1、Designation: D5461 06 (Reapproved 2012)Standard Test Method forRubber Compounding MaterialsWet Sieve Analysis ofPowdered Rubber Compounding Materials1This standard is issued under the fixed designation D5461; the number immediately following the designation indicates the year oforiginal adoption or,
2、 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 a procedure for the qualitativeevaluation of aggregate s
3、ize and aggregate size distribution ofpowdered rubber accelerators and other compounding materi-als which are insoluble in water.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 This standard does not purport to address
4、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. Terminology2.1 Definitions:2.1.1 aggregatea cluster of ind
5、ividual particles making upthe mass of the material.2.1.2 aggregate size distributionthe distribution of aggre-gates obtained by passing wetted rubber chemicals throughstacked sieves of known mesh which are arranged in order ofdecreasing size.3. Summary of Test Method3.1 A sample of powdered rubber
6、chemical is wetted with adilute aqueous solution of soap and defoamer. The sample istransported by water flow through stacked sieves arranged inorder of decreasing mesh size. The material retained on theface of each sieve is dried in an oven. The dry mass of retainedmaterial is obtained for each sie
7、ve. The percent retainedmaterial is calculated on the basis of original sample mass.Individual masses and percentages are summed to evaluate theaggregate size distribution for the sample.4. Significance and Use4.1 This test method is used to evaluate the suitability ofpowdered rubber chemicals, part
8、icularly accelerators, for usein rubber compounds that require very small particle clusters toachieve a uniform cross-linked network. This test method isintended to be used to ensure that no excessively large particlesare present that would result in network “flaws” and todetermine that the powdered
9、 product follows a typical patternof size distribution.4.2 In view of the inherent variability in this type of method,it is recommended that the results be used only in a semi-quantitative sense; that is, comparisons within a laboratory orrelative comparisons of samples against reference samples, or
10、both.5. Apparatus5.1 Standard Sieves, stainless steel, 200 mm (approximately8 in.) diameter containing selected stainless steel wire clothswith openings in the range of 45 to 250 m. (This correspondsto 325 to 60 mesh sieves.)NOTE 1If the 200 mm diameter sieves are not available, the smaller76 mm dia
11、meter sieves can be used. In this case, the sample mass shouldbe reduced from 50 to 10 g.5.2 Analytical Balance, 150 g capacity, 1.0 mg sensitivity.5.3 Convection Oven, controlled at 70 6 2C. For lowmelting materials, the oven temperature should be set 10Cbelow the melting point.5.4 Aluminum Weighin
12、g Dishes, disposable, 55 to 60 mmdiameter, approximately 1 g mass.5.5 No. 6 Stiff Bristle Artist Brush, having 10 to 45 mm longbristles.1This test method is under the jurisdiction of ASTM Committee D11 on Rubberand is the direct responsibility of Subcommittee D11.11 on Chemical Analysis.Current edit
13、ion approved May 1, 2012. Published July 2012. Originally approvedin 1993. Last previous edition approved in 2006 as D5461 06. DOI: 10.1520/D5461-06R12.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6. Reagents and Materials6.1 Dete
14、rgent, sodium alkylbenzenesulfonate (SABS), 40 %active or equivalent.6.2 Silicone Defoamer,2water soluble.6.3 Soap Solution, prepared by adding 100 g of SABS and200 cm3silicone defoamer to 20 dm3water.7. Procedure7.1 Place the soap solution in a suitable carboy on a shelf orstand over a sink and dis
15、charge the solution from the bottom ofthe container through 6 mm (0.25 in.) rubber tubing connectedto a bottom outlet. A pinch-clamp serves as a control valve.7.2 Assemble pre-cleaned sieves (200 or 76 mm) into astack, with the largest sieve opening on top. For example:Sieve Size Sieve Opening, mTop
16、 60 250100 150200 75270 53Bottom 325 457.3 Place the sieve stack in the sink under the discharge linefor the soap solution and under a sink tap equipped with anaerator.7.4 Wet the surface of each screen with water and soapsolution.7.5 Tare a series of commercially available aluminumweighing dishes,
17、corresponding to each sieve. Take care tomaintain the “dish to sieve” correspondence.7.6 Weigh 50 + 0.1 g sample for 200 mm sieve or10.0 + 0.1 g sample for 76 mm sieve of the test material into a1dm3screw cap bottle equipped with a vinyl or TFE-fluorocarbon insert.7.7 Add 100 cm soap solution to the
18、 bottle and screw thecap onto the bottle.7.8 Agitate and mix the contents of the bottle by gentleshaking. Make sure the contents are thoroughly wetted asdetermined by visual inspection. Absence of foam, bubbles,and visible chunks indicates complete wetting.7.9 Pour the contents of the bottle onto th
19、e top sieve in thesieve stack. Ensure complete transfer of the sample by washingthe bottle two to three times with 50 cm3portions of water.7.10 Gently wash the sample through the sieve with a smallstream of soap solution. Switch to an aerated stream of waterto finish washing the sample through the s
20、ieve. If necessary,alternate the use of water and soap solution to assure completetransport of sample through the sieve breaking up agglomeratesusing a stiff bristle brush. (Clean the brush with water oversieve.)7.11 When transfer is complete, wash the residue to themiddle of the sieve with a gentle
21、 stream of water. Take care toensure that all soap residue is rinsed from the remainingsample.7.12 Remove the top sieve from the stack and wipe excesswater from the sieve sides and bottom with a dry lint-freeabsorbent towel and set aside.7.13 Repeat 7.10 through 7.12 for all sieves in the stack.7.14
22、 Dry each sieve plus residue in a 70C convection ovenfor 1 h. (Low melting materials should be dried at 10C belowthe melting point.)7.15 Remove the sieves from the oven and allow them tocool to ambient temperature.7.16 Remove the residue from the sieve by gently tappingthe sides while pouring the so
23、lids into a tared, properly labeledaluminum weighing dish.NOTE 2It may be possible to avoid this transfer when using thesmaller 76 mm sieves. In that case, the sieves should be tared initially, thenreweighed following drying and cooling to ambient temperature.7.17 Record the quantity of residue cont
24、ained on each sieve.8. Calculation8.1 Calculate the percent retained on each sieve as follows:Retained % 5AB3 100 (1)where:A = mass of residue, g, andB = mass of sample, g.8.1.1 Residue mass should be accumulated for successivesieves. To determine the residue mass on a finer sieve, it isnecessary to
25、 sum the masses of residues collected on all coarsersieves and add it to the mass from the selected sieve.8.2 The amount of sample passing through each sieve isdetermined by subtracting the percent of material collected onthe sieve and all coarser sieves from 100.8.3 The amount of material passing t
26、hrough all sieves isdetermined by subtracting the total amount retained on allsieves from 100.9. Report9.1 Report the following information:9.1.1 Proper sample identification,9.1.2 Identification of each sieve used,9.1.3 Mass retained on each sieve in grams,9.1.4 Percent of material passing through
27、each sieve, and9.1.5 Percent of material passing through all sieves.10. Precision and Bias10.1 Due to the qualitative nature of this test method,classical precision testing is not appropriate. A pilot round-robin precision test gave unacceptably large between-laboratory variations.11. Keywords11.1 p
28、article size; rubber compounding materials; wet sieveanalysis2The sole source of supply of the apparatus (Dow-Corning FG-10) known to thecommittee at this time is Dow-Corning, Midland, MI. If you are aware of alternativesuppliers, please provide this information to ASTM International Headquarters.Yo
29、ur comments will receive careful consideration at a meeting of the responsibletechnical committee,1which you may attend.D5461 06 (2012)2ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this stan
30、dard are expressly advised that determination of the validity of any such patent 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 and
31、if not revised, either reapproved or withdrawn. Your comments are invited either 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, w
32、hich you may attend. If you feel that your comments have not received a fair 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
33、,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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D5461 06 (2012)3
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