ASTM_D_5461-06R2017.pdf

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recommendations isued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.Designation:D5461-06(Reapproved 2017)INTERNATIONALStandard Test Method forRubber Compounding Materials-Wet 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,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon(8)indicates an editorial change since the last revision or reapproval.1.Scopematerial is obtained for each sieve.The percent retained1.1 This test method covers a procedure for the qualitativematerial is calculated on the basis of original sample mass.evaluation of aggregate size and aggregate size distribution ofIndividual masses and percentages are summed to evaluate thepowdered rubber accelerators and other compounding materi-aggregate size distribution for the sample.als which are insoluble in water.4.Significance and Use1.2 The values stated in SI units are to be regarded as thestandard.The values given in parentheses are for information4.1 This test method is used to evaluate the suitability ofonly.powdered rubber chemicals,particularly accelerators,for usein rubber compounds that require very small particle clusters to1.3 This standard does not purport to address all of theachieve a uniform cross-linked network.This test method issafety concerns,if any,associated with its use.It is theintended to be used to ensure that no excessively large particlesresponsibility of the user of this standard to establish appro-are present that would result in network flaws and topriate safety and health practices and determine the applica-determine that the powdered product follows a typical patternbility of regulatory limitations prior to use.of size distribution.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-4.2 In view of the inherent variability in this type of method,ization established in the Decision on Principles for theit is recommended that the results be used only in a semi-Development of International Standards,Guides and Recom-quantitative sense;that is,comparisons within a laboratory ormendations issued by the World Trade Organization Technicalrelative comparisons of samples against reference samples,orBarriers to Trade(TBT)Committee.both.2.Terminology5.Apparatus2.1 Definitions:5.1 Standard Sieves,stainless steel,200 mm(approximately2.1.1 aggregate-a cluster of individual particles making up8 in.)diameter containing selected stainless steel wire clothsthe mass of the material.with openings in the range of 45 to 250 um.(This corresponds2.1.2 aggregate size distribution-the distribution of aggre-to 325 to 60 mesh sieves.)gates obtained by passing wetted rubber chemicals throughNoTE 1-If the 200 mm diameter sieves are not available,the smallerstacked sieves of known mesh which are arranged in order of76 mm diameter sieves can be used.In this case,the sample mass shoulddecreasing size.be reduced from 50 to 10 g.5.2 Analytical Balance,150 g capacity,1.0 mg sensitivity.3.Summary of Test Method5.3 Convection Oven,controlled at 70 2C.For low3.1 A sample of powdered rubber chemical is wetted with amelting materials,the oven temperature should be set 10Cdilute aqueous solution of soap and defoamer.The sample isbelow the melting point.transported by water flow through stacked sieves arranged inorder of decreasing mesh size.The material retained on the5.4 Aluminum Weighing Dishes,disposable,55 to 60 mmface of each sieve is dried in an oven.The dry mass of retaineddiameter,approximately 1 g mass.5.5 No.6 Stiff Bristle Artist Brush,having 10 to 45 mm longbristles.This test method is under the jurisdiction of ASTM Committee D11 on Rubberand Rubber-like Materials and is the direct responsibility of Subcommittee D11.11on Chemical Analysis.6.Reagents and MaterialsCurrent edition approved May 1,2017.Published July 2017.Originally approvedin 1993.Last previous edition approved in 2012 as D5461-06(2012).DOI:6.1 Detergent,sodium alkylbenzenesulfonate(SABS),40%10.1520/D5461-06R17.active or equivalent.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United StatesCopyright by ASTM Intl(all rights reserved);Sat Sep 30 22:26:46 EDT 2017 1Downloaded/printed byUniversity of Edinburgh(University of Edinburgh)pursuant to License Agreement.No further reproductions authorized.D5461-06(2017)6.2 Silicone Defoamer;water soluble.7.12 Remove the top sieve from the stack and wipe excess6.3 Soap Solution,prepared by adding 100 g of SABS andwater from the sieve sides and bottom with a dry lint-free200 cmsilicone defoamer to 20 dm water.absorbent towel and set aside.7.Procedure7.13 Repeat 7.10 through 7.12 for all sieves in the stack.7.1 Place the soap solution in a suitable carboy on a shelf or7.14 Dry each sieve plus residue in a 70C convection ovenstand over a sink and discharge the solution from the bottom offor 1 h.(Low melting materials should be dried at 10C belowthe container through 6 mm(0.25 in.)rubber tubing connectedthe melting point.)to a bottom outlet.A pinch-clamp serves as a control valve.7.15 Remove the sieves from the oven and allow them to7.2 Assemble pre-cleaned sieves(200 or 76 mm)into acool to ambient temperature.stack,with the largest sieve opening on top.For example:7.16 Remove the residue from the sieve by gently tappingSieve SizeSieve Opening,umthe sides while pouring the solids into a tared,properly labeledTop60250aluminum weighing dish.10015020075NoTE 2-It may be possible to avoid this transfer when using the27053smaller 76 mm sieves.In that case,the sieves should be tared initially,thenBottom32545reweighed following drying and cooling to ambient temperature.7.3 Place the sieve stack in the sink under the discharge line7.17 Record the quantity of residue contained on each sieve.for the soap solution and under a sink tap equipped with anaerator.8.Calculation7.4 Wet the surface of each screen with water and soap8.1 Calculate the percent retained on each sieve as follows:solution.7.5 Tare a series of commercially available aluminumRetained%=10(1)weighing dishes,corresponding to each sieve.Take care towhere:maintain the dish to sieve correspondence.A=mass of residue,g,and7.6 Weigh 50+0.1 g sample for 200 mm sieve orB=mass of sample,g.10.0+0.1 g sample for 76 mm sieve of the test material into aI dm3 screw cap bottle equipped with a vinyl or TFE-8.1.1 Residue mass should be accumulated for successivefluorocarbon insert.sieves.To determine the residue mass on a finer sieve,it isnecessary to sum the masses of residues collected on all coarser7.7 Add 100 cm soap solution to the bottle and screw thesieves and add it to the mass from the selected sieve.cap onto the bottle.8.2 The amount of sample passing through each sieve is7.8 Agitate and mix the contents of the bottle by gentledetermined by subtracting the percent of material collected onshaking.Make sure the contents are thoroughly wetted asthe sieve and all coarser sieves from 100.determined by visual inspection.Absence of foam,bubbles,and visible chunks indicates complete wetting.8.3 The amount of material passing through all sieves isdetermined by subtracting the total amount retained on all7.9 Pour the contents of the bottle onto the top sieve in thesieves from 100.sieve stack.Ensure complete transfer of the sample by washingthe bottle two to three times with 50 cm portions of water.9.Report7.10 Gently wash the sample through the sieve with a small9.1 Report the following information:stream of soap solution.Switch to an aerated stream of water9.1.1 Proper sample identification,to finish washing the sample through the sieve.If necessary,9.1.2 Identification of each sieve used,alternate the use of water and soap solution to assure complete9.1.3 Mass retained on each sieve in grams,transport of sample through the sieve breaking up agglomerates9.1.4 Percent of material passing through each sieve,andusing a stiff bristle brush.(Clean the brush with water over9.1.5 Percent of material passing through all sieves.sieve.)7.11 When transfer is complete,wash the residue to the10.Precision and Biasmiddle of the sieve with a gentle stream of water.Take care to10.1 Due to the qualitative nature of this test method,ensure that all soap residue is rinsed from the remainingclassical precision testing is not appropriate.A pilot round-sample.robin precision test gave unacceptably large between-laboratory variations.2 The 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 alternative11.Keywordssuppliers,please provide this information to ASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsible11.1 particle size;rubber compounding materials;wet sievetechnical committee,which you may attend.analysisCopyright by ASTM Intl(all rights reserved);Sat Sep 30 22:26:46 EDT 20172Downloaded/printed byUniversity of Edinburgh(University of Edinburgh)pursuant to License Agreement.No further reproductions authorized.D5461-06(2017)ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard.Users of this standard 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 andif 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,which you may attend.If you feel that your comments have not received a fair hearing you shoulcmake 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.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 Copyright Clearance Center,222Rosewood Drive,Danvers,MA 01923,Tel:(978)646-2600;http:/ by ASTM Intl(all rights reserved);Sat Sep 30 22:26:46 EDT 20173Downloaded/printed byUniversity of Edinburgh(University of Edinburgh)pursuant to License Agreement.No further reproductions authorized