1、Designation: E 1019 03Standard Test Methods forDetermination of Carbon, Sulfur, Nitrogen, and Oxygen inSteel and in Iron, Nickel, and Cobalt Alloys1This standard is issued under the fixed designation E 1019; 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 (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
3、 These test methods2cover the determination of carbon,sulfur, nitrogen, and oxygen, in steel and in iron, nickel, andcobalt alloys having chemical compositions within the follow-ing limits:Element Concentration Range, %Aluminum 0.001 to 18.00Antimony 0.002 to 0.03Arsenic 0.0005 to 0.10Beryllium 0.00
4、1 to 0.05Bismuth 0.001 to 0.50Boron 0.0005 to 1.00Cadmium 0.001 to 0.005Calcium 0.001 to 0.05Carbon 0.001 to 4.50Cerium 0.005 to 0.05Chromium 0.005 to 35.00Cobalt 0.01 to 75.0Columbium 0.002 to 6.00Copper 0.005 to 10.00Hydrogen 0.0001 to 0.0030Iron 0.01 to 100.0Lead 0.001 to 0.50Magnesium 0.001 to 0
5、.05Manganese 0.01 to 20.0Molybdenum 0.002 to 30.00Nickel 0.005 to 84.00Nitrogen 0.0005 to 0.50Oxygen 0.0005 to 0.03Phosphorus 0.001 to 0.90Selenium 0.001 to 0.50Silicon 0.001 to 6.00Sulfur (Metal ReferenceMaterials)0.002 to 0.35Sulfur (Potassium Sulfate) 0.001 to 0.600Tantalum 0.001 to 10.00Telluriu
6、m 0.001 to 0.35Tin 0.002 to 0.35Titanium 0.002 to 5.00Tungsten 0.005 to 21.00Vanadium 0.005 to 5.50Zinc 0.005 to 0.20Zirconium 0.005 to 2.5001.2 The test methods appear in the following order:SectionsCarbon, Total, by the CombustionInstrumental MeasurementMethod 10-20Nitrogen by the Inert Gas Fusion
7、Thermal Conductivity Method 32-42Oxygen by the Inert Gas Fusion Method 43-54Sulfur by the Combustion-Infrared Absorption Method (Calibrationwith Metal Reference Materials) 55-65Sulfur by the CombustionInfrared Absorption Method (PotassiumSulfate Calibration) 21-311.3 This standard does not purport t
8、o 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 the applica-bility of regulatory limitations prior to use. Specific hazardsstatements are given in Section 6.
9、2. Referenced Documents32.1 ASTM Standards:E29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE50 Practices for Apparatus, Reagents, and Safety Precau-tions for Chemical Analysis of MetalsE 135 Terminology Relating to Analytical Chemistry forMetals, Ore
10、s, and Related MaterialsE 1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE 1806 Practice for Sampling Steel and Iron for Determi-nation of Chemical CompositionE 173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Analysi
11、s of Metals3. Terminology3.1 For definition of terms used in this test method, refer toTerminology E 135.1These 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,
12、 Steel, and Ferroalloys.Current edition approved Oct. 1, 2003. Published November 2003. Originallyapproved in 1984. Last previous edition approved in 2002 as E 1019 02.2Some of these test methods represent revisions of test methods covered byASTM Methods E 350, E 351, E 352, E 353, and E 354 which a
13、ppear in the AnnualBook of ASTM Standards, Vol 03.05.3For 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 website.1Copyrig
14、ht ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4. Significance and Use4.1 These test methods for the chemical analysis of metalsand alloys are primarily intended to test such materials forcompliance with compositional specifications. It is
15、assumedthat all who use these test methods will be trained analysts,capable of performing common laboratory procedures skill-fully and safely. It is expected that work will be performed ina properly equipped laboratory.5. Apparatus and Reagents5.1 Apparatus and reagents required for each determinati
16、onare listed in separate sections preceding the procedure.6. Hazards6.1 For hazards to be observed in the use of certain reagentsin this test method, refer to Practices E50.6.2 Use care when handling hot crucibles and operatingfurnaces to avoid personal injury by either burn or electricalshock.7. Sa
17、mpling7.1 For procedures for sampling the materials, refer to thoseparts of Practice E 1806.8. Rounding Calculated Values8.1 Calculated values shall be rounded to the desired num-ber of places as directed in Practice E29.9. Interlaboratory Studies9.1 These test methods have been evaluated in accorda
18、ncewith Practice E 173 (discontinued 1997). The ReproducibilityR2of E 173 corresponds to the Reproducibility Index R ofE 1601. The Repeatability R1of E 173 corresponds to theRepeatability Index r of E 1601.TOTAL CARBON BY THE COMBUSTIONINSTRUMENTAL MEASUREMENT METHOD10. Scope10.1 This test method co
19、vers the determination of carbon inconcentrations from 0.005 % to 4.5 %.11. Summary of Test Method11.1 The carbon is converted to carbon dioxide by combus-tion in a stream of oxygen.11.1.1 Thermal Conductivity MethodThe carbon dioxideis absorbed on a suitable grade of zeolite, released by heatingthe
20、 zeolite, and swept by helium or oxygen into a chromato-graphic column. Upon elution, the amount of carbon dioxide ismeasured in a thermistor-type conductivity cell. Refer to Fig. 1.11.1.2 Infrared (IR) Absorption, Method A The amount ofcarbon dioxide is measured by infrared (IR) absorption. Car-bon
21、 dioxide (CO2) absorbs IR energy at a precise wavelengthwithin the IR spectrum. Energy of this wavelength is absorbedas the gas passes through a cell body in which the IR energy istransmitted. All other IR energy is eliminated from reachingthe detector by a precise wavelength filter. Thus, the absor
22、ptionof IR energy can be attributed to only CO2and its concentra-tion is measured as changes in energy at the detector. One cellis used as both a reference and a measure chamber. Totalcarbon, as CO2, is monitored and measured over a period oftime. Refer to Fig. 2.11.1.3 Infrared (IR) Absorption, Met
23、hod B The detectorconsists of an IR energy source, a separate measure chamberand reference chamber, and a diaphragm acting as one plate ofa parallel plate capacitor. During specimen combustion, theflow of CO2with its oxygen gas carrier is routed through themeasure chamber while oxygen alone passes t
24、hrough thereference chamber. Energy from the IR source passes throughboth chambers, simultaneously arriving at the diaphragm(capacitor plate). Part of the IR energy is absorbed by the CO2present in the measure chamber while none is absorbed passingthrough the reference chamber. This creates an IR en
25、ergyimbalance reaching the diaphragm, thus distorting it. Thisdistortion alters the fixed capacitance creating an electric signalchange that is amplified for measurement as CO2. Total carbon,as CO2, is monitored and measured over a period of time.Refer to Fig. 3.11.1.4 Infrared (IR) Absorption, Meth
26、od C, Closed LoopThe combustion is performed in a closed loop, where CO andCO2are detected in the same infrared cell. Each gas ismeasured with a solid state energy detector. Filters are used topass the appropriate IR wavelength to each detector. In theabsence of CO and CO2, the energy received by ea
27、ch detectoris maximum. During combustion, the IR absorption propertiesof CO and CO2gases in the chamber cause a loss of energy;therefore a loss in signal results which is proportional toconcentrations of each gas in the closed loop. Total carbon, asCO2plus CO, is monitored and measured over a period
28、 oftime. Refer to Fig. 4.11.2 This test method is written for use with commercialanalyzers, equipped to carry out the above operations automati-cally and calibrated using steels of known carbon content.12. Interferences12.1 The elements ordinarily present do not interfere.13. Apparatus13.1 Combustio
29、n and Measurement ApparatusSee Figs.1-4.13.2 CruciblesUse crucibles that meet or exceed thespecifications of those recommended by the manufacturer ofthe instrument used and preheat in a suitable furnace for notless than 40 min at more than 1000C. Remove from thefurnace and cool in air for 90 6 15 s
30、before use. Crucibles maybe placed in a desiccator for periods of 1 h prior to use.13.3 Crucible TongsCapable of handling recommendedcrucibles.14. Reagents14.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall confo
31、rm to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,E1019032where such specifications are available.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy
32、 of the determination.14.2 AcetoneThe residue after evaporation must be0.0005 %.14.3 Copper (Low Carbon), granular (10 to 30 mesh) (Note1).14.4 Magnesium Perchlorate, (known commercially as An-hydrone).14.5 Oxygen, Ultra High Purity (purity: 99.95 %minimum)Other grades of oxygen may be used if low a
33、ndconsistent blank readings are obtained, or the oxygen may bepurified as described in Practices E50.14.6 Platinum or Platinized Silica, heated to 350C for theconversion of carbon monoxide to carbon dioxide.14.7 Sodium Hydroxide, on clay (known commercially asAscarite II).14.8 Tungsten (Low Carbon),
34、 12 to 20 mesh (Note 1).14.9 Tungsten-Tin (Low Carbon), 20 to 40 mesh.NOTE 1The accelerator should contain no more than 0.001 % carbon.If necessary, wash three times with acetone by decantation to remove4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washingto
35、n, 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, Inc. (USPC), Rockville,MD.AHigh Purity O
36、xygen MCO2Collection TrapBOxygen Regulator (2 Stage) NFurnace Combustion ExhaustCSodium Hydroxide Impregnated Clay/Magnesium Perchlorate OFurnace Purge ExhaustDSecondary Pressure Regulator PMetal Connector To Use Oxygen As Carrier GasEFlowmeter QHigh Purity HeliumFInduction Furnace RHelium Regulator
37、 (2 Stage)GCombustion Tube SChromagraphic ColumnHDust Trap TTC Cell/ReadoutIManganese Dioxide UMeasure FlowmeterJHeated CO to CO2Converter VReference FlowmeterKMagnesium Perchlorate WFurnace Power StatLValve Manifold* May be sealed chamber ifoxygen is carrier gas.* Not required if oxygen iscarrier g
38、as.FIG. 1 Apparatus for Determination of Carbon by the Combustion Thermal Conductivity MethodE1019033organic contaminants and dry at room temperature. The mesh size iscritical to the inductive coupling which heats the sample.15. Preparation of Apparatus15.1 Assemble the apparatus as recommended by t
39、he manu-facturer.15.2 Test the furnace and analyzer to ensure the absence ofleaks and make the required electrical power connections.Prepare the analyzer for operation according to the manufac-turers instructions. Make a minimum of two determinationsusing the specimen and accelerator as directed in
40、18.1.2 and18.1.3 before attempting to calibrate the system or determinethe blank.16. Sample Preparation16.1 The sample should be uniform in size, but not finerthan 40 mesh.16.2 Wash in acetone and dry at 70 to 100C.17. Calibration17.1 Calibration Reference Materials (Note 2):17.1.1 For Range I, 0.00
41、5 % to 0.10 % carbon, select threecertified reference materials containing approximately0.005 %, 0.05 %, and 0.10 % carbon and designate them asCalibrants A, B, and C, respectively.17.1.2 For Range II, 0.10 % to 1.25 % carbon, select twocertified reference materials containing approximately 0.12 %an
42、d 1.00 % carbon and designate them as Calibrants BB andCC, respectively.17.1.3 For Range III, 1.25 % to 4.50 % carbon, select twocertified reference materials containing approximately 1.25 %and 4.00 % carbon and designate them as Calibrants BBB andCCC, respectively.NOTE 2The uncertainty of results o
43、btained using this test method isdependent on the uncertainty of the values assigned to the calibrationreference materials. The homogeneity of the reference materials must beconsidered as well, if it was not included in the derivation of the publisheduncertainty values.17.2 Adjustment of Response of
44、 Measurement System:17.2.1 Transfer 1.0 g of Calibrant B, weighed to the nearest1 mg, and 1.5 g of accelerator, weighed to the nearest 5 mg, toa preburned crucible.17.2.2 Proceed as directed in 18.1.2 and 18.1.3.17.2.3 Repeat 17.2.1 and 17.2.2 until the absence of drift isindicated.Adjust the signal
45、 to provide a reading within 60.003of the certified percent carbon value for the certified referencematerial.17.3 Determination of Blank ReadingRange I:17.3.1 Transfer 1.0 g of Calibrant A, weighed to the nearest1 mg, and 1.5 g of accelerator, weighed to the nearest 5 mg,into a preburned crucible.17
46、.3.2 Proceed as directed in 18.1.2 and 18.1.3.17.3.3 Repeat 17.3.1 and 17.3.2 a sufficient number of timesto establish that low (less than 0.002 % of carbon) andconsistent (60.0002 % of carbon) readings are obtained. Blankvalues are equal to the total result of the accelerator andCalibrant A minus t
47、he certified value for the certified referencematerial.17.3.4 Record the average value of at least three blankdeterminations.17.3.5 If the blank readings are too high or inconsistent,determine the cause, correct it, and repeat the steps as directedin 17.3.1-17.3.4.17.3.6 Enter the average blank valu
48、e in the analyzer (Note3); refer to manufacturers instructions. This mechanism willelectronically compensate for the blank value.NOTE 3If the unit does not have this function, the blank value mustbe subtracted from the total result prior to any calculation.17.4 Determination of Blank ReadingRange II
49、Proceedas directed in 17.3.17.5 Determination of Blank ReadingRange III:17.5.1 Transfer 0.5 g of Calibrant A, weighed to the nearest1 mg, and 1.5 g of accelerator, weighed to the nearest 5 mg, toa preburned crucible.17.5.2 Proceed as directed in 17.3.2-17.3.6.17.6 CalibrationRange I (0.005 % to 0.10 % carbon):17.6.1 Weigh four 1.0 g specimens of Calibrant C, to thenearest 1 mg, the place in preburned crucibles. To each, add 1.5g of accelerator, weighed to the nearest 5 mg.17.6.2 Follow the calibration procedure recommended bythe manuf
