ASTM E1019-2011 6250 Standard Test Methods for Determination of Carbon Sulfur Nitrogen and Oxygen in Steel Iron Nickel and Cobalt Alloys by Various Combustion and Fusion Techniques.pdf

1、Designation: E1019 11Standard 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 E1019; the number immediately following the designation indicate

2、s 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.1. Scope1.1 These test methods cover the determination of

3、carbon,sulfur, nitrogen, and oxygen, in steel, iron, nickel, and cobaltalloys having chemical compositions within the followinglimits:Element Concentration Range, %Aluminum 0.001 to 18.00Antimony 0.002 to 0.03Arsenic 0.0005 to 0.10Beryllium 0.001 to 0.05Bismuth 0.001 to 0.50Boron 0.0005 to 1.00Cadmi

4、um 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 75.0Niobium 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 0.05Manganese 0.01 to 20.0Molybdenum 0.002 to 30.00Nickel

5、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 10.00Tellurium 0.001 to 0.35Tin 0.002 to 0.35Titanium 0.002 to 5.00Tun

6、gsten 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 Method 10-20Nitrogen by the Inert Gas FusionThermal ConductivityTest Method32-42Oxygen by the In

7、ert 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 Sulfate Calibration) 21-311.3 The values stated in SI units are to be regarded asstandard. No ot

8、her 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 standard to establish appro-priate safety and health practices and determine the applica-bility

9、of regulatory limitations prior to use. Specific hazardsstatements are given in Section 6.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE50 Practices for Apparatus, Rea

10、gents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Analysis of Metals3E1601 Practice for Condu

11、cting an Interlaboratory Study toEvaluate the Performance of an Analytical Method1These 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

12、.Current edition approved March 15, 2011. Published June 2011. Originallyapproved in 1984. Last previous edition approved in 2008 as E1019 08. DOI:10.1520/E1019-11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Boo

13、k of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. The last 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, U

14、nited States.E1806 Practice for Sampling Steel and Iron for Determina-tion of Chemical Composition3. Terminology3.1 For definition of terms used in this test method, refer toTerminology E135.4. Significance and Use4.1 These test methods for the chemical analysis of metalsand alloys are primarily int

15、ended to test such materials forcompliance with compositional specifications. 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 laborato

16、ry.5. Apparatus and Reagents5.1 Apparatus and reagents required for each 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 an

17、d operatingfurnaces to avoid personal injury by either burn or electricalshock.7. Sampling7.1 For procedures for sampling the materials, refer to thoseparts of Practice E1806.8. Rounding Calculated Values8.1 Calculated values shall be rounded to the desired num-ber of places as directed in Practice

18、E29.9. Interlaboratory Studies9.1 These test methods have been evaluated in accordancewith Practice E173. The Reproducibility R2of Practice E173corresponds to the Reproducibility Index R of Practice E1601.The Repeatability R1of Practice E173 corresponds to theRepeatability Index r of Practice E1601.

19、TOTAL CARBON BY THE COMBUSTIONINSTRUMENTAL MEASUREMENT TEST METHOD10. 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 Cond

20、uctivity Test MethodThe carbon di-oxide is absorbed on a suitable 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

21、 (IR) Absorption, Test Method ATheamount of carbon dioxide is measured 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. Al

22、l other IR energy iseliminated from reaching the detector by a precise 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 CO

23、2, is monitored andmeasured over a period of time. Refer to Fig. 2.11.1.3 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-ti

24、on, the flow of CO2with its oxygen gas carrier is routedthrough the 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 CO2pre

25、sent in the measure chamber while none isabsorbed passing through 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 carbo

26、n, as CO2, is monitored and measured over aperiod of time. Refer to 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 ar

27、e used topass the appropriate IR wavelength to each detector. In theabsence of CO and CO2, the energy received by each detectoris at its maximum. During combustion, the IR absorptionproperties of CO and CO2gases in the chamber cause a loss ofenergy; therefore a loss in signal results which is propor

28、tionalto concentrations of each gas in the closed loop. Total carbon,as CO2plus CO, is monitored and measured over a period oftime. 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 o

29、f known carbon content.12. Interferences12.1 For the scope of elements typically found in materialsto be tested by this method refer to 1.1.13. Apparatus13.1 Combustion and Measurement ApparatusSee Figs.1-4.13.2 CruciblesUse crucibles that meet or exceed thespecifications of the instrument manufactu

30、rer and prepare thecrucibles by heating in a suitable furnace for not less than 40min at approximately 1000 C. Remove from the furnace andcool before use. Crucibles may be stored in a desiccator priorto use. Heating of crucibles is particularly important whenanalyzing for low levels of carbon and ma

31、y not be required ifthe material to be analyzed has higher levels of carbon such asE1019 112that found in pig iron. Above certain concentrations, asdetermined by the testing laboratory, the nontreatment ofcrucibles will have no adverse effect. The analytical ranges forthe use of untreated crucibles

32、shall be determined by the testinglaboratory and supporting data shall be maintained on file tovalidate these ranges.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 int

33、ended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use wit

34、hout lessening theaccuracy of the determination.14.2 AcetoneThe residue after evaporation shall be30), t may be set equal to 2 at the 95 %confidence level. At its discretion, the laboratory may choose to set asmaller range for the acceptable test result.17.6.4 Weigh at least two 1.0 g specimens of C

35、alibrant B,weighed to the nearest 1 mg, and transfer them to crucibles. Toeach, add approximately 1.5 g of accelerator.17.6.5 Treat each specimen as directed in 18.1.2 and 18.1.3before proceeding to the next one.17.6.6 Record the results of 17.6.4 and 17.6.5 and comparethem to the certified carbon v

36、alue of Calibrant B. The resultshould agree with the certified value within a suitable confi-dence interval (see Note 4). If the result agrees with thecertified value within the uncertainty provided on the certificateof analysis, the calibration is acceptable. Also, if the certifiedvalue falls withi

37、n an interval calculated as described in Eq 1,the calibration is acceptable. If not, refer to the manufacturersinstructions for checking the linearity of the system.NOTE 5The use of 1.5 g of accelerator may not be sufficient for alldeterminators. The required amount is determined by the analyzer use

38、d,induction coil spacing, position of the crucible in the induction coil, ageand strength of the oscillator tube, and type of crucible being used. Use theamount required to produce proper sample combustion using the sameamount throughout the entire test method.17.7 CalibrationRange II (0.10 % to 1.2

39、5 % carbon):17.7.1 Proceed as directed in 17.6.1-17.6.3, using CalibrantCC.17.7.2 Proceed as directed in 17.6.4-17.6.6, using CalibrantBB.17.8 CalibrationRange III (1.25 % to 4.50 % carbon):17.8.1 Weigh four 0.5 g specimens of Calibrant CCC, to thenearest 1 mg, and place in crucibles. To each, add a

40、pproxi-mately 1.5 g of accelerator. Follow the calibration procedurerecommended by the manufacturer. Use Calibrant CCC as theprimary calibrant and analyze at least three specimens todetermine the calibration slope. Treat each specimen, asdirected in 18.1.2 and 18.1.3, before proceeding to the nexton

41、e.17.8.2 Confirm the calibration by analyzing Calibrant CCCfollowing the calibration procedure. The result should agreewith the certified value within a suitable confidence interval(see Note 4). If the result agrees with the certified value withinthe uncertainty provided on the certificate of analys

42、is, thecalibration is acceptable.Also, if the certified value falls withinan interval calculated as described in Eq 1, the calibration isacceptable.17.8.3 If not, repeat 17.8.1 and 17.8.2.17.8.4 Weigh at least two 0.5 g specimens of CalibrantBBB, weighed to the nearest 1 mg, and transfer to crucible

43、s. Toeach, add approximately 1.5 g of accelerator.17.8.5 Treat each specimen as described in 18.1.2 and18.1.3 before proceeding to the next one.17.8.6 Record the results of 17.8.4 and 17.8.5 and compareto the certified carbon value of Calibrant BBB. The resultE1019 116should agree with the certified

44、 value within a suitable confi-dence interval (see Note 4). If the result agrees with thecertified value within the uncertainty provided on the certificateof analysis, the calibration is acceptable. Also, if the certifiedvalue falls within an interval calculated as described in Eq 1,the calibration

45、is acceptable. If not, refer to manufacturersinstructions for checking the linearity of the analyzer (Note 6).NOTE 6Verify the calibration when: (1) a different lot of crucibles isused, (2) a different lot of accelerator is used, (3) the system has been inuse for 4 h, (4) the oxygen supply has been

46、changed, and (5) the systemhas been idle for 1 h. Verification should consist of analyzing at least onespecimen of each calibrant. Recalibrate as necessary.18. Procedure18.1 ProcedureRange I:18.1.1 Stabilize the furnace and analyzer as directed inSection 15. Transfer approximately 1.0 g of specimen

47、andapproximately 1.5 g of accelerator to a crucible. (See 13.2.)18.1.2 Place the crucible on the furnace pedestal and raisethe pedestal into position. Use crucible tongs to handle thecrucibles.18.1.3 Refer to the manufacturers recommended procedureregarding entry of specimen mass and blank value. St

48、art theanalysis cycle.18.2 ProcedureRange IIProceed as directed in 18.1.18.3 ProcedureRange IIIProceed as directed in 18.1,using a 0.5 g specimen.19. Calculation19.1 The calibration function of the equipment shall yield alinear plot described by Eq 2.Y 5 mX 1 b (2)where:Y = measurement response,M =

49、slope,X = calibrant concentration, andb = Y intercept.Calculation of the calibration function shall be done using alinear least squares regression. Some manufacturers recom-mend the use of a curve weighting factor where the calibrantconcentration is derived as 1/X. It is acceptable to use this typeof curve weighting.19.2 Since most modern commercially available instru-ments calculate mass fraction concentrations directly, includ-ing corrections for blank and sample mass, manual calculationsby the analyst are not required.NOTE 7If the analyzer does not com