1、Designation: E 1019 08Standard Test Methods forDetermination of Carbon, Sulfur, Nitrogen, and Oxygen inSteel, Iron, Nickel, and Cobalt Alloys by VariousCombustion and Fusion Techniques1This standard is issued under the fixed designation E 1019; the number immediately following the designation indica
2、tes the year oforiginal adoption or, 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 t
3、he Department of Defense.1. Scope1.1 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 0.03
4、Arsenic 0.0005 to 0.10Beryllium 0.001 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 100.0Le
5、ad 0.001 to 0.50Magnesium 0.001 to 0.05Manganese 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
6、0.600Tantalum 0.001 to 10.00Tellurium 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 MeasurementTest Met
7、hod 10-20Nitrogen by the Inert Gas FusionThermal ConductivityTest Method32-42Oxygen by the Inert Gas Fusion Test Method 43-54Sulfur by the Combustion-Infrared Absorption Test Method(Calibration with Metal Reference Materials) 55-65Sulfur by the CombustionInfrared Absorption Test Method(Potassium Sul
8、fate Calibration) 21-311.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 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 sta
9、ndard 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 6.2. Referenced Documents2.1 ASTM Standards:3E29 Practice for Using Significant Digits in Test Data toDetermine Conform
10、ance with SpecificationsE50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE 135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE 173 Practice for Conducting Interlaboratory Studies ofMethod
11、s for Chemical Analysis of Metals4E 1601 Practice for Conducting an Interlaboratory Study to1These 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
12、Ferroalloys.Current edition approved Nov. 1, 2008. Published November 2008. Originallyapproved in 1984. Last previous edition approved in 2003 as E 1019 03.2Some of these test methods represent revisions of test methods covered by TestMethods E 350, E 351, E 352, E 353, and E 354, which appear in th
13、e Annual Bookof 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.4Withdrawn. The las
14、t approved version of this historical standard is referencedon www.astm.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.Evaluate the Performance of an Analytical MethodE 1806 Practice for Sampling Steel and Iron for Determi-natio
15、n of Chemical Composition3. Terminology3.1 For definition of terms used in this test method, refer toTerminology E 135.4. Significance and Use4.1 These test methods for the chemical analysis of metalsand alloys are primarily intended to test such materials forcompliance with compositional specificat
16、ions. It is 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
17、 determinationare 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 electrica
18、lshock.7. Sampling7.1 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 evaluate
19、d in accordancewith Practice E 173. The Reproducibility R2of Practice E 173corresponds to the Reproducibility Index R of Practice E 1601.The Repeatability R1of Practice E 173 corresponds to theRepeatability Index r of Practice E 1601.TOTAL CARBON BY THE COMBUSTIONINSTRUMENTAL MEASUREMENT TEST METHOD
20、10. Scope10.1 This test method covers 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 Test MethodThe carbon di-oxide is absorbed on a suitable
21、grade of zeolite, released byheating the zeolite, and swept by helium or oxygen into achromatographic column. Upon elution, the amount of carbondioxide is measured in a thermistor-type conductivity cell.Refer to Fig. 1.11.1.2 Infrared (IR) Absorption, Test Method ATheamount of carbon dioxide is meas
22、ured by infrared (IR)absorption. Carbon dioxide (CO2) absorbs IR energy at aprecise wavelength within the IR spectrum. Energy of thiswavelength is absorbed as the gas passes through a cell body inwhich the IR energy is transmitted. All other IR energy iseliminated from reaching the detector by a pre
23、cise wavelengthfilter. Thus, the absorption of IR energy can be attributed toonly CO2and its concentration is measured as changes inenergy at the detector. One cell is used as both a reference anda measure chamber. Total carbon, as CO2, is monitored andmeasured over a period of time. Refer to Fig. 2
24、.11.1.3 Infrared (IR) Absorption, Test Method BThe detec-tor consists of an IR energy source, a separate measurechamber and reference chamber, and a diaphragm acting as oneplate of a parallel plate capacitor. During specimen combus-tion, the flow of CO2with its oxygen gas carrier is routedthrough th
25、e measure chamber while oxygen alone passesthrough the reference chamber. Energy from the IR sourcepasses through both chambers, simultaneously arriving at thediaphragm (capacitor plate). Part of the IR energy is absorbedby the CO2present in the measure chamber while none isabsorbed passing through
26、the reference chamber. This createsan IR energy imbalance reaching the diaphragm, thus distort-ing it. This distortion alters the fixed capacitance creating anelectric signal change that is amplified for measurement asCO2. Total carbon, as CO2, is monitored and measured over aperiod of time. Refer t
27、o Fig. 3.11.1.4 Infrared (IR) Absorption, Test Method C, ClosedLoopThe combustion is performed in a closed loop, whereCO and CO2are 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 t
28、heabsence of CO and CO2, the energy received by each 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, asC
29、O2plus CO, is monitored and measured over a period of time.Refer to Fig. 4.11.2 This test method is written for use with commercialanalyzers, equipped to perform the above operations automati-cally and calibrated using steels of known carbon content.12. Interferences12.1 The elements ordinarily pres
30、ent do not interfere.13. Apparatus13.1 Combustion and Measurement ApparatusSee Figs.1-4.13.2 CruciblesUse crucibles that meet or exceed thespecifications of the instrument manufacturer and preheat in asuitable furnace for not less than 40 min at approximately1000 C. Remove from the furnace and cool
31、before use.Crucibles may be stored in a desiccator prior to use. Preheatingof crucibles is particularly important for low levels of carbon.It may not be required for the determination of higher levels ofcarbon such as those found in pig iron.E101908213.3 Crucible TongsCapable of handling recommended
32、crucibles.14. Reagents14.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are avai
33、lable.5Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.14.2 AcetoneThe residue after evaporation must be 0.0005 %.14.3 Copper (Low Carbon), granular (10 to 30 mesh) (Note1).1
34、4.4 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 andconsistent blank readings are obtained, or the oxygen may bepurified as described in Practices E50.14.6 Platinum or Platinized Silica, hea
35、ted to 350 C for theconversion of carbon monoxide to carbon dioxide.14.7 Sodium Hydroxide, on clay (known commercially asAscarite II).14.8 Tungsten (Low Carbon) Accelerator, 12 to 20 mesh(Note 1).14.9 Tungsten-Tin (Low Carbon) Accelerator,20to40mesh or 12 to 20 mesh.5Reagent Chemicals, American Chem
36、ical 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 Ltd., Poole, Dorset, U.K. (http:/), and the UnitedStates PharmacopeiaNational Formulary, U.S
37、. Pharmacopeial Convention, Inc.(USPC), Rockville, MD (http:/www.usp.org/USPNF).AHigh Purity Oxygen MCO2Collection TrapBOxygen Regulator (2 Stage) NFurnace Combustion ExhaustCSodium Hydroxide Impregnated Clay/Magnesium Perchlorate OFurnace Purge ExhaustDSecondary Pressure Regulator PMetal Connector
38、To Use Oxygen As Carrier GasEFlowmeter QHigh Purity HeliumFInduction Furnace RHelium Regulator (2 Stage)GCombustion Tube SChromagraphic ColumnHDust Trap TTC Cell/ReadoutIManganese Dioxide UMeasure FlowmeterJHeated CO to CO2Converter VReference FlowmeterKMagnesium Perchlorate WFurnace Power StatLValv
39、e Manifold* May be sealed chamber ifoxygen is carrier gas.* Not required if oxygen iscarrier gas.FIG. 1 Apparatus for Determination of Carbon by the Combustion Thermal Conductivity Test MethodE1019083NOTE 1The accelerator should contain no more than 0.001 % carbon.If necessary, wash three times with
40、 acetone by decantation to removeorganic contaminants and dry at room temperature. The mesh size iscritical to the inductive coupling which heats the sample. Some manufac-turers of accelerators may not certify the mesh size on a lot to lot basis.These accelerators may be considered acceptable for us
41、e without verifyingthe mesh size.15. Preparation of Apparatus15.1 Assemble the apparatus as recommended by the 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
42、-turers instructions. Make a minimum of two determinationsusing the specimen and accelerator as directed in 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 If necessary, w
43、ash in acetone or another suitablesolvent and dry.17. Calibration17.1 Calibration Reference Materials (Note 2):17.1.1 For Range I, 0.005 % to 0.10 % carbon, select threecertified reference materials containing approximately0.005 %, 0.05 %, and 0.10 % carbon and designate them asCalibrants A, B, and
44、C, respectively. Some labs may useaccelerator with a certified carbon value as Calibrant A.17.1.2 For Range II, 0.10 % to 1.25 % carbon, select twocertified reference materials containing approximately 0.12 %and 1.00 % carbon and designate them as Calibrants BB andCC, respectively.17.1.3 For Range I
45、II, 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 obtained using this test method isdependent on the uncertainty of the values assigned to th
46、e 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 Measurement System:17.2.1 Transfer 1.0 g of Calibrant B, weighed to the nearest1 mg, and
47、approximately 1.5 g of accelerator to a preheatedcrucible. Some manufacturers provide scoops that dispenseapproximately 1.5 g of accelerator. Once it is verified that thescoop delivers this approximate weight, it is acceptable to usethis device for routine dispensing of accelerator.17.2.2 Proceed as
48、 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 to provide a reading within6 0.003 of the certified percent carbon value for the certifiedreference material.17.3 Determination of Blank ReadingRange I:17.3.1 Add approximately 1.
49、5 g of accelerator into a pre-heated crucible. If required, 1.0 g of Calibrant A, weighed tothe nearest 1 mg, may be added to the crucible.17.3.2 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 (6 0.0002 % of carbon) readings are obtained.Blank values are equal to the total result of the accelerator. IfCalibrant A was used, blank values are equal to the total resultof the accelerator and Calibrant A minus the c
