1、Designation: D 1243 95 (Reapproved 2000)e1Standard 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
2、year 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.e1NOTEReference to ISO 1628-2 was corrected editorially in March 2000.1. Scope1.1 This test method covers the determinati
3、on of the dilutesolution viscosity of vinyl chloride polymers in cyclohex-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 vi
4、scosity may be used as described inthe Appendix, but any change from the 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.
5、 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.NOTE 2Although this test method and ISO 1628-2-1998 differ inapproach or detail, data obtained by either are technically
6、 equivalent.2. Referenced Documents2.1 ASTM Standards:D 445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and the Calculation of DynamicViscosity)2D 883 Terminology Relating to Plastics2D 1600 Terminology for Abbreviated Terms Relating toPlastics3D 1755 Specification for Poly
7、(Vinyl Chloride) Resins3D 2857 Test Method for Dilute Solution Viscosity of Poly-mers4E 77 Method for Verification and Calibration of Liquid-in-Glass Thermometers52.2 ISO Standard:ISO 1628-2-1998 Determination of Viscosity Number andLimiting Viscosity NumberPart 2: Poly(Vinyl Chloride)Resins62.3 Nat
8、ional Institute of Standards and Technology Circu-lar:7C-434 Testing of Glass Volumetric Apparatus3. Terminology3.1 Definitions: Definitions are in accordance with Termi-nology D 883 and Terminology D 1600, unless otherwiseindicated.4. Summary of Test Method4.1 A sample of resin is dissolved in cycl
9、ohexanone to makea solution of specified concentration. Inherent viscosity (loga-rithmic viscosity 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 Visco
10、sity of Polymers.35. Significance and Use5.1 Dilute solution viscosity values for vinyl chloride 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-da
11、nce with National Institute of Standards and TechnologyCircular C-434.6.3 Viscometer, Ubbelohde Series U-1 or Cannon-Ubbelohde No. 75.1This test method is under the jurisdiction of ASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materials(Sectio
12、n D20.15.07).Current edition approved March 15, 1995. Published May 1995. Originallypublished as D 1243 52 T. Last previous edition D 1243 79 (1990)e1.This edition contains changes in Sections 1 and 2 to include an ISO equivalencystatement.2Annual Book of ASTM Standards, Vols 05.01 and 10.03.3Annual
13、 Book of ASTM Standards, Vol 08.01.4Annual Book of ASTM Standards, Vol 08.02.5Annual Book of ASTM Standards, Vol 14.03.6Available from American National Standards Institute, 11 W. 42nd St., 13thFloor, New York, NY 10036.7Available from National Institute of Standards and Technology, U. S. Dept. ofCo
14、mmerce, Washington, DC 20234.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.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 Funne
15、l, fritted-glass.86.7 Thermometer, standard, in accordance with MethodE 77.7. 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 Dissolve
16、 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 into a t
17、ared, 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 exceed 1
18、2 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 fritted-glass
19、filter 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 the so
20、lvent 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 viscosi
21、ty (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 (logarithmic vi
22、scosity 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 Bias911.1 An interlaboratory test program utilizing this testmethod was carried out in 1973 involving seven
23、 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 %confidence
24、 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 refere
25、e method.12. Keywords12.1 dilute solution viscosity; inherent viscosity; intrinsicviscosity; relative viscosity; specific viscosity; test method;vinyl chloride polymers8Filters may be obtained from Corning Glass, No. 36060 “Coarse” type.9Supporting data are available from ASTM Headquarters. Request
26、RR: D20-1112.D 12432APPENDIX(Nonmandatory Information)X1. OTHER EXPRESSIONS FOR VISCOSITYX1.1 DefinitionsX1.1.1 relative viscosityratio of the flow time of a speci-fied solution of the polymer to the flow time of the puresolvent. The International Union of Pure and Applied Chem-istry (IUPAC) term fo
27、r relative viscosity is viscosity ratio.X1.1.2 specific viscosityrelative viscosity minus one. Spe-cific viscosity represents the increase in viscosity that may beattributed to the polymeric solute.X1.1.3 reduced viscosityratio of the specific viscosity tothe concentration. Reduced viscosity is a me
28、asure of thespecific capacity of the polymer to increase the relativeviscosity. The IUPAC term for reduced viscosity is viscositynumber.X1.1.4 inherent viscosityratio of the natural logarithm ofthe relative viscosity to the concentration. The IUPAC term forinherent viscosity is logarithmic viscosity
29、 number.X1.1.5 intrinsic viscosity limit of the reduced and inher-ent viscosities as the concentration of the polymeric soluteapproaches zero and represents the capacity of the polymer toincrease viscosity. Interactions between solvent and polymermolecules have the affect of yielding different intri
30、nsic viscosi-ties for the same polymer in various solvents. 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 solutio
31、n viscosity data,the reduced and inherent viscosities (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
32、 a point of zeroconcentration of the solute which represents 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;
33、 therefore, the greatest accuracy isobtained at less than 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 pl
34、ot of either type of viscosity will permit thecalculation 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)10permitsa good approximation of intrinsic viscosity (limiting visc
35、ositynumber). This method makes use of equations derived 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 foundsuit
36、able for poly(vinyl chloride) resins:h514hrel2 1!/C# 1FS34ln hrelD/CGwhere C = concentration of polymer, g/100 mL.10The boldface numbers in parentheses refer to the list of references at the endof this test method.FIG. X1.1 Example of Plot to Determine Intrinsic Viscosity.D 12433REFERENCES(1) Billme
37、yer, 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 64,1942, p. 2716.(4) International Union of Pure and Applied Chemistry, Journal ofPo
38、lymer 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 asserted in connection with any item mentionedin this standard. Users of this standar
39、d 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 andif
40、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 committee, whic
41、h 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 19428-2959,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).D 12434
