ASTM D1243-95(2000)e1
(Test Method)Standard Test Method for Dilute Solution Viscosity of Vinyl Chloride Polymers
Standard Test Method for Dilute Solution Viscosity of Vinyl Chloride Polymers
SIGNIFICANCE AND USE
Dilute solution viscosity values for vinyl chloride polymers are related to the average molecular size of that portion of the polymer that dissolves in the solvent.
SCOPE
1.1 This test method covers the determination of the dilute solution viscosity of vinyl chloride polymers in cyclohexanone. The viscosity is expressed in terms of inherent viscosity (logarithmic viscosity number). The test method is limited to those materials that give clear, uniform solutions at the test dilution.
Note 1--Other expressions for viscosity may be used as described in the Appendix, but any change from the test method as specified shall be stated in 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 responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
Note 2--Although this test method and ISO 1628-2-1998 differ in approach or detail, data obtained by either are technically equivalent.
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Designation:D1243–95 (Reapproved 2000)
Standard Test Method for
Dilute Solution Viscosity of Vinyl Chloride Polymers
This standard is issued under the fixed designation D 1243; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Reference to ISO 1628-2 was corrected editorially in March 2000.
1. Scope E 77 Method for Verification and Calibration of Liquid-in-
Glass Thermometers
1.1 This test method covers the determination of the dilute
2.2 ISO Standard:
solution viscosity of vinyl chloride polymers in cyclohex-
ISO 1628-2-1998 Determination of Viscosity Number and
anone.The viscosity is expressed in terms of inherent viscosity
LimitingViscosity Number—Part 2: Poly(Vinyl Chloride)
(logarithmic viscosity number). The test method is limited to
Resins
those materials that give clear, uniform solutions at the test
2.3 National Institute of Standards and Technology Circu-
dilution.
lar:
NOTE 1—Other expressions for viscosity may be used as described in
C-434 Testing of Glass Volumetric Apparatus
the Appendix, but any change from the test method as specified shall be
stated in the report.
3. Terminology
1.2 The values stated in SI units are to be regarded as the
3.1 Definitions: Definitions are in accordance with Termi-
standard.
nology D 883 and Terminology D 1600, unless otherwise
1.3 This standard does not purport to address all of the
indicated.
safety concerns, if any, associated with its use. It is the
4. Summary of Test Method
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4.1 Asampleofresinisdissolvedincyclohexanonetomake
bility of regulatory limitations prior to use.
a solution of specified concentration. Inherent viscosity (loga-
rithmicviscositynumber)iscalculatedfromthemeasuredflow
NOTE 2—Although this test method and ISO 1628-2-1998 differ in
times of the solvent and of the polymer solution.
approach or detail, data obtained by either are technically equivalent.
NOTE 3—For additional information, refer to Test Method D 445 and
2. Referenced Documents
Test Method D 2857 for Dilute Solution Viscosity of Polymers.
2.1 ASTM Standards:
5. Significance and Use
D 445 Test Method for Kinematic Viscosity of Transparent
and Opaque Liquids (and the Calculation of Dynamic
5.1 Dilute solution viscosity values for vinyl chloride poly-
Viscosity)
mersarerelatedtotheaveragemolecularsizeofthatportionof
D 883 Terminology Relating to Plastics
the polymer that dissolves in the solvent.
D 1600 Terminology for Abbreviated Terms Relating to
6. Apparatus
Plastics
D 1755 Specification for Poly(Vinyl Chloride) Resins
6.1 Transfer Pipets.
D 2857 Test Method for Dilute Solution Viscosity of Poly-
6.2 Volumetric Flasks, 100-mL, glass-stoppered, in accor-
mers
dance with National Institute of Standards and Technology
Circular C-434.
6.3 Viscometer, Ubbelohde Series U-1 or Cannon-
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
Ubbelohde No. 75.
and is the direct responsibility of Subcommittee D20.15 onThermoplastic Materials
(Section D20.15.07).
Current edition approved March 15, 1995. Published May 1995. Originally
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published as D 1243 – 52 T. Last previous edition D 1243 –79 (1990) .
This edition contains changes in Sections 1 and 2 to include an ISO equivalency Annual Book of ASTM Standards, Vol 14.03.
statement. Available from American National Standards Institute, 11 W. 42nd St., 13th
Annual Book of ASTM Standards, Vols 05.01 and 10.03. Floor, New York, NY 10036.
3 7
Annual Book of ASTM Standards, Vol 08.01. Available from National Institute of Standards and Technology, U. S. Dept. of
Annual Book of ASTM Standards, Vol 08.02. Commerce, Washington, DC 20234.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D1243
6.4 Water Bath,at306 0.5°C, controlled to within 6 9. Calculation
0.01°C.
9.1 Calculate the relative and inherent viscosity (viscosity
6.5 Timer, as specified in Test Method D 445, graduated in
ratio and logarithmic viscosity number) as follows:
divisions of 0.1 s or less.
h 5 t/t
8 rel o
6.6 Filter Funnel, fritted-glass.
h 5 ~ln !/C
inh hrel
6.7 Thermometer, standard, in accordance with Method
E 77.
where:
h = relative viscosity (viscosity ratio),
rel
7. Materials
t = efflux time of the solution,
7.1 Solvent—Cyclohexanone, analytical reagent grade or t = efflux time of the pure solvent,
o
laboratory-distilled technical grade, boiling between 155 and C = weight of sample used (8.1) per 100 mL of
solution,
156°C at 760 mm Hg has been found acceptable if stored in a
h = inherent viscosity (logarithmic viscosity num-
closed container.
inh
ber), and
ln h = natural logarithm of relative viscosity (viscosity
8. Procedure
rel
ratio).
8.1 Dissolve duplicates of resin as follows: Weigh 0.26
0.002 g of the sample (moisture content below 0.1 %) and
10. Report
transfer it to a 100-mL glass-stoppered volumetric flask. Take
10.1 Report the average inherent viscosity of two analyses
care to transfer all of the weighed resin into the flask. As an
to the nearest 0.01.
alternative method, the resin (0.26 0.002 g) may be weighed
directly into a tared, 100-mL glass-stoppered volumetric flask. 9
11. Precision and Bias
8.2 Add 50 to 70 mL of cyclohexanone to the flask, taking
11.1 An interlaboratory test program utilizing this test
care to wet the resin so that lumps do not form.
method was carried out in 1973 involving seven laboratories,
8.3 Heat the flask at 85 6 10°C until the resin is dissolved.
each performing pairs of determinations on one polymer.
Occasional shaking will reduce the time required for solution.
Heating should not exceed 12 h and should preferably be less
NOTE 5—See Specification D 1755, Table 3, for inherent viscosity
value of ASTM PVC Reference Standard No. 1.
to minimize degradation. If any gel-like particles can be seen,
prepare a new solution.
11.2 Precision—The following values of precision have
8.4 Cool the solution to the test temperature by immersing
beencalculatedfromtheinterlaboratorytestpr
...
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