ASTM D3591-97

Standard Test Method for Determining Logarithmic Viscosity Number of Poly(Vinyl Chloride) (PVC) in Formulated Compounds

SCOPE
1.1 This test method covers the determination of the logarithmic viscosity number of poly(vinyl chloride) (PVC) homopolymers after compounding or processing.  
1.2 It is the basic assumption of this technique that the formulation of the compounded resin is known and that any additives present can be separated from the resin by extraction with diethyl ether. This is necessary to permit adjustment of the amount of sample used in the test to give a resin concentration in cyclohexanone of 0.2 + 0.002 g/100 mL.  
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 precautionary statements are given in 6.3 and 7.4.1.
Note 1- This test method and ISO 1628-2 are not equivalent.

General Information

• Status: Historical
• Publication Date: 09-Jan-1997
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.70 - Analytical Methods

Relations

• Replaced By: ASTM D3591-97(2003) - Standard Test Method for Determining Logarithmic Viscosity Number of Poly(Vinyl Chloride) (PVC) in Formulated Compounds
• Effective Date: 10-Mar-2003
• Referred By: ASTM D2857-22 - Standard Practice for Dilute Solution Viscosity of Polymers
• Effective Date: 10-Jan-1997

Standards Content (Sample)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.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.
Designation: D 3591 – 97
Standard Test Method for
Determining Logarithmic Viscosity Number of Poly(Vinyl
Chloride) (PVC) in Formulated Compounds
This standard is issued under the fixed designation D 3591; 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 * Determine the Precision of a Test Method
2.2 ISO Standard:
1.1 This test method covers the determination of the loga-
1628-2 Plastics—Determination of Viscosity Number and
rithmic viscosity number of poly(vinyl chloride) (PVC) ho-
Limiting Viscosity Number—Part 2: Poly (Vinyl Chlo-
mopolymers after compounding or processing.
ride) Resins
1.2 It is the basic assumption of this technique that the
formulation of the compounded resin is known and that any
3. Terminology
additives present can be separated from the resin by extraction
3.1 Units and symbols used in this test method are those
with diethyl ether. This is necessary to permit adjustment of the
recommended in Practice E 380.
amount of sample used in the test to give a resin concentration
3.2 Definitions of Terms Specific to This Standard:
in cyclohexanone of 0.2 6 0.002 g/100 mL.
3.2.1 The term logarithmic viscosity number is defined by
1.3 This standard does not purport to address all of the
the equation is 9.1.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
4.1 The sample is pressed into a thin film and extracted to
bility of regulatory limitations prior to use. Specific precau-
remove the plasticizer.
tionary statements are given in 6.3 and 7.4.1.
4.2 The plasticizer-free film is dissolved in cyclohexanone
NOTE 1—This test method and ISO 1628-2 are not equivalent.
and centrifuged to remove insoluble matter.
4.3 The viscosity of the cyclohexanone solution is measured
2. Referenced Documents
in accordance with Test Method D 1243.
2.1 ASTM Standards:
D 445 Test Method for Kinematic Viscosity of Transparent 5. Significance and Use
and Opaque Liquids (the Calculation of Dynamic Viscos-
5.1 The logarithmic viscosity number provides information
ity)
on the effect of compounding or processing of PVC.
D 446 Specification and Operating Instructions for Glass
5.2 Exposure of PVC compositions to shear or to high
Capillary Kinematic Viscometers
temperatures can result in a change in the logarithmic viscosity
D 1243 Test Method for Dilute Solution Viscosity of Vinyl
number of the resin.
Chloride Polymers
D 2124 Method for Analysis of Components in Poly(Vinyl 6. Apparatus
Chloride) Compounds Using an Infrared Spectrophoto-
6.1 Centrifuge, capable of 2500 rpm with 100-mL sample
metric Technique
container.
E 1 Specification for ASTM Thermometers
6.2 Heated Hydraulic Press, capable of 620-kN ram force
E 380 Practice for the Use of International System of Units
and a temperature of 165°C.
(SI)
6.3 Soxhlet Extraction Apparatus with a 150-mL flask and
E 691 Practice for Conducting an Interlaboratory Study to
a 27 by 100-mm thimble.
6.4 Volumetric Flasks, 100-mL.
6.5 Viscometers.
This test method is under the jurisdiction of ASTM Committee D-20 on Plastics
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
Current edition approved Jan. 10, 1997. Published May 1997. Originally
published as D 3591 – 77. Last previous edition D 3591 – 77 (1991).
2 6
Annual Book of ASTM Standards, Vol 05.01. Available from American National Standards Institute, 11 W. 42nd St., 13th
Annual Book of ASTM Standards, Vol 08.01. Floor, New York, NY 10036.
4 7
Annual Book of ASTM Standards, Vol 14.03. Cannon Fenske No. 75 or Ubbelohde No. 1 have been found satisfactory for
Annual Book of ASTM Standards, Vol 14.02. this purpose.
*A Summary of Changes section appears at the end of this standard.
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 3591
6.6 Infrared Spectrophotometer, see 5.4 of Method D 2124.
7. Reagents
7.1 Cyclohexanone, high-purity (see Annex A1).
7.2 Diethyl Ether, anhydrous, reagent grade.
7.3 Caution—Safety precautions should be taken to avoid
personal contact, to eliminate toxic vapors, and to guard
against explosive hazards in accordance with the hazardous
nature of the particular reagent being used.
8. Procedure
8.1 Prepare the PVC sample for extraction by pressing a
film. The film should be 0.02 to 0.5 mm (1 to 2 mil) thick.
Prepare two films in order to make duplicate runs.
8.1.1 Heat the hydraulic press to 165°C (330°F).
8.1.2 Place2gof sample between two sheets of aluminum
foil and insert into the press.
8.1.3 Allow the sample to come to temperature for 2.5 min.
During the next 0.5 min, increase the force on the sample to
620 kN. Maintain the force for 3 min, then cool while
FIG. 1 Calibration Curve, 1 % Plasticizer in PVC Resin at 5.8 μm
maintaining the force.
8.2 Weigh, to 60.2 mg, approximately1gof pressed film
into a 27 by 100-mm extraction thimble.
8.3 Place the thimble in a Soxhlet extraction apparatus fitted
with a tared 150-mL flask, and extract with 120 mL of diethyl
ether for 20 h.
8.4 Remove the tared 150-mL flask containing the diethyl
ether and extracted plasticizer from the extraction apparatus,
and gently heat to boil off the ether.
8.4.1 Caution—When evaporating a quantity of ether to
near dryness, precautions should be taken to guard against an
explosive hazard, due to peroxides which may be in the ether
or which may have been formed during use.
8.5 Place the flask in an evacuated desiccator for a mini-
mum of1hto remove the last traces of ether.
8.6 Weigh, to 60.2 mg, the flask containing the extracted
plasticizer.
8.7 Calculate the percentage plasticizer as follows:
Plasticizer, % 5 A 3 100 /B (1)
~ !
where:
A = weight of extracted plasticizer (7.6), and
FIG. 2 Acceptable Residual Plasticizer,
B = sample weight (7.2).
Less than 0.05 % at 5.8 μm
8.8 Dry the film to remove all solvent.
8.8.1 The extracted film must be free of plasticizer. Errors in
where:
excess of 10 % will result from small residual amounts of
F = weight of extracted film, g,
plasticizer. Examine the extracted film by infrared spectros-
P = plasticizer, %, and
copy to ascertain that the plasticizer level is less than 0.05 % in
R = PVC, %.
order to obtain satisfactory results. An example for a carbonyl
8.10 Weigh a sample of extracted film as determined in 8.9
containing plasticizer is shown in Fig. 1 and Fig. 2.
and transfer to a 100-mL glass-stopped volumetric flask. Take
8.9 Determine the sample size of the extracted film that will
care to transfer all of the weighed sample.
yield 0.02 6 0.002 g of PVC resin as follows:
8.11 Add 50 to 70 mL of cyclohexanone to the flask. Make
sure that all the sample is in the solvent and not attached to the
100 2 P
F 5 3 0.2 (2)
neck of the flask.
R
8.11.1 Use freshly distilled cyclohexanone. Serious errors of
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 3591
greater than 10 % can oc
...