1、Designation: D1977 03 (Reapproved 2008)D1977 16Standard Test Method forNickel and Vanadium in FCC Equilibrium Catalysts byHydrofluoric/Sulfuric Acid Decomposition and AtomicSpectroscopic Analysis1This standard is issued under the fixed designation D1977; the number immediately following the designat
2、ion 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 () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determ
3、ination of nickel and vanadium in equilibrium catalysts where the vanadium and nickelconcentrations are greater than 50 and 25 mg/kg, respectively.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 This standard does not
4、purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D
5、1193 Specification for Reagent WaterD3766 Terminology Relating to Catalysts and CatalysisE105 Practice for Probability Sampling of MaterialsE177 Practice for Use of the Terms Precision and Bias in ASTM Test MethodsE288 Specification for Laboratory Glass Volumetric FlasksE456 Terminology Relating to
6、Quality and StatisticsE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method2.2 U.S. Federal Specification:3Federal Specification NNN-P-395C Tolerance for Class A Pipets3. Terminology3.1 DefinitionsSee Terminology D3766.4. Summary of Test Method4.1 The test
7、 specimen (as received) is decomposed with hydrofluoric and sulfuric acids. After complete volatilization of thehydrofluoric acid and cooling, the sulfate salts are diluted to the appropriate concentration range for analysis by flame atomicabsorption, direct current plasma emission, or inductively c
8、oupled plasma emission spectroscopies. The instrument is calibratedwith matrix-matched standards. Solutions of the test specimen are analyzed.5. Significance and Use5.1 This test method is a procedure by which catalyst samples may be compared on an inter- or intra-laboratory basis. Catalystproducers
9、 and user should find this test method to be of value.1 This test method is under the jurisdiction of ASTM Committee D32 on Catalysts and is the direct responsibility of Subcommittee D32.03 on Chemical Composition.Current edition approved April 1, 2008March 1, 2016. Published April 2008April 2016. O
10、riginally approved in 1991. Last previous edition approved in 20032008 asD197703. 03 (2008). DOI: 10.1520/D1977-03R08.10.1520/D1977-16.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume info
11、rmation, refer to the standards Document Summary page on the ASTM website.3 Available from Standardization Documents Order Desk, Bldg. 4 Section D, DLA Document Services, Building 4/D, 700 Robbins Ave., Philadelphia, PA 19111-5094,Attn: NPODS.http:/quicksearch.dla.mil.This document is not an ASTM st
12、andard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all ca
13、ses only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16. Interferences6.1 The enhancement of alumina in the samples are overcome by u
14、sing matrix-matched standards. Any dilutions needed toachieve the working ranges for vanadium and nickel must contain the same Al2O3 (7800 ppm) concentration as the standards.6.2 If using optical emission, consult tables showing interfering line near analyte lines; if significant overlap occurs, one
15、 mustapply interelement correction or choose an alternate emission line.7. Apparatus7.1 Analytical Balance, capable of weighing to nearest 0.1 mg.7.2 Hot Plate, capable of maintaining 250 6 10C at surface.7.3 TFEPTFE Fluorocarbon Beaker, 250 mL.mL and PTFE watch glass.7.4 Volumetric Flasks, borosili
16、cate glass, 50, 100, 250, 500, and 1000-mL capacity conforming to Specification E288.7.5 Pipettes, borosilicate glass, 5, 10, and 25 mL, conforming to Federal Specification NNN-P-395C.7.6 Bottles, polyethylene, 100 and 1000 mL.8. Reagents8.1 Purity of ReagentsReagent grade chemicals shall be used in
17、 all tests. Unless otherwise indicated, it is intended that allreagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where suchspecifications are available.4 Other grades may be used, provided it is first ascertained that the reagent is of s
18、ufficient purity topermit its use without lessening the accuracy of the determination.8.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean type IV reagent water, wateror better, as defined in Specification D1193.8.3 Required Reagents:8.3.1 Hydrofluoric Acid
19、(HF), concentrated, 48 %.8.3.2 Sulfuric Acid, (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, thencool.8.3.4 Hydrochloric Acid, concentrated, 38 %.8.3.5 Hydrochloric Acid, 19 volume %, add slowly, w
20、hile stirring, one part of concentrated HCl (38 %) to one part of water,then cool.8.3.6 Nitric Acid (HNO3), concentrated, 70 %.8.3.7 Reference Standard Solution1000 mg/L nickel (see Note 1).NOTE 1If emission spectrometry is to be used, standards must contain no interfering element(s) in concentratio
21、n(s) great enough to yield aninterference of more 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, dissolve 184.5 g of AlCl36H2O in water and dilute
22、to 1 L and store ina polyethylene bottle.8.3.11 Hydrogen Peroxide3 % solution.9. Sampling9.1 The selection of a representative analytical sample from the bulk material is outside the scope of this test method. Partiesusing this test method for comparison purposes will have agreed on the selection of
23、 an analytical sample. If a sampling procedureis desired, Practice E105 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 Al2O3 and 10 %hydrochloric acid by transferring 0, 5.0, 20.0, and 50.0 mLof the
24、1000-mg/Lsolution to 1000-mLvolumetric flasks containing 200mLof the 39 000-mgLAl2O3 solution and 100 mLconcentrated hydrochloric acid. Dilute solutions to volume with distilled waterand store in polyethylene bottles.4 Reagent Chemicals, American Chemical Society Specifications, American Chemical So
25、ciety, Washington, DC. For Suggestions on the testing of reagents not listed bythe American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC),(USP), Rock
26、ville, MD.D1977 16210.2 VanadiumPrepare standard solutions containing 0, 10.0, 25.0, 50.0 and 100.0 mg/L V in a matrix of 7800 mg/L Al2O3and 10 % hydrochloric acid by transferring 0, 10.0, 25.0, 50.0, and 100.0 mL of the 1000-mg/L solution to 1000-mL volumetricflasks containing 200 mL of the 39 000-
27、mgL Al2O3 solution and 100 mL concentrated hydrochloric acid. Dilute solutions tovolume with distilled water and store in polyethylene bottles.11. Procedure11.1 Weigh three test specimens of approximately 2.0 g each to the nearest 0.1 mg and transfer to 250-mL TFE-fluorocarbonPTFE-fluorocarbon beake
28、rs. A reagent blank should be carried along with each set of samples.11.2 Add First, add 10 mL 48 % sulfuric acid, then 10 mL concentrated nitric acid, and 10 mL concentrated hydrofluoricacid.acid at last.11.3 Transfer beaker and contents to a hot plate (no hotter than 250C to avoid melting the beak
29、er) and evaporate to neardryness.11.4 Remove beaker from hot plate and cool to ambient temperature.11.5 Add 20 mL 19 % hydrochloric acid and 30 mL 3% hydrogen peroxide, cover with a PTFE watch glass and return beakerto hot plate.11.6 Heat solution to boiling and continue to boil until all the salts
30、are dissolved.11.7 After dissolution is complete, remove beaker from hot plate and cool to ambient temperature.11.8 Wash watch glass, catching washings in the beaker, and transfer solution quantitatively to a polymethylpentene (PMP)plastic 100-mL volumetric flask. Dilute to volume with water and mix
31、 well.11.9 Using direct current argon plasma spectrometry (DCP), inductively coupled argon plasma spectrometry (ICP), or atomicabsorption spectrophotometry (AAS), determine concentration of analytes in solutions of test specimens. If apparent concentrationis greater than that of the most concentrate
32、d standard, perform an additional dilution so that result is bracketed by two or morestandards. If internal standard is required, calibration standard must match preparation sample matrix.12. Calculations12.1 Calculate the concentration of nickel and vanadium as follows:mg/Lmetal5C3DS (1)where:where
33、:C = concentration of metal in solution, mg/kg,D = volume equivalent of dilution used for analysis; if solution 10.8 is used directly, D = 100 mL. If a further dilution is needed,D = 100 mL V2/V1, where V1 is the aliquot of solution 10.8 and V2 is the volume to which it was diluted, andS = Sample ma
34、ss.13. Precision and Bias13.1 Test ProgramAn interlaboratory study was conducted in which the named property was measured in three separate testmaterials in eight separate laboratories. Practice E691, modified for non-uniform data sets, was followed for the data reductionperiod.13.2 PrecisionPairs o
35、f test results obtained by a procedure similar to that described in the study are expected to differ inabsolute value by less than 2.772 S, where 2.772 S is the 95 % probability interval limit on the difference between two test results,and S is the appropriate estimate of standard deviation. Definit
36、ions and usage are given in Terminology E456 and Practice E177,respectively.D1977 163Test Resultsfor Ni(Consensus Mean)95 % RepeatabilityInterval(Within Laboratory)95 % ReproducibilityInterval(Between Laboratories)Test Resultsfor Ni(Consensus Mean)95 % RepeatabilityInterval(Within Laboratory)95 % Re
37、producibilityInterval(Between Laboratories)208 mg/kg 8 mg/kg(3.9 % of mean)14 mg/kg(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 % Reprodu
38、cibilityInterval(Between Laboratories)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(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 m
39、g/kg(2.4% of mean)531 mg/kg(15.9 % of mean)13.3 BiasThis test method described is without known bias since there is by definition no absolute standard for comparison.14. Keywords14.1 acid decomposition; atomic spectroscopy; ECAT; FCC equilibrium catalysts; nickel; vanadiumASTM International takes no
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