1、Designation: D5291 16Standard 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 adoption or, in the
2、 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. Scope*1.1 These test methods cover the instrumental determinationof carbon, hydrogen, and nitrog
3、en 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 nitrogen analysis. The
4、se 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 % nitrogen, or both,s
5、uch 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-oxygenateblends, or gas
6、oline 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 address all of the
7、safety 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 Practice for Manual Sa
8、mpling 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 In these test me
9、thods, 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 process.In other syste
10、ms, 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 following:3.2.1 Th
11、e 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-sponding gases takes
12、 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 the jurisdiction
13、 of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and are the direct responsibilityof Subcommittee D02.03 on Elemental Analysis.Current edition approved Oct. 1, 2016. Published October 2016. Originallyapproved in 1992. Last previous edition approved in 2015 as D5291 10 (2015)
14、.DOI: 10.1520/D5291-16.2For 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 section appears
15、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 hydrogen and the
16、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 There are sev
17、eral 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 mixedgases is
18、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 nitrogenmeasurement, the ca
19、rbon 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 thoroughly homog-e
20、nized 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 nitrogen,carbon
21、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, and H2O in
22、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 1050 C, thr
23、ough 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 trioxide an
24、d 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 individual componen
25、ts 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 in the samp
26、le 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.NOTE 1Other instrument models in addition
27、 to the four included hereare available in the marketplace; however, no precision statements havebeen generated for them.3.5 In all cases, the concentrations of carbon, hydrogen andnitrogen are calculated as functions of the following:3.5.1 The measured instrumental responses,3.5.2 The values for re
28、sponse 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 computations auto-matically can be included in the instrumentation utilized forthese test methods.4. Significance and Use4.1 This is the first ASTM sta
29、ndard covering the simultane-ous determination of carbon, hydrogen, and nitrogen in petro-leum products and lubricants.4.2 Carbon, hydrogen, and particularly nitrogen analysesare useful in determining the complex nature of sample typescovered by this test method. The CHN results can be used toestima
30、te the processing and refining potentials and yields in thepetrochemical industry.4.3 The concentration of nitrogen is a measure of thepresence of nitrogen containing additives. Knowledge of itsconcentration can be used to predict performance. Somepetroleum products also contain naturally occurring
31、nitrogen.Knowledge of hydrogen content in samples is helpful inaddressing their performance characteristics. Hydrogen tocarbon ratio is useful to assess the performance of upgradingprocesses.5. Apparatus5.1 Since a variety of instrumental components and configu-rations can be satisfactorily utilized
32、 for these test methods, nospecifications are given here with respect to overall systemdesign.5.2 Functionally, however, the following are specified for allinstruments:3The sole source of supply of the Leco CHN-600 instrument known to thecommittee at this time is Leco Corporation, 3000 Lakeview Ave.
33、, 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 responsible technical committee1, which you may attend.5The sole source of supply of the Perkin E
34、lmer 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, and 1500 instrumentsknown to the committee at this time is Carlo Erba Strumentazione, Strada R
35、ivoltana,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 1625.2.1 The conditions for combustion of the sample must besuch that (for the full range of applicab
36、le samples) the subjectcomponents are completely converted to carbon dioxide, watervapor (except for hydrogen associated with volatile halides andsulfur oxides), and nitrogen or nitrogen oxides. Generally,instrumental conditions that affect complete combustion in-clude availability of the oxidant, t
37、emperature, and time.5.2.2 Representative aliquots of the combustion gases mustthen be treated:5.2.2.1 To liberate (as water vapor) hydrogen present 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
38、obtained must beincluded with the materials originally present in these aliquots.5.2.4 Additional treatment of the aliquots (prior to detec-tion) depends on the detection scheme utilized for the instru-ment (see Note 2).NOTE 2These additional treatments can be provided by the instru-mental component
39、s 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 interference.Additionally, for each analyte, either:5.2.5.1 The detectors must provide linear responses withrespect to concentration over the full range of possibl
40、e con-centrations from the applicable samples, or5.2.5.2 The system must include provisions for appropri-ately evaluating nonlinear responses so 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 (au
41、xiliary) computation schemes.5.2.7 Lastly, except for those systems where the concentra-tion data are output directly, the instrument must include 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
42、,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,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 o
43、r Pipettes, to transfer the test specimens tocapsules.6. Reagents6.1 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
44、Society,where such specifications are available.8Other 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.6.2 Calibration StandardsTable 1 lists the pure organiccompounds most commonl
45、y 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 Gases: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 n
46、eeded, and6.3.4 Carbon Dioxide.6.4 Additional Reagents (as Specified by the InstrumentManufacturer)This specification covers the reagents utilizedto provide for the functional requirements cited in 5.2.2 and5.2.3. These reagents can vary substantially for differentinstruments. Consequently, these re
47、agents 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 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 Cata
48、lyst, and6.4.1.7 Magnesium Oxide,4,9for liquids.8Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole
49、, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.9The sole source 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-di
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