1、Designation: D1243 14D1243 15Standard 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, the year of last r
2、evision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method covers the determination of the dilute solution viscosity of vinyl chloride polymers in cyclohexanone. The
3、viscosity 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 change from the test meth
4、od 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 establish appropriate s
5、afety and health practices and determine the applicability of regulatorylimitations prior to use.NOTE 2This standard and ISO 1628-2 address the same subject matter, but differ in technical content.2. Referenced Documents2.1 ASTM Standards:2D445 Test Method for Kinematic Viscosity of Transparent and
6、Opaque Liquids (and Calculation of Dynamic Viscosity)D446 Specifications and Operating Instructions for Glass Capillary Kinematic ViscometersD883 Terminology Relating to PlasticsD1600 Terminology for Abbreviated Terms Relating to PlasticsD1755 Specification for Poly(Vinyl Chloride) ResinsD2857 Pract
7、ice for Dilute Solution Viscosity of PolymersE2251 Specification for Liquid-in-Glass ASTM Thermometers with Low-Hazard Precision Liquids2.2 ISO Standard:ISO 1628-2 Determination of Viscosity Number and Limiting Viscosity NumberPart 2: Poly(Vinyl Chloride) Resins32.3 National Institute of Standards a
8、nd Technology Circular:4C-434 Testing of Glass Volumetric Apparatus3. Terminology3.1 DefinitionsDefinitions are in accordance with Terminology D883 and Terminology D1600, unless otherwise indicated.4. Summary of Test Method4.1 A sample of resin is dissolved in cyclohexanone to make a solution of spe
9、cified concentration. Inherent viscosity(logarithmic viscosity number) is calculated from the measured flow times of the solvent and of the polymer solution.NOTE 3For additional information, refer to Test Method D445 and Test Method D2857 for Dilute Solution Viscosity of Polymers.1 This test method
10、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 Oct. 1, 2014Oct. 1, 2015. Published October 2014October 2015. Originally approved in 1952. Last previous edition approved in 2
11、0082014 asD1243 - 95 (2008).D1243 - 14. DOI: 10.1520/D1243-14.10.1520/D1243-15.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on
12、 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 Standards and Technology (NIST), 100 Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http:/www.nist.gov.This d
13、ocument 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 technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions
14、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 standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. Uni
15、ted States15. Significance and Use5.1 Dilute solution viscosity values 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
16、National Institute of Standards and Technology CircularC-434.6.3 Viscometer, ASTM Ubbelohde Size 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 4Operating instructions c
17、an be found in Specification D446.6.4 Water Bath, set at 30.0 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 divi
18、sions of 0.1 s or less.6.6 Filter Funnel, fritted-glass.funnel, Hirsh-Type; borosilicate glass; w/coarse fritted disc, pore size: 4060 m.6.7 Thermometer, standard, in accordance with Method E2251.7. Materials7.1 SolventCyclohexanone, analytical reagent grade or laboratory-distilled technical grade,
19、boiling between 155 and 156Cat 760 mm Hg has been found acceptable if stored in a closed container.8. Procedure8.1 Dissolve duplicates of resin as follows: Weigh 0.2 6 0.002 g of the sample (moisture content below 0.1 %) and transfer itto a 100-mLglass-stoppered volumetric flask. Take care to transf
20、er all of the weighed resin into the flask.As an alternative method,weigh the resin (0.2 6 0.002 g) directly into a tared, 100-mL glass-stoppered volumetric 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
21、until the resin is dissolved. Occasional shaking will reduce the time required for solution. Takecare that heating time does not exceed 12 h, preferably less, to minimize degradation. If any gel-like particles can be seen, preparea new solution.8.4 Cool the solution to the test temperature by immers
22、ing flask in the 30C bath for a minimum time of 30 min and adjust toa solution volume of 100 mL. Filter through a fritted-glass filter filter, as described in 6.6, directly into the viscometer.8.5 Measure at 30.0 6 0.5C the flow time of the prepared solution (8.4) and of the pure solvent (aged at 85
23、 6 10C) in theviscometer.Allow 10 min for the viscometer to come to temperature equilibrium after placing it in the water bath. If the flow timeof the solution or the solvent differs by more than 0.1 % on repeat runs on the same filling, the result is suspect.NOTE 5Keep the Ubbelohde viscometer clea
24、n when not in use.Acetone may be used to flush the pure solvent (Cyclohexanone) and enable subsequentdrying. 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
25、) as follows: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,C = weight of sample used (8.1) per 100 mL of solution,inh = inherent viscosity (logarithmic viscosity number), andln rel = natural logarithm of
26、relative viscosity (viscosity ratio).10. Report10.1 Report the average inherent viscosity of two analyses to the nearest 0.01.D1243 15211. Precision and Bias511.1 An interlaboratory test program utilizing this test method was carried out in 1973 involving seven laboratories, eachperforming pairs of
27、determinations on one polymer.11.2 PrecisionThe following values of precision have been calculated from the interlaboratory test program at a 95 %confidence level:Within-laboratory precision (within one pair ofanalyses)1.4 % of meanBetween-laboratories precision (between averages ofanalyses)2.2 % of
28、 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; test m
29、ethod; 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 (IUPAC)
30、term for relative viscosity is viscosity ratio.X1.1.2 specific viscosityrelative viscosity minus one. Specific viscosity represents the increase in viscosity that may beattributed to the polymeric solute.X1.1.3 reduced viscosityratio of the specific viscosity to the concentration. Reduced viscosity
31、is a measure of the specificcapacity of the polymer to 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 viscosity is logarithmic
32、 viscosity number.X1.1.5 intrinsic viscositylimit 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 havethe affect of yielding differ
33、ent intrinsic viscosities for the same polymer in various solvents. The IUPAC term for intrinsic viscosityis limiting viscosity number.X1.2 Determination of Intrinsic Viscosity (Limiting Viscosity Number)X1.2.1 To determine the intrinsic viscosity (limiting viscosity number) of a polymer from dilute
34、 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 are then plotted against the respective concentrations. The two lines thusobtained c
35、onverge 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 this convergence.X1.2.2 At higher concentrations the viscosity curves may deviate f
36、rom linearity; therefore, the greatest accuracy is obtained at lessthan 0.5 gdl (0.005 gmL) of solution. Since extrapolation of either reduced viscosity or inherent viscosity (viscosity or5 Supporting data are available from ASTM Headquarters. Request RR:D20-1112.D1243 153logarithmic viscosity numbe
37、r) 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 Number)X
38、1.3.1 The mathematical method of Billmeyer (1)6 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 written whi
39、ch can be used to estimate intrinsic viscosity (limiting viscositynumber). The following equation has been found suitable for poly(vinyl chloride) resins:iv 5 14 rel 21!/C#134lnrel!/C#where C = concentration of polymer, g/100 mL.REFERENCES(1) Billmeyer, F. W., Jr., Journal of Polymer Science, Vol 4,
40、 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 of Polymer Science, Vol 8, 1952, p. 269.(5) Streeter,
41、 D. J., and Boyer, R. F., Industrial and Engineering Chemistry, Vol 43, 1951, p. 1790.SUMMARY OF CHANGESCommittee D20 has identified the location of selected changes to this standard since the last issue (D1243 - 95(2008)D1243 - 14) that may impact the use of this standard. (October 1, 2014)2015)(1)
42、 Reworded 6.6ISO statement in accordance with, added pore size of D4968 - 09 in40 Note 2.60m.(2) Removed year reference from ISO standard in old Footnote 5.Note 2.(3) Removed E77 reference in Section 2, removed Mercury reference.(4) Added E2251 reference in Section 2.(5) Added D446 reference in Sect
43、ion 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 6.6 The boldface numbers in
44、parentheses refer to the list of references at the end of this test method.FIG. X1.1 Example of Plot to Determine Intrinsic Viscosity.D1243 154(13) Removed Note 5, ASTM PVC resin is no longer referenced in D1755.(3) RevisedReworded 8.1, 8.3, 8.4, and added reference to 8.56.6.(15) Changed 11.2 wordi
45、ng from values and pairs to analysis.(16) Replaced Intrinsic Viscosity equation in X1.3.1(17) Updated Summary of Changes.ASTM 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 expres
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48、end. 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.
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