1、Designation: D1514 04 (Reapproved 2011)Standard Test Method forCarbon BlackSieve Residue1This standard is issued under the fixed designation D1514; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number
2、 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 waterwash sieve residue in regular untreated carbon blacks. It maynot be applicable to oil-t
3、reated carbon blacks because the oilwould prevent proper wetting of the black by water.1.2 The values stated in SI units are to be regarded as thestandard. The values in parentheses are for information only.1.3 This standard does not purport to address all of thesafety concerns, if any, associated w
4、ith 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. For specificprecautionary statements, see Section 6.2. Referenced Documents2.1 ASTM Standards:2D1799 Practi
5、ce for Carbon BlackSampling PackagedShipmentsD1900 Practice for Carbon BlackSampling Bulk Ship-mentsD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3. Summary of Tes
6、t Method3.1 A sample of carbon black is washed with water througha wire-mesh screen of a specified size until all that remains isa non-carbon black residue. This residue is dried, weighed, andthe amount of residue is expressed as mg/kg (ppm) of theoriginal sample.4. Significance and Use4.1 The quant
7、ity of sieve residue of carbon black is impor-tant in some molded or extruded products as it may relate to thesurface appearance of those products. The maximum residue ineach application is normally determined and agreed to betweenthe user and the producer.5. Apparatus5.1 Sieve and Filtering Apparat
8、us,3, 4as shown in Fig. 1.5.2 Balance, with a sensitivity of 0.01 g.5.3 Analytical Balance, with a sensitivity of 0.1 mg.5.4 Oven, gravity-convection type, capable of temperatureregulation within 61C at 125C and temperature uniformitywithin 65C.5.5 Sieves, of either phosphor bronze or stainless stee
9、l. Thesieve shall be in accordance with Specification E11. The sieveto be used shall be agreed upon between the purchaser and theseller.5.6 Weighing Dishes.6. Precautions6.1 Keep the apparatus clean at all times to prevent con-tamination.6.2 Examine the sieves each time they are used to make suretha
10、t no cracks or holes have developed.6.3 Examine the strainer periodically to ascertain that thefilter screen is in good condition.7. Sampling7.1 Samples shall be taken in accordance with PracticeD1799 or Practice D1900.1This test method is under the jurisdiction of ASTM Committee D24 on CarbonBlack
11、and is the direct responsibility of Subcommittee D24.31 on Non-CarbonBlack Components of Carbon Black.Current edition approved May 1, 2011. Published July 2011. Originally approvedin 1957. Last previous edition approved in 2004 as D1514 04. DOI: 10.1520/D1514-04R11.2For referenced ASTM standards, vi
12、sit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Sieve and filtering apparatus, available from Titan Specialties, Inc., P.O. Box2316, Pampa, TX
13、 70066-2316, has been found suitable. The A2000 Test Set fromKrahnen IQS, GmbH, Paffrather Str. 1315, D-51069 Koeln, Germany, has beenfound suitable. An ASTM specified apparatus modified with an enlarged funnel legID (5.080 cm or 2.0 in.) and sieve screen OD (6.032 cm or 2.375 in.) has also beenfoun
14、d suitable.4The sole source of supply of housing No. 20 and cartridge No. 30 known to thecommittee at this time is Amtec, Plymouth Products Division, 562 Indiana Ave.,Sheboygan, WI 53081. If you are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Yo
15、ur comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.8. Calibration8.1 Calculate the sieve residue to the nearest mg/kg
16、 (ppm)as follows:R 5 W/S! 3 106(1)where:R = sieve residue, mg/kg (ppm),W = mass of sieve residue, g, andS = mass of sample, g.9. Procedure9.1 Prior to making a test, clean the strainer by openingvalves A and B and closing valve C as shown in Fig. 1. Allowthe strainer to wash for 2 min.9.2 Close valv
17、e B and open valve C. With valves A and Ccompletely open, regulate the water pressure by means of areducing valve. The recommended water pressure is 207 6 34kPa (30 6 5 lbf/in.2).9.3 After the water pressure has been regulated, attach thesieve holder with a 50-mm (2-in.) diameter sieve to the funnel
18、and allow the water to run through it for 3 min. Stop the waterflow by closing valves A and C. Examine the sieve forparticles; if none are observed, the apparatus is ready for use.9.4 Weigh 100.0 g of the carbon black on the balance.9.5 Attach the proper sieve to the funnel and start the waterflow b
19、y opening valves A and C.9.6 Add the carbon black slowly to the funnel to preventplugging of the sieve.NOTE 1If desired, it shall be permissible to disperse the carbon blackin water using a high speed stirring apparatus. It shall also be permissibleto utilize wetting agents to facilitate dispersion.
20、 Care must be taken toensure that all of the solid material is transferred from the vessel used fordispersing the black into the funnel of the washing apparatus.9.7 Use a gentle stream of water from the hose attached tovalve D to wash down any carbon black on the sides of thefunnel.9.8 Continue wash
21、ing until the wash water coming throughthe sieve is clear.9.9 Remove the sieve holder and sieve from the funnel andrub the residue lightly with the finger to disaggregate any hardcarbon black lumps which may not have been thoroughly wetby the water.9.10 Replace the sieve holder and sieve and wash fo
22、r anadditional 2 min.9.11 Remove the sieve holder and sieve and dry for1hat125C.9.12 Transfer the dried residue to a piece of smooth whitebond paper and rub gently to remove any carbon blackremaining on the residue. Rub until the white paper no longershows any smears.NOTE 2The purpose of gently rubb
23、ing the residue is to remove anyblack that may be clinging to the gritty residue. Do not apply excessiveforce when rubbing, as this action may fracture the residue allowing it toescape, or may trap the residue in the paper causing a low gritdetermination. Similarly, do not wear gloves when performin
24、g this step, asthe residue may be trapped in the glove material, giving a low result.9.13 Brush all the loose residue to a tared weighing dish andweigh to the nearest 0.1 mg using the analytical balance.10. Report10.1 Report the following information:10.1.1 Proper identification of the sample,10.1.2
25、 Identification of the sieve number, and10.1.3 Result of the determinations reported to the nearestmg/kg (ppm).11. Precision and Bias11.1 These precision statements have been prepared inaccordance with Practice D4483. Refer to this practice forterminology and other statistical details.11.2 The preci
26、sion results in this precision and bias sectiongive an estimate of the precision of this test method with thematerials used in the particular interlaboratory program de-scribed below. The precision parameters should not be used foracceptance or rejection testing of any group of materialswithout docu
27、mentation that they are applicable to those par-ticular materials and the specific testing protocols of the testmethod. Any appropriate value may be used from Table 1.Atype 1 interlaboratory precision program was conducted asdetailed in Table 2. Both repeatability and reproducibilityrepresent short-
28、term (daily) testing conditions. The testing wasperformed using two operators in each laboratory performingthe test once on each of two days (total of four tests). A testresult is the value obtained from a single determination.Acceptable difference values were not measured. The betweenoperator compo
29、nent of variation is included in the calculatedvalues for (r) and (R).NOTE 1Industrial/O.E.M. filter and pleated polyester fabric reusablecartridges have been found to be a satisfactory strainer.1NOTE 2Corrosion-free piping must be used.NOTE 3Detailed drawings can be obtained from Test MethodD1514 8
30、8a.NOTE 4Spray nozzle: Part No. 460.746.30 BE available from LechlerInc., 445 Kautz Rd., St. Charles, IL 60174, or Titan Specialties Inc., P.O.Box 2316, Pampa, TX 70066-2316.FIG. 1 Schematic Diagram of Apparatus for Sieve ResidueDeterminationD1514 04 (2011)211.3 The results of the precision calculat
31、ions for this test aregiven in Table 1. The materials are arranged in ascending“mean level” order.11.4 RepeatabilityThe pooled relative repeatability, (r),ofthis test method has been established as 80.8 %. Any othervalue in Table 1 may be used as an estimate of repeatability, asappropriate. The diff
32、erence between two single test results (ordeterminations) found on identical test material under therepeatability conditions prescribed for this test will exceed therepeatability on an average of not more than once in 20 casesin the normal and correct operation of the method. Two singletest results
33、that differ by more than the appropriate value fromTable 1 must be suspected of being from different populationsand some appropriate action taken.NOTE 3Appropriate action may be an investigation of the test methodprocedure or apparatus for faulty operation or the declaration of asignificant differen
34、ce in the two materials, samples, and so forth, whichgenerated the two test results.11.5 ReproducibilityThe pooled relative reproducibility,(R), of this test method has been established as 180 %. Anyother value in Table 1 may be used as an estimate ofreproducibility, as appropriate. The difference b
35、etween twosingle and independent test results found by two operatorsworking under the prescribed reproducibility conditions indifferent laboratories on identical test material will exceed thereproducibility on an average of not more than once in 20 casesin the normal and correct operation of the met
36、hod. Two singletest results produced in different laboratories that differ bymore than the appropriate value from Table 1 must besuspected of being from different populations and some appro-priate investigative or technical/commercial action taken.11.6 BiasIn test method terminology, bias is the dif
37、fer-ence between an average test value and the reference (true) testproperty value. Reference values do not exist for this testmethod, since the value or level of the test property isexclusively defined by the test method. Bias, therefore, cannotbe determined.12. Keywords12.1 carbon black; non-carbo
38、n black residue; sieve residue;water wash sieve residueASTM 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
39、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
40、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 hear
41、ing 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. Individual reprints (single or multiple copies) of this standard
42、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/).TABLE 1 Preci
43、sion Parameters for D1514 Sieve Residue, (Type 1(No. 325 Sieve) Precision)Units mg/kg (ppm)Material Mean Level Sr (r) SR (R)IRB#6 (N330) 18.3 6.0 93.3 13.1 203N762 18.3 7.4 114 9.7 150SRB A5 (N135) 20.8 5.1 69.5 9.7 132N550 64.3 10.4 45.9 24.7 109N650 75.7 20.2 75.6 46.7 174Average 39.5Pooled Values 11.3 80.8 25.1 180TABLE 2 Interlaboratory Precision ProgramNominal Test Period Material Number of LaboratoriesMarch 1996 N650 49October 1996 IRB#6 (N330) 41March 1997 N762 45September 1997 SRB A5 (N135) 42March 1998 N550 47D1514 04 (2011)3
