1、Designation: D7578 101Standard Guide forCalibration Requirements for Elemental Analysis ofPetroleum Products and Lubricants1This standard is issued under the fixed designation D7578; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision,
2、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.1NOTEUpdated Table 8 to correct Referenced Document editorially in August 2011.1. Scope1.1 This guide covers different
3、 ways by which the testmethods used for elemental analysis of petroleum product andlubricant samples are calibrated before the sample analysis.1.2 Uniform practice for test method calibration is benefi-cial in standardizing the procedures, and obtaining consistentresults across different laboratorie
4、s.1.3 This guide includes only the basic steps for generallyencountered instrument types. Anything out of the ordinarymay require special procedures. See individual test methods forinstructions to handle such situations.1.4 This guide is not a substitute for a thorough understand-ing of the actual t
5、est method to be used, caveats it contains, andadditional instrument preparation that may be required.1.5 The user should not expand the scope of the testmethods to materials or concentrations outside the scope of thetest methods being used.1.6 This guide should also be applicable to sample prepa-ra
6、tion of non-petroleum based bio-fuels for elemental analysis.Work is underway on these aspects in Subcommittee D02.03.As more information becomes available, it will be added to thisstandard.1.7 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in
7、 thisstandard.1.8 This standard does not purport to address 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
8、. Referenced Documents2.1 ASTM Standards:2D129 Test Method for Sulfur in Petroleum Products (Gen-eral Bomb Method)D445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and Calculation of Dynamic Viscos-ity)D482 Test Method for Ash from Petroleum ProductsD808 Test Method for Chlo
9、rine in New and Used PetroleumProducts (Bomb Method)D874 Test Method for Sulfated Ash from Lubricating Oilsand AdditivesD892 Test Method for Foaming Characteristics of Lubricat-ing OilsD1018 Test Method for Hydrogen In Petroleum FractionsD1091 Test Methods for Phosphorus in Lubricating Oilsand Addit
10、ivesD1266 Test Method for Sulfur in Petroleum Products(Lamp Method)D1318 Test Method for Sodium in Residual Fuel Oil (FlamePhotometric Method)D1548 Test Method for Vanadium in Navy Special FuelOil3D1552 Test Method for Sulfur in Petroleum Products(High-Temperature Method)D1839 Test Method for Amyl N
11、itrate in Diesel FuelsD2622 Test Method for Sulfur in Petroleum Products byWavelength Dispersive X-ray Fluorescence SpectrometryD2784 Test Method for Sulfur in Liquefied PetroleumGases (Oxy-Hydrogen Burner or Lamp)D3120 Test Method for Trace Quantities of Sulfur in LightLiquid Petroleum Hydrocarbons
12、 by Oxidative Microcou-lometryD3228 Test Method for Total Nitrogen in Lubricating Oils1This guide 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 Feb. 15, 2010. P
13、ublished March 2010. DOI: 10.1520/D7578-10.2For 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.1Copyright ASTM In
14、ternational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.and Fuel Oils by Modified Kjeldahl MethodD3230 Test Method for Salts in Crude Oil (ElectrometricMethod)D3231 Test Method for Phosphorus in GasolineD3237 Test Method for Lead in Gasoline by Atomic Ab-sorp
15、tion SpectroscopyD3246 Test Method for Sulfur in Petroleum Gas by Oxida-tive MicrocoulometryD3340 Test Method for Lithium and Sodium in LubricatingGreases by Flame PhotometerD3341 Test Method for Lead in GasolineIodine Mono-chloride MethodD3348 Test Method for Rapid Field Test for Trace Lead inUnlea
16、ded Gasoline (Colorimetric Method)D3605 Test Method for Trace Metals in Gas Turbine Fuelsby Atomic Absorption and Flame Emission SpectroscopyD3831 Test Method for Manganese in Gasoline By AtomicAbsorption SpectroscopyD4045 Test Method for Sulfur in Petroleum Products byHydrogenolysis and Rateometric
17、 ColorimetryD4046 Test Method for Alkyl Nitrate in Diesel Fuels bySpectrophotometryD4047 Test Method for Phosphorus in Lubricating Oils andAdditives by Quinoline Phosphomolybdate MethodD4294 Test Method for Sulfur in Petroleum and PetroleumProducts by Energy Dispersive X-ray Fluorescence Spec-tromet
18、ryD4307 Practice for Preparation of Liquid Blends for Use asAnalytical StandardsD4628 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 Oxida
19、tive Combustion andChemiluminescence DetectionD4927 Test Methods for Elemental Analysis of Lubricantand Additive ComponentsBarium, Calcium, Phospho-rus, Sulfur, and Zinc by Wavelength-Dispersive X-RayFluorescence SpectroscopyD4929 Test Methods for Determination of Organic ChlorideContent in Crude Oi
20、lD4951 Test Method for Determination of Additive Ele-ments in Lubricating Oils by Inductively Coupled PlasmaAtomic Emission SpectrometryD5056 Test Method for Trace Metals in Petroleum Coke byAtomic AbsorptionD5059 Test Methods for Lead in Gasoline by X-Ray Spec-troscopyD5184 Test Methods for Determi
21、nation of Aluminum andSilicon in Fuel Oils by Ashing, Fusion, InductivelyCoupled Plasma Atomic Emission Spectrometry, andAtomic Absorption SpectrometryD5185 Test Method for Determination of Additive Ele-ments, Wear Metals, and Contaminants in Used Lubricat-ing Oils and Determination of Selected Elem
22、ents in BaseOils by Inductively Coupled Plasma Atomic EmissionSpectrometry (ICP-AES)D5291 Test Methods for Instrumental Determination ofCarbon, Hydrogen, and Nitrogen in Petroleum Productsand LubricantsD5384 Test Methods for Chlorine in Used Petroleum Prod-ucts (Field Test Kit Method)D5453 Test Meth
23、od 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 Atomic Emission Spectrom-etry (ICP-AES)D5622 Test Methods for Determin
24、ation of Total Oxygen inGasoline and Methanol Fuels by Reductive PyrolysisD5708 Test Methods for Determination of Nickel, Vana-dium, and Iron in Crude Oils and Residual Fuels byInductively Coupled Plasma (ICP)Atomic Emission Spec-trometryD5762 Test Method for Nitrogen in Petroleum and Petro-leum Pro
25、ducts by Boat-Inlet ChemiluminescenceD5800 Test Method for Evaporation Loss of LubricatingOils by the Noack MethodD5863 Test Methods for Determination of Nickel, Vana-dium, Iron, and Sodium in Crude Oils and Residual Fuelsby Flame Atomic Absorption SpectrometryD6334 Test Method for Sulfur in Gasolin
26、e by WavelengthDispersive X-Ray FluorescenceD6443 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)D6445 Test Method
27、 for Sulfur in Gasoline by Energy-Dispersive X-ray Fluorescence Spectrometry3D6470 Test Method for Salt in Crude Oils (PotentiometricMethod)D6481 Test Method for Determination of Phosphorus, Sul-fur, Calcium, and Zinc in Lubrication Oils by EnergyDispersive X-ray Fluorescence SpectroscopyD6595 Test
28、Method 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 Fluorescenc
29、eD6728 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-etryD6792 Practice for Quality System in Petroleum
30、Productsand Lubricants Testing LaboratoriesD6920 Test Method for Total Sulfur in Naphthas, Distil-lates, Reformulated Gasolines, Diesels, Biodiesels, and3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.D7578 1012Motor Fuels by Oxidative Combustion and El
31、ectrochemi-cal DetectionD7039 Test Method for Sulfur in Gasoline and Diesel Fuelby Monochromatic Wavelength Dispersive X-ray Fluores-cence SpectrometryD7040 Test Method for Determination of Low Levels ofPhosphorus in ILSAC GF 4 and Similar Grade Engine Oilsby Inductively Coupled Plasma Atomic Emissi
32、on Spec-trometryD7041 Test Method for Determination of Total Sulfur inLight Hydrocarbons, Motor Fuels, and Oils by Online GasChromatography with Flame Photometric DetectionD7111 Test Method for Determination of Trace Elements inMiddle Distillate Fuels by Inductively Coupled PlasmaAtomic Emission Spe
33、ctrometry (ICP-AES)D7171 Test Method for Hydrogen Content of Middle Dis-tillate Petroleum Products by Low-Resolution PulsedNuclear Magnetic Resonance SpectroscopyD7212 Test Method for Low Sulfur in Automotive Fuels byEnergy-Dispersive X-ray Fluorescence Spectrometry Us-ing a Low-Background Proportio
34、nal CounterD7220 Test Method for Sulfur in Automotive Fuels byPolarization X-ray Fluorescence SpectrometryD7260 Practice for Optimization, Calibration, and Valida-tion of Inductively Coupled Plasma-Atomic EmissionSpectrometry (ICP-AES) for Elemental Analysis of Petro-leum Products and LubricantsD730
35、3 Test Method for Determination of Metals in Lubri-cating Greases by Inductively Coupled Plasma AtomicEmission SpectrometryD7318 Test Method for Existent Inorganic Sulfate in Etha-nol by Potentiometric TitrationD7319 Test Method for Determination of Existent andPotential Sulfate and Inorganic Chlori
36、de in Fuel Ethanolby Direct Injection Suppressed Ion ChromatographyD7328 Test Method for Determination of Existent andPotential Inorganic Sulfate and Total Inorganic Chloride inFuel Ethanol by Ion Chromatography Using AqueousSample InjectionD7343 Practice for Optimization, Sample Handling, Cali-brat
37、ion, and Validation of X-ray Fluorescence Spectrom-etry Methods for Elemental Analysis of Petroleum Prod-ucts and LubricantsD7455 Practice for Sample Preparation of Petroleum andLubricant Products for Elemental AnalysisE77 Test Method for Inspection and Verification of Ther-mometersE319 Practice for
38、 the Evaluation of Single-Pan MechanicalBalancesE898 Test Method of Testing Top-Loading, Direct-ReadingLaboratory Scales and Balances2.2 NIST Standard:4NIST Special Publication 260-136 Definitions of Terms andModes Used at NIST for Value-Assignment of ReferenceMaterials for Chemical Measurements2.3
39、ISO Standard:5ISO Guide 30 Terms and definitions used in connection withreference materials3. Terminology3.1 Definitions:3.1.1 calibration standard, nmaterial with a certifiedvalue for a relevant property, issued by or traceable to anational organization such as NIST, and whose properties areknown w
40、ith sufficient accuracy to permit its use to evaluate thesame property of another sample. D67923.1.2 certified reference material, CRM, nreference ma-terial one or more of whose property values are certified by atechnically valid procedure, accompanied by a traceable cer-tificate or other documentat
41、ion which is issued by a certifyingbody. ISO Guide 303.1.3 check standard, nmaterial having an assigned(known) value (reference value) used to determine the accu-racy of the measurement system or instrument. This standard isnot used to calibrate the measurement instrument or system.D71713.1.4 refere
42、nce material, RM, nmaterial with acceptedreference value(s), accompanied by an uncertainty at a statedlevel of confidence for desired properties, which may be usedfor calibration or quality control purposes in the laboratory.3.1.4.1 DiscussionSometimes these may be prepared “in-house” provided the r
43、eference values are established usingstandard primary procedures with known precision uncertain-ties. See below for further discussion. D67923.1.5 traceability, nproperty of the result of a measure-ment or the value of a standard whereby it can be related tostated references, usually national or int
44、ernational standards,through an unbroken chain of comparisons all having stateduncertainties. D67924. Summary of Guide4.1 This guide covers procedures used for calibrating instru-ments or methods for the analysis of petroleum products orlubricant samples for elemental analysis measurements. Themeans
45、 of calibration may vary from none to elaborate depen-dent on the test method and the measurement technique used.Test method requirements will take precedence over this guidewhere applicable.4.2 This guide may also be applicable to non-petroleumbased biofuels. Work is underway to validate this.5. Si
46、gnificance and Use5.1 Crude oil, petroleum, petroleum products, additives,biofuels, and lubricants are routinely analyzed for their el-emental content such as chlorine, nitrogen, hydrogen, phos-phorus, sulfur, and various metals using a variety of analyticaltechniques. Some of these methods require
47、little to no methodcalibration; some others require only simple one step calibra-tion; while others require elaborate calibration routine beforethe product is analyzed for its elemental content.4Available from National Institute of Standards and Technology (NIST), 100Bureau Dr., Stop 1070, Gaithersb
48、urg, MD 20899-1070, http:/www.nist.gov.5Available from International Organization for Standardization (ISO), 1, ch. dela Voie-Creuse, Case postale 56, CH-1211, Geneva 20, Switzerland, http:/www.iso.ch.D7578 10135.2 Fairly often it can be shown that the round robin resultsby a co-operator are all bia
49、sed 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 estimate or the data being dropped fromthe study as an outlier.5.2.1 Another cause of such discrepancies could be differentor inadequate calibration practice used in the laboratory. Mosttest methods spell out the calibration requirements but often donot quote the frequency required letting the laboratories usegood laboratory pr
