1、Designation: D 4572 89 (Reapproved 2005)Standard Test Method forRubber ChemicalsWet Sieve Analysis of Sulfur1This standard is issued under the fixed designation D 4572; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of la
2、st revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the evaluation of the particlesize distribution of the coarse fraction of sulfur. It is limited
3、 tothe measurement of those particles greater than 45 m (No. 325sieve).1.2 This standard does not purport to address 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 th
4、e applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustries3. Significance and Use3.1 This test method is used to evaluate sulfur for suitab
5、ilityas a rubber vulcanizing agent. Sulfur particles must be signifi-cantly small enough to dissolve in rubber during cure andproduce a uniform network of cross-links. This test method isused as a quality control method to ensure that no excessivelylarge sulfur particles are present and to see if th
6、e productfollows a typical pattern of size distribution.3.2 This procedure is necessary when problems of the sulfurcaking occur with the use of the dry sieving procedure forparticle size.4. Apparatus4.1 Standard Sieves, stainless steel, 76 mm diameter con-taining selected stainless steel wire cloth
7、in the range of 45 to250 m mesh count.4.2 No. 6 Stiff Bristle Artist Brush, having 10 to 15 mm longbristles.4.3 Balance, with a minimum capacity of 150 g sensitive to0.001 g.4.4 Oven, circulating air type, controlled to 70 6 2C.5. Materials5.1 Liquid Detergent.6. Procedure6.1 Weigh 10.0 g of the sul
8、fur sample into a 250-cm3beaker.Wet the sulfur with 25 mL of water. Mix thoroughly with aglass stirring rod to guarantee wetting all the sulfur.NOTE 1A 1 % solution of a liquid detergent may be used if the sulfursample does not wet out properly.6.2 Weigh each cleaned and dried sieve to the nearest 0
9、.001g. Assemble preweighed stainless steel sieves in order ofdescending fineness with the coarsest screen on top. Carefullytransfer the wetted sulfur to top screen using additional waterto wash all of the sulfur out of the beaker. Wash the sulfurthrough the top sieve with a gentle stream of water fr
10、om anozzle and detergent (see 5.1) as needed. Tap or vibrate thescreen while washing. Finally, break up all agglomerated sulfurparticles using the brush. Clean sulfur from the bristles of thebrush using wash water. Be careful that the wash water doesnot back up on the finer sieves causing the sulfur
11、 slurry tooverflow the sieve sides.6.3 Remove the top sieve. Wash off any residual sulfurslurry on the underside of the sieve. Repeat the washingprocedure described in 6.2 ensuring total transport of the finesulfur particles through each successive sieve.6.4 Carefully dry the sides of the sieves wit
12、h a lint freetowel, and place each sieve separately in a drying oven at 70Cfor1horuntil the sulfur is dry. Remove the sieves and cool atleast12 h in a dessicator.6.5 Weigh each sieve to the nearest 0.001 g. When theamount of sulfur on the coarser sieves is very small (a fewparticles), it may be appr
13、opriate to brush the particles on to apreweighed glassine weighing paper and weigh the sulfurdirectly.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 edition approved May 1, 2005. Publishe
14、d May 2005. Originallyapproved in 1986. Last previous edition approved in 1999 as D 4572 89(1999).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Docu
15、ment Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7. Calculation7.1 Calculate the percent retained on each sieve, P,asfollows:P 5M1M23 100 (1)where:M1= mass residue, g, andM2= mass sample, g.7.1.1 I
16、n order to determine how much would be retained ona finer sieve, it is necessary to accumulate the mass of materialcollected on all the sieves and add it to the mass of materialfrom the selected sieve.7.2 The amount of material passing through each sieve isdetermined by subtracting the percent of th
17、e material collectedon the sieve from 100.8. Report8.1 Report the following information:8.1.1 Proper identification of samples,8.1.2 Identification of each sieve used,8.1.3 Percent retained on each sieve, and8.1.4 Percent material passing through each sieve.9. Precision and Bias39.1 This precision a
18、nd bias section has been prepared inaccordance with Practice D 4483. Refer to Practice D 4483 forterminology and other statistical details.9.2 The precision results in this precision and bias sectiongive an estimate of the precision of this test method with thematerials (rubbers) used in the particu
19、lar interlaboratory pro-grams as described below. The precision parameters should notbe used for acceptance/rejection testing of any group ofmaterials without documentation that they are applicable tothose particular materials and the specific testing protocols thatinclude this test method.9.3 A Typ
20、e 1 (interlaboratory) precision was evaluated in1986. Both repeatability and reproducibility are short term. Aperiod of a few days separates replicate test results.Atest resultis the mean value, as specified by this test method, obtained ontwo determinations or measurements of the property or param-
21、eter in question.9.4 Three different materials were used in the interlabora-tory program. These were tested in seven laboratories on twodifferent days.9.5 The results of the precision calculations for repeatabilityand reproducibility are given in Table 1. Values for r and R aregiven for 250, 180, 15
22、0, and 75 m mesh wet sieve tests.9.6 RepeatabilityThe repeatability, r, of this test methodhas been established as the appropriate value tabulated inTable 1. Two single test results, obtained under normal testmethod procedures, that differ by more than this tabulated r(for any given level) must be c
23、onsidered as derived fromdifferent or nonidentical sample populations.9.7 ReproducibilityThe reproducibility, R, of this testmethod has been established as the appropriate value tabulatedin Table 1. Two single test results obtained in two differentlaboratories, under normal test method procedures, t
24、hat differby more than the tabulated R (for any given level) must beconsidered to have come from different or nonidentical samplepopulations.9.8 BiasIn test method terminology, bias is the differencebetween an average test value and the reference (or true) testproperty value. Reference values have n
25、ot been evaluated forthis test method. Bias, therefore, cannot be determined.10. Keywords10.1 sulfur; wet sieveASTM 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 advise
26、d 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 re
27、approved 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 y
28、ou 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,United States. Individua
29、l 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).3Supporting data have been filed at ASTM International Headquarters an
30、d maybe obtained by requesting Research Report RR: D111048.TABLE 1 Type 1 Precision ResultsSulfur, Percent Through Wet-Sieve (25075 m Mesh)MaterialMean TestLevel250 m mesh 180 m mesh 150 m mesh 75 m meshrARBrRrRrROil Treated, 90 % Insoluble SulfurAC0.014 0.014 0.022 0.179 0.044 0.626 0.213 2.26Oil T
31、reated, 90 % Insoluble SulfurBC0.034 0.034 0.028 0.104 0.058 0.150 0.218 5.53General Purpose Ground SulfurC0.01 0.01 0.030 0.030 0.105 0.146 0.457 6.06Ar = repeatability = 2.83 (Sr) (within laboratories).BR = reproducibility = 2.83 (Sr) (between laboratories).CMaterial test levels for all three materials are essentially equal (99.93 100.0) for the 250100 m mesh tests. For 75 m mesh, the test levels vary from 94.08 to 96.39.D 4572 89 (2005)2
