ASTM E1019-2018 1250 Standard Test Methods for Determination of Carbon Sulfur Nitrogen and Oxygen in Steel Iron Nickel and Cobalt Alloys by Various Combustion and Inert Gas Fusion .pdf

1、Designation: E1019 18Standard Test Methods forDetermination of Carbon, Sulfur, Nitrogen, and Oxygen inSteel, Iron, Nickel, and Cobalt Alloys by VariousCombustion and Inert Gas Fusion Techniques1This standard is issued under the fixed designation E1019; the number immediately following the designatio

2、n indicates 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 agenc

3、ies of the U.S. Department of Defense.1. Scope1.1 These test methods cover the determination of carbon,sulfur, nitrogen, and oxygen, in steel, iron, nickel, and cobaltalloys having chemical compositions within the followinglimits:Element Mass Fraction Range, %Aluminum 0.001 to 18.00Antimony 0.002 to

4、 0.03Arsenic 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 75.0Niobium 0.002 to 6.00Copper 0.005 to 10.00Hydrogen 0.0001 to 0.0030Iron 0.01 to 100.

5、0Lead 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 0.002 to 0.35Tantalum 0.001 to 10.00Tellurium 0.001 to 0.35Tin 0.002 to

6、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 Combustion and InfraredAbsorption or Thermal Conductivity Detection TestMethod1020Nitrogen by the Inert Ga

7、s Fusion and Thermal Conduc-tivity Detection Test Method3242Oxygen by the Inert Gas Fusion and Infrared Absorp-tion or Thermal Conductivity Detection Test Method4354Sulfur by the Combustion-Infrared Absorption DetectionTest Method5565Sulfur by the CombustionInfrared Absorption TestMethod (Potassium

8、Sulfate Calibration) Discontinued201821311.3 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 th

9、e user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.Specific hazards statements are given in Section 6.1.5 This international standard was developed in accor-dance with internationally r

10、ecognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1193 Specificati

11、on for Reagent WaterE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications1These test methods are under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and are the directresponsibility of Subcommittee E

12、01.01 on Iron, Steel, and Ferroalloys.Current edition approved April 15, 2018. Published June 2018. Originallyapproved in 1984. Last previous edition approved in 2011 as E1019 11. DOI:10.1520/E1019-18.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Servi

13、ce at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in ac

14、cordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1E50 Practices for Apparatus,

15、Reagents, 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 Metals (Withdrawn1998)3E1601

16、 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE1806 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 Us

17、e4.1 These test methods for the chemical analysis of metalsand alloys are primarily intended 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-full

18、y 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 determinationare listed in separate sections preceding the procedure.5.2 These methods were originally developed for oldertechnology manual

19、instrumentation with the flow schematicsindicated. Current commercially available instruments aremore automated and may have slightly different flow schemat-ics and should be capable of producing data meeting orexceeding the precision and bias requirements.6. Hazards6.1 For hazards to be observed in

20、 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. Sampling7.1 For procedures to sample the materials, refer to thoseparts of Practice E1806.8. Rounding C

21、alculated Values8.1 Rounding of test results obtained using these test meth-ods shall be performed as directed in Practice E29, RoundingMethod, unless an alternative rounding method is specified bythe customer or applicable material specification.9. Interlaboratory Studies9.1 These test methods have

22、 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.TOTAL CARBON BY THE COMBUSTION ANDINFRARED ABSORPTION OR

23、THERMALCONDUCTIVITY DETECTION TEST METHOD10. Scope10.1 This test method covers the determination of carbonfrom 0.005 % to 4.5 %.11. Summary of Test Method11.1 The carbon is converted to carbon dioxide (CO2)bycombustion in a stream of oxygen.11.1.1 Thermal Conductivity Test MethodThe CO2isabsorbed on

24、 a suitable grade of zeolite, released by heating thezeolite, and swept by helium or oxygen into a chromatographiccolumn. Upon elution, the amount of CO2is measured in athermistor-type conductivity cell. Refer to Fig. 1 for example.11.1.2 Infrared (IR) Absorption, Test Method ATheamount of CO2is mea

25、sured by infrared (IR) absorption. CO2absorbs IR energy at a precise wavelength within the IRspectrum. Energy of this wavelength is absorbed as the gaspasses through a cell body in which the IR energy is transmit-ted. All other IR energy is eliminated from reaching thedetector by a precise wavelengt

26、h filter. Thus, the absorption ofIR energy can be attributed to only CO2and its amount ismeasured as changes in energy at the detector. One cell is usedas both a reference and a measure chamber. Total carbon, asCO2, is measured over a period of time. Refer to Fig. 2 forexample.11.1.3 Infrared (IR) A

27、bsorption, 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 specimencombustion, the flow of CO2with its oxygen carrier gas isrouted through the measure chamber while o

28、xygen alonepasses through the reference chamber. Energy from the IRsource passes through both chambers, simultaneously arrivingat the diaphragm (capacitor plate). Part of the IR energy isabsorbed by the CO2present in the measure chamber whilenone is absorbed passing through the reference chamber. Th

29、iscreates an IR energy imbalance reaching the diaphragm, thusdistorting it. This distortion alters the capacitance creating anelectric signal change that is amplified for measurement asCO2. Total carbon, as CO2, is measured over a period of time.Refer to Fig. 3 for example.11.1.4 Infrared (IR) Absor

30、ption, Test Method C, ClosedLoopThe combustion is performed in a closed loop, wherecarbon monoxide (CO) and CO2are detected in the sameinfrared cell. Each gas is measured with a solid state energydetector. Filters are used to pass the appropriate IR wavelengthto each detector. In the absence of CO a

31、nd CO2, the energyreceived by each detector is at its maximum. During3The last approved version of this historical standard is referenced onwww.astm.org.E1019 182combustion, the IR absorption properties of CO and CO2gasesin the chamber cause a loss of energy; therefore a loss in signalresults which

32、is proportional to amounts of each gas in theclosed loop. Total carbon, as CO2plus CO, is measured over aperiod of time. Refer to Fig. 4 for example.11.2 This test method is written for use with commercialanalyzers, equipped to perform the above operations automati-cally and calibrated using referen

33、ce materials of known carboncontent.12. Interferences12.1 The elements ordinarily present in iron, steel, nickel,and cobalt alloys do not interfere.13. Apparatus13.1 Combustion and Measurement ApparatusSee Figs.1-4 for examples.13.2 CruciblesUse crucibles that meet or exceed thespecifications of the

34、 instrument manufacturer 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.13.2.1 The analytical ranges for the use of untreated cru-cibles shall b

35、e determined by the testing laboratory andsupporting data shall be maintained on file to validate theseranges. Heating of crucibles is particularly important whenAHigh Purity Oxygen MCO2Absorber ZeoliteBOxygen Regulator (2 Stage) NFurnace Combustion ExhaustCSodium Hydroxide Impregnated Clay and Magn

36、esium Perchlo-rateOFurnace Purge ExhaustDSecondary Pressure Regulator PMetal Connector To Use Oxygen As Carrier GasEFlowmeter QHigh Purity HeliumFInduction Furnace RHelium Regulator (2 Stage)GCombustion Tube SChromatographic ColumnHDust Trap TTC Cell/ReadoutIManganese Dioxide UMeasure FlowmeterJHeat

37、ed CO to CO2Converter (suitable catalyst) VReference FlowmeterKMagnesium Perchlorate (Note 1 in 14.4) WFurnace Power SupplyLValve 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 Con

38、ductivity Detection Test MethodE1019 183analyzing for low levels of carbon and may not be required ifthe material to be analyzed has higher levels of carbon such asthat found in pig iron (3.5% or greater). Above certain carbonmass fractions, as determined by the testing laboratory, thenon-treatment

39、of crucibles will have no adverse effect.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 conform to the specifications of the Commit-tee

40、 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 without lessening theaccuracy of the determination.14.2 AcetoneThe residue afte

41、r evaporation shall be30), t may beset equal to 2 at the 95 % confidence level.At its discretion, the laboratorymay choose to set a smaller range for the acceptable test result.17.6.4 Weigh at least two 1.0 g specimens of B, weighed tothe nearest 1 mg, and transfer them to crucibles. To each, addapp

42、roximately 1.5 g of accelerator.17.6.4.1 The use of 1.5 g of accelerator may not be sufficientfor all determinators. The required amount is determined by theanalyzer used, induction coil spacing, position of the cruciblein the induction coil, age and strength of the oscillator tube, andtype of cruci

43、ble being used. Use the amount required toproduce proper sample combustion using the same amountthroughout the entire test method.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 certifi

44、ed carbon value of B. The result should agreewith the certified value within a suitable confidence interval(see Note 4 in 17.6.3). If the result agrees with the certifiedvalue within the uncertainty provided on the certificate ofanalysis, the calibration is acceptable. Also, if the certifiedvalue fa

45、lls within 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.17.7 CalibrationRange II (0.10 % to 1.25 % carbon):17.7.1 Proceed as directed in 17.6.1 17.6.3, using CC.17.7.2 Proceed as dir

46、ected in 17.6.4 17.6.6, using BB.17.8 CalibrationRange III (1.25 % to 4.50 % carbon):17.8.1 Weigh four 0.5 g specimens of CCC, to the nearest 1mg, and place in crucibles. To each, add approximately 1.5 g ofaccelerator. Follow the calibration procedure recommended bythe manufacturer. Use CCC as the p

47、rimary calibration RM andanalyze at least three specimens to determine the calibrationslope. Treat each specimen, as directed in 18.1.2 and 18.1.3,before proceeding to the next one.17.8.2 Confirm the calibration by analyzing CCC followingthe calibration procedure. If the result agrees with the certi

48、fiedvalue within the uncertainty provided on the certificate ofanalysis, the calibration is acceptable. Also, if the certifiedvalue falls within an interval calculated as described in Eq 1,the calibration is acceptable. See Note 4 in 17.6.3.17.8.3 If not, repeat 17.8.1 and 17.8.2.17.8.4 Weigh at lea

49、st two 0.5 g specimens of BBB, weighedto the nearest 1 mg, and transfer to crucibles. To each, addapproximately 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 BBB. The result should agreewith the certified value within a suitable confidence interval(see Note 4 in 17.6.3). If the result agrees with the certifiedvalue within the uncertainty provided on the certificate ofanalys