1、Designation: D 7455 08An American National StandardStandard Practice forSample Preparation of Petroleum and Lubricant Productsfor Elemental Analysis1This standard is issued under the fixed designation D 7455; the number immediately following the designation indicates the year oforiginal adoption or,
2、 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 This practice covers different means by which petro-leum product and lubricant s
3、amples may be prepared before 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 forinstruction
4、s to handle such situations.1.3 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 con
5、centrations outside the scope 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 D02.0
6、3; asinformation becomes available, 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.
7、 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:2D86 Test Method for Distillation of Petroleum Products atAtmospheric Pressure
8、D 129 Test Method for Sulfur in Petroleum Products (Gen-eral Bomb Method)D 482 Test Method for Ash from Petroleum ProductsD 808 Test Method for Chlorine in New and Used Petro-leum Products (Bomb Method)D 874 Test Method for Sulfated Ash from Lubricating Oilsand AdditivesD 1018 Test Method for Hydrog
9、en In Petroleum FractionsD 1091 Test Methods for Phosphorus in Lubricating Oilsand AdditivesD 1266 Test Method for Sulfur in Petroleum Products(Lamp Method)D 1318 Test Method for Sodium in Residual Fuel Oil(Flame Photometric Method)D 1548 Test Method for Vanadium in Navy Special FuelOil3D 1552 Test
10、Method for Sulfur in Petroleum Products(High-Temperature Method)D 2622 Test Method for Sulfur in Petroleum Products byWavelength Dispersive X-ray Fluorescence SpectrometryD 2784 Test Method for Sulfur in Liquefied PetroleumGases (Oxy-Hydrogen Burner or Lamp)D 3120 Test Method for Trace Quantities of
11、 Sulfur in LightLiquid Petroleum Hydrocarbons by Oxidative Microcou-lometryD 3228 Test Method for Total Nitrogen in Lubricating Oilsand Fuel Oils by Modified Kjeldahl MethodD 3230 Test Method for Salts in Crude Oil (ElectrometricMethod)D 3231 Test Method for Phosphorus in GasolineD 3237 Test Method
12、for Lead in Gasoline by AtomicAbsorption SpectroscopyD 3246 Test Method for Sulfur in Petroleum Gas by Oxi-dative MicrocoulometryD 3340 Test Method for Lithium and Sodium in LubricatingGreases by Flame PhotometerD 3341 Test Method for Lead in GasolineIodineMonochloride MethodD 3348 Test Method for R
13、apid Field Test for Trace Lead inUnleaded Gasoline (Colorimetric Method)1This practice is under the jurisdiction of ASTM Committee D02 on PetroleumProducts and Lubricants and is the direct responsibility of Subcommittee D02.03 onElemental Analysis.Current edition approved May 1, 2008. Published June
14、 2008.2For 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.3Withdrawn.1Copyright ASTM International, 100 Barr Harb
15、or Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.D 3605 Test Method for Trace Metals in Gas Turbine Fuelsby Atomic Absorption and Flame Emission SpectroscopyD 3701 Test Method for Hydrogen Content of AviationTurbine Fuels by Low Resolution Nuclear Magnetic Reso-nance Spectromet
16、ryD 3831 Test Method for Manganese in Gasoline By AtomicAbsorption SpectroscopyD 4045 Test Method for Sulfur in Petroleum Products byHydrogenolysis and Rateometric ColorimetryD 4047 Test Method for Phosphorus in Lubricating Oils andAdditives by Quinoline Phosphomolybdate MethodD 4057 Practice for Ma
17、nual Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD 4294 Test Method for Sulfur in Petroleum and PetroleumProducts by Energy Dispersive X-ray Fluorescence Spec-trometryD 4628 Test Method for Analysis of Barium, Calcium,Magnesium,
18、 and Zinc in Unused Lubricating Oils byAtomic Absorption SpectrometryD 4629 Test Method for Trace Nitrogen in Liquid Petro-leum Hydrocarbons by Syringe/Inlet Oxidative Combus-tion and Chemiluminescence DetectionD 4808 Test Methods for Hydrogen Content of Light Dis-tillates, Middle Distillates, Gas O
19、ils, and Residua byLow-Resolution Nuclear Magnetic Resonance Spectros-copyD 4927 Test Methods for Elemental Analysis of Lubricantand Additive ComponentsBarium, Calcium, Phospho-rus, Sulfur, and Zinc by Wavelength-Dispersive X-RayFluorescence SpectroscopyD 4929 Test Methods for Determination of Organ
20、ic Chlo-ride Content in Crude OilD 4951 Test Method for Determination of Additive Ele-ments in Lubricating Oils by Inductively Coupled PlasmaAtomic Emission SpectrometryD 5056 Test Method for Trace Metals in Petroleum Coke byAtomic AbsorptionD 5059 Test Methods for Lead in Gasoline by X-RaySpectrosc
21、opyD 5184 Test Methods for Determination of Aluminum andSilicon in Fuel Oils by Ashing, Fusion, InductivelyCoupled Plasma Atomic Emission Spectrometry, andAtomic Absorption SpectrometryD 5185 Test Method for Determination of Additive Ele-ments, Wear Metals, and Contaminants in Used Lubricat-ing Oils
22、 and Determination of Selected Elements in BaseOils by Inductively Coupled Plasma Atomic EmissionSpectrometry (ICP-AES)D 5291 Test Methods for Instrumental Determination ofCarbon, Hydrogen, and Nitrogen in Petroleum Productsand LubricantsD 5384 Test Methods for Chlorine in Used PetroleumProducts (Fi
23、eld Test Kit Method)D 5453 Test Method for Determination of Total Sulfur inLight Hydrocarbons, Spark Ignition Engine Fuel, DieselEngine Fuel, and Engine Oil by Ultraviolet FluorescenceD 5600 Test Method for Trace Metals in Petroleum Coke byInductively Coupled Plasma Atomic Emission Spectrom-etry (IC
24、P-AES)D 5622 Test Methods for Determination of Total Oxygen inGasoline and Methanol Fuels by Reductive PyrolysisD 5708 Test Methods for Determination of Nickel, Vana-dium, and Iron in Crude Oils and Residual Fuels byInductively Coupled Plasma (ICP)Atomic Emission Spec-trometryD 5762 Test Method for
25、Nitrogen in Petroleum and Petro-leum Products by Boat-Inlet ChemiluminescenceD 5863 Test Methods for Determination of Nickel, Vana-dium, Iron, and Sodium in Crude Oils and Residual Fuelsby Flame Atomic Absorption SpectrometryD 6334 Test Method for Sulfur in Gasoline by WavelengthDispersive X-Ray Flu
26、orescenceD 6443 Test Method for Determination of Calcium, Chlo-rine, Copper, Magnesium, Phosphorus, Sulfur, and Zinc inUnused Lubricating Oils and Additives by WavelengthDispersive X-ray Fluorescence Spectrometry (Mathemati-cal Correction Procedure)D 6445 Test Method for Sulfur in Gasoline by Energy
27、-Dispersive X-ray Fluorescence SpectrometryD 6470 Test Method for Salt in Crude Oils (PotentiometricMethod)D 6481 Test Method for Determination of Phosphorus,Sulfur, Calcium, and Zinc in Lubrication Oils by EnergyDispersive X-ray Fluorescence SpectroscopyD 6595 Test Method for Determination of Wear
28、Metals andContaminants in Used Lubricating Oils or Used HydraulicFluids by Rotating Disc Electrode Atomic Emission Spec-trometryD 6667 Test Method for Determination of Total VolatileSulfur in Gaseous Hydrocarbons and Liquefied PetroleumGases by Ultraviolet FluorescenceD 6728 Test Method for Determin
29、ation of Contaminants inGas Turbine and Diesel Engine Fuel by Rotating DiscElectrode Atomic Emission SpectrometryD 6732 Test Method for Determination of Copper in JetFuels by Graphite Furnace Atomic Absorption Spectrom-etryD 6920 Test Method for Total Sulfur in Naphthas, Distil-lates, Reformulated G
30、asolines, Diesels, Biodiesels, andMotor Fuels by Oxidative Combustion and Electrochemi-cal DetectionD 7039 Test Method for Sulfur in Gasoline and Diesel Fuelby Monochromatic Wavelength Dispersive X-ray Fluores-cence SpectrometryD 7040 Test Method for Determination of Low Levels ofPhosphorus in ILSAC
31、 GF 4 and Similar Grade Engine Oilsby Inductively Coupled Plasma Atomic Emission Spec-trometryD 7041 Test Method for Determination of Total Sulfur inLight Hydrocarbons, Motor Fuels, and Oils by Online GasChromatography with Flame Photometric DetectionD 7111 Test Method for Determination of Trace Ele
32、ments inMiddle Distillate Fuels by Inductively Coupled PlasmaAtomic Emission Spectrometry (ICP-AES)D7455082D 7171 Test Method for Hydrogen Content of MiddleDistillate Petroleum Products by Low-Resolution PulsedNuclear Magnetic Resonance SpectroscopyD 7212 Test Method for Low Sulfur inAutomotive Fuel
33、s byEnergy-Dispersive X-ray Fluorescence Spectrometry Us-ing a Low-Background Proportional CounterD 7220 Test Method for Sulfur in Automotive Fuels byPolarization X-ray Fluorescence SpectrometryD 7303 Test Method for Determination of Metals in Lubri-cating Greases by Inductively Coupled Plasma Atomi
34、cEmission SpectrometryD 7318 Test Method for Total Inorganic Sulfate in Ethanolby Potentiometric TitrationD 7319 Test Method for Determination of Total and Poten-tial Sulfate and Inorganic Chloride in Fuel Ethanol byDirect Injection Suppressed Ion ChromatographyD 7328 Test Method for Determination o
35、f Total and Poten-tial Inorganic Sulfate and Total Inorganic Chloride in FuelEthanol by Ion Chromatography Using Aqueous SampleInjectionWK16905 Practice for Sampling, Storage, and Handling ofHydrocarbon Samples for Mercury Analysis3. Summary of Practice3.1 This practice covers alternate ways of prep
36、aring apetroleum product or lubricant sample for elemental analysismeasurements. The means of preparation of samples may varyfrom no special steps to extensive detailed procedures depen-dent on the sample matrix and the measurement technique to beused.3.2 This practice may also be applicable to non-
37、petroleumbased biofuels. Work is underway to validate the applicabilityto these types of materials.4. Significance and Use4.1 Crude oil, petroleum, petroleum products, additives, andlubricants are routinely analyzed for their elemental contentsuch as chlorine, nitrogen, phosphorus, sulfur, and vario
38、usmetals using a variety of analytical techniques. Some of thesetest methods require little to no sample preparation; someothers require only simple dilutions; while others requireelaborate sample decomposition before the product is analyzedfor its elemental content.4.2 Fairly often it can be shown
39、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 instructions in the test methods can be a causalfactor of such errors.Afurther consequence is an unnecessarilylarge reproducibility
40、 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 consistent resultsacross the laboratories.5. Gross Sample Preparation5.1 Collection of a meaningful and representative sample isoften
41、 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 sampling and allsubsequent analysis steps. Good laboratory practices in thisarea can include:5.1.1 The sample received by the labora
42、tory for analysisneeds to be stored in a designated specific storage locationwhile awaiting analysis. This area, whenever possible, shall notcontain materials with high levels of specific elements thatcould contaminate other samples requiring trace element analy-sis.5.1.2 All laboratory equipment us
43、ed 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 g
44、ases and dust particles.5.1.4 Wear clean, fresh, protective, and impermeable glovesfor sample preparation for trace element analysis, appropriatefor the materials being handled. Test the gloves to confirm thatthey do not contain interfering elements or elements of interest,since they may cause conta
45、mination. The development of cleanarea sample handling protocols is encouraged.5.2 All laboratory samples should be collected in accor-dance with Practices D 4057 and D 4177. The personnelcollecting the samples should be properly trained in sampling,since invalid sampling can lead to invalid results
46、. The respon-sibility of the laboratory starts on receipt of the sample in thelaboratory.5.2.1 It would be useful for the laboratory personnel toassist the plant personnel in securing a representativecontamination-free sample. Often inappropriate or uncleancontainers are used to collect the samples
47、in plant or field. Itwould help if the laboratory can provide pre-cleaned samplecontainers to the plant personnel collecting the samples.5.2.1.1 The clean container, lid, liner seal, and liner adhe-sive shall not contaminate the sample, and the sample shall notcompromise the integrity of the contain
48、er.5.2.1.2 Consult Department of Transportation packagingguidelines or other appropriate sources, such as placing in aHazmat-Pak, taping caps in place after securing tightlycontainer/liner compatibility, judicious use of vermiculite as apacking material considering contamination as well as usersafet
49、y from inhaled dust, etc.5.2.2 To preserve sample integrity and prevent the loss ofvolatile components, which can be present in some samples,they shall not be kept uncovered any longer than necessary.Samples need to be analyzed as soon as possible after takingfrom the bulk supplies to prevent loss of volatile species orcontamination.5.3 Before taking an aliquot of the bulk sample, ensure thatthe sample is well-mixed and homogenous. This can beensured, if necessary, by the use of an ultrasonic device orvigorously stirring with a magnetic or mechanical stirrer orshaker. Purge the sampl
