1、Designation: D5291 10 (Reapproved 2015)Standard Test Methods forInstrumental Determination of Carbon, Hydrogen, andNitrogen in Petroleum Products and Lubricants1This standard is issued under the fixed designation D5291; the number immediately following the designation indicates the year oforiginal a
2、doption 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 instrumental determinationof carbon, hyd
3、rogen, and nitrogen in laboratory samples ofpetroleum products and lubricants. Values obtained representthe total carbon, the total hydrogen, and the total nitrogen.1.2 These test methods are applicable to samples such ascrude oils, fuel oils, additives, and residues for carbon andhydrogen and nitro
4、gen analysis. These test methods weretested in the concentration range of at least 75 mass % to 87mass % for carbon, at least 9 mass % to 16 mass % forhydrogen, and 0.1 mass % to 2 mass % for nitrogen.1.3 The nitrogen test method is not applicable to lightmaterials or those containing 0.75 mass % ni
5、trogen, or both,such as gasoline, jet fuel, naphtha, diesel fuel, or chemicalsolvents.1.3.1 However, using Test Method D levels of 0.1 mass %nitrogen in lubricants could be determined.1.4 These test methods are not recommended for the analy-sis of volatile materials such as gasoline, gasoline-oxygen
6、ateblends, or gasoline type aviation turbine fuels.1.5 The results of these tests can be expressed as mass %carbon, hydrogen or nitrogen.1.6 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.7 This standard does not purport to a
7、ddress 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.2. Referenced Documents2.1 ASTM Standards:2D4057 Pract
8、ice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System Performance3. Summary of Test Methods3.1
9、 In these test methods, carbon, hydrogen, and nitrogenare determined concurrently in a single instrumental procedure.With some systems, the procedure consists of simply weighinga portion of the sample, placing the portion in the instrument,and initiating the (subsequently automatic) analytical proce
10、ss.In other systems, the analytical process, to some degree, ismanually controlled.3.2 The actual process can vary substantially from instru-ment to instrument, since a variety of means can be utilized toeffect the primary requirements of the test methods. Allsatisfactory processes provide for the f
11、ollowing:3.2.1 The conversion of the subject materials (in theirentirety) to carbon dioxide, water vapor, and elementalnitrogen, respectively, and3.2.2 The subsequent, quantitative determination of thesegases in an appropriate gas stream.3.3 The conversion of the subject materials to their corre-spo
12、nding gases takes place largely during combustion of thesample at an elevated temperature in an atmosphere of purifiedoxygen. Here, a variety of gaseous materials are produced,including the following:3.3.1 Carbon dioxide from the oxidation of organic andelemental carbon,1These test methods are under
13、 the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and are the direct responsibilityof Subcommittee D02.03 on Elemental Analysis.Current edition approved April 1, 2015. Published June 2015. Originallyapproved in 1992. Last previous edition approved in 2010 as
14、D5291 10. DOI:10.1520/D5291-10R15.2For 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.*A Summary of Changes secti
15、on appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.3.2 Hydrogen halides from organic halides (and organichydrogen, as required),3.3.3 Water vapor from the oxidation of (the remaining)organic hydrog
16、en and the liberation of moisture,3.3.4 Nitrogen and nitrogen oxides from the oxidation oforganic nitrogen, and3.3.5 Sulfur oxides from the oxidation of organic sulfur. Insome systems, sulfurous and sulfuric acids can also be obtainedfrom a combination of the sulfur oxides and the water vapor.3.4 Th
17、ere are several accepted ways of isolating the desiredgaseous products and quantitatively determining them. Theseare as follows:3.4.1 Test Method A3,4From the combustion product gasstream, oxides of sulfur are removed with calcium oxide in thesecondary combustion zone. A portion of the remaining mix
18、edgases is carried by helium gas over a hot copper train to removeoxygen, and reduce NOxto N2, over NaOH to remove CO2,and over magnesium perchlorate to remove H2O. The remain-ing elemental nitrogen is measured by the thermal conductivitycell. Simultaneously, but separately from the nitrogenmeasurem
19、ent, the carbon and hydrogen selective infrared cellsmeasure the CO2and H2O levels.3.4.2 Test Method B4,5From the combustion product gasstream (which is cleaned from sulfur oxides, excess oxygen,etc. as in 3.4.1), the remaining CO2, water vapor, and N2areflushed into a mixing chamber and are thoroug
20、hly homog-enized at a precise volume, temperature, and pressure. Afterhomogenization, the chamber is depressurized to allow thegases to pass through a heated column, where the gasesseparate as a function of selective retention times. The sepa-ration occurs in a stepwise steady-state manner for nitro
21、gen,carbon dioxide, and water.3.4.3 Test Method C4,6The combustion product gasstream, after full oxidation of component gases, is passed overheated copper to remove excess oxygen and reduce NOxto N2gas. The gases are then passed through a heated chromato-graphic column to separate and elute N2,CO2,
22、and H2O in thatorder. The individual eluted gases are measured by a thermalconductivity detector.3.4.4 Test Method D4,7The organic samples are packedinto lightweight containers of oxidizable metal and dropped atpreset times into a vertical quartz, inconel, or stainless steelreactor, heated at about
23、1050 C, through which a constant flowof helium is maintained. When the samples are introduced, thehelium stream is temporarily enriched with pure oxygen. Flashcombustion takes place primed by the oxidation of the con-tainer. Quantitative combustion is then achieved by passing thegases over chromium
24、trioxide and cupric oxide. The mixture ofthe combustion gases is transferred over copper at about640 C (840 C in a steel reactor) to eliminate the excess ofoxygen; then without stopping, it is introduced into thechromatographic column heated to about 120 C (50 C forFlash EA 1112 units). The individu
25、al components are thenseparated by elution in the order nitrogen, carbon dioxide, andwater by a dedicated Poropak column (active carbon columnfor Flash EA 1112 units for nitrogen determination) andmeasured by a thermal conductivity detector. With dedicatedsoftware the percentage of elements present
26、in the sample arecalculated. The instrument is calibrated with standard pureorganic compounds. K-factors or linear regression can be usedfor instrument calibration. The typical operator analysis timefor a single sample is about 4 min, and the total elapsed timeis 8 min.3.5 In all cases, the concentr
27、ations of carbon, hydrogen andnitrogen are calculated as functions of the following:3.5.1 The measured instrumental responses,3.5.2 The values for response per unit mass for the elements(established via instrument calibration), and3.5.3 The mass of the sample.3.6 A capability for performing these co
28、mputations auto-matically can be included in the instrumentation utilized forthese test methods.4. Significance and Use4.1 This is the first ASTM standard covering the simultane-ous determination of carbon, hydrogen, and nitrogen in petro-leum products and lubricants.4.2 Carbon, hydrogen, and partic
29、ularly nitrogen analysesare useful in determining the complex nature of sample typescovered by this test method. The CHN results can be used toestimate the processing and refining potentials and yields in thepetrochemical industry.4.3 The concentration of nitrogen is a measure of thepresence of nitr
30、ogen containing additives. Knowledge of itsconcentration can be used to predict performance. Somepetroleum products also contain naturally occurring nitrogen.Knowledge of hydrogen content in samples is helpful inaddressing their performance characteristics. Hydrogen tocarbon ratio is useful to asses
31、s the performance of upgradingprocesses.5. Apparatus5.1 Since a variety of instrumental components and configu-rations can be satisfactorily utilized for these test methods, nospecifications are given here with respect to overall systemdesign.5.2 Functionally, however, the following are specified fo
32、r allinstruments:5.2.1 The conditions for combustion of the sample must besuch that (for the full range of applicable samples) the subjectcomponents are completely converted to carbon dioxide, watervapor (except for hydrogen associated with volatile halides and3The sole source of supply of the Leco
33、CHN-600 instrument known to thecommittee at this time is Leco Corporation, 3000 Lakeview Ave., St. Joseph, MI49085.4If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of the resp
34、onsible technical committee1, which you may attend.5The sole source of supply of the Perkin Elmer 240C, 2400 series and CEC240XA and 440 instruments known to the committee at this time is Perkin ElmerCorporation, Main Ave., Norwalk, CT 06856.6The sole source of supply of the Carlo Erba 1106, 1108, a
35、nd 1500 instrumentsknown to the committee at this time is Carlo Erba Strumentazione, Strada Rivoltana,20090 Rodano, Milan, Italy.7The sole source of supply of the Flash EA instruments known to the committeeat this time is Thermo Fisher Scientific, Strada Rivoltana, 20090 Milano, Italy.D5291 10 (2015
36、)2sulfur oxides), and nitrogen or nitrogen oxides. Generally,instrumental conditions that affect complete combustion in-clude availability of the oxidant, temperature, and time.5.2.2 Representative aliquots of the combustion gases mustthen be treated:5.2.2.1 To liberate (as water vapor) hydrogen pre
37、sent ashydrogen halides and sulfur oxyacids, and5.2.2.2 To reduce (to the element) nitrogen present asnitrogen oxides.5.2.3 The water vapor and nitrogen so obtained must beincluded with the materials originally present in these aliquots.5.2.4 Additional treatment of the aliquots (prior to detec-tion
38、) depends on the detection scheme utilized for the instru-ment (see Note 1).NOTE 1These additional treatments can be provided by the instru-mental components utilized to satisfy 5.2.2.5.2.5 The detection system (in its full scope) must deter-mine the analytical gases individually and without interfe
39、rence.Additionally, for each analyte, either:5.2.5.1 The detectors must provide linear responses withrespect to concentration over the full range of possible con-centrations from the applicable samples, or5.2.5.2 The system must include provisions for appropri-ately evaluating nonlinear responses so
40、 that they can beaccurately correlated with these concentrations.5.2.6 Such provisions can be integral to the instrumentation,or they can be provided by (auxiliary) computation schemes.5.2.7 Lastly, except for those systems where the concentra-tion data are output directly, the instrument must inclu
41、de anappropriate readout device for the detector responses.5.3 Additionally consumables needed for the analyses in-clude:5.3.1 Tin Capsules, large and small,5.3.2 Ceramic Crucibles,5.3.3 Copper Capsules,5.3.4 Tin Plugs,5.3.5 Tin Boats,5.3.6 Copper Plugs,5.3.7 Aluminum Capsules,5.3.8 Combustion Tubes
42、,5.3.9 Adsorption Tubes,5.3.10 Nickel Capsules, and5.3.11 Reduction Tubes.5.4 Analytical Balance, capable of weighing to the nearest0.00001 g.5.5 Syringes or Pipettes, to transfer the test specimens tocapsules.6. Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless
43、 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 available.8Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently hi
44、gh purity to permit its use without lessening theaccuracy of the determination.6.2 Calibration StandardsTable 1 lists the pure organiccompounds most commonly used to calibrate the instrumentsoperated according to 3.4.1 3.4.3; other suitable purecompounds can also be used.6.3 Carrier and Combustion G
45、ases:6.3.1 Oxygen, high purity (99.998 %),6.3.2 Helium, high purity (99.995 %),6.3.3 Compressed Air, Nitrogen, or Argon, for operatingpneumatic valves, if needed, and6.3.4 Carbon Dioxide.6.4 Additional Reagents (as Specified by the InstrumentManufacturer)This specification covers the reagents utiliz
46、edto provide for the functional requirements cited in 5.2.2 and5.2.3. These reagents can vary substantially for differentinstruments. Consequently, these reagents shall be those rec-ommended by the manufacturer. Specifically, these reagentswill be for:6.4.1 Test Method A3,4:6.4.1.1 Sodium Hydroxide
47、Coated Silica,6.4.1.2 Quartz Wool,6.4.1.3 Magnesium Perchlorate,6.4.1.4 Copper Turnings,6.4.1.5 Coated Calcium Oxide (Furnace Reagent),6.4.1.6 Nitrogen Catalyst, and6.4.1.7 Magnesium Oxide,4,9for liquids.8Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washingt
48、on, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.9The sole sou
49、rce of supply of Com-aid, a registered trademark of Leco, knownto the committee at this time is Leco Corporation, 3000 Lakeview Ave., St Joseph,MI 49085.TABLE 1 Calibration Standards for CHN Instrumental AnalysisA,BCompoundMolecularFormulaCarbon,Mass%HydrogenMass %NitrogenMass %Acetanilide C8H9NO 71.09 6.71 10.36Atropine C17H23NO370.56 8.01 4.84Benzoic acid C7H6O268.84 4.95 . . .Cyclohexanone- C12H14N4O451.79 5.07 20.142,4-dinitrophenylhydrazoneCystine C6H12N2O4S229.99 5.03 11.66Diphenyl C12H1093.46 6.54 . .EDTA C10H16N2O841.10 5.52 9.59Imidazol C3H4N252.92 5.92 41.15
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