods, refer to Terminology E135.4. Significance and Use4.1 These test methods for the chemical analysis of metals and alloys
28、 are primarily intended as referee methods to test suchmaterials for compliance with compositional specifications particularly those under the jurisdiction of ASTM Committee A1 onSteel, Stainless Steel, and Related Alloys. It is assumed that all who use these test methods will be trained analysts ca
29、pable ofperforming common laboratory procedures skillfully and safely. It is expected that work will be performed in a properly equippedlaboratory under appropriate quality control practices such as those described in Guide E882.5. Apparatus, Reagents, and Instrumental Practices5.1 ApparatusSpeciali
30、zed apparatus requirements are listed in the “Apparatus” Section in each method. In some casesreference may be made to Practices E50.5.2 Reagents:5.2.1 Purity of ReagentsUnless otherwise indicated, all reagents used in these test methods shall conform to the “ReagentGrade” Specifications of the Amer
31、ican Chemical Society.5 Other chemicals may be used, provided it is first ascertained that they2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document
32、 Summary page on the ASTM website.3 The last approved version of this historical standard is referenced on www.astm.org.4 Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.5 “Reagent Chemicals,American Chemical Society Spec
33、ifications,”Am.American Chemical Soc.,Society, Washington, DC. For suggestions on the testing of Reagents notlisted by the American Chemical Society, see“ Reagent Chemicals and Standards,” by Joseph Rosin, D. Van Nostrand Co., Inc., New York, NY, and see the “United StatesPharmacopeia.” United State
34、s United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Rockville, MD 20852.Inc. (USPC), Rockville, MD.E352 133are of sufficiently high purity to permit their use without adversely affecting the expected performance of the determination, asindicated in the section on “Pre
35、cision and Bias.”5.2.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water as defined byType conforming to Type I or Type II of Specification D1193. Type III or IV may be used if they effect no measurable change inthe blank or sample.5.3 Photometr
36、icSpectrophotometric PracticePhotometricSpectrophotometric practice prescribed in these test methods shallconform to Practice E60.6. Hazards6.1 For precautions to be observed in the use of certain reagents and equipment in these methods, refer to Practices E50.7. Sampling7.1 For procedures for sampl
37、ing the material, reference shall be made to Practice E1806.8. Interlaboratory Studies and Rounding Calculated Values8.1 These test methods have been evaluated using in accordance with Practice E173 or ISO 5725. (withdrawn 1997) or ISO5725. The Reproducibility R2 of E173 corresponds to the Reproduci
38、bility Index R of E1601. The Repeatability R1 of E173corresponds to the Repeatability Index r of E1601.8.2 Calculated values shall be rounded to the desired number of places as directed in 3.4 to 3.6in accordance with the RoundingMethod of Practice E29.MANGANESE BY THE METAPERIODATEPHOTOMETRIC METHO
39、DMANGANESE BY THE METAPERIODATE SPECTROPHOTOMETRIC METHOD9. Scope9.1 This method covers the determination of manganese in concentrationscompositions from 0.10 % to 5.00 %.5.00 %.10. Summary of Method10.1 Manganous ions are oxidized to permanganate ions by treatment with periodate. Tungsten when pres
40、ent at concentra-tionscompositions greater than 0.5 % 0.5 % is kept in solution with phosphoric acid. Solutions of the samples are fumed withperchloricHClO4 acid so that the effect of periodate is limited to the oxidation of manganese. PhotometricSpectrophotometricmeasurement is made at approximatel
41、y 545 nm.11. Concentration Range11.1 The recommended concentration range is 0.15 mg to 0.8 mg of manganese per 50 mL of solution, using a 1-cm cell (Note1) and a spectrophotometer with a band width of 10 nm or less.NOTE 1This method has been written for cells having a 1-cm light path and a “narrow-b
42、and” instrument. The concentration range depends upon bandwidth and spectral region used as well as cell optical path length. Cells having other dimensions may be used, provided suitable adjustments can be madein the amounts of sample and reagents used.12. Stability of Color12.1 The color is stable
43、for at least 24 h.13. Interferences13.1 PerchloricHClO4 acid treatment, 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 colored ions in the sample solution undergo no further change in colorquality upon tr
44、eatment with metaperiodate ion, the following precautions must be observed when filter photometers are used:Select a filter with maximum transmittance between 545 nm and 565 nm. The filter must transmit not more than 5 % of itsmaximum at a wavelength shorter than 530 nm. The band width of the filter
45、 should be less than 30 nm when measured at 50 %of its maximum transmittance. Similar restrictions apply with respect to the wavelength region employed when other“ wide-band”instruments are used.13.2 The spectral transmittance curve of permanganate ions exhibits two useful minima, one at approximate
46、ly 526 nm, and theother at 545 nm. The latter is recommended when a “narrow-band” spectrophotometer is used.E352 13413.3 Tungsten, when present in amounts of more than 0.5 % interferes by producing a turbidity in the final solution. A specialprocedure is provided for use with samples containing more
47、 than 0.5 % tungsten which eliminates the problem by preventing theprecipitation of the tungsten.14. Reagents14.1 Manganese, Standard Solution (1 mL = 0.032 mg Mn)Transfer the equivalent of 0.4000 g of assayed, high-puritymanganese (purity: 99.99 % minimum), to a 500-mL volumetric flask and dissolve
48、 in 20 mL of HNO3 by heating. Cool, dilute tovolume, and mix. Using a pipet, transfer 20 mL to a 500-mL volumetric flask, dilute to volume, and mix.14.2 Nitric-Phosphoric Acid MixtureCautiously, while stirring, add 100 mL of HNO3 and 400 mL of H3PO4 to 400 mL ofwater. Cool, dilute to 1 L, and mix. P
49、repare fresh as needed.14.3 Potassium Metaperiodate Solution (7.5 g/L)Dissolve 7.5 g of potassium metaperiodate (KIO4) in 200 mL of hot HNO3(1 + 1), add 400 mL of H3PO4, cool, dilute to 1 L, and mix.14.4 Water, Pretreated with MetaperiodateAdd 20 mL of KIO4 solution to 1 L of water, mix, heat at not less than 90C 90C for 20 min to 30 min, and cool. Use this water to dilute solutions to volume that have been treated with KIO4 solution to oxidizemanganese, and thus avoid reduction of permanganate ions by any reducing agents in the untreated water
