ASTM D7455-2014 2049 Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis《元素分析用石油和润滑产品样品制备的标准实施规程》.pdf

1、Designation: D7455 14Standard Practice forSample Preparation of Petroleum and Lubricant Productsfor Elemental Analysis1This standard is issued under the fixed designation D7455; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the y

2、ear 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 This practice covers different means by which petro-leum product and lubricant samples may be prepared before

3、themeasurement of their elemental content using different analyti-cal techniques.1.2 This practice includes only the basic steps for generallyencountered sample types. Anything out of the ordinary mayrequire special procedures. See individual test methods forinstructions to handle such situations.1.

4、3 This practice is not a substitute for a thorough under-standing of the actual test method to be used, caveats the testmethod contains, and additional sample preparation that maybe required.1.4 The user should not expand the scope of the testmethods to materials or concentrations outside the scope

5、of thetest methods being used without thoroughly understanding theimplications of such deviations.1.5 This practice may also be applicable to sample prepa-ration of non-petroleum based bio-fuels for elemental analysis.Currently, work is ongoing inASTM Subcommittee D02.03; asinformation becomes avail

6、able, it will be added to this stan-dard.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 thesafety concerns, if any, associated with its use. It is theresponsibility of th

7、e 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:2C1234 Practice for Preparation of Oils and Oily WasteSamples by High-Pressure, High-Temperature Digestionfo

8、r Trace Element DeterminationsD86 Test Method for Distillation of Petroleum Products atAtmospheric PressureD129 Test Method for Sulfur in Petroleum Products (Gen-eral High Pressure Decomposition Device Method)D482 Test Method for Ash from Petroleum ProductsD808 Test Method for Chlorine in New and Us

9、ed PetroleumProducts (High Pressure Decomposition Device Method)D874 Test Method for Sulfated Ash from Lubricating Oilsand AdditivesD1018 Test Method for Hydrogen In Petroleum FractionsD1091 Test Methods for Phosphorus in Lubricating Oils andAdditivesD1266 Test Method for Sulfur in Petroleum Product

10、s (LampMethod)D1318 Test Method for Sodium in Residual Fuel Oil (FlamePhotometric Method)D1548 Test Method for Vanadium in Heavy Fuel Oil1(Withdrawn 1997)3D1552 Test Method for Sulfur in Petroleum Products (High-Temperature Method)D2622 Test Method for Sulfur in Petroleum Products byWavelength Dispe

11、rsive X-ray Fluorescence SpectrometryD2784 Test Method for Sulfur in Liquefied Petroleum Gases(Oxy-Hydrogen Burner or Lamp)D3120 Test Method for Trace Quantities of Sulfur in LightLiquid Petroleum Hydrocarbons by Oxidative Microcou-lometry1This practice is under the jurisdiction of ASTM Committee D0

12、2 on PetroleumProducts, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom-mittee D02.03 on Elemental Analysis.Current edition approved May 1, 2014. Published May 2014. Originallyapproved in 2008. Last previous edition approved in 2008 as D7455 08. DOI:10.1520/D7455-14.2For refe

13、renced 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.3The last approved version of this historical standard is referenced o

14、nwww.astm.org.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1D3228 Test Method for Total Nitrogen in Lubricating Oilsand Fuel Oils by Modified Kjeldahl MethodD3230 Test

15、 Method for Salts in Crude Oil (ElectrometricMethod)D3231 Test Method for Phosphorus in GasolineD3237 Test Method for Lead in Gasoline byAtomicAbsorp-tion SpectroscopyD3246 Test Method for Sulfur in Petroleum Gas by Oxida-tive MicrocoulometryD3340 Test Method for Lithium and Sodium in LubricatingGre

16、ases by Flame Photometer (Withdrawn 2013)3D3341 Test Method for Lead in GasolineIodine Mono-chloride MethodD3348 Test Method for Rapid Field Test for Trace Lead inUnleaded Gasoline (Colorimetric Method)D3605 Test Method for Trace Metals in Gas Turbine Fuelsby Atomic Absorption and Flame Emission Spe

17、ctroscopyD3701 Test Method for Hydrogen Content of AviationTurbine Fuels by Low Resolution Nuclear MagneticResonance SpectrometryD3831 Test Method for Manganese in Gasoline By AtomicAbsorption SpectroscopyD4045 Test Method for Sulfur in Petroleum Products byHydrogenolysis and Rateometric Colorimetry

18、D4047 Test Method for Phosphorus in Lubricating Oils andAdditives by Quinoline Phosphomolybdate MethodD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD4294 Test Method for Sulfur in Petroleum and PetroleumPr

19、oducts by Energy Dispersive X-ray Fluorescence Spec-trometryD4628 Test Method for Analysis of Barium, Calcium,Magnesium, and Zinc in Unused Lubricating Oils byAtomic Absorption SpectrometryD4629 Test Method for Trace Nitrogen in Liquid PetroleumHydrocarbons by Syringe/Inlet Oxidative Combustion andC

20、hemiluminescence DetectionD4808 Test Methods for Hydrogen Content of LightDistillates, Middle Distillates, Gas Oils, and Residua byLow-Resolution Nuclear Magnetic Resonance Spectros-copyD4927 Test Methods for Elemental Analysis of Lubricantand Additive ComponentsBarium, Calcium,Phosphorus, Sulfur, a

21、nd Zinc by Wavelength-DispersiveX-Ray Fluorescence SpectroscopyD4929 Test Methods for Determination of Organic ChlorideContent in Crude OilD4951 Test Method for Determination of Additive Elementsin Lubricating Oils by Inductively Coupled PlasmaAtomic Emission SpectrometryD5056 Test Method for Trace

22、Metals in Petroleum Coke byAtomic AbsorptionD5059 Test Methods for Lead in Gasoline by X-Ray Spec-troscopyD5184 Test Methods for Determination of Aluminum andSilicon in Fuel Oils by Ashing, Fusion, InductivelyCoupled Plasma Atomic Emission Spectrometry, andAtomic Absorption SpectrometryD5185 Test Me

23、thod for Multielement Determination ofUsed and Unused Lubricating Oils and Base Oils byInductively Coupled Plasma Atomic Emission Spectrom-etry (ICP-AES)D5291 Test Methods for Instrumental Determination ofCarbon, Hydrogen, and Nitrogen in Petroleum Productsand LubricantsD5384 Test Methods for Chlori

24、ne in Used Petroleum Prod-ucts (Field Test Kit Method)D5453 Test Method for Determination of Total Sulfur inLight Hydrocarbons, Spark Ignition Engine Fuel, DieselEngine Fuel, and Engine Oil by Ultraviolet FluorescenceD5600 Test Method for Trace Metals in Petroleum Coke byInductively Coupled Plasma A

25、tomic Emission Spectrom-etry (ICP-AES)D5622 Test Methods for Determination of Total Oxygen inGasoline and Methanol Fuels by Reductive PyrolysisD5708 Test Methods for Determination of Nickel,Vanadium, and Iron in Crude Oils and Residual Fuels byInductively Coupled Plasma (ICP) Atomic EmissionSpectrom

26、etryD5762 Test Method for Nitrogen in Petroleum and Petro-leum Products by Boat-Inlet ChemiluminescenceD5863 Test Methods for Determination of Nickel,Vanadium, Iron, and Sodium in Crude Oils and ResidualFuels by Flame Atomic Absorption SpectrometryD6334 Test Method for Sulfur in Gasoline by Waveleng

27、thDispersive X-Ray FluorescenceD6443 Test Method for Determination of Calcium, Chlorine,Copper, Magnesium, Phosphorus, Sulfur, and Zinc inUnused Lubricating Oils and Additives by WavelengthDispersive X-ray Fluorescence Spectrometry (Mathemati-cal Correction Procedure)D6445 Test Method for Sulfur in

28、Gasoline by Energy-Dispersive X-ray Fluorescence Spectrometry (Withdrawn2009)3D6470 Test Method for Salt in Crude Oils (PotentiometricMethod)D6481 Test Method for Determination of Phosphorus,Sulfur, Calcium, and Zinc in Lubrication Oils by EnergyDispersive X-ray Fluorescence SpectroscopyD6595 Test M

29、ethod for Determination of Wear Metals andContaminants in Used Lubricating Oils or Used HydraulicFluids by Rotating Disc Electrode Atomic Emission Spec-trometryD6667 Test Method for Determination of Total VolatileSulfur in Gaseous Hydrocarbons and Liquefied PetroleumGases by Ultraviolet Fluorescence

30、D6728 Test Method for Determination of Contaminants inGas Turbine and Diesel Engine Fuel by Rotating DiscElectrode Atomic Emission SpectrometryD6732 Test Method for Determination of Copper in JetFuels by Graphite Furnace Atomic Absorption Spectrom-etryD7455 142D6920 Test Method for Total Sulfur in N

31、aphthas, Distillates,Reformulated Gasolines, Diesels, Biodiesels, and MotorFuels by Oxidative Combustion and Electrochemical De-tectionD7039 Test Method for Sulfur in Gasoline, Diesel Fuel, JetFuel, Kerosine, Biodiesel, Biodiesel Blends, andGasoline-Ethanol Blends by Monochromatic WavelengthDispersi

32、ve X-ray Fluorescence SpectrometryD7040 Test Method for Determination of Low Levels ofPhosphorus in ILSAC GF 4 and Similar Grade EngineOils by Inductively Coupled Plasma Atomic EmissionSpectrometryD7041 Test Method for Determination of Total Sulfur inLight Hydrocarbons, Motor Fuels, and Oils by Onli

33、ne GasChromatography with Flame Photometric DetectionD7111 Test Method for Determination of Trace Elements inMiddle Distillate Fuels by Inductively Coupled PlasmaAtomic Emission Spectrometry (ICP-AES)D7171 Test Method for Hydrogen Content of Middle Dis-tillate Petroleum Products by Low-Resolution Pu

34、lsedNuclear Magnetic Resonance SpectroscopyD7212 Test Method for Low Sulfur in Automotive Fuels byEnergy-Dispersive X-ray Fluorescence Spectrometry Us-ing a Low-Background Proportional CounterD7220 Test Method for Sulfur in Automotive, Heating, andJet Fuels by Monochromatic Energy Dispersive X-rayFl

35、uorescence SpectrometryD7260 Practice for Optimization, Calibration, and Valida-tion of Inductively Coupled Plasma-Atomic EmissionSpectrometry (ICP-AES) for Elemental Analysis of Petro-leum Products and LubricantsD7303 Test Method for Determination of Metals in Lubri-cating Greases by Inductively Co

36、upled Plasma AtomicEmission SpectrometryD7318 Test Method for Existent Inorganic Sulfate in Ethanolby Potentiometric TitrationD7319 Test Method for Determination of Existent and Po-tential Sulfate and Inorganic Chloride in Fuel Ethanol andButanol by Direct Injection Suppressed Ion Chromatog-raphyD73

37、28 Test Method for Determination of Existent and Po-tential Inorganic Sulfate and Total Inorganic Chloride inFuel Ethanol by Ion Chromatography Using AqueousSample InjectionD7343 Practice for Optimization, Sample Handling,Calibration, and Validation of X-ray Fluorescence Spec-trometry Methods for El

38、emental Analysis of PetroleumProducts and LubricantsD7482 Practice for Sampling, Storage, and Handling ofHydrocarbons for Mercury AnalysisD7620 Test Method for Determination of Total Sulfur inLiquid Hydrocarbon Based Fuels by Continuous Injection,Air Oxidation and Ultraviolet Fluorescence DetectionD

39、7622 Test Method for Total Mercury in Crude Oil UsingCombustion and Direct Cold Vapor Atomic AbsorptionMethod with Zeeman Background CorrectionD7623 Test Method for Total Mercury in Crude Oil UsingCombustion-Gold Amalgamation and Cold Vapor AtomicAbsorption MethodD7691 Test Method for MultielementAn

40、alysis of Crude OilsUsing Inductively Coupled Plasma Atomic EmissionSpectrometry (ICP-AES)D7740 Practice for Optimization, Calibration, and Valida-tion of Atomic Absorption Spectrometry for Metal Analy-sis of Petroleum Products and LubricantsD7751 Test Method for Determination of Additive Elementsin

41、 Lubricating Oils by EDXRF AnalysisD7757 Test Method for Silicon in Gasoline and RelatedProducts by Monochromatic Wavelength DispersiveX-ray Fluorescence SpectrometryD7876 Practice for Practice for Sample Decomposition Us-ing Microwave Heating (With or Without Prior Ashing)for Atomic Spectroscopic E

42、lemental Determination inPetroleum Products and Lubricants3. Summary of Practice3.1 This practice covers alternate ways of preparing apetroleum product or lubricant sample for elemental analysismeasurements. The means of preparation of samples may varyfrom no special steps to extensive detailed proc

43、edures depen-dent on the sample matrix and the measurement technique to beused.3.2 This practice may also be applicable to non-petroleumbased biofuels. Work is underway to validate the applicabilityto these types of materials.4. Significance and Use4.1 Crude oil, petroleum, petroleum products, addit

44、ives, andlubricants are routinely analyzed for their elemental contentsuch as chlorine, nitrogen, phosphorus, sulfur, and variousmetals using a variety of analytical techniques. Some of thesetest methods require little to no sample preparation; someothers require only simple dilutions; while others

45、requireelaborate sample decomposition before the product is analyzedfor its elemental content.4.2 Fairly often it can be shown that the round robin resultsby a co-operator are all biased with respect to those from otherlaboratories. Presumably, the failure to follow good laboratorypractices and inst

46、ructions in the test methods can be a causalfactor of such errors.Afurther consequence is an unnecessarilylarge reproducibility estimate or the data being dropped fromthe study as an outlier.4.3 Uniform practice for sample preparation is beneficial instandardizing the procedures and obtaining consis

47、tent resultsacross the laboratories.5. Gross Sample Preparation5.1 Collection of a meaningful and representative sample isoften the most critical step in an analytical procedure. In traceelement analysis, in particular, extreme care must be taken toavoid contamination of the samples during the sampl

48、ing and allsubsequent analysis steps. Good laboratory practices in thisarea can include:D7455 1435.1.1 The sample received by the laboratory for analysisneeds to be stored in a designated specific storage locationwhile awaiting analysis. This area, whenever possible, shall notcontain materials with

49、high levels of specific elements thatcould contaminate other samples requiring trace element analy-sis.5.1.2 All laboratory equipment used specifically for traceelement analysis need to be free of any source of contamina-tion. This may require that specific equipment be used only fortrace element analysis.5.1.3 Use working surfaces that can be decontaminatedeasily if a spillage occurs. The atmosphere needs to be free ofinterfering gases and dust particles.5.1.4 Wear clean, fresh, protective, and impermeable glovesfor sample preparation for trace element analysis, appropriatefor