1、Designation: D 4513 97 (Reapproved 2006)Standard Test Method forParticle Size Distribution of Catalytic Materials by Sieving1This standard is issued under the fixed designation D 4513; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision
2、, 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 determination of particlesize distribution of catalytic powder material usi
3、ng a sievinginstrument and is one of several found valuable for themeasurement of particle size. This test method is particularlysuitable for particles in the 20 to 420-m range.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonl
4、y.1.3 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-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced
5、 Documents2.1 ASTM Standards:2E11 Specification for Wire Cloth and Sieves for TestingPurposesE 161 Specification for Precision Electroformed SievesE 177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE 456 Terminology Relating to Quality and Statistics3. Summary of Test Method3.
6、1 A 50 % relative humidity-equilibrated sample of knownweight is allowed to fractionate on a series of various sizesieves to allow the various particle sizes to be collected onsuccessively smaller sieve openings.3.2 The sample fraction collected on each sieve of the seriesis weighed and its fraction
7、al part of the original sample isdetermined.4. Significance and Use4.1 This test method can be used to determine particle sizedistributions of catalysts and supports for materials specifica-tions, manufacturing control, and research and developmentwork.5. Apparatus5.1 Laboratory Sieving Instrument,
8、automatic with timerpreferred.5.2 U.S. Standard Sieves, or equivalent, to include microme-tres (mesh) 420(40), 250(60), 177(80), 149(100), 105(140),74(200), 44(325) and electroformed 30 and 20 micrometres.Because of their superior uniformity and resistance to distor-tion or damage during use, electr
9、oformed sieves, preferablywith square holes, are recommended. Sieves with diametersbetween 6 and 10 cm are suggested.5.3 Ultrasonic Cleaning Tank, 100 W.5.4 Transmitted Light Microscope, 300 magnification, withcalibrated scale eyepiece.5.5 Heat Gun Dryer, (hair dryer or equivalent).5.6 Analytical Ba
10、lance, capable of weighing to 0.001 g.5.7 Sample Splitter, Chute Type, or Spinning Riffler, withspinning riffler preferred.6. Reagents6.1 Antistatic Coating, (record cleaning spray or equiva-lent.)6.2 Alcohol-Water SolutionOne part ethanol to nine partsdeionized or distilled water.7. Sampling7.1 The
11、 sample must be free-flowing and homogeneous. Ifparticle size segregation is apparent to either the eye or fromobservation under a microscope, remix and resample thematerial using the proper riffling procedure.1This test method is under the jurisdiction of ASTM Committee D32 onCatalysts and is the d
12、irect responsibility of Subcommittee D32.02 on Physical-Mechanical Properties.Current edition approved April 1, 2006. Published April 2006. Originallyapproved in 1985. Last previous edition approved in 2001 as D 451397(2001)e1.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orc
13、ontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7.2 Equilibrate the
14、 sample at 20 to 25C (68 to 77F) in adesiccator with a humidity level of 50 %. A 24-h period isusually sufficient.8. Calibration and Standardization8.1 Prior to use, check all sieves for damage or impropercleaning. If woven-wire sieves are used rather than the pre-ferred electroformed sieves, it is
15、especially important tocarefully inspect the wire surface for wear, misalignment, tears,creases, or separation along the edges.NOTE 1Specifications for wire cloth sieves are described in Specifi-cation E11and specifications for electroformed sieves are described inSpecification E 161.9. Procedure9.1
16、 Select appropriate sieves for the sample being analyzed,typically the 149, 105, 74, 44, and 20-m sieves.NOTE 2For optimum results, the estimated particle size should bedetermined by microscopic examination at 100300X. Sieves may then beselected to cover the size range of the particles.9.2 Clean 44
17、and 20-m sieves prior to use in an ultrasonicbath using a 10 % ethanol, 90 % water mixture. Dry the sievesin a low temperature air jet (hair dryer or equivalent) and allowto equilibrate at room temperature for 30 min before obtainingthe tare weights.9.3 Tare each sieve and the fines collector pan, r
18、ecordingeach weight to the nearest 0.001 g.9.4 After taring, moisten a sheet of tissue paper withantistatic spray and coat the inside wall surface of each sieveby rubbing with the coated tissue.9.5 Place the sieves in a vertical stack in descending orderby mesh size (largest on top).9.6 Weigh a suit
19、able amount of sample obtained by riffling,normally 0.5 to 1.0 g, and transfer into the largest mesh sieveat the top of the stack.9.7 Complete the assembly of the apparatus.9.8 Turn on and adjust to provide rapid transport through thesieves.9.9 Continue sieving for 2 min after no further separation
20、isdetectable.NOTE 3After completion of sieving, none of the sieves should containmore than two to three particle layers. For most powder samples, 0.5 g ofsample provides a satisfactory quantity distribution.9.10 Stop the sieve action.9.11 Remove sieves carefully and weigh each sieve and thepan separ
21、ately. Note the gross weight for each one and recordabove the corresponding tare weight.9.12 Sum the weight of sample on each sieve and the pan toobtain the total weight of the recovered sample. The totalweight of recovered material should check within 5 mg of thestarting sample weight.NOTE 4Examine
22、 the sieve fractions under a microscope to determinewhether the sieve particles in each fraction are within the size rangebetween the sieve and the next coarser sieve. If appreciable finer or coarserparticles are present, tackiness is indicated. Dry and reequilibrate thesample and repeat the analysi
23、s.10. Presentation10.1 Calculate the weight percent of sample on each sieveby multiplying the net weight of each fraction by 100 anddividing by the total weight the total weight of recoveredsample.Weight % sieve fraction 5 100 3 S 2 T!/Wwhere:S = total weight after sieving, g,T = tare weight of siev
24、e, g, andW = total weight of recovered sample, g.10.1.1 Calculate the cumulative percentage passing througheach sieve by adding its fractional percentage to the fractionalpercentage of all coarser sieves, and subtracting the total from100 %. See Table 1 for an example of the calculations andpresenta
25、tion.10.2 Median Particle SizeThe median particle size maybe determined by plotting the cumulative percentage dataagainst the mesh size and determining the size correspondingto 50 %.11. Precision and Bias (Note 5)11.1 Agreement among individual measurements was deter-mined using an equilibrium fluid
26、 cracking catalyst. Experimen-tal repeatability was measured for a number of analyses in eachof five laboratories. Experimental reproducibility was deter-mined by comparison of results from all seven of the labora-tories participating in the round-robin testing program. Pairs oftest results obtained
27、 by a procedure similar to that describedherein are expected to differ in absolute value by less than2.77S, where 2.77S is the 95 % probability limit on thedifference between two test results, and S is the appropriateestimate of standard deviation.NOTE 5Use of the terms “repeatability,” “reproducibi
28、lity,” “preci-sion,” and “bias” are in accordance with Terminology E 456 and PracticeE 177.11.1.1 Experimental Repeatability3Repeatability is usedto designate the ability of an instrument to report the sameanswer assuming no sample bias or operator influence. Ameasure of instrument repeatability is
29、the standard deviation ofa number of runs. The results of testing the equilibrium fluidcatalytic cracking catalyst sample in each of five laboratoriesproduced an average standard deviation of the interpolated3Supporting data have been filed at ASTM International Headquarters and maybe obtained by re
30、questing Research Report RR:D32-1015.TABLE 1 Presentation of Data Weight of Sample Used, 0.610 gSieve No.Mesh SizemicronsNet Weight,gWeight %Sieve FractionCumulative %Passing100 149 0.037 6.1 93.9140 105 0.034 5.6 88.3200 74 0.083 13.6 74.7325 44 0.193 31.6 43.1635 20 0.196 32.1 11.0Pan 0.067 11.0To
31、tal weight recovered 0.610 100.0D 4513 97 (2006)2weight percent median diameter of 0.39 m, corresponding toa 2.77S % value of 61.7 %.11.1.2 Experimental Reproducibility3Reproducibilityamong instruments is used to measure the ability of severalinstruments to produce results which should be the same.
32、Thisparameter takes into account any manufacturing differences ininstruments, any bias in formulating the samples, and anyoperator influence in performing the analyses. Experimentalreproducibility of the seven laboratories when analyzing theequilibrium fluid catalytic cracking catalyst sample materi
33、alresulted in a median (50th percentile) value of 64.3 m with astandard deviation of 1.9 m, corresponding to a 2.77S % valueof 68.2 %.11.2 BiasStandard reference material is not presentlyavailable for determining bias.12. Keywords12.1 catalyst; particle size; sieves; sievingASTM International takes
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37、ddress 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 4513 97 (2006)3
