1、Designation: D7578 10Standard 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, t
2、he 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 guide covers different ways by which the testmethods used for elemental analysis of petroleum product
3、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 laboratories.1.3 This guide includes only the basic steps for generallyencountered instrume
4、nt 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 test method to be used, caveats it contains, andadditional instrument preparation
5、 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-ration of non-petroleum based bio-fuels for elemental analysis.Work is underway on
6、 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 thisstandard.1.8 This standard does not purport to address all of thesafety con
7、cerns, 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:2D129 Test Method for Sulfur in Petrole
8、um 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 Chlorine in New and Used PetroleumProducts (Bomb Method)D874 Test Method for Sulfate
9、d 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 AdditivesD1266 Test Method for Sulfur in Petroleum Products(Lamp Method)D1318 Test Me
10、thod 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 Nitrate in Diesel FuelsD2622 Test Method for Sulfur in Petroleum Products byWavel
11、ength 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 by Oxidative Microcou-lometryD3228 Test Method for Total Nitrogen in Lubricatin
12、g Oilsand 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-sorption Spectroscopy1This practice is under the jurisdiction of ASTM Committee D02 on Petroleu
13、mProducts and Lubricants and is the direct responsibility of Subcommittee D02.03 onElemental Analysis.Current edition approved Feb. 15, 2010. Published March 2010. DOI: 10.1520/D7578-10.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceas
14、tm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshoho
15、cken, PA 19428-2959, United States.D3246 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 GasolineIodineMonochloride MethodD3348 Test Method for Rapid Field Test for Tr
16、ace Lead inUnleaded 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
17、 and Rateometric 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 Fluoresc
18、ence Spec-trometryD4307 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 Syr
19、inge/Inlet Oxidative 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 ChlorideCon
20、tent in Crude OilD4951 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 Met
21、hods for Determination 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
22、of Selected Elements 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
23、)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 Atomic Emission Spectrom-etry (ICP-AES)D5622 Test Meth
24、ods for Determination 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 an
25、d Petro-leum Products 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 S
26、ulfur in Gasoline 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)D
27、6445 Test Method 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 Spectro
28、scopyD6595 Test 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 Ultravi
29、olet FluorescenceD6728 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 Syst
30、em in Petroleum Productsand Lubricants Testing LaboratoriesD6920 Test Method for Total Sulfur in Naphthas, Distil-lates, Reformulated Gasolines, Diesels, Biodiesels, andMotor Fuels by Oxidative Combustion and Electrochemi-cal DetectionD7039 Test Method for Sulfur in Gasoline and Diesel Fuelby Monoch
31、romatic Wavelength Dispersive X-ray Fluores-cence SpectrometryD7040 Test Method for Determination of Low Levels ofPhosphorus in ILSAC GF 4 and Similar Grade Engine OilsD7578 102by Inductively Coupled Plasma Atomic Emission Spec-trometryD7041 Test Method for Determination of Total Sulfur inLight Hydr
32、ocarbons, 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 Spectrometry (ICP-AES)D7171 Test Method for Hydrogen Content of Middle Dis-tillate
33、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 Proportional CounterD7220 Test Method for Sulfur in Automotive Fuels byPolarization X-ray
34、 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 LubricantsD7303 Test Method for Determination of Metals in Lubri-cating Greases by Inductively
35、 Coupled Plasma AtomicEmission SpectrometryD7318 Test Method for Total Inorganic Sulfate in Ethanolby Potentiometric TitrationD7319 Test Method for Determination of Total and Poten-tial Sulfate and Inorganic Chloride in Fuel Ethanol byDirect Injection Suppressed Ion ChromatographyD7328 Test Method f
36、or Determination of Total and Poten-tial Inorganic Sulfate and Total Inorganic Chloride in FuelEthanol by Ion Chromatography Using Aqueous SampleInjectionD7343 Practice for Optimization, Sample Handling, Cali-bration, and Validation of X-ray Fluorescence Spectrom-etry Methods for Elemental Analysis
37、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 the Evaluation of Single-Pan MechanicalBalancesE898 Test Method of Testing Top-Loading
38、, 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 ISO Standard:5ISO Guide 30 Terms and definitions used in connection withreference mater
39、ials3. 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 with sufficient accuracy to permit its use to evaluate thesame property of another sampl
40、e. 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 documentation which is issued by a certifyingbody. ISO Guide 303.1.3 check standard, nmaterial ha
41、ving 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 reference material, RM, nmaterial with acceptedreference value(s), accompanied by an uncertai
42、nty 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 reference values are established usingstandard primary procedures with known precision u
43、ncertain-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 international standards,through an unbroken chain of comparisons all having stateduncertai
44、nties. 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 of calibration may vary from none to elaborate depen-dent on the test method and the m
45、easurement 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. Significance and Use5.1 Crude oil, petroleum, petroleum products, additives,biofuels, and
46、 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 little to no methodcalibration; some others require only simple one step calibra-tion;
47、while others require elaborate calibration routine beforethe product is analyzed for its elemental content.5.2 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 laboratorypract
48、ices 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.4Available from National Institute of Standards and Technology (NIST), 100Bureau Dr., Stop 1070,
49、 Gaithersburg, 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 1035.2.1 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 practices for this task. Thus, uniform practicefor instrument calibration would be beneficial i
