ASTM D7111-2005 Standard Test Method for Determination of Trace Elements in Middle Distillate Fuels by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)《用感应耦合等离子体原子.pdf
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1、Designation: D 7111 05An American National StandardStandard Test Method forDetermination of Trace Elements in Middle Distillate Fuelsby Inductively Coupled Plasma Atomic EmissionSpectrometry (ICP-AES)1This standard is issued under the fixed designation D 7111; the number immediately following the de
2、signation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the
3、 determination of selectedelements in middle distillate fuels by inductively coupledplasma atomic emission spectrometry (ICP-AES). The specificelements are listed in Table 1. The concentration range of thistest method is approximately 0.1 to 2.0 mg/kg. The test methodmay be used for concentrations o
4、utside of this range; however,the precision statements may not be applicable. Middle distil-late fuels covered in this test method have all distillationfractions contained within the boiling range of 150 to 390C.This includes, but is not limited to, diesel fuels and aviationturbine fuels.1.2 This te
5、st method is not intended to analyze insolubleparticulates. However, very small particulate matter (smallerthan a micrometre) will be carried into the plasma and beincluded in the quantitative analysis.1.3 This test method may give a result that is higher than thetrue value if an analyte is present
6、in the sample in a form whichis sufficiently volatile. For example, hexamethyldisiloxane willgenerate a biased high result for silicon.1.4 The values stated in SI units are to be regarded asstandard.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its
7、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:2D 2880 Specification for Gas Turbine Fuel OilsD 3605 Test Method for Trac
8、e Metals in Gas Turbine Fuelsby Atomic Absorption and Flame Emission SpectroscopyD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4306 Practice for Aviation Fuel Sample Containers forTests Affected by Trace ContaminationD 5185 Test Method for Determination of Additive Ele-ment
9、s, Wear Metals, and Contaminants in Used Lubricat-ing Oils and Determination of Selected Elements in BaseOils by Inductively Coupled Plasma Atomic EmissionSpectrometry (ICP-AES)D 6299 Practice for Applying Statistical Quality AssuranceTechniques to Evaluate Analytical Measurement SystemPerformanceD
10、6792 Guide for Quality System in Petroleum Productsand Lubricants Testing Laboratories2.2 Military Standard:MIL-F-16884J Military Specification, Fuel, Naval Distil-late33. Terminology3.1 Definitions:1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants
11、 and is the direct responsibility of SubcommitteeD02.03 on Elemental Analysis.Current edition approved April 1, 2005. Published May 2005.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume i
12、nformation, refer to the standards Document Summary page onthe ASTM website.3Naval Sea Systems Command (NAVSEA), SEA03R42, 1333 Isaac Hull Ave.,SE, Washington, DC 20376.TABLE 1 Elements and Recommended WavelengthsElement Wavelengths, nmAluminum 308.215, 396.153Barium 455.403, 493.408Calcium 393.366C
13、hromium 267.716, 283.563Copper 324.752Iron 259.939Lithium 670.784Lead 224.688, 283.306Magnesium 279.553Manganese 257.610Molybdenum 204.597, 281.616Nickel 221.648, 341.476Potassium 766.490Sodium 588.995Silicon 251.611Silver 328.068Titanium 334.940Vanadium 310.230Zinc 213.8571Copyright ASTM Internatio
14、nal, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.1 calibration, nthe determination of the values of thesignificant parameters by comparison with values indicated bya set of reference standards.3.1.2 calibration curve, nthe graphical or mathematicalrepresen
15、tation of a relationship between the assigned (known)values of standards and the measured responses from themeasurement system.3.1.3 calibration standard, na standard having an ac-cepted value (reference value) for use in calibrating a measure-ment instrument or system.3.1.4 detection limit, na stat
16、ed limiting value that desig-nates the lowest concentration that can be determined withconfidence and that is specific to the analytical procedure used.3.1.5 emission spectroscopy, nmeasurement of the energyspectrum emitted by or from an object under some form ofenergetic stimulation; for example, l
17、ight or electrical discharge.3.1.6 inductively coupled plasma, na high temperaturedischarge generated by passing an ionizable gas through amagnetic field induced by a radio frequency coil surroundingthe tubes that carry the gas.3.1.7 radio frequency, nthe range of frequencies between3 kHz and 300 GH
18、z.3.1.8 standard, na physical or chemical reference used asa basis for comparison or calibration.3.2 Definitions of Terms Specific to This Standard:3.2.1 detection limit, nthe lowest concentration value foran element that can be determined by ICP analysis and that iscalculated by multiplying three t
19、imes the standard deviation often repetitive element analyses of the blank solution.3.2.2 internal standard, na chemical standard having anaccepted value (and added to the fuel test specimen andcalibration standard) to determine the emission intensity ratioof an element to the internal standard.4. S
20、ummary of Test Method4.1 Calibration standards are prepared by mixing organo-metallic standard materials in kerosine. An internal standardmaterial is added to the calibration standards and fuel samples.The calibration standards and the fuel samples are aspiratedinto the ICP-AES instrument. The conce
21、ntrations of the ele-ments in the fuel are calculated by comparing emissionintensity ratios of the fuel and calibration standards to theinternal standard.5. Significance and Use5.1 Trace elemental analysis is used to indicate the level ofcontamination of middle distillate fuels. Trace metals in turb
22、inefuels can cause corrosion and deposition on turbine compo-nents at elevated temperatures. Some diesel fuels have speci-fication limit requirements for trace metals to guard againstengine deposits. Trace level copper in middle distillate aviationturbine fuel can significantly accelerate thermal in
23、stability ofthe fuel leading to oxidation and production of detrimentalinsoluble deposits in the engine.5.2 Gas turbine fuel oil Specification D 2880 providesrecommended upper limits for five trace metals (calcium, lead,sodium, potassium, and vanadium). Military specificationMIL-F-16884J for naval d
24、istillate fuel sets requirements formaximum concentrations of the same five metals. Both speci-fications designate Test Method D 3605, an atomic absorption/flame emission method, for the quantitative analysis of four ofthe metals. Test Method D 3605 does not cover potassium. Thistest method provides
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