ASTM D1977-2003(2008) Standard Test Method for Nickel and Vanadium in FCC Equilibrium Catalysts by Hydrofluoric Sulfuric Acid Decomposition and Atomic Spectroscopic Analysis《用氢氟酸 硫.pdf

1、Designation: D 1977 03 (Reapproved 2008)Standard Test Method forNickel and Vanadium in FCC Equilibrium Catalysts byHydrofluoric/Sulfuric Acid Decomposition and AtomicSpectroscopic Analysis1This standard is issued under the fixed designation D 1977; the number immediately following the designation in

2、dicates 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 determinati

3、on of nickel andvanadium in equilibrium catalysts where the vanadium andnickel concentrations are greater than 50 and 25 mg/kg,respectively.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport t

4、o 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. Referenced Documents2.1 ASTM Standards:2D 1193 S

5、pecification for Reagent WaterD 3766 Terminology Relating to Catalysts and CatalysisE 105 Practice for Probability Sampling Of MaterialsE 177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE 288 Specification for Laboratory Glass Volumetric FlasksE 456 Terminology Relating to Qu

6、ality and StatisticsE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 U.S. Federal Specification:3Federal Specification NNN-P-395C Tolerance for Class APipets3. Terminology3.1 DefinitionsSee Terminology D 3766.4. Summary of Test Method4.1 The test s

7、pecimen (as received) is decomposed withhydrofluoric and sulfuric acids.After complete volatilization ofthe hydrofluoric acid and cooling, the sulfate salts are diluted tothe appropriate concentration range for analysis by flameatomic absorption, direct current plasma emission, or induc-tively coupl

8、ed plasma emission spectroscopies. The instrumentis calibrated with matrix-matched standards. Solutions of thetest specimen are analyzed.5. Significance and Use5.1 This test method is a procedure by which catalystsamples may be compared on an inter- or intra-laboratorybasis. Catalyst producers and u

9、ser should find this test methodto be of value.6. Interferences6.1 The enhancement of alumina in the samples are over-come by using matrix-matched standards. Any dilutionsneeded to achieve the working ranges for vanadium and nickelmust contain the same Al2O3(7800 ppm) concentration as thestandards.6

10、.2 If using optical emission, consult tables showing inter-fering line near analyte lines; if significant overlap occurs, onemust apply interelement correction or choose an alternateemission line.7. Apparatus7.1 Analytical Balance, capable of weighing to nearest0.1 mg.7.2 Hot Plate, capable of maint

11、aining 250 6 10C atsurface.7.3 TFE Fluorocarbon Beaker, 250 mL.7.4 Volumetric Flasks, borosilicate glass, 50, 100, 250, 500,and 1000-mL capacity conforming to Specification E 288.1This test method is under the jurisdiction of ASTM Committee D32 onCatalysts and is the direct responsibility of Subcomm

12、ittee D32.03 on ChemicalComposition.Current edition approved April 1, 2008. Published April 2008. Originallyapproved in 1991. Last previous edition approved in 2003 as D 197703.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. F

13、or Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.1Copyright ASTM International, 100 Barr Harbor Drive,

14、 PO Box C700, West Conshohocken, PA 19428-2959, United States.7.5 Pipettes, borosilicate glass, 5, 10, and 25 mL, conform-ing to Federal Specification NNN-P-395C.7.6 Bottles, polyethylene, 100 and 1000 mL.8. Reagents8.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless othe

15、rwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society, wheresuch specifications are available.4Other grades may be used,provided it is first ascertained that the reagent is of sufficientpurity to permit

16、its use without lessening the accuracy of thedetermination.8.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean type IV reagent water, asdefined in Specification D 1193.8.3 Required Reagents:8.3.1 Hydrofluoric Acid (HF), concentrated, 48 %.8.3.2 Sulfuric Acid

17、,(H2SO4), concentrated, 98 %.8.3.3 Sulfuric Acid, 49 volume %, add slowly, while stirring,one part of concentrated H2SO4(98 %) to one part of water,then cool.8.3.4 Hydrochloric Acid, concentrated, 38 %.8.3.5 Hydrochloric Acid, 19 volume %, add slowly, whilestirring, one part of concentrated HCl (38

18、%) to one part ofwater, then cool.8.3.6 Nitric Acid (HNO3), concentrated, 70 %.8.3.7 Reference Standard Solution1000 mg/L nickel (seeNote 1).NOTE 1If emission spectrometry is to be used, standards must containno interfering element(s) in concentration(s) great enough to yield aninterference of more

19、than 0.1% of the analytical response.8.3.8 Reference Standard Solution1000 mg/L vanadium(see Note 1).8.3.9 Aluminum Chloride, reagent grade, AlCl36H2O8.3.10 Aluminum Stock Solution39 000 mg/L Al2O3, dis-solve 184.5 g of AlCl36H2O in water and dilute to 1 L andstore in a polyethylene bottle.8.3.11 Hy

20、drogen Peroxide3 % solution.9. Sampling9.1 The selection of a representative analytical sample fromthe bulk material is outside the scope of this test method.Parties using this test method for comparison purposes willhave agreed on the selection of an analytical sample. If asampling procedure is des

21、ired, Practice E 105 is recommended.10. Preparation of Standards10.1 NickelPrepare standard solutions containing 0, 5.0,20.0, and 50.0 mg/L Ni in a matrix of 7800 mg/L Al2O3and10 % hydrochloric acid by transferring 0, 5.0, 20.0, and50.0 mL of the 1000-mg/L solution to 1000-mL volumetricflasks contai

22、ning 200 mL of the 39 000-mg/L Al2O3solutionand 100 mL concentrated hydrochloric acid. Dilute solutions tovolume with distilled water and store in polyethylene bottles.10.2 VanadiumPrepare standard solutions containing 0,10.0, 25.0, 50.0 and 100.0 mg/L V in a matrix of 7800 mg/LAl2O3and 10 % hydroch

23、loric acid by transferring 0, 10.0, 25.0,50.0, and 100.0 mL of the 1000-mg/L solution to 1000-mLvolumetric flasks containing 200 mL of the 39 000-mg/LAl2O3solution and 100 mL concentrated hydrochloric acid. Dilutesolutions to volume with distilled water and store in polyeth-ylene bottles.11. Procedu

24、re11.1 Weigh three test specimens of approximately 2.0 geach to the nearest 0.1 mg and transfer to 250-mL TFE-fluorocarbon beakers. A reagent blank should be carried alongwith each set of samples.11.2 Add 10 mL 48 % sulfuric acid, 10 mL concentratednitric acid, and 10 mL concentrated hydrofluoric ac

25、id.11.3 Transfer beaker and contents to a hot plate (no hotterthan 250C to avoid melting the beaker) and evaporate to neardryness.11.4 Remove beaker from hot plate and cool to ambienttemperature.11.5 Add 20 mL 19 % hydrochloric acid and 30 mL 3%hydrogen peroxide, cover with watch glass and return be

26、aker tohot plate.11.6 Heat solution to boiling and continue to boil until allthe salts are dissolved.11.7 After dissolution is complete, remove beaker from hotplate and cool to ambient temperature.11.8 Wash watch glass, catching washings in the beaker, andtransfer solution quantitatively to a 100-mL

27、 volumetric flask.Dilute to volume with water and mix well.11.9 Using direct current argon plasma spectrometry (DCP),inductively coupled argon plasma spectrometry (ICP), oratomic absorption spectrophotometry (AAS), determine con-centration of analytes in solutions of test specimens. If appar-ent con

28、centration is greater than that of the most concentratedstandard, perform an additional dilution so that result isbracketed by two or more standards.12. Calculations12.1 Calculate the concentration of nickel and vanadium asfollows:mg/L metal 5C 3 DS(1)where:C = concentration of metal in solution, mg

29、/kg,D = volume equivalent of dilution used for analysis; ifsolution 10.8 is used directly, D = 100 mL. If a furtherdilution is needed, D = 100 mL 3 V2/V1, where V1isthe aliquot of solution 10.8 and V2is the volume towhich it was diluted, andS = Sample mass.4Reagent Chemicals, American Chemical Socie

30、ty Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeia

31、l Convention, Inc. (USPC), Rockville,MD.D 1977 03 (2008)213. Precision and Bias13.1 Test ProgramAn interlaboratory study was con-ducted in which the named property was measured in threeseparate test materials in eight separate laboratories. PracticeE 691, modified for non-uniform data sets, was foll

32、owed forthe data reduction period.13.2 PrecisionPairs of test results obtained by a proce-dure similar to that described in the study are expected to differin absolute value by less than 2.772 S, where 2.772 S is the95 % probability interval limit on the difference between twotest results, and S is

33、the appropriate estimate of standarddeviation. Definitions and usage are given in TerminologyE 456 and Practice E 177, respectively.Test Resultsfor Ni(Consensus Mean)95 % RepeatabilityInterval(Within Laboratory)95 % ReproducibilityInterval(Between Laboratories)208 mg/kg 8 mg/kg(3.9 % of mean)14 mg/k

34、g(6.7 % of mean)152 mg/kg 5 mg/kg(3.3 % of mean)24 mg/kg(15.8 % of mean)437 mg/kg 9 mg/kg(2.1 % of mean)31 mg/kg(7.1 % of mean)Test Results for V(Consensus Mean)95 % RepeatabilityInterval(Within Laboratory)95 % ReproducibilityInterval(Between Laboratories)1191 mg/kg 43 mg/kg(3.6 % of mean)201 mg/kg(

35、16.9 % of mean)1898 mg/kg 72 mg/kg(3.8 % of mean)303 mg/kg(16.0 % of mean)3346 mg/kg 82 mg/kg(2.4% of mean)531 mg/kg(15.9 % of mean)13.3 BiasThis test method described is without knownbias since there is by definition no absolute standard forcomparison.14. Keywords14.1 acid decomposition; atomic spe

36、ctroscopy; ECAT; FCCequilibrium catalysts; nickel; vanadiumASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such pat

37、ent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited eit

38、her for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair

39、hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 1977 03 (2008)3