ASTM D7085-2004(2010)e1 0625 Standard Guide for Determination of Chemical Elements in Fluid Catalytic Cracking Catalysts by X-ray Fluorescence Spectrometry (XRF)《X射线荧光光谱法(XRF)测定流化床.pdf
《ASTM D7085-2004(2010)e1 0625 Standard Guide for Determination of Chemical Elements in Fluid Catalytic Cracking Catalysts by X-ray Fluorescence Spectrometry (XRF)《X射线荧光光谱法(XRF)测定流化床.pdf》由会员分享,可在线阅读,更多相关《ASTM D7085-2004(2010)e1 0625 Standard Guide for Determination of Chemical Elements in Fluid Catalytic Cracking Catalysts by X-ray Fluorescence Spectrometry (XRF)《X射线荧光光谱法(XRF)测定流化床.pdf(10页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: D7085 04 (Reapproved 2010)1Standard Guide forDetermination of Chemical Elements in Fluid CatalyticCracking Catalysts by X-ray Fluorescence Spectrometry(XRF)1This standard is issued under the fixed designation D7085; the number immediately following the designation indicates the year ofo
2、riginal adoption or, 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.1NOTEUpdated Scope and text to reflect the use of ppm and SI units edito
3、rially in April 2010.1. Scope1.1 This guide covers several comparable procedures for thequantitative chemical analysis of up to 29 elements in fluidcatalytic cracking (FCC) catalyst by X-ray fluorescence spec-trometry (XRF). Additional elements may be added.1.2 This guide is applicable to fresh FCC
4、catalyst, equilib-rium FCC catalyst, spent FCC catalyst, and FCC catalyst fines.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3.1 The units of ppm (mg/kg) are used instead of wt% inTables X2.3-X2.5 for reporting concentr
5、ation of certain ele-ments because of industry convention and because most ofthese elements are present at trace levels.1.4 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-pr
6、iate safety and health practices and determine the applica-bility of regulatory requirements prior to use.2. Referenced Documents2.1 ASTM Standards:2C982 Guide for Selecting Components for Energy-Dispersive X-Ray Fluorescence (XRF) Systems3C1118 Guide for Selecting Components for Wavelength-Dispersi
7、ve X-Ray Fluorescence (XRF) SystemsD1977 Test Method for Nickel and Vanadium in FCCEquilibrium Catalysts by Hydrofluoric/Sulfuric Acid De-composition and Atomic Spectroscopic AnalysisE1172 Practice for Describing and Specifying aWavelength-Dispersive X-Ray SpectrometerE1361 Guide for Correction of I
8、nterelement Effects inX-Ray Spectrometric AnalysisE1621 Guide for X-Ray Emission Spectrometric AnalysisE1622 Practice for Correction of Spectral Line Overlap inWavelength-Dispersive X-Ray Spectrometry33. Summary of Guide3.1 The test specimen is prepared with a clean, uniform, flatsurface. Two common
9、ly used test methods of preparing testspecimens are listed: briquetting a powder (Test Method A,Sections 8-15) and fusing a powder into a glass bead (TestMethod B, Sections 16-23). This surface of the fused orbriquetted specimen is irradiated with a primary source of Xrays. The secondary X rays prod
10、uced in the specimen arecharacteristic of the chemical elements present in the speci-men. Two types of XRF instrumentation may be used to collectand process the X-ray spectra. Using a wavelength-dispersiveX-ray spectrometer, the secondary X rays produced in thespecimen are dispersed according to the
11、ir wavelength bymeans of crystals or synthetic multilayers. The X-ray intensi-ties are measured by detectors set at selected wavelengths andrecorded as counts (number of X rays impinging on thedetector per unit time). Concentrations of the elements aredetermined from the measured intensities using c
12、alibrationcurves prepared from suitable reference materials. Using anenergy-dispersive X-ray spectrometer, the secondary X raysproduced in the specimen are sent to a detector where the entireX-ray spectrum is electronically sorted according to the X-ray1This guide is under the jurisdiction of ASTM C
13、ommittee D32 on Catalysts andis the direct responsibility of Subcommittee D32.03 on Chemical Composition.Current edition approved April 1, 2010. Published May 2010. Originallyapproved in 2004. Last previous edition approved in 2004 as D7085041.DOI:10.1520/D7085-04R10E01.2For referenced ASTM standard
14、s, 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. The last approved version of this historical standard is referencedon www.astm
15、.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.energy and processed into counts using a multichannel ana-lyzer. The principal advantages of the wavelength-dispersiveX-ray spectrometer are resolution and detection limit. Theprin
16、cipal advantages of the energy-dispersive X-ray spectrom-eter are speed and a generally lower equipment cost.4. Significance and Use4.1 The chemical composition of fresh FCC catalyst andequilibrium FCC catalyst is a predictor of catalyst perfor-mance. The analysis of catalyst fines also provides inf
17、ormationon the performance of the FCC unit and the fines collectiondevice(s).4.2 The chemical composition of equilibrium FCC catalystis a measure of the hazardous nature or toxicity of the materialfor purposes of disposal or secondary use.5. Apparatus5.1 X-ray Spectrometer, wavelength or energy-disp
18、ersivesystem equipped with a vacuum sample chamber. Refer toGuide C982, Guide C1118, and Practice E1172 for informationon specifying XRF systems.5.2 Muffle Furnace, capable of operating at 600C.5.3 Hot Plate, capable of maintaining a constant 200C.5.4 Porcelain Dishes, of a suitable size for calcini
19、ng 50-gsample aliquots.5.5 Vacuum Oven, capable of maintaining 60C. This isrequired only if catalyst fines are to be analyzed.5.6 Vacuum Desiccators, useful for storing fusion beads orpressed pellets.5.7 Fusion Equipment:5.7.1 Fusion Furnace or Fluxing Device, capable of oper-ating at 1100C.5.7.2 Fu
20、sion Crucibles and Molds, graphite or plati-num5 % gold alloy, sized to match the specimen holder of theX-ray spectrometer.5.8 Pressed Pellet Equipment:5.8.1 Grinders or Pulverizers, manual (such as agate, mul-lite, alumina, tungsten carbide, or boron carbide mortar andpestle) or automated (typicall
21、y with a tungsten carbide grindingvessel). Avoid steel grinding vessels.5.8.2 Mixer Mill, useful for blending ground sample andbinder prior to preparing a pressed powder specimen.5.8.3 Mixing Vials, sized to match the mixer mill.5.8.4 Briquetting Press, capable of maintaining a reproduc-ible pressur
22、e of at least 25 000 psi. This is required only if thepressed powder method is utilized. Match mold size to thespecimen holder of the X-ray spectrometer. Typical sizes are 25to 40 mm.6. Reagents6.1 Reagents for Fusion Techniques:6.1.1 Fluxes, lithium borates or carbonates or mixtures, ofultrahigh pu
23、rity.6.1.2 Non-Wetting Agents, such as lithium or ammoniumiodide, are frequently added to the flux, as are oxidizing agentssuch as lithium, potassium, or ammonium nitrate. Take carethat adding non-wetting or oxidizing reagents does not causespectral interference with the analytes of interest.6.2 Rea
24、gents for Pressed Pellet Techniques:6.2.1 Heavy Absorber, barium or hafnium oxides are com-monly used as heavy absorbers, if that technique is applied.6.2.2 Binders, required for the pressed powder technique.These should not contribute any spectral interference. Micro-crystalline wax or cellulose wi
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