ASTM D1243-95(2008)
(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 2008)
Standard Test Method for
Dilute Solution Viscosity of Vinyl Chloride Polymers
This standard is issued under the fixed designation D1243; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2.2 ISO Standard:
ISO 1628-2-1998 Determination of Viscosity Number and
1.1 This test method covers the determination of the dilute
LimitingViscosity Number—Part 2: Poly(Vinyl Chloride)
solution viscosity of vinyl chloride polymers in cyclo-
Resins
hexanone. The viscosity is expressed in terms of inherent
2.3 National Institute of Standards and Technology Circu-
viscosity (logarithmic viscosity number). The test method is
lar:
limited to those materials that give clear, uniform solutions at
C-434 Testing of Glass Volumetric Apparatus
the test dilution.
NOTE 1—Other expressions for viscosity may be used as described in 3. Terminology
the Appendix, but any change from the test method as specified shall be
3.1 Definitions: Definitions are in accordance with Termi-
stated in the report.
nology D883 and Terminology D1600, unless otherwise indi-
1.2 The values stated in SI units are to be regarded as the
cated.
standard.
4. Summary of Test Method
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4.1 Asampleofresinisdissolvedincyclohexanonetomake
responsibility of the user of this standard to establish appro-
a solution of specified concentration. Inherent viscosity (loga-
priate safety and health practices and determine the applica-
rithmicviscositynumber)iscalculatedfromthemeasuredflow
bility of regulatory limitations prior to use.
times of the solvent and of the polymer solution.
NOTE 2—Although this test method and ISO 1628-2-1998 differ in
NOTE 3—For additional information, refer to Test Method D445 and
approach or detail, data obtained by either are technically equivalent.
Test Method D2857 for Dilute Solution Viscosity of Polymers.
2. Referenced Documents 5. Significance and Use
5.1 Dilute solution viscosity values for vinyl chloride poly-
2.1 ASTM Standards:
mersarerelatedtotheaveragemolecularsizeofthatportionof
D445 Test Method for Kinematic Viscosity of Transparent
the polymer that dissolves in the solvent.
and Opaque Liquids (and Calculation of Dynamic Viscos-
ity)
6. Apparatus
D883 Terminology Relating to Plastics
D1600 TerminologyforAbbreviatedTermsRelatingtoPlas- 6.1 Transfer Pipets.
tics
6.2 Volumetric Flasks, 100-mL, glass-stoppered, in accor-
D1755 Specification for Poly(Vinyl Chloride) Resins
dance with National Institute of Standards and Technology
D2857 Practice for Dilute Solution Viscosity of Polymers
Circular C-434.
E77 Test Method for Inspection and Verification of Ther-
6.3 Viscometer, Ubbelohde Series U-1 or Cannon-
mometers
Ubbelohde No. 75.
6.4 Water Bath, at 306 0.5°C, controlled to within 6
0.01°C.
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materi-
6.5 Timer, as specified in Test Method D445, graduated in
als.15.07).
divisions of 0.1 s or less.
Current edition approved March 1, 2008. Published April 2008. Originally
ε1
approved in 1952. Last previous edition approved in 2000 as D1243 - 95(2000) .
DOI: 10.1520/D1243-95R08.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM 4th Floor, New York, NY 10036, http://www.ansi.org.
Standards volume information, refer to the standard’s Document Summary page on Available from National Institute of Standards and Technology (NIST), 100
the ASTM website. Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http://www.nist.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1243 − 95 (2008)
6.6 Filter Funnel, fritted-glass. η 5 t/t
rel o
6.7 Thermometer, standard, in accordance with Method η 5 ln /C
~ !
inh ηrel
E77.
where:
7. Materials
η = relative viscosity (viscosity ratio),
rel
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
156°C at 760 mm Hg has been found acceptable if stored in a
solution,
closed container.
η = inherent viscosity (logarithmic viscosity number),
inh
and
8. Procedure
ln η = natural logarithm of relative viscosity (viscosity
rel
8.1 Dissolve duplicates of resin as follows: Weigh 0.26
ratio).
0.002 g of the sample (moisture content below 0.1 %) and
transfer it to a 100-mL glass-stoppered volumetric flask. Take
10. Report
care to transfer all of the weighed resin into the flask. As an
alternative method, the resin (0.26 0.002 g) may be weighed
10.1 Report the average inherent viscosity of two analyses
directly into a tared, 100-mL glass-stoppered volumetric flask.
to the nearest 0.01.
8.2 Add 50 to 70 mL of cyclohexanone to the flask, taking
11. Precision and Bias
care to wet the resin so that lumps do not form.
8.3 Heat the flask at 85 6 10°C until the resin is dissolved.
11.1 An interlaboratory test program utilizing this test
Occasional shaking will reduce the time required for solution.
method was carried out in 1973 involving seven laboratories,
Heating should not exceed 12 h and should preferably be less
each performing pairs of determinations on one polymer.
to minimize degradation. If any gel-like particles can be seen,
NOTE 5—See Specification D1755,Table 3, for inherent viscosity value
prepare a new solution.
of ASTM PVC Reference Standard No. 1.
8.4 Cool the solution to the test temperature by immersing
11.2 Precision—The following values of precision have
flaskinthe30°Cbathforaminimumtimeof30minandadjust
beencalculatedfromtheinterlaboratorytestprogramata95 %
to a solution volume of 100 mL. Filter through a fritted-glass
confidence level:
filter directly into the viscometer.
Within-laboratory precision (within one pair of values) 1.4 % of mean
8.5 Measure at
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation:D 1243–95 (Reapproved 2000) Designation: D1243 – 95 (Reapproved
2008)
Standard Test Method for
Dilute Solution Viscosity of Vinyl Chloride Polymers
This standard is issued under the fixed designation D1243; 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 (´) indicates an editorial change since the last revision or reapproval. ´ NOTE—Reference to ISO 1628-2 was
corrected editorially in March 2000.
1. 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 1628-2-1998differ in approach or detail, data obtained by either are technically equivalent.
2. Referenced Documents
2.1 ASTM Standards:
D445 Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and the Calculation of Dynamic Viscosity)
D883 Terminology Relating to Plastics
D1600 Terminology for Abbreviated Terms Relating to Plastics
D1755 Specification for Poly(Vinyl Chloride) Resins
D2857 Test Method Practice for Dilute Solution Viscosity of Polymers
E77 Method for Verification and Calibration of Liquid-in-Glass Thermometers Test Method for Inspection and Verification of
Thermometers
2.2 ISO Standard:
ISO 1628-2-1998 Determination of Viscosity Number and Limiting Viscosity Number—Part 2: Poly(Vinyl Chloride) Resins
2.3 National Institute of Standards and Technology Circular:
C-434 Testing of Glass Volumetric Apparatus
3. Terminology
3.1 Definitions: Definitions are in accordance with Terminology D 883D 883 and Terminology D 1600D 1600Definitions are
in accordance with Terminology D883 and Terminology D1600, unless otherwise indicated.
4. Summary of Test Method
4.1 A sample of resin is dissolved in cyclohexanone to make a solution of specified concentration. Inherent viscosity
(logarithmic viscosity number) is calculated from the measured flow times of the solvent and of the polymer solution.
This test method is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materials
(Section D20.15.07).
on Thermoplastic Materials.15.07).
Current edition approved March 15, 1995. Published May 1995. Originally published as D 1243–52T. Last previous edition D 1243–79 (1990)
´1
Current edition approved March 1, 2008. Published April 2008. Originally approved in 1952. Last previous edition approved in 2000 as D1243 - 95(2000) .
This edition contains changes in Sections 1 and 2 to include an ISO equivalency statement. DOI: 10.1520/D1243-95R08.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vols 05.01 and 10.03.volume information, refer to the standard’s Document Summary page on the ASTM website.
Annual Book of ASTM Standards, Vol 08.01.
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
Annual Book of ASTM Standards, Vol 08.02.
Available from National Institute of Standards and Technology (NIST), 100 Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http://www.nist.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D1243 – 95 (2008)
NOTE 3—For additional information, refer to Test Method D 445D445 and Test Method D 2857D2857 for Dilute Solution Viscosity of Polymers.
5. Significance and Use
5.1 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.
6. Apparatus
6.1 Transfer Pipets.
6.2 Volumetric Flasks, 100-mL, glass-stoppered, in accordance with National Institute of Standards and Technology Circular
C-434.
6.3 Viscometer, Ubbelohde Series U-1 or Cannon-Ubbelohde No. 75.
6.4 Water Bath,at306 0.5°C, controlled to within 6 0.01°C.
6.5 Timer, as specified in Test Method D 445D445, graduated in divisions of 0.1 s or less.
6.6 Filter Funnel, fritted-glass.
6.7 Thermometer, standard, in accordance with Method E 77E77.
7. Materials
7.1 Solvent—Cyclohexanone, analytical reagent grade or laboratory-distilled technical grade, boiling between 155 and 156°C
at 760 mm Hg has been found acceptable if stored in a closed container.
8. Procedure
8.1 Dissolve duplicates of resin as follows: Weigh 0.26 0.002 g of the sample (moisture content below 0.1 %) and transfer it
toa100-mLglass-stopperedvolumetricflask.Takecaretotransferalloftheweighedresinintotheflask.Asanalternativemethod,
the resin (0.26 0.002 g) may be weighed 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 10°C until the resin is dissolved. Occasional shaking will reduce the time required for solution.
Heatingshouldnotexceed12handshouldpreferablybelesstominimizedegradation.Ifanygel-likeparticlescanbeseen,prepare
a new solution.
8.4 Cool the solution to the test temperature by immersing flask in the 30°C bath for a minimum time of 30 min and adjust to
a solution volume of 100 mL. Filter through a fritted-glass filter directly into the viscometer.
8.5 Measure at 30°C the flow time of the prepared solution (8.4) and of the pure solvent (aged at 85 6 10°C) in the viscometer.
Allow10minfortheviscometertocometotemperatureequilibriumafterplacingitinthewaterbath.Theflowtimeofthesolution
or the solvent should be within 0.1 % on repeat runs on the same filling.
NOTE 4—Keep the Ubbelohde viscometer clean when not in use. Acetone may be used as a cleaning flush. The viscometer may be stored filled with
pure solvent or it may be stored dry.
9. Calculation
9.1 Calculate the relative and inherent viscosity (viscosity ratio and lo
...
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