Dilute Solution Viscosity of Vinyl Chloride Polymers: Standard Test Method For
Dilute Solution Viscosity of Vinyl Chloride Polymers: Standard Test Method For
Dilute Solution Viscosity of Vinyl Chloride Polymers: Standard Test Method For
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6.4.1 The temperature of the bath medium shall not vary by enable subsequent drying. The viscometer may be stored filled with pure
more than 60.02°C of the selected temperature in accordance solvent or it may be stored dry.
with Test Method D445. 9. Calculation
6.5 Timer, as specified in Test Method D445, graduated in 9.1 Calculate the relative and inherent viscosity (viscosity
divisions of 0.1 s or less. ratio and logarithmic viscosity number) as follows:
6.6 Filter Funnel, funnel, Hirsh-Type; borosilicate glass; η rel 5 t/t o
w/coarse fritted disc, pore size: 40–60 µm.
η inh 5 ~ ln ηrel! /C
6.7 Thermometer, standard, in accordance with Method
E2251. where:
ηrel = relative viscosity (viscosity ratio),
7. Materials t = efflux time of the solution,
7.1 Solvent—Cyclohexanone, analytical reagent grade or to = efflux time of the pure solvent,
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 ηinh = inherent viscosity (logarithmic viscosity number),
closed container. and
ln ηrel = natural logarithm of relative viscosity (viscosity
8. Procedure ratio).
8.1 Dissolve duplicates of resin as follows: Weigh 0.2 6 10. Report
0.002 g of the sample (moisture content below 0.1 %) and
10.1 Report the average inherent viscosity of two analyses
transfer it to a 100-mL glass-stoppered volumetric flask. Take
to the nearest 0.01.
care to transfer all of the weighed resin into the flask. As an
alternative method, weigh the resin (0.2 6 0.002 g) directly 11. Precision and Bias5
into a tared, 100-mL glass-stoppered volumetric flask.
11.1 An interlaboratory test program utilizing this test
8.2 Add 50 to 70 mL of cyclohexanone to the flask, taking method was carried out in 1973 involving seven laboratories,
care to wet the resin so that lumps do not form. each performing pairs of determinations on one polymer.
8.3 Heat the flask at 85 6 10°C until the resin is dissolved. 11.2 Precision—The following values of precision have
Occasional shaking will reduce the time required for solution. been calculated from the interlaboratory test program at a 95 %
Take care that heating time does not exceed 12 h, preferably confidence level:
less, to minimize degradation. If any gel-like particles can be Within-laboratory precision (within one pair of 1.4 % of mean
seen, prepare a new solution. analyses)
Between-laboratories precision (between averages of 2.2 % of mean
8.4 Cool the solution to the test temperature by immersing analyses)
flask in the 30°C bath for a minimum time of 30 min and adjust
11.3 Bias—No justifiable statement of bias can be made for
to a solution volume of 100 mL. Filter through a fritted-glass
this test method, since the true value of the property cannot be
filter, as described in 6.6, directly into the viscometer.
established by an accepted referee method.
8.5 Measure at 30.0 6 0.5°C the flow time of the prepared
solution (8.4) and of the pure solvent (aged at 85 6 10°C) in 12. Keywords
the viscometer. Allow 10 min for the viscometer to come to 12.1 dilute solution viscosity; inherent viscosity; intrinsic
temperature equilibrium after placing it in the water bath. If the viscosity; relative viscosity; specific viscosity; test method;
flow time of the solution or the solvent differs by more than vinyl chloride polymers
0.1 % on repeat runs on the same filling, the result is suspect.
NOTE 5—Keep the Ubbelohde viscometer clean when not in use. 5
Supporting data are available from ASTM Headquarters. Request RR:D20-
Acetone may be used to flush the pure solvent (Cyclohexanone) and 1112.
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APPENDIX
(Nonmandatory Information)
X1.1 Definitions
X1.1.1 relative viscosity—ratio of the flow time of a speci-
fied solution of the polymer to the flow time of the pure
solvent. The International Union of Pure and Applied Chem-
istry (IUPAC) term for relative viscosity is viscosity ratio.
X1.1.2 specific viscosity—relative viscosity minus one.
Specific viscosity represents the increase in viscosity that may
be attributed to the polymeric solute.
X1.1.3 reduced viscosity—ratio of the specific viscosity to FIG. X1.1 Example of Plot to Determine Intrinsic Viscosity.
the concentration. Reduced viscosity is a measure of the
specific capacity of the polymer to increase the relative
viscosity. The IUPAC term for reduced viscosity is viscosity X1.2.2 At higher concentrations the viscosity curves may
number. deviate from linearity; therefore, the greatest accuracy is
obtained at less than 0.5 g ⁄dl (0.005 g ⁄mL) of solution. Since
X1.1.4 inherent viscosity—ratio of the natural logarithm of extrapolation of either reduced viscosity or inherent viscosity
the relative viscosity to the concentration. The IUPAC term for (viscosity or logarithmic viscosity number) curves to infinite
inherent viscosity is logarithmic viscosity number. dilution will give the same value for intrinsic viscosity (limit-
X1.1.5 intrinsic viscosity—limit of the reduced and inherent ing viscosity number), a plot of either type of viscosity will
viscosities as the concentration of the polymeric solute ap- permit the calculation of valid intrinsic viscosity (limiting
proaches zero and represents the capacity of the polymer to viscosity number) data.
increase viscosity. Interactions between solvent and polymer
molecules have the affect of yielding different intrinsic viscosi- X1.3 Estimation of Intrinsic Viscosity (Limiting Viscosity
ties for the same polymer in various solvents. The IUPAC term Number)
for intrinsic viscosity is limiting viscosity number. X1.3.1 The mathematical method of Billmeyer (1)6 permits
a good approximation of intrinsic viscosity (limiting viscosity
X1.2 Determination of Intrinsic Viscosity (Limiting Vis- number). This method makes use of equations derived from the
cosity Number) power series expansion of viscosity versus concentration.
X1.2.1 To determine the intrinsic viscosity (limiting viscos- Neglecting the higher order terms, equations may be written
ity number) of a polymer from dilute solution viscosity data, which can be used to estimate intrinsic viscosity (limiting
the reduced and inherent viscosities (viscosity and logarithmic viscosity number). The following equation has been found
viscosity number) of solutions of various concentrations of the suitable for poly(vinyl chloride) resins:
polymer are determined at constant temperature and these 1 3
values are then plotted against the respective concentrations. η iv 5
4
@ ~ η rel 2 1 ! /C # 1 4 @ ln~ η rel!/C #
The two lines thus obtained converge to a point of zero
concentration of the solute which represents the intrinsic where C = concentration of polymer, g/100 mL.
viscosity (limiting viscosity number) of the polymer in that
solvent at the temperature of the determination. Fig. X1.1 6
The boldface numbers in parentheses refer to the list of references at the end of
illustrates this convergence. this test method.
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REFERENCES
(1) Billmeyer, F. W., Jr., Journal of Polymer Science, Vol 4, 1949, p. 83. (4) International Union of Pure and Applied Chemistry, Journal of
(2) Cragg, L. H., and Fern, C. R. H., Journal of Polymer Science, Vol 10, Polymer Science, Vol 8, 1952, p. 269.
1953, p. 185. (5) Streeter, D. J., and Boyer, R. F., Industrial and Engineering
(3) Huggins, M. L., Journal of the American Chemical Society, Vol 64, Chemistry, Vol 43, 1951, p. 1790.
1942, p. 2716.
SUMMARY OF CHANGES
Committee D20 has identified the location of selected changes to this standard since the last issue (D1243 - 14)
that may impact the use of this standard. (October 1, 2015)
(1) Reworded 6.6, added pore size of 40 – 60µm. (3) Reworded 8.4, added reference to 6.6.
(2) Removed old Footnote 5.
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