1、Designation: D5644 01 (Reapproved 2013)D5644 18Standard Test MethodsMethod forRubber Compounding MaterialsDetermination of ParticleSize Distribution of Recycled Vulcanizate ParticulateRubber1This standard is issued under the fixed designation D5644; the number immediately following the designation i
2、ndicates 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 () indicates an editorial change since the last revision or reapproval.1. Scope1.1 TheseThis test methods describemethod d
3、escribes the procedures for determining average particle size distribution ofrecycled vulcanizate particulate.particulate rubber by the Ro-tap sieve test method for 90 m (170 mesh) or larger particles.1.2 Method A describes the Ro-tap sieve test method for 60 mesh or coarser particles.1.3 Method B d
4、escribes the ultrasonic technique combined with optical microscope especially suitable for 80 mesh or finerparticles. This procedure is based on Test Method D3849.1.2 The values stated in SI units are to be regarded as the standard.1.3 This standard does not purport to address all of the safety conc
5、erns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use.1.4 This international standard was developed in accorda
6、nce with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Stan
7、dards:2D297 Test Methods for Rubber ProductsChemical AnalysisD1416 Test Methods for Rubber from Synthetic SourcesChemical Analysis (Withdrawn 1996)3D1566 Terminology Relating to RubberD3182 Practice for RubberMaterials, Equipment, and Procedures for Mixing Standard Compounds and Preparing StandardVu
8、lcanized SheetsD3191 Test Methods for Carbon Black in SBR (Styrene-Butadiene Rubber)Recipe and Evaluation ProceduresD3192 Test Methods for Carbon Black Evaluation in NR (Natural Rubber)D3849 Test Method for Carbon BlackMorphological Characterization of Carbon Black Using Electron MicroscopyD5603 Cla
9、ssification for Rubber Compounding MaterialsRecycled Vulcanizate Particulate RubberE11 Specification for Woven Wire Test Sieve Cloth and Test SievesE105 Practice for Probability Sampling of Materials3. Terminology3.1 Definitions:3.1.1 parent compound, noriginal compound used in the product.3.1.2 rec
10、ycled vulcanizate rubber, nvulcanized rubber that has been processed to give particulates or other forms of differentshapes, sizes, and size distributions.1 TheseThis test methods aremethod is under the jurisdiction of ASTM Committee D11 on Rubber and Rubber-like Materials and areis the direct respo
11、nsibility ofSubcommittee D11.20 on Compounding Materials and Procedures.Current edition approved Nov. 1, 2013June 1, 2018. Published January 2014July 2018. Originally approved in 1994. Last previous edition approved in 20082013 asD5644 01 (2008)(2013).1. DOI: 10.1520/D5644-01R13.10.1520/D5644-18.2 F
12、or referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to pr
13、ovide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof th
14、e standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.1.3 DiscussionThe words “vulcanizate” and “vulcanized rubber” are interchangeable. Additional terminology asso
15、ciatedwith this classification can be found in Terminology D1566.4. Significance and Use4.1 The particulate size distribution of vulcanizate particulate rubber is used for the purpose of assigning a product mesh oraverage particle size designation.4.2 The product designation for mesh size for the Ro
16、-tap method (MethodA, as follows) is based on the size designation screenwhich allows a range for the upper limit retained of maximum 5 % for up to 850 m (20 mesh) particles, maximum 10 % for600850 to 150 m (30(20 to 100 mesh), and maximum 15 % for 128125 to 7520 m (120 to 200635 mesh). No rubber pa
17、rticlesshall be retained on the zero screen (see Table 1,2, Classification D5603).4.3 For Method A, the The weight percent retained on a specific screen is noted whereas in Method B (ultrasonic technique),the number of particles at a particular size is counted.noted.4.4 Method B addresses problems t
18、hat may be caused by tackiness and static electrical forces that recycled rubber particles exerton each other to form agglomerates, especially for 80 mesh or finer particles. This method eliminates agglomerate formation byultrasonically dispersing the particles.4.5 Both methods can be used as a qual
19、ity control tool.5. Method A: The Ro-tap Method5.1 Summary of Test Method:5.1.1 Method ARo-tap Method:5.1.1.1 A 100 6 1 g specimen of the recycled rubber is combined with a fixed amount of talc and placed on top of a series ofmesh sieves, with the coarsest sieve being on top and the finest on the bo
20、ttom. The specimen is placed in a Ro-tap shaker for 10to 20 min, depending on the grade of the recycled rubber. The weight of the rubber retained on the individual sieves is thenrecorded and the mesh designation of the product determined.5. Summary of Test Method5.1 Ro-tap Method, Mechanical Vibrato
21、ry Sieve ShakerA100 6 1 g specimen of the recycled rubber is combined with a fixedamount of flowing agent (for example, hydrous magnesium silicate (talc), fumed, aluminum oxide, fumed silica, or calciumcarbonate) and placed on top of a series of mesh sieves, with the coarsest sieve being on top and
22、the finest on the bottom. Thespecimen is placed in a Ro-tap shaker for 10 to 20 min, depending on the grade of the recycled rubber. The weight of the rubberretained on the individual sieves is then recorded and the mesh designation of the product determined.6. Apparatus6.1 Mechanical Sieve Shaker3Th
23、is is a mechanically operated sieve shaker that imparts a uniform rotary and tapping motionto a stack of 200-mm (8-in.) 200 mm (7.9 in.) sieves in accordance with 6.2. The sieve shaker should be adjusted to accommodatea stack of sieves, receiver pan, and cover plate. The bottom stops should be adjus
24、ted to give a clearance of 1.5 mm (0.06 in.)between the bottom plate and the screens so that the screens will be free to rotate. The sieve shaker machine shall be powered withan electric motor operating 28.75 to 29.17 Hz (1725 to 1750 rpm). This will produce 2.33 to 2.60 Hz and 280 to 320 rotarymoti
25、ons/min. The cover plate shall be fitted with a cork stopper that shall extend from 3.00 to 9.00 mm (0.118 to 0.354 in.) abovethe metal recess. At no time, shall a rubber, wood, or other material other than cork be permitted.6.2 Standard Sieves, stainless steel or brass, 200 mm (7.9 in.) in diameter
26、 in accordance with Specification E11. The sieve setshould include a lid and a bottom pan.6.3 Balance, Digital Scale with Tare Function, with a sensitivity of weighing at a minimum 0.1 g.6.4 Brush.Brushes:6.4.1 A Tyler Model 1778-SB soft brass wire brush for cleaning sieves 100 425 m (40) mesh and c
27、oarser.6.4.2 A nylon bristle brush for cleaning sieves finer than 100 425 m (40) mesh.6.5 Jar, Glass or Metal Measuring Cup, with a capacity of 500 cm3 (1 pint) with large opening.pint).6.6 Glass Wide-Mouth Jar with Lid, with capacity of 500 cm3 (1 pint).6.7 Rubber Balls, 4 with a diameter from 25 t
28、o 50 mm (1 to 2 in.) or Plastic Rings,plastic rings with a height of 20 6 3 mm,an outside diameter of 60 6 3 mm, and an inside diameter of 58 6 3 mm. The height of the balls or rings must be lesssless than3 The last approved version of this historical standard is referenced on www.astm.org.3 The Ro-
29、Tap Sieve Shaker meets the specified conditions and has been found satisfactory for this purpose,purpose and is available from many scientific laboratorysuppliers.4 Available from various sieve manufacturing suppliers.D5644 182the depth of the screens being used. Enough balls or rings are needed to
30、have Use two balls or two plastic rings per sieve. test screenas per 7.1.5. Balls and rings are not to be used simultaneously.6.8 Talcum Powders, Flow Agent (same as 5.1), usually some mixture of magnesium silicate, silica, magnesium oxide,magnesium-aluminum silicate with at least 90 % of the partic
31、les being less than 40 m (approximately 400 mesh) in size.7. Procedure7.1 Select test screens appropriate to the particle size distribution of the product being tested. A set of two to six sieves and areceiver pan are normally used. The actual number of sieves is to be agreed upon by vendor and cust
32、omer.7.2 Clean each screen with brush (see 6.4), making sure all particles are removed from both sides of screen.7.1 Stack test screens in order of increasing mesh size with smallest number on top (coarsest) and highest number on bottom(finest). For products of 425 m (40 mesh) or finer, add two rubb
33、er balls or plastic rings per sieve. For products coarser than 425m (40 mesh), the use of rubber balls or plastic rings as agitation aid is optional. Rubber balls and plastic rings are not to be usedsimultaneously. Same size balls shall be used on any one screen.Selection and Preparation of Test Scr
34、eens:7.1.1 Select test screens appropriate to the particle size distribution of the product being tested. A set of two to six sieves anda receiver pan are normally used. The actual number of sieves is to be agreed upon by vendor and customer.7.1.2 Verify each screen has been cleaned of all particles
35、 on both sides of screen with brush (see 6.4).7.1.3 Stack test screens in order of increasing mesh size with smallest number on top (coarsest) and highest number on bottom(finest).7.1.4 Add bottom receiver pan to stack.7.1.5 Verify rubber balls or plastic rings are in place in test screens; For prod
36、ucts of 425 m (40 mesh) or finer, add two rubberballs or two plastic rings per sieve. For products coarser than 425 m (40 mesh), the use of rubber balls or plastic rings as anagitation aid is optional. Rubber balls and plastic rings are not to be mixed on any test screen.7.4 Add bottom receiver pan
37、to stack.7.2 Obtain approximately 150 to 200 g of vulcanizate particulate rubber from the lot (refer to Practice E105). Preparation ofSpecimen:7.2.1 Obtain approximately 150 to 200 g of vulcanizate particulate rubber from the lot (refer to Practice E105).7.2.2 Place an empty glass or metal measuring
38、 cup on digital scale. Press tare feature to determine tare weight of measuringcup.7.2.3 Using the glass or metal measuring cup weigh 100 g of specimen to the nearest gram.7.2.4 Transfer 100 g of specimen into glass jar as defined in 6.6.7.3 Prepare a 100-g specimen as follows:Preparation of Flow Ag
39、ent:7.3.1 Weigh 100 g of specimen to the nearest gram.Place empty glass or metal measuring cup on digital scale; press tare featureto determine tare weight of measuring cup.7.3.2 Weigh talc according to Using the empty glass or metal measuring cup weigh flow agent per product gradationdesignation. F
40、or products designated coarser than 300 m (50 mesh), weigh 5.060.1 g of talc. flow agent. For products designated300 m (50 mesh) or finer, weigh 15.0 6 0.1 g of talc.flow agent.7.3.3 Add talc to specimen.flow agent to specimen in glass jar as defined in 6.6 and seal glass jar with lid.7.3.4 Mix thor
41、oughly by placing talc and specimen in a 500-cmThoroughly 3 (1-pt) jar and shake the glass jar for a minimumof 1 min,min until agglomerates are broken and talc flow agent is uniformly mixed.mixed or dispersed.7.4 Place the specimen on the top sieve and place a cover on the Remove specimen and flow a
42、gent from glass jar and placeon top screen. Place cover on top of stack.7.5 Place the stack in the shaker.7.6 Activate the shaker for 10 min for products designated coarser then 300 m (50 mesh). For products designated 300 m (50mesh) or finer, activate the shaker for 20 min.7.7 After the shaker comp
43、letes the appropriate cycle, remove the stack.7.8 Starting with the top sieve, remove the screened fraction by gently tapping its contents to one side and pouring the contentson the balance and recording its mass to the nearest 0.1 g. Record any mass less than 0.1 g as trace.Determine and Record Res
44、ults:7.8.1 Place empty glass or metal measuring cup on digital scale; press tare feature to determine tare weight of measuring cup;7.8.2 Starting with the top sieve, remove the screened fraction by gently tapping its contents to one side and pouring the contentsinto the metal or glass measuring cup
45、and recording its mass to the nearest 0.1 g. Record any mass less than 0.1 g as trace.7.8.3 Brush any material adhering to the bottom of the screen onto the next finer screen.7.8.4 Empty the glass or metal measuring cup and set the specimen aside.7.8.5 Repeat 7.8.1 7.8.4 until all sieves in the stac
46、k and the bottom pan have been emptied, weighed, and recorded. This givesthe weight retained on each screen.D5644 1837.12 Brush any material adhering to the bottom of the screen onto the next finer screen.7.13 Zero the balance in preparation for weighing the retained contents of the next screen.7.14
47、 Repeat 7.11 to 7.12 until all sieves in the stack and the bottom pan have been emptied, weighed, and recorded. This givespercent retained on each screen.8. Calculation8.1 The sum of the masses of each fraction from the sieves and the bottom pan shall not be less than the original mass of thespecime
48、n plus mass of talc flow agent less 2 g, or greater than the original mass of the specimen plus 100 % of talc flow agentadded. Repeat test if either of these conditions occurs.8.2 To adjust for the addition of talc to the specimen, the mass of the contents of the bottom pan is adjusted by the follow
49、ingequation: calculate the relative fractions of the samples that are retained on each screen and the pan, create a list of all screens usedin the procedure including the top screen (zero screen) and pan.x 5y 2z 2100! (1)where:x = mass of rubber in bottom pan,y = total mass of contents in bottom pan, andz = total mass of contents of all six sieves plus bottom pan.8.2.1 Adjacent to each entry on the list, record the retained weight on each screen and pan. Sum total of the values for eachscreen including the pan to obtain the total weight retained f
