1、Designation: D1511 12 (Reapproved 2017)Standard Test Method forCarbon BlackPellet Size Distribution1This standard is issued under the fixed designation D1511; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisio
2、n. 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 the determination of the pelletsize distribution of carbon black.1.2 The values stated in SI units are to
3、be regarded as thestandard. The values given in parentheses are for informationonly.1.3 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, health, and environment
4、al practices and deter-mine the applicability of regulatory limitations prior to use.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Gu
5、ides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1799 Practice for Carbon BlackSampling PackagedShipmentsD1900 Practice for Carbon BlackSampling Bulk Ship-mentsD4483 Practice for Evaluating Precisi
6、on for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD5817 Practice for Carbon Black, PelletedReduction,Blending, and Drying of Gross Samples for TestingE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3. Summary of Test Method3.1 A sample of carbon black
7、is shaken in a sieve shaker toseparate the pellets by size with specified series of sievescreens arranged with progressively smaller openings. Thepercentage, by mass, of carbon black retained on each sieve isweighed to calculate the pellet size distribution.4. Significance and Use4.1 The variation i
8、n the size of the pellets may relate to thelevel of dispersion and to the ease of handling. Due to the manyother variables that influence dispersion and handling, thesignificance of pellet size must be determined by the user.5. Apparatus5.1 Riffle Sample Splitter as specified in Practice D5817.5.2 B
9、alance with a sensitivity of 0.1 g.5.3 SievesU.S. Standard Sieves or equivalent, conformingto Specification E11. Sieve Nos. 10, 18, 35, 60, and 120,having openings respectively of 2000, 1000, 500, 250, and 125m, shall be used. The sieves shall be 25 mm (1 in.) in heightand 200 mm (8 in.) in diameter
10、.5.4 Bottom receiver pan and top sieve cover.5.5 Sieve ShakerAny equipment that will vibrate or shakea stack of sieves in a manner that will allow the pellets toseparate into size fractions without excessive pellet breakage.The following three types of shakers have been found satis-factory for deter
11、mining the pellet size distribution of pelletedcarbon black.5.5.1 Mechanical Sieve Shaker3The Mechanical SieveShaker shall impart a uniform rotary and tapping motion to astack of sieves as described in 5.3. The shaker machine shall bepowered with an electric motor producing constant oscillationto th
12、e sieve stack providing 280 to 320 rotary motions/min and140 to 160 taps per minute. The cover plate shall be fitted with1This test method is under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.51 on Carbon BlackPellet Properties.Current e
13、dition approved Dec. 1, 2017. Published December 2017. Originallyapproved in 1957. Last previous edition approved in 2012 as D1511 12. DOI:10.1520/D1511-12R17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of
14、ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The following devices have been found suitable: the Ro-Tap Siever and the AS200 tap. The sole sources of supply known to the committee at this time are,respectively, WS Tyler, 8570 Tyler Blvd., Mentor,
15、 OH 44060, E-mail:, and Retsch Inc., 74 Walker Lane, Newton, PA18940, E-mail:. If you are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou m
16、ay attend.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopmen
17、t of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1a cork stopper that shall extend 3 to 9 mm (18 to38 in.) abovethe metal recess. Materials other than cork, such as rubber orwood, are unacceptable. The amplitu
18、de of the hammer shall beset at 3.30 6 0.15 cm (1516 6116 in.).5.5.2 Vibratory Siever4The Retsch Sieve Shaker AS200has variable timer and amplitude settings. When set at 3 minand 0.5 amplitude, the AS200 provides satisfactory results. Itaccommodates a stack of sieves as described in 5.3.5.5.3 Automa
19、tic Sieve Shaker5The Gradex 2000 automati-cally performs all of the required steps including the weighingof the sample and the individual fractions retained on eachsieve. The equipment consists of a balance, autofeed system,electric motor that imparts a uniform rotary motion, pneumati-cally operated
20、 rods to provide the tapping action, and computerand software to record and perform analyses. Shake time of 1min provides satisfactory test results. The test sieves aredescribed in 5.3.NOTE 1Top sieve cover is not needed for the Gradex 2000.NOTE 2The Gradex is supplied with one standard tapping rod.
21、 It isrecommended that two additional tapping rods be installed to provideadditional tapping action.6. Sampling6.1 Lot samples shall be taken in accordance with PracticesD1799 or D1900.6.2 Practice D5817 shall be used for blending or reducingsamples.7. Procedure7.1 Prepare carbon black for testing a
22、s noted in Section 6.NOTE 3It is not good practice to weigh out the test portion by pouringit directly from the sample container since the smaller pellets will tend toremain in the container while the larger pellets pour out first. Dipping theblack from the container is the preferred technique.7.2 P
23、repare the sieve assembly by stacking the sieves in thefollowing order from bottom to top: Bottom receiver pan, No.120, No. 60, No. 35, No. 18, No. 10, and top sieve cover.NOTE 4Top sieve cover is not needed for the Gradex 2000.7.3 Mechanical and Vibratory Sieve Shakers:7.3.1 Weigh 100.0 g of carbon
24、 black.7.3.2 Transfer weighed carbon black to the top sieve.7.3.3 Install the sieve cover and transfer the sieve assemblyto the shaker. The stack in the shaker should be adjusted toeliminate looseness.7.3.4 Start the shaker and allow it to shake as noted below:7.3.4.1 Mechanical Shaker1 min with ham
25、mer operating.7.3.4.2 Vibratory Shaker3 min and 0.5 mm amplitude.7.3.5 Remove the sieve assembly from the apparatus andweigh individually the carbon black retained on each sieve andbottom receiver pan to the nearest 0.1 g.7.3.6 Record the data and calculate as noted in Section 8.7.4 Automatic Sieve
26、Shaker:7.4.1 Follow the manufacturers instructions to load soft-ware and configure the shake time to 1 min.7.4.2 Transfer the sieve assembly to the automatic sieveshaker.7.4.3 Weigh or measure approximately 100 g of carbonblack.7.4.4 Transfer measured carbon black to the autofeed con-tainer.7.4.5 En
27、ter the sample identification into the operatingprogram. Repeat steps 7.4.3 7.4.5 as required for consecutivesamples. Up to six samples may be identified at one time.7.4.6 Start the testing sequence according to the manufac-turers operating instructions.7.4.7 Retrieve report from the computer.8. Cal
28、culation8.1 Calculate the pellet size distribution of the sample to thenearest 0.1 % as follows:Sieve No. Mass Retained, g Percent Retained10 _ _18 _ _35 _ _60 _ _120 _ _Pan _ _Total _ _9. Report9.1 Report the following information:9.1.1 Proper identification of the sample,9.1.2 Result obtained from
29、 a single determination, reportedto the nearest 0.1 %.9.1.3 Apparatus used to determine test values.4The sole source of supply of the Retsch Sieve Shaker AS200 known to thecommittee at this time is Retsch Inc., 74 Walker Lane, Newtown, PA18940, E-mail:. If you are aware of alternative suppliers, ple
30、ase provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend.5The sole source of supply of the Gradex 2000 known to the committee at thistime is Rotex, Inc., 1230 Knowlton Stre
31、et, Cincinnati, OH 45223, E-mail:. If you are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend.TABLE 1 Precision-Type 1 Carbon Bl
32、ack-Pellet Size Distribution+10AMaterialMeanLevel,%Within Laboratories Between LaboratoriesSr r (r) SR R (R)Sample 2 0.62 0.08 0.21 34.36 0.27 0.76 121.45Sample 3 1.77 0.23 0.64 36.08 0.49 1.39 78.37Sample 1 3.52 0.32 0.90 25.58 1.33 3.75 106.64pooled oraveragevalues 1.97 0.23 0.65 32.94 0.83 2.35 1
33、19.29AThis is short term precision (days) with:p =7,q = 3, and n =4.Symbols are defined as follows:Sr = Within laboratory standard deviation,r = repeatability (in measured units),(r) = repeatability (in percent),SR = Between laboratory standard deviation,R = reproducibility (in measured units), and(
34、R) = reproducibility (in percent).D1511 12 (2017)210. Precision and Bias610.1 This precision and bias section has been prepared inaccordance with Practice D4483. Refer to Practice D4483 forterminology and other statistical details.10.2 The precision results in this precision and bias give anestimate
35、 of the precision described as follows. The precisionparameters should not be used for acceptance/rejection testingof materials without documentation that they are applicable tothose particular materials and the specific testing protocols thatinclude this test method.10.3 A Type 1 inter-laboratory p
36、recision program was con-ducted in 1988 to determine the testing precision of threesamples (Sample 1, Sample 2, and Sample 3) according to thistest method. Both repeatability and reproducibility representshort term testing conditions. The program was conducted byseven laboratories testing three samp
37、les twice on each of twodifferent days. A test result is the value obtained from a singledetermination. Acceptable differences were not measured.10.4 RepeatabilityThe repeatability, r, of the specificscreen fraction has been established as the value tabulated inTables 1-6. Two single test results (o
38、r determinations) thatdiffer by more than r must be considered suspect and dictatesthat some appropriate investigative action be taken.10.5 ReproducibilityThe reproducibility, R, of the specificscreen fraction has been established as the value tabulated inTables 1-6. Two single test results (or dete
39、rminations) thatdiffer by more than R must be considered suspect and dictatesthat some appropriate investigative action be taken.10.6 BiasBias is the difference between an average testvalue and the reference (true) test property value. Referencevalues do not exist for this test method since the valu
40、e or levelof the test property is exclusively defined by the test method.Therefore, bias cannot be determined.11. Keywords11.1 carbon black; pellet size distribution6Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D24-1007.TABLE
41、2 Precision-Type 1 Carbon Black-Pellet Size Distribution+18AMaterialMeanLevel,%Within Laboratories Between LaboratoriesSr r (r) SR R (R)Sample 2 24.89 1.36 3.84 15.42 6.27 17.75 71.31Sample 1 45.27 2.14 6.06 13.39 7.50 21.21 46.85Sample 3 72.75 2.34 6.63 9.11 2.98 8.43 11.59pooled oraveragevalues 47
42、.64 1.99 5.64 11.84 5.90 16.69 35.04AThis is short term precision (days) with:p =7,q = 3, and n =4.Symbols are defined as follows:Sr = Within laboratory standard deviation,r = repeatability (in measured units),(r) = repeatability (in percent),SR = Between laboratory standard deviation,R = reproducib
43、ility (in measured units), and(R) = reproducibility (in percent).TABLE 3 Precision-Type 1 Carbon Black-Pellet Size Distribution+35AMaterialMeanLevel,%Within Laboratories Between LaboratoriesSr r (r) SR R (R)Sample 3 20.66 1.43 4.05 19.61 2.03 5.76 27.88Sample 1 32.48 1.03 2.91 8.96 5.70 16.13 49.65S
44、ample 2 43.02 0.88 2.48 5.76 1.33 3.77 8.76pooled oraveragevalues 32.05 1.14 3.21 10.03 3.58 10.12 31.59AThis is short term precision (days) with:p =7,q = 3, and n =4.Symbols are defined as follows:Sr = Within laboratory standard deviation,r = repeatability (in measured units),(r) = repeatability (i
45、n percent),SR = Between laboratory standard deviation,R = reproducibility (in measured units), and(R) = reproducibility (in percent).TABLE 4 Precision-Type 1 Carbon Black-Pellet Size Distribution+60AMaterialMeanLevel,%Within Laboratories Between LaboratoriesSr r (r) SR R (R)Sample 3 2.97 0.65 1.84 6
46、1.94 1.07 3.03 101.92Sample 1 11.90 1.22 3.45 28.97 3.28 9.29 78.04Sample 2 21.36 1.12 3.18 14.86 2.21 6.25 29.25pooled oraveragevalues 12.08 1.03 2.91 24.07 2.37 6.70 55.44AThis is short term precision (days) with:p =7,q = 3, and n =4.Symbols are defined as follows:Sr = Within laboratory standard d
47、eviation,r = repeatability (in measured units),(r) = repeatability (in percent),SR = Between laboratory standard deviation,R = reproducibility (in measured units), and(R) = reproducibility (in percent).D1511 12 (2017)3ASTM International takes no position respecting the validity of any patent rights
48、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 tim
49、e 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 me
