1、 IT IS THE USERS RESPONSIBILITY TO ESTABLISH APPROPRIATE PRECAUTIONARY PRACTICES AND TO DETERMINE THE APPLICABILITY OF REGULATORY LIMITATIONS PRIOR TO USE. EFFECTIVE HEALTH AND SAFETY PRACTICES ARE TO BE FOLLOWED WHEN UTILIZING THIS PROCEDURE. FAILURE TO UTILIZE THIS PROCEDURE IN THE MANNER PRESCRIB
2、ED HEREIN CAN BE HAZARDOUS. MATERIAL SAFETY DATA SHEETS (MSDS) OR EXPERIMENTAL MATERIAL SAFETY DATA SHEETS (EMSDS) FOR ALL OF THE MATERIALS USED IN THIS PROCEDURE SHOULD BE REVIEWED FOR SELECTION OF THE APPROPRIATE PERSONAL PROTECTION EQUIPMENT (PPE). COPYRIGHT 2000, 2012 UOP LLC. All rights reserve
3、d. Nonconfidential UOP Methods are available from ASTM International, 100 Barr Harbor Drive, P.O. Box C700, West Conshohocken, PA 19428-2959, USA. The UOP Methods may be obtained through the ASTM website, www.astm.org, or by contacting Customer Service at serviceastm.org, 610.832.9555 FAX, or 610.83
4、2.9585 PHONE. Automated Crush Strength of Spherical and Extruded Catalysts UOP Method 967-12 Scope This method is for determining the piece crush strength (PCS) of spherical and extruded catalysts using the Lloyds LS1 motorized sample stand fitted with a load cell. The method applies primarily to pa
5、rticles having a nominal diameter of 1.6-mm (1/16-inch), but may also be used for particles up to 3.2-mm (1/8-inch) in diameter. The measurement range is from 1 N (Newtons) to 500 N. Test apparatus other than the Lloyds may be used provided comparable results are obtained. For statistical purposes,
6、the number of particles crushed is set at a minimum of 50, however, more may be analyzed to improve the precision of the PCS measurement. Data generated using this method can be made comparable to those generated using UOP Method 914, “Automated Crush Strength of Catalysts or Molecular Sieves,” and
7、UOP Method 973, “Automated Crush Strength of Extruded Catalysts,” if instrument parameters are set to specific values. General instrument settings that can be used for the Lloyd instrument are listed in Appendix A. References Lloyds LS1 Instrument Manual, included with instrument Nexygen Plus Softwa
8、re Manual, included with instrument UOP Method 914, “Automated Crush Strength of Catalysts or Molecular Sieves,” www.astm.org UOP Method 973, “Automated Crush Strength of Extruded Catalysts,” www.astm.org UOP Method 999, “Precision Statements in UOP Methods,” www.astm.org Outline of Method A represe
9、ntative sample of catalyst (spherical or extrudate) is riffled to obtain approximately, but not less than, 50 pieces. Moisture content affects crush strength. Therefore, by default, the catalyst is heated to bring the moisture content to a low, consistent level. The sample may also be non-heated per
10、 customer request. Each catalyst piece is placed between the measuring load cell and the flat base plate and subjected to a compressive load. The peak force required to crush the piece is recorded and the procedure is repeated until a minimum of 50 pieces in the riffled sample have been crushed. The
11、 average crush strength is calculated at the conclusion of the test. The percent of pieces which crush above or below a given value (product specification or customer driven) is reported. In addition, the 2 of 7 967-12 crush strength data can be graphically displayed as a histogram. Results are repo
12、rted in Newtons (N) but other units can be calculated. Apparatus References to catalog numbers and suppliers are included as a convenience to the method user. Other suppliers may be used. Brush, round, camels hair, Fisher Scientific, Cat. No. 03-670, or, VWR, Cat. No. 17216-048 Calibration weights,
13、Class 3, Fisher Scientific, Cat. No. 02-225-26P Computer, personal, for running Nexygen software, and capable of running ExcelTM, MinitabTM or similar software to develop a histogram and perform post-analysis calculations; see Nexygen software for minimum requirements and compatibility, JLW Instrume
14、nts Printer, any model compatible with the computer Crucible, porcelain, Coors 60230, Fisher Scientific, Cat. No. 08-693A, or, VWR, Cat. No. 25313-039 Forceps, blunt-pointed, straight, 127-mm length, Fisher Scientific, Cat. No. 08-890, or, VWR, Cat. No. 25720-043 Hot plate, capable of 200C, Fisher S
15、cientific, Cat. No. 11-600-16H, or, VWR, Cat. No. 12365-450 Muffle furnace, capable of 500C, VWR, Cat. No. 30604-158 Riffler, Fisher Scientific, Cat. No. 04-942D, or, VWR, Cat. No. 56720-083 Software (optional), Minitab or other equivalent for displaying histogram, and Excel or equivalent for post-a
16、nalysis calculations Software (required), Nexygen Plus, to control the LS1 and collect data from load cell, JLW Instruments Surface temperature disc, used to verify hotplate temperature, PTC Instruments Test stand and gauge, Lloyds, Cat. No. Machine Type LS1 Motorized Test Stand with Cat. No. 500N a
17、nd Cat. No. 20N Load Cells with Cat. No. 100N and Cat. No. 5N Futek sensors, respectively, JLW Instruments. The instrument includes flat and chisel tips. Use the flat tip for spheres and the chisel tip for extrudates. Reagents and Materials References to catalog numbers and suppliers are included as
18、 a convenience to the method user. Other suppliers may be used. Reference catalysts, spherical or extruded, the same type as samples Procedure The analyst is expected to be familiar with general laboratory practices and the equipment being used. Dispose of all used reagents, materials, and samples i
19、n an environmentally safe manner according to local regulations. Validation and Calibration The Lloyds instrument manual must be read and thoroughly understood before use. Validate 3 of 7 967-12 instrument performance as per the manufacturers instructions monthly when samples are being analyzed, or
20、when indicated by rule violations, trend shifts, or out of control SPC data. Detailed instructions for instrument calibration are supplied by the instrument manufacturer and are given in Appendix B. It is recommended that the user select suitable reference material for weekly quality control measure
21、ment. This material should be uniform and sufficient material should be obtained to last for at least six months, preferably one to five years. The reference should be well riffled and stored in sealed containers to reduce moisture absorption. Instrument Setup 1. Set the Lloyds reference point to 18
22、.5 mm for all materials sizes up to 3.2-mm diameter following the manufacturers instructions. 2. Select and run appropriate analysis program in the NexyGen Plus software. Table 1 lists general parameter settings for the available choices. Other instrument parameters may be used, based upon the sampl
23、e type. It is the laboratorys responsibility to show correlation with the general parameter settings. To avoid confusion, the parameters in Table 1 are listed as they appear on the instrument screen. Not all parameters are used. Test Code and Test Name designations may differ from site to site. Tabl
24、e 1 General Parameter Settings, Lloyds Instrument Test Direction: Compression Preload/Stress: NA Preload Speed: 120 mm/min Test Speed: Extension Rate: NA Automatically Zero at Start: Load at Extension Return to Zero Sample Height: No parameters checked Sample Area: No parameters checked Limits Stop
25、Test: Load 400 N Configure Break Detection: 1 N Results: Maximum, Minimum, Average Sample Analysis 1. Riffle the sample down to approximately, but not less than, 50 whole spheres. Skip to Step 5 if heating in a muffle furnace is not required: UOP Method 914 equivalent. 2. Transfer the riffled sample
26、 to a crucible and place in a 500C muffle furnace for one hour. Keep a monolayer of sample or use additional crucible. CAUTION: Wear appropriate personal protective equipment and use tongs when transferring crucibles to the muffle furnace and from the muffle furnace to the hot plate. 3. Remove the c
27、rucible containing the sample from the muffle furnace, and place in a desiccator. 4. Remove the still hot crucible from desiccator and quickly transfer the crucible to a hot plate set at 4 of 7 967-12 a minimum of 200C. Tests have shown that crush strength decreases with increasing sample moisture c
28、ontent. Start crush strength testing no more than 20 minutes after removal of the sample from the muffle furnace. 5. Select program in NexyGen by choosing batch from library and following steps to rename and start program. See Table 1 for selections. The NexyGen software will control the LS1 until t
29、he analysis is completed. 6. Position a hot sample sphere or extrudate at the center of the bottom plate using the blunt forceps. CAUTION: Take precautions to avoid burns when picking up a sphere from the crucible on the hot plate. The sphere must remain centered and not be allowed to roll from this
30、 position. Only whole spheres are to be crushed. Orient extrudates perpendicular to the chisel tip. 7. Press “Start“ to begin movement of the motor-driven gauge. After the catalyst is crushed, the moveable anvil automatically returns to the preset start position. 8. Brush the crushed material from t
31、he anvil and base plate into the utility tray with the camels hair brush. 9. Insert the next sphere or extrudate immediately. 10. Repeat Steps 6 through 9 until a minimum of 50 spheres or extrudates riffled from the original sample have been crushed (testing of a larger number of spheres may be requ
32、ested). Calculations The calculation of average crush strength is pre-programmed into the Nexygen Software. Reports can be configured and saved for later use. Report values to the nearest whole number if in N, or the nearest tenth if in lbf (pound-force). Multiply the raw N value from the instrument
33、 printout times 0.2248 to convert to lbf. Equation 1 is the manual calculation of average crush strength. XS C = (1) where: C = average crush strength, N or lbf S = sum of the recorded strengths for all spheres or extrudates crushed, N or lbf X = number of spheres crushed If requested, calculate the
34、 percent of spheres having crush strength above or below a given value and report to the nearest tenth of a percent using Equation 2. Refer to the specification for the particular product or customer. XP100 B = (2) where: B = spheres having a crush strength above or below a given value, % P = number
35、 of spheres or extrudates crushed having a crush strength above or below a given value X = previously defined, Equation 1 100 = factor to convert to percent Transfer the data to the personal computer equipped with Excel or Minitab to perform the calculations and display a histogram. 5 of 7 967-12 Re
36、port values to the nearest whole number if in N, or the nearest tenth if in lbf. Multiply the raw N value from the instrument printout times 0.2248 to convert to lbf. Report Report all values listed below in N to the nearest whole number. Average crush strength, from the instrument printout (or as c
37、alculated in Equation1). Percent of spheres or extrudates having a crush strength above or below a given value, as calculated in Equation 2. Maximum crush strength - choose the highest value from the spheres crushed. Minimum crush strength - choose the lowest value from the spheres crushed. Precisio
38、n The precision statements were determined using UOP Method 999. Repeatability, Site Precision, and Reproducibility A nested design was carried out for determining crush strength of a reference spherical reforming catalyst with two analysts in each of three laboratories. Each analyst carried out tes
39、ts on two separate days, performing four tests each day. The total number of tests performed was 32. Using a stepwise analysis of variance procedure, the within-day estimated standard deviation (esd) was calculated and is listed in Table 2. Two tests performed by the same analyst on the same day sho
40、uld not differ by more than the repeatability allowable difference shown in Table 2 with 95% confidence. Two tests performed in one laboratory by different analysts on different days should not differ by more than the site precision allowable difference shown in Table 2 with 95% confidence. Two test
41、s performed in different laboratories by different analysts on different days should not differ by more than the reproducibility allowable difference shown in Table 2 with 95% confidence. The data in Table 2 are a short-term estimate of repeatability. When the test is run routinely, a control standa
42、rd and chart should be used to develop a better estimate of the long-term repeatability. Table 2 Repeatability and Site Precision, Newtons Repeatability Site Precision Reproducibility Mean Within- Day esd Allowable Difference Within- Lab esd Allowable Difference Within- Lab esd Allowable Difference
43、45 1.8 5 1.9 6 2.5 8 Time for Analysis The elapsed time for a single analysis is 1.8 hours, with a labor requirement of 0.5 hour. Suggested Suppliers Fisher Scientific, 711 Forbes Ave., Pittsburgh, PA 15219, USA (412-562-8300) JLW Instruments, Inc., 14 North Peoria St., Suite B-101, Chicago, IL 606
44、07, USA (312-666-0595) PTC Instruments, 2301 Federal Ave., Los Angeles, CA 90064, USA (310-478-1134) VWR International, 1310 Goshen Parkway, West Chester, PA 19380, USA (610-431-1700) 6 of 7 967-12 Appendix A Alternative Instrumentation Other instrument manufacturers have equipment that may be us
45、ed to determine the crush strength of particles. Listed below is equipment from Chatillon and Erweka, and general settings for that can be used as a starting point for setting up that equipment for crush strength determinations for the sample types described in the body of the method. Results obtain
46、ed using the equipment below may not compare directly with results obtained using the equipment listed in the body of the method. Apparatus References to catalog numbers and suppliers are included as a convenience to the method user. Other suppliers may be used. The following apparatus are alternati
47、ves to those listed in the body of the method. Test stand and gauge, Chatillon, Cat. No. TCD-200 Motorized Test Stand, Cat. No. SPK-FM200-019, with a DFS-100 digital force gauge, Cat. No. S-DFS-0100, includes Nexygen DF series software, JLW Instruments Tablet hardness tester, Model TBH, Erweka Proce
48、dure Table A1 lists general parameter settings for Chatillon and Erweka instruments. Table A1 General Parameter Settings, Chatillon and Erweka UOP Method 967-00 and UOP Method 973-01 equivalent (Chatillon) UOP Method 914-92 equivalent (Erweka) Test Direction: Compression Compression Preload/Stress:
49、1.0 N No Preload Preload Speed: 120 mm/min 120 mm/min Extension Rate: 12.7 mm/min 120 mm/min Automatically Zero at Start: Load at Extension Load at Extension Return to Zero Sample Height: No parameters checked No parameters checked Sample Area: No parameters checked No parameters checked Limits Stop Test: Load 400 N Load 400 N Configure Break Detection: 1 N 1 N Results: Maximum, Minimum, Average Maximum, Minimum, Average 7 of 7 967-12 Appendix B Instrument Calibratio
