1、Designation: D 4315 94 (Reapproved 2006)Standard Test Methods forRubber Compounding MaterialZinc Oxide1This standard is issued under the fixed designation D 4315; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last rev
2、ision. 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 These test methods cover chemical and physical tests forzinc oxide that are considered to be important to its use inrubber co
3、mpounding.1.2 The tests appear in the following order:Test SectionZinc Oxide 5Lead and Cadmium 6Sulfur 7Heat Loss 8Surface Area 9Sieve Residue 101.3 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 stand
4、ard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use For specificprecautions, see 5.2.2. Referenced Documents2.1 ASTM Standards:2D 280 Test Methods for Hygroscopic Moisture (and OtherMatter Volatile Under the Test Condition
5、s) in PigmentsD 1193 Specification for Reagent WaterD 3037 Test Methods for Carbon BlackSurface Area byNitrogen Adsorption3D 3040 Practice for Preparing Precision Statements forStandards Related to Rubber and Rubber Testing3D 3280 Test Methods for Analysis of White Zinc PigmentsD 4075 Test Methods f
6、or Rubber CompoundingMaterialsFlame Atomic Absorption AnalysisDetermination of MetalsE11 Specification for Wire Cloth and Sieves for TestingPurposes3. Significance and Use3.1 These test methods may be used for quality control ofzinc oxide used as a compounding material and for researchand developmen
7、t studies where zinc oxide is used in a rubbermix.4. Reagents4.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.4.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean Type IV reagent water inaccordance with Specification D 1193.ZINC OXIDE5.
8、 Procedure for Determination of % Zinc Oxide5.1 Analysis of white zinc pigments is covered in TestMethods D 3280.5.2 Reagents and safety precautions for Test MethodsD 3280 apply.5.3 Section 6 of Test Methods D 3280 describes the analysisof total zinc in zinc oxide using diphenylamine as internalindi
9、cator.5.4 Section 7 of Test Methods D 3280 describes the analysisof total zinc in zinc oxide using uranyl acetate as externalindicator.LEAD AND CADMIUM6. Procedure for Determination of Lead and Cadmium inZinc Oxide6.1 Test Methods D 4075 is the standard test method formetal analysis in compounding m
10、aterials using the flameatomic absorption technique.Analysis for cadmium and lead inzinc oxide are described in Sections 11 through 20 of TestMethods D 4075.SULFUR7. Procedure for Determination of Sulfur in Zinc Oxide7.1 Analysis of white zinc pigments is covered in TestMethods D 3280.7.2 Reagents a
11、nd safety precautions for Test MethodsD 3280 apply.1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and are the direct responsibility of Subcommittee D11.20 on CompoundingMaterials and Procedures.Current edition approved Oct. 1, 2006. Published November 2006. Originallya
12、pproved in 1984. Last previous edition approved in 2001 as D 4315 94 (2001).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 Document Summary page onth
13、e ASTM website.3Withdrawn.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7.3 Section 9 of Test Methods D 3280 describes the analysisof total sulfur in zinc oxide.HEAT LOSS8. Procedure for Determining Heat Loss in Zinc Oxide8.1 Use T
14、est Methods D 280, Method A, for pigments thatdo not decompose at 110C.SURFACE AREA9. Surface Area of Zinc Oxide9.1 Use Procedure D of Test Methods D 3037. Test MethodsD 3037 are written for carbon black using a flowing gas surfacearea analyzer. It shall be followed with the following excep-tions:9.
15、2 Sections 33.11 and 33.12 shall read:Accurately weigh a clean, dry, empty sample cell and record the mass.Using a small funnel, pour the zinc oxide into the sample cell using the fol-lowing table as a guide for the approximate sample mass:Surface Area, 103m2/kg Zinc Oxide Mass, g940.200.350.500.709
16、.3 Section 33.16 shall read:Outgas the Zinc Oxide at 200C for 20 min9.4 Section 33.21 shall read:An attenuator setting of one is usually satisfactoryfor the surface areas and masses.NOTE 1See 9.2.9.5 Sections 33.33.1, 33.33.2 and 33.33.3 should be disre-garded as not relevant as there are currently
17、no ASTMapproved reference standards for zinc oxide surface areas.SIEVE RESIDUE10. Procedure for Sieve Residue of Zinc Oxide10.1 Apparatus:10.1.1 Sieves, 75-mm (3-in.) or 200-mm (8-in.) with 45-m(325-mesh) wire cloth.410.1.2 Balance, with a sensitivity of 60.1 mg.10.1.3 Drying Oven, maintained at 100
18、 6 10C.10.1.4 Weighing Dish.10.1.5 Aerator, for hose connected to a tap-water supply.10.2 Reagents:10.2.1 Tap Water.10.3 Sampling:10.3.1 Sampling shall be at the discretion of the analyst toobtain a representative sample of the lot to be tested.10.4 Procedure:10.4.1 Weigh a 10 to 100-g sample to 60.
19、1 g in a suitableweighing dish. Small samples are used with the 75-mm (3-in.)sieve, large samples for the 200-mm (8-in.) sieve.10.4.2 Place the sample in the sieve and wash with a streamof tap water, directed onto the sieve from a hose. If any lumpsare detected after most of the zinc oxide has passe
20、d through thesieve, gently manipulate the lumps to break them up usingfinger tips or a small brush. This operation serves to break upany persistent lumps of zinc oxide but is not stringent enoughto force coarse, hard particles through the sieve. Continuewashing with tap water until no more residue w
21、ill pass throughthe sieve. When no more residue will pass through the sieve,place the sieve in an oven maintained at 100C until it is dry.10.4.3 Remove the sieve from the oven and transfer anyweighable residue to a small weighing dish, which has beenpreviously weighed to 60.1 mg and weigh.10.5 Calcu
22、lations:10.5.1 Calculate the percent sieve residue R as follows:R 5 W/S 3 100 (1)where:R = sieve residue, %,W = mass of sieve residue, g, andS = mass of sample, g.10.6 Report:10.6.1 The report shall include the following information:10.6.1.1 Proper identification of the sample.10.6.1.2 Results of tw
23、o individual percent sieve residuedeterminations and their average.11. Precision and Bias11.1 Precision and bias statements are in the process ofbeing prepared in the form specified by Practice D 3040. Theywill be added to these test methods when completed.12. Keywords12.1 chemical and physical test
24、s for zinc oxide; heat loss;lead and cadmium in zinc oxide; sieve residue; sulfur in zincoxide; surface area; zinc oxide; zinc oxide percentASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this
25、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
26、 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 committe
27、e, which you may attend. If you 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-
28、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).4Detailed requirements for this sieve are given in Specification E11.D 4315 94 (2006)2
