ASTM D4603-96
(Test Method)Standard Test Method for Determining Inherent Viscosity of Poly(Ethylene Terephthalate) (PET) by Glass Capillary Viscometer
Standard Test Method for Determining Inherent Viscosity of Poly(Ethylene Terephthalate) (PET) by Glass Capillary Viscometer
SCOPE
1.1 This test method is for the determination of the inherent viscosity of poly(ethylene terephthalate) (PET) soluble at 0.50% concentration in a 60/40 phenol/1,1,2,2-tetrachloroethane solution by means of a glass capillary viscometer. Some highly crystalline forms of PET may not be soluble in this solvent mixture and will require a different procedure.
1.2 The inherent viscosity values obtained by this test method are comparable with those obtained using differential viscometry described in Test Method D 5225.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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. Specific hazards statements are given in Section 8.
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
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Designation: D 4603 – 96
Standard Test Method for
Determining Inherent Viscosity of Poly(Ethylene
Terephthalate) (PET) by Glass Capillary Viscometer
This standard is issued under the fixed designation D 4603; 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.
1. Scope E 1 Specification for ASTM Thermometers
E 380 Practice for Use of the International System of Units
1.1 This test method is for the determination of the inherent
(SI)
viscosity of poly(ethylene terephthalate) (PET) soluble at
E 691 Practice for Conducting an Interlaboratory Study to
0.50 % concentration in a 60/40 phenol/1,1,2,2-
Determine the Precision of a Test Method
tetrachloroethane solution by means of a glass capillary vis-
2.2 ISO Standard:
cometer. Some highly crystalline forms of PET may not be
1628/5-1986 Determination of Viscosity Number and Lim-
soluble in this solvent mixture and will require a different
iting Number—Part 5
procedure.
2.3 NIST Standard:
1.2 The inherent viscosity values obtained by this test
C 602 Testing of Glass Volumetric Apparatus
method are comparable with those obtained using differential
viscometry described in Test Method D 5225.
3. Terminology
1.3 The values stated in SI units are to be regarded as the
3.1 Units, symbols, and abbreviations used in this test
standard. The values given in parentheses are for information
method are those recommended in Practice E 380.
only.
3.2 Definitions of Terms Specific to This Standard:
1.4 This standard does not purport to address all of the
3.2.1 inherent viscosity (also known as the logarithmic
safety concerns, if any, associated with its use. It is the
viscosity number)—defined by the equation given in 11.1.
responsibility of the user of this standard to establish appro-
3.2.2 PET—as outlined in Practice D 1972. The PET acro-
priate safety and health practices and determine the applica-
nym may be used to avoid trademark infringement and to
bility of regulatory limitations prior to use. Specific hazards
comply with various state or federal laws.
statements are given in Section 8.
4. Summary of Test Method
2. Referenced Documents
4.1 The inherent viscosity is determined by measuring the
2.1 ASTM Standards:
flow time of a solution of known polymer concentration and
D 445 Test Method for Kinematic Viscosity of Transparent
the flow time of the pure solvent in a capillary viscometer at a
and Opaque Liquids (and the Calculation of Dynamic
fixed temperature. The inherent viscosity value is calculated
Viscosity)
from the flow time values.
D 446 Specification for Operating Instructions for Glass
Capillary Kinematic Viscometers
5. Significance and Use
D 1972 Practice for Generic Marking of Plastic Products
5.1 The inherent viscosity is relatable to the composition
D 4019 Test Method for Moisture in Plastics by Coulom-
and molecular weight of a polyester resin. It must be controlled
etry
so that the processability and end properties of the resin remain
D 5225 Test Method for Measuring Solution Viscosity of
in a desired range.
Polymers with a Differential Viscometer
6. Apparatus
6.1 Cannon Ubbelohde Type 1B Viscometer, as described in
This test method is under the jurisdiction of ASTM Committee D-20 on Plastics
Specifications and Operating Instructions D 446.
and is the direct responsibility of Subcommittee D20.70.05 on Analytical Methods.
Current edition approved Nov. 10, 1996. Published May 1997. Originally
published as D 4603 – 86. Last previous edition D 4603 – 91.
This edition includes a title change and revised precision and bias statement. Annual Book of ASTM Standards, Vol 14.03.
2 7
Annual Book of ASTM Standards, Vol 05.01. Annual Book of ASTM Standards, Vol 14.02.
3 8
Annual Book of ASTM Standards, Vol 08.01. Available from American National Standards Institute, 11 W. 42nd St., 13th
Annual Book of ASTM Standards, Vol 08.02. Floor, New York, NY 10036.
5 9
Annual Book of ASTM Standards, Vol 08.03. Available from the National Institute of Standards and Technology, U.S.
Department of Commerce, Washington, DC 20234.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 4603
6.2 Viscometer Holder. testing equipment should also be obtained from their suppliers
6.3 Electric Timer, readable to 0.1 s, as described in Test and consulted before use.
Method D 445.
9. Conditioning
6.4 Constant Temperature Bath, control label at 30°C
(86°F) 6 0.01°C (0.02°F).
9.1 If the sample of PET contains 0.5 % or more of inert
6.5 Kinematic Viscosity Thermometer ASTM 118 (for use at
material such as titanium dioxide or glass fiber, determine the
30°C), conforming to Specification E 1.
amount of inert material accurately by a procedure suitable for
6.6 Temperature Controllable Magnetic Stirring Hot Plate.
the type of inert material present.
6.7 TFE-Fluorocarbon Plastic-Coated Stirring Bars and a
9.2 If the sample is suspected of being wet (in excess of the
Magnetic Bar Retriever.
moisture level derived from exposure to ambient humidity
6.8 Volumetric Flasks and Stoppers, 50-mL capacity, con-
conditions), dry the sample in an oven for a suggested
forming to the standards of accuracy in NIST Circular No.
minimum of2hat 65°C (149°F)6 5°C (9°F) or until a
C 602.
constant weight of 6 0.1 % is reached. Moisture picked up
6.9 Analytical Balance, with readout to 0.0001 g.
from ambient humidity will weigh 0.30 % and can be neglected
6.10 Borosilicate Funnels.
in this procedure. (See Note 1.)
6.11 Stainless Steel Filter Screening, 325-mesh or finer.
NOTE 1—Test Method D 4019 or another suitable technical method
6.12 Aspirator.
may be used to determine moisture content.
6.13 Wiley Mill Grinder, with 20-mesh stainless steel
9.3 If the sample is difficult to dissolve, it may be desirable
screen.
to grind it to a 20-mesh screen size in a Wiley Mill. Care must
6.14 Drying Oven, for equipment.
be taken not to overheat the sample during the grinding
7. Reagents and Materials
operation. A low temperature can be maintained by grinding in
the presence of dry ice or liquid nitrogen. Grind a 15 to 20- g
7.1 Purity of Reagents—Reagent grade chemicals shall be
sample, representative of the entire lot being tested. Drying
used in all tests. Unless otherwise indicated, it is intended that
may be necessary after the dry ice grinding step.
all reagents shall conform to the specifications of the Commit-
tee on Analytical Reagents of the American Chemical Society
10. Procedure
where such specifications are available. Other grades may be
used, providing it is first ascertained that the reagent is of 10.1 Accurately weigh between 0.2475 and 0.2525 g (accu-
sufficiently high purity to permit its use without lessening the rate to 60.0002 g) of sample into a clean, dry 50-mL
accuracy of the determination. volumetric flask. If the sample contains more than 0.5 % inert
7.2 Phenol/1,1,2,2-tetrachloroethane Solution, (PET), material, weigh the amount of sample necessary to give the
60/40 weight % mixture (0.5 % moisture maximum, protected specified amount of PET.
in such a manner as to maintain this maximum level). The PET 10.2 Place a TFE-fluorocarbon plastic-coated stirring bar
should be protected against the degradation which can occur into the flask and add approximately 25 mL of solvent. Prepare
during the heating stage in 10.3 through the addition of a one flask without any sample present. Cap the flasks.
hydrogen chloride scavenger to the solvent, such as 0.2 weight 10.3 Place the flasks in steel beakers and place on a
% n-octyl-bis-(isoethyl mercaptoacetate). magnetic hot plate which has been preheated to 110°C (230°F)
7.3 Reagent Grade Methylene Chloride and Acetone, rins- 6 10°C (18°F). Heat the flasks for 15 min while stirring.
ing solvents. Remove flasks and inspect for undissolved PET. If a sample
7.4 Chromic Acid, cleaning solution. does not dissolve completely, extend the stirring time for up to
30 more min while inspecting the sample at 10-min intervals.
8. Hazards
If the sample fails to dissolve completely at this time, this
8.1 The solvent used in this procedure is a mixture of 60
procedure is not applicable.
weight % phenol and 40 weight % 1,1,2,2-tetrachloroethane.
10.4 When the samples have completely dissolved, remove
Both compounds and the mixture are toxic and require care in
the flasks from the hot plate and allow them to cool to
handling. Reference should be made to the material safety data
approximately room temperature. Remove the stirring bars
sheets available from the suppliers of these compounds for
with a magnetic
...
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