ASTM D1243-1995(2008) Standard Test Method for Dilute Solution Viscosity of Vinyl Chloride Polymers《氯乙烯聚合物的稀溶液粘度的标准试验方法》.pdf

1、Designation: D 1243 95 (Reapproved 2008)Standard Test Method forDilute Solution Viscosity of Vinyl Chloride Polymers1This standard is issued under the fixed designation D 1243; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the ye

2、ar of last 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 determination of the dilutesolution viscosity of vinyl chloride polymers in cyclohe

3、x-anone. The viscosity is expressed in terms of inherent viscosity(logarithmic viscosity number). The test method is limited tothose materials that give clear, uniform solutions at the testdilution.NOTE 1Other expressions for viscosity may be used as described inthe Appendix, but any change from the

4、 test method as specified shall bestated in the report.1.2 The values stated in SI units are to be regarded as thestandard.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

5、-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.NOTE 2Although this test method and ISO 1628-2-1998 differ inapproach or detail, data obtained by either are technically equivalent.2. Referenced Documents2.1 ASTM Standards:2D 445 Test Method

6、 for Kinematic Viscosity of Transparentand Opaque Liquids (and Calculation of Dynamic Viscos-ity)D 883 Terminology Relating to PlasticsD 1600 Terminology for Abbreviated Terms Relating toPlasticsD 1755 Specification for Poly(Vinyl Chloride) ResinsD 2857 Practice for Dilute Solution Viscosity of Poly

7、mersE77 Test Method for Inspection and Verification of Ther-mometers2.2 ISO Standard:ISO 1628-2-1998 Determination of Viscosity Number andLimiting Viscosity NumberPart 2: Poly(Vinyl Chloride)Resins32.3 National Institute of Standards and Technology Circu-lar:4C-434 Testing of Glass Volumetric Appara

8、tus3. Terminology3.1 Definitions: Definitions are in accordance with Termi-nology D 883 and Terminology D 1600, unless otherwiseindicated.4. Summary of Test Method4.1 Asample of resin is dissolved in cyclohexanone to makea solution of specified concentration. Inherent viscosity (loga-rithmic viscosi

9、ty number) is calculated from the measured flowtimes of the solvent and of the polymer solution.NOTE 3For additional information, refer to Test Method D 445 andTest Method D 2857 for Dilute Solution Viscosity of Polymers.5. Significance and Use5.1 Dilute solution viscosity values for vinyl chloride

10、poly-mers are related to the average molecular size of that portion ofthe polymer that dissolves in the solvent.6. Apparatus6.1 Transfer Pipets.6.2 Volumetric Flasks, 100-mL, glass-stoppered, in accor-dance with National Institute of Standards and TechnologyCircular C-434.6.3 Viscometer, Ubbelohde S

11、eries U-1 or Cannon-Ubbelohde No. 75.6.4 Water Bath,at306 0.5C, controlled to within 60.01C.6.5 Timer, as specified in Test Method D 445, graduated indivisions of 0.1 s or less.6.6 Filter Funnel, fritted-glass.56.7 Thermometer, standard, in accordance with MethodE77.1This test method is under the ju

12、risdiction of ASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materi-als.15.07).Current edition approved March 1, 2008. Published April 2008. Originallyapproved in 1952. Last previous edition approved in 2000 as D 1243 - 95(2000)e1.2For referenc

13、ed 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 onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd S

14、t.,4th Floor, New York, NY 10036, http:/www.ansi.org.4Available from National Institute of Standards and Technology (NIST), 100Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http:/www.nist.gov.5Filters may be obtained from Corning Glass, No. 36060 “Coarse” type.1Copyright ASTM International, 10

15、0 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7. Materials7.1 SolventCyclohexanone, analytical reagent grade orlaboratory-distilled technical grade, boiling between 155 and156C at 760 mm Hg has been found acceptable if stored in aclosed container.8. Procedure8.1 D

16、issolve duplicates of resin as follows: Weigh 0.260.002 g of the sample (moisture content below 0.1 %) andtransfer it to a 100-mL glass-stoppered volumetric flask. Takecare to transfer all of the weighed resin into the flask. As analternative method, the resin (0.26 0.002 g) may be weigheddirectly i

17、nto a tared, 100-mL glass-stoppered volumetric flask.8.2 Add 50 to 70 mL of cyclohexanone to the flask, takingcare to wet the resin so that lumps do not form.8.3 Heat the flask at 85 6 10C until the resin is dissolved.Occasional shaking will reduce the time required for solution.Heating should not e

18、xceed 12 h and should preferably be lessto minimize degradation. If any gel-like particles can be seen,prepare a new solution.8.4 Cool the solution to the test temperature by immersingflask in the 30C bath for a minimum time of 30 min and adjustto a solution volume of 100 mL. Filter through a fritte

19、d-glassfilter directly into the viscometer.8.5 Measure at 30C the flow time of the prepared solution(8.4) and of the pure solvent (aged at 85 6 10C) in theviscometer. Allow 10 min for the viscometer to come totemperature equilibrium after placing it in the water bath. Theflow time of the solution or

20、 the solvent should be within 0.1 %on repeat runs on the same filling.NOTE 4Keep the Ubbelohde viscometer clean when not in use.Acetone may be used as a cleaning flush. The viscometer may be storedfilled with pure solvent or it may be stored dry.9. Calculation9.1 Calculate the relative and inherent

21、viscosity (viscosityratio and logarithmic viscosity number) as follows:hrel5 t/tohinh5 lnhrel!/Cwhere:hrel= relative viscosity (viscosity ratio),t = efflux time of the solution,to= efflux time of the pure solvent,C = weight of sample used (8.1) per 100 mL ofsolution,hinh= inherent viscosity (logarit

22、hmic viscosity num-ber), andln hrel= natural logarithm of relative viscosity (viscosityratio).10. Report10.1 Report the average inherent viscosity of two analysesto the nearest 0.01.11. Precision and Bias611.1 An interlaboratory test program utilizing this testmethod was carried out in 1973 involvin

23、g seven laboratories,each performing pairs of determinations on one polymer.NOTE 5See Specification D 1755, Table 3, for inherent viscosityvalue of ASTM PVC Reference Standard No. 1.11.2 PrecisionThe following values of precision havebeen calculated from the interlaboratory test program at a 95 %con

24、fidence level:Within-laboratory precision (within one pair of values) 1.4 % of meanBetween-laboratories precision (between averages ofpairs)2.2 % of mean11.3 BiasNo justifiable statement of bias can be made forthis test method, since the true value of the property cannot beestablished by an accepted

25、 referee method.12. Keywords12.1 dilute solution viscosity; inherent viscosity; intrinsicviscosity; relative viscosity; specific viscosity; test method;vinyl chloride polymersAPPENDIX(Nonmandatory Information)X1. OTHER EXPRESSIONS FOR VISCOSITYX1.1 DefinitionsX1.1.1 relative viscosityratio of the fl

26、ow time of a speci-fied solution of the polymer to the flow time of the pure solvent.The International Union of Pure and Applied Chemistry(IUPAC) term for relative viscosity is viscosity ratio.X1.1.2 specific viscosityrelative viscosity minus one. Spe-cific viscosity represents the increase in visco

27、sity that may beattributed to the polymeric solute.X1.1.3 reduced viscosityratio of the specific viscosity tothe concentration. Reduced viscosity is a measure of thespecific capacity of the polymer to increase the relativeviscosity. The IUPAC term for reduced viscosity is viscositynumber.X1.1.4 inhe

28、rent viscosityratio of the natural logarithm ofthe relative viscosity to the concentration. The IUPAC term forinherent viscosity is logarithmic viscosity number.X1.1.5 intrinsic viscosity limit of the reduced and inherentviscosities as the concentration of the polymeric solute ap-proaches zero and r

29、epresents the capacity of the polymer toincrease viscosity. Interactions between solvent and polymer6Supporting data are available from ASTM Headquarters. Request RR: D20-1112.D 1243 95 (2008)2molecules have the affect of yielding different intrinsic viscosi-ties for the same polymer in various solv

30、ents. The IUPAC termfor intrinsic viscosity is limiting viscosity number.X1.2 Determination of Intrinsic Viscosity (LimitingViscosity Number)X1.2.1 To determine the intrinsic viscosity (limiting viscos-ity number) of a polymer from dilute solution viscosity data,the reduced and inherent viscosities

31、(viscosity and logarithmicviscosity number) of solutions of various concentrations of thepolymer are determined at constant temperature and thesevalues are then plotted against the respective concentrations.The two lines thus obtained converge to a point of zeroconcentration of the solute which repr

32、esents the intrinsicviscosity (limiting viscosity number) of the polymer in thatsolvent at the temperature of the determination. Fig. X1.1illustrates this convergence.X1.2.2 At higher concentrations the viscosity curves maydeviate from linearity; therefore, the greatest accuracy isobtained at less t

33、han 0.5 g/mL of solution. Since extrapolationof either reduced viscosity or inherent viscosity (viscosity orlogarithmic viscosity number) curves to infinite dilution willgive the same value for intrinsic viscosity (limiting viscositynumber), a plot of either type of viscosity will permit thecalculat

34、ion of valid intrinsic viscosity (limiting viscosity num-ber) data.X1.3 Estimation of Intrinsic Viscosity (Limiting ViscosityNumber)X1.3.1 The mathematical method of Billmeyer (1)7permitsa good approximation of intrinsic viscosity (limiting viscositynumber). This method makes use of equations derive

35、d from thepower series expansion of viscosity versus concentration.Neglecting the higher order terms, equations may be writtenwhich can be used to estimate intrinsic viscosity (limitingviscosity number). The following equation has been foundsuitable for poly(vinyl chloride) resins:h514hrel2 1!/C# 1

36、S34ln hrelD/Cwhere C = concentration of polymer, g/100 mL.REFERENCES(1) Billmeyer, F. W., Jr., Journal of Polymer Science, Vol 4, 1949, p. 83.(2) Cragg, L. H., and Fern, C. R. H., Journal of Polymer Science, Vol 10,1953, p. 185.(3) Huggins, M. L., Journal of the American Chemical Society, Vol 64,194

37、2, p. 2716.(4) International Union of Pure and Applied Chemistry, Journal ofPolymer Science, Vol 8, 1952, p. 269.(5) Streeter, D. J., and Boyer, R. F., Industrial and Engineering Chemistry,Vol 43, 1951, p. 1790.ASTM International takes no position respecting the validity of any patent rights asserte

38、d 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 time by th

39、e 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

40、careful consideration at a meeting of theresponsible technical committee, 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 Internat

41、ional, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,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).7The boldface numbers in parentheses refer to the list of references at the end ofthis test method.FIG. X1.1 Example of Plot to Determine Intrinsic Viscosity.D 1243 95 (2008)3