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. SAFETY DATA SHEETS (SDS) OR EXPERIMENTAL SAFETY DATA SHEETS (ESDS) FOR ALL OF THE MATERIALS USED IN THIS PROCEDURE SHOULD BE REVIEWED FOR SELECTION OF THE APPROPRIATE PERSONAL PROTECTION EQUIPMENT (PPE). COPYRIGHT 1980, 2014 UOP LLC. All rights reserved. Nonconfidential U
3、OP 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 610.832.9585 PHONE. Size D
4、istribution of Charcoal Particles UOP Method 801-14 Scope This method is for determining the size distribution of charcoal and charcoal supported catalyst particles by screening through appropriate ASTM Series testing sieves. Reference UOP Method 999, “Precision Statements in UOP Methods,” www.astm.
5、org Outline of Method A representative 100-mL sample is placed on the top of a nest of appropriate mesh size, 8-inch diameter sieves with a bottom pan. The nest is covered, placed in a sieve shaker and shaken for 5 minutes. The material retained on each sieve and in the pan is weighed, and the weigh
6、t-percent of is then calculated. Apparatus References to catalog numbers and suppliers are included as a convenience to the method user. Other suppliers may be used. Balance, readability 0.01 g, with digital interface. See the shaker manufacturers software or representative for balance compatibility
7、. Brush, paint, VWR, Cat. No. 17230-060, used to clean the sieves Computer, compatible with shaker interface and software Riffler, sample splitter, VWR, Cat. No. 56723-250 Sieve bottom pan and cover, stainless steel, 203-mm (8-inch) diameter, 51-mm (2-inch) height, Retsch Part Nos. 697203050 and 326
8、620002, respectively, VWR, Cat. Nos. 66004-848 and 14214-620, respectively Sieve shaker, with clamp cover, Retsch Model AS 200 Control with Easy Clamp, VWR Cat. No. 66004-956. Easy Sieve software is included. This sieve shaker employs a specific throwing motion with angular momentum; different resul
9、ts may be obtained if other sieve shakers are used. Substitution is permitted only if equivalent results are demonstrated. 2 of 4 801-14 Sieves, ASTM Series, stainless steel wire cloth, stainless steel frame, 203-mm (8-inch) diameter, 51-mm (2-inch) height. Sieve sizes and nest designations are dete
10、rmined by the size of the material to be tested and any specifications related to the material. Table 1 is a list of suggested sieves to be used. Sieves may be added or deleted depending upon the materials to be tested and test requirements. Important: If the results will be compared between laborat
11、ories, the sieves must be “Matched” test sieves from the same manufacturer. Table 1 Part Numbers for Sieves ASTM Series Size Opening Retsch Part Number VWR Catalog Number No. 10 2.00 mm 60150002000 66004-896 No. 20 0.85 mm 60150000850 66004-886 No. 30 0.60 mm 60150000600 66004-882 Reagents and Mater
12、ials References to catalog numbers and suppliers are included as a convenience to the method user. Other suppliers may be used. Gloves, disposable, nitrile, VWR, Cat. Nos. 32919-000 through -008, corresponding to hand sizes XS through XL Procedure The analyst is expected to be familiar with general
13、laboratory practices and the equipment being used. Wear gloves whenever incidental contact with sample is possible. Dispose of all supplies and samples in an environmentally safe manner according to local regulations. The steps below are written specifically for the Retsch Model AS 200 Control shake
14、r listed in Apparatus. 1. Using approximately 500 g of sample, riffle to obtain a 50 to 75 g representative sample of the material to be tested. Follow instructions supplied with the riffler for proper riffling procedure. 2. Open the Easy Sieve program. Click on “Sieve Analysis” in the menu bar. Cho
15、ose one of the programs under the task file list from the drop down menu. Edit the parameters and sample information and press “OK.” The parameters listed in Table 2 have been found suitable for the charcoal samples. Please refer to the manual for the Retsch Sieve Shaker prior to starting an analysi
16、s for operating instructions and for editing the screens from the program. Table 2 Sieve Shaker Parameters Amplitude 1 Time 5 min Sample size 100 mL 3. Tare the balance and place the empty bottom pan on the balance. Press the “PRINT” button on the balance to transmit the weight of the pan to the pro
17、gram. 4. Tare the balance and place the finest mesh sieve on the bottom pan. Press the “PRINT” button on the balance to transmit the weight of the screen to the program. Repeat for each additional screen used for the analysis. 5. Tare the balance and place the sample onto the top screen. Press “PRIN
18、T” to transmit the weight 3 of 4 801-14 of the sample. Remove screens from the balance and place on the Retsch sieve shaker. Attach and secure the screens with the clamp cover. Press “OK” on the screen prompts to start sieving. 6. Re-zero the balance. 7. When the analysis is finished, loosen the cla
19、mps on the cover, remove the top screen, and place on the balance. Press “PRINT” to transmit weight to appropriate place in the program. Repeat for each screen until all the screens are complete. When finished, click on the “CALCULATE” button on the screen. For a table of numeric data, go to “RESULT
20、S barb2right TABLE” or simply press “F5.” 8. Clean the screens before the next sample, brushing the underside of the screen to remove material lodged in the mesh. Calculations Calculations are performed by the data system. For information, the equivalent manual calculation is shown in Equation 1. Am
21、ount on each sieve and in bottom pan = B A100 (1) where: A = material on a given sieve, g B = total material recovered, g 100 = factor to convert to percent Report Report results to the nearest 0.1 mass-% as follows: Particle Size of charcoal, mass-% Retained on ASTM No. 10 Through ASTM No. 10, on A
22、STM No. 20 Through ASTM No. 20, on ASTM No. 30 Through ASTM No. 30 For some applications of this method, only the “Through ASTM No. 30” need be reported. Precision Precision statements were determined using UOP Method 999, “Precision Statements in UOP Methods.” Repeatability and Site Precision A nes
23、ted design was carried out for determining impurities in one batch of charcoal by two analysts on two separate days, performing two analyses each day for a total of eight analyses. Using a stepwise analysis of variance procedure, the within-day estimated standard deviations (esd) were calculated at
24、the concentration means listed in Table 3. Two analyses performed in one laboratory by the same analyst on the same day should not differ by more than the repeatability allowable differences shown in Table 3 with 95% confidence. Two analyses performed in one laboratory by different analysts on diffe
25、rent days should not differ by more than the site precision allowable differences shown in Table 3 with 95% confidence. The data in Table 3 represent short-term estimates of the repeatability of the method. When the test is run routinely, use of a control standard and a control chart is recommended
26、to generate an estimate of long-term repeatability. 4 of 4 801-14 Table 3 Repeatability and Site Precision, mass-% Repeatability Site Precision On Screen Mean Within- Day esd Allowable Difference Within- Lab esd Allowable Difference No. 10 0.1 0.08 0.3 0.08 0.3 No. 20 73.5 3.00 9.8 3.54 13.9 No. 30
27、25.5 2.89 9.4 3.34 13.1 Through No. 30 0.9 0.22 0.8 0.29 1.1 Reproducibility There is insufficient data to calculate the reproducibility of the test at this time. Time for Analysis The elapsed time for one analysis is 0.75 hour. The labor requirement is 0.40 man-hour. Suggested Suppliers VWR Interna
28、tional is listed as the supplier for all of the apparatus including the Retsch sieve shaker and related parts. Alternatively, the sieve shaker and related parts may be purchased directly from Retsch. Retsch Inc., 74 Walker Lane, Newton, PA 18940, USA, 1-267-757-0351, VWR International, 1310 Goshen Parkway, West Chester, PA 19380, USA, 1-610-431-1700,
