1、Designation: D1243 95 (Reapproved 2008)D1243 14Standard Test Method forDilute Solution Viscosity of Vinyl Chloride Polymers1This standard is issued under the fixed designation D1243; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision,
2、the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope Scope*1.1 This test method covers the determination of the dilute solution viscosity of vinyl chloride polyme
3、rs in cyclohexanone. Theviscosity is expressed in terms of inherent viscosity (logarithmic viscosity number). The test method is limited to those materialsthat give clear, uniform solutions at the test dilution.NOTE 1Other expressions for viscosity may be used as described in the Appendix, but any c
4、hange from the test method as specified shall be statedin the report.1.2 The values stated in SI units are to be regarded as the standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to
5、 establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.NOTE 2Although this test method and ISO 1628-2-1998 differ in approach or detail, data obtained by either are technically equivalent. This standardand ISO 1628-2 address the same
6、subject matter, but differ in technical content.2. Referenced Documents2.1 ASTM Standards:2D445 Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and Calculation of Dynamic Viscosity)D446 Specifications and Operating Instructions for Glass Capillary Kinematic ViscometersD883 Ter
7、minology Relating to PlasticsD1600 Terminology for Abbreviated Terms Relating to PlasticsD1755 Specification for Poly(Vinyl Chloride) ResinsD2857 Practice for Dilute Solution Viscosity of PolymersE77E2251 Test Method for Inspection and Verification of ThermometersSpecification for Liquid-in-GlassAST
8、M Thermometerswith Low-Hazard Precision Liquids2.2 ISO Standard:ISO 1628-2-19981628-2 Determination of Viscosity Number and Limiting Viscosity NumberPart 2: Poly(Vinyl Chloride)Resins32.3 National Institute of Standards and Technology Circular:4C-434 Testing of Glass Volumetric Apparatus3. Terminolo
9、gy3.1 Definitions: DefinitionsDefinitions are in accordance with Terminology D883 and Terminology D1600, unless otherwiseindicated.4. Summary of Test Method4.1 A sample of resin is dissolved in cyclohexanone to make a solution of specified concentration. Inherent viscosity(logarithmic viscosity numb
10、er) is calculated from the measured flow times of the solvent and of the polymer solution.1 This test method is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.15 on ThermoplasticMaterials.15.07).Current edition approved March 1, 2008Oct.
11、 1, 2014. Published April 2008October 2014. Originally approved in 1952. Last previous edition approved in 20002008 asD1243 - 95 (2008).(2000)1. DOI: 10.1520/D1243-95R08.10.1520/D1243-14.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceas
12、tm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.4 Available from National Institute of Standa
13、rds and Technology (NIST), 100 Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http:/www.nist.gov.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technica
14、lly possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this sta
15、ndardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1NOTE 3For additional information, refer to Test Method D445 and Test Method D2857 for Dilute Solution Viscosity of Polymers.5. Significance and Use5.1 Dilute solution viscosity valu
16、es for vinyl chloride polymers are related to the average molecular size of that portion of thepolymer that dissolves in the solvent.6. Apparatus6.1 Transfer Pipets.6.2 Volumetric Flasks, 100-mL, glass-stoppered, in accordance with National Institute of Standards and Technology CircularC-434.6.3 Vis
17、cometer, ASTM Ubbelohde Series U-1Size 1 or Cannon-Ubbelohde No. 75.NOTE 4ASTM Ubbelohde Size 1 is a commonly used name for a specific viscometer type, which is neither supplied nor endorsed by ASTMInternational.NOTE 5Operating instructions can be found in Specification D446.6.4 Water Bath, set at 3
18、0630.0 6 0.5C, controlled to within 6 0.01C.6.4.1 The temperature of the bath medium shall not vary by more than 60.02C of the selected temperature in accordance withTest Method D445.6.5 Timer, as specified in Test Method D445, graduated in divisions of 0.1 s or less.6.6 Filter Funnel, fritted-glass
19、.56.7 Thermometer, standard, in accordance with Method E77E2251.7. Materials7.1 SolventCyclohexanone, analytical reagent grade or laboratory-distilled technical grade, boiling between 155 and 156Cat 760 mm Hg has been found acceptable if stored in a closed container.8. Procedure8.1 Dissolve duplicat
20、es of resin as follows: Weigh 0.26 0.2 6 0.002 g of the sample (moisture content below 0.1 %) andtransfer it to a 100-mL glass-stoppered volumetric flask. Take care to transfer all of the weighed resin into the flask. As analternative method, weigh the resin (0.26 0.002 g) may be weighed (0.2 6 0.00
21、2 g) directly into a tared, 100-mL glass-stopperedvolumetric flask.8.2 Add 50 to 70 mL of cyclohexanone to the flask, taking care 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.Heat
22、ing should not exceed 12 h and should preferably be less Take care that heating time does not exceed 12 h, preferably less,to minimize degradation. If any gel-like particles can be seen, prepare a new solution.8.4 Cool the solution to the test temperature by immersing flask in the 30C bath for a min
23、imum time of 30 min and adjust toa solution volume of 100 mL. Filter through a fritted-glass filter directly into the viscometer.8.5 Measure at 30C 30.0 6 0.5C the flow time of the prepared solution (8.4) and of the pure solvent (aged at 85 6 10C)in the viscometer. Allow 10 min for the viscometer to
24、 come to temperature equilibrium after placing it in the water bath. The Ifthe flow time of the solution or the solvent should be within differs by more than 0.1 % on repeat runs on the same filling. filling,the result is suspect.NOTE 6Keep the Ubbelohde viscometer clean when not in use. Acetone may
25、 be used as a cleaning flush. to flush the pure solvent (Cyclohexanone)and enable subsequent drying. The viscometer may be stored filled with pure solvent or it may be stored dry.9. Calculation9.1 Calculate the relative and inherent viscosity (viscosity ratio and logarithmic viscosity number) as fol
26、lows:rel 5t/t oinh 5ln rel!/Cwhere:rel = relative viscosity (viscosity ratio),t = efflux time of the solution,to = efflux time of the pure solvent,5 Filters may be obtained from Corning Glass, No. 36060 “Coarse” type.D1243 142C = weight of sample used (8.1) per 100 mL of solution,inh = inherent visc
27、osity (logarithmic viscosity number), andln rel = natural logarithm of relative viscosity (viscosity ratio).10. Report10.1 Report the average inherent viscosity of two analyses to the nearest 0.01.11. Precision and Bias611.1 An interlaboratory test program utilizing this test method was carried out
28、in 1973 involving seven laboratories, eachperforming pairs of determinations on one polymer.NOTE 5See Specification D1755, Table 3, for inherent viscosity value of ASTM PVC Reference Standard No. 1.11.2 PrecisionThe following values of precision have been calculated from the interlaboratory test pro
29、gram at a 95 %confidence level:Within-laboratory precision (within one pair of values) 1.4 % of meanBetween-laboratories precision (between averages ofpairs)2.2 % of meanWithin-laboratory precision (within one pair ofanalyses)1.4 % of meanBetween-laboratories precision (between averages ofanalyses)2
30、.2 % of mean11.3 BiasNo justifiable statement of bias can be made for this test method, since the true value of the property cannot beestablished by an accepted referee method.12. Keywords12.1 dilute solution viscosity; inherent viscosity; intrinsic viscosity; relative viscosity; specific viscosity;
31、 test method; vinylchloride polymersAPPENDIX(Nonmandatory Information)X1. OTHER EXPRESSIONS FOR VISCOSITYX1.1 DefinitionsX1.1.1 relative viscosityratio of the flow time of a specified solution of the polymer to the flow time of the pure solvent. TheInternational Union of Pure and Applied Chemistry (
32、IUPAC) term for relative viscosity is viscosity ratio. relative viscosityratioof the flow time of a specified solution of the polymer to the flow time of the pure solvent. The International Union of Pure andApplied Chemistry (IUPAC) term for relative viscosity is viscosity ratio.X1.1.2 specific visc
33、osityrelative viscosity minus one. Specific viscosity represents the increase in viscosity that may be attributedto the polymeric solute. specific viscosityrelative viscosity minus one. Specific viscosity represents the increase in viscosity thatmay be attributed to the polymeric solute.X1.1.3 reduc
34、ed viscosityratio of the specific viscosity to the concentration. Reduced viscosity is a measure of the specificcapacity of the polymer to increase the relative viscosity. The IUPAC term for reduced viscosity is viscosity number. reducedviscosityratio of the specific viscosity to the concentration.
35、Reduced viscosity is a measure of the specific capacity of the polymerto increase the relative viscosity. The IUPAC term for reduced viscosity is viscosity number.X1.1.4 inherent viscosityratio of the natural logarithm of the relative viscosity to the concentration. The IUPAC term forinherent viscos
36、ity is logarithmic viscosity number. inherent viscosityratio of the natural logarithm of the relative viscosity to theconcentration. The IUPAC term for inherent viscosity is logarithmic viscosity number.6 Supporting data are available from ASTM Headquarters. Request RR:D20-1112.D1243 143X1.1.5 intri
37、nsic viscosity limit of the reduced and inherent viscosities as the concentration of the polymeric solute approacheszero and represents the capacity of the polymer to increase viscosity. Interactions between solvent and polymer molecules have theaffect of yielding different intrinsic viscosities for
38、 the same polymer in various solvents. The IUPAC term for intrinsic viscosity islimiting viscosity number. intrinsic viscositylimit of the reduced and inherent viscosities as the concentration of the polymericsolute approaches zero and represents the capacity of the polymer to increase viscosity. In
39、teractions between solvent and polymermolecules have the affect of yielding different intrinsic viscosities for the same polymer in various solvents. The IUPAC term forintrinsic viscosity is limiting viscosity number.X1.2 Determination of Intrinsic Viscosity (Limiting Viscosity Number)X1.2.1 To dete
40、rmine the intrinsic viscosity (limiting viscosity number) of a polymer from dilute solution viscosity data, thereduced and inherent viscosities (viscosity and logarithmic viscosity number) of solutions of various concentrations of the polymerare determined at constant temperature and these values ar
41、e then plotted against the respective concentrations. The two lines thusobtained converge to a point of zero concentration of the solute which represents the intrinsic viscosity (limiting viscosity number)of the polymer in that solvent at the temperature of the determination. Fig. X1.1 illustrates t
42、his convergence.X1.2.2 At higher concentrations the viscosity curves may deviate from linearity; therefore, the greatest accuracy is obtained at lessthan 0.50.5 g g/mLdl (0.005 gmL) of solution. Since extrapolation of either reduced viscosity or inherent viscosity (viscosity orlogarithmic viscosity
43、number) curves to infinite dilution will give the same value for intrinsic viscosity (limiting viscosity number),a plot of either type of viscosity will permit the calculation of valid intrinsic viscosity (limiting viscosity number) data.X1.3 Estimation of Intrinsic Viscosity (Limiting Viscosity Num
44、ber)X1.3.1 The mathematical method of Billmeyer (1)7 permits a good approximation of intrinsic viscosity (limiting viscositynumber). This method makes use of equations derived from the power series expansion of viscosity versus concentration.Neglecting the higher order terms, equations may be writte
45、n which can be used to estimate intrinsic viscosity (limiting viscositynumber). The following equation has been found suitable for poly(vinyl chloride) resins:5 14 rel 21!/C#1FS34lnrelD/CGiv 5 14 rel 21!/C#134lnrel!/C#where C = concentration of polymer, g/100 mL.REFERENCES(1) Billmeyer, F. W., Jr.,
46、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. 2716.7 The boldface numbers in parentheses refer to the list of references at the end o
47、f this test method.FIG. X1.1 Example of Plot to Determine Intrinsic Viscosity.D1243 144(4) International Union of Pure and Applied Chemistry, Journal of Polymer Science, Vol 8, 1952, p. 269.(5) Streeter, D. J., and Boyer, R. F., Industrial and Engineering Chemistry, Vol 43, 1951, p. 1790.SUMMARY OF
48、CHANGESCommittee D20 has identified the location of selected changes to this standard since the last issue (D1243 - 95(2008) that may impact the use of this standard. (October 1, 2014)(1) Reworded ISO statement in accordance with D4968 - 09 in Note 2.(2) Removed year reference from ISO standard in N
49、ote 2.(3) Removed E77 reference in Section 2, removed Mercury reference.(4) Added E2251 reference in Section 2.(5) Added D446 reference in Section 2.(6) Removed year reference from ISO standard in 2.2.(7) Revised 6.3, changed Ubbelohde U-1 tube to Ubbelohde size 1.(8) Added new Note 5 referencing D446.(9) Revised 6.4.(10) Added 6.4.1.(11) In 6.7, replaced E77 reference with E2251.(12) Changed old Note 4 to Note 6.(13) Removed Note 5, ASTM PVC resin is no longer referenced in D1755.(14) Revised 8.1, 8.3, 8.4, and 8.5.(15) Ch
