ASTM D3591-97(2011)
(Test Method)Standard Test Method for Determining Logarithmic Viscosity Number of Poly(Vinyl Chloride) (PVC) in Formulated Compounds
Standard Test Method for Determining Logarithmic Viscosity Number of Poly(Vinyl Chloride) (PVC) in Formulated Compounds
SIGNIFICANCE AND USE
The logarithmic viscosity number provides information on the effect of compounding or processing of PVC.
Exposure of PVC compositions to shear or to high temperatures can result in a change in the logarithmic viscosity number of the resin.
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 7.3 and 8.4.1.
Note 1—This test method and ISO 1628-2 are not equivalent.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D3591 − 97 (Reapproved 2011)
Standard Test Method for
Determining Logarithmic Viscosity Number of Poly(Vinyl
Chloride) (PVC) in Formulated Compounds
This standard is issued under the fixed designation D3591; 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 Determine the Precision of a Test Method
IEEE/ASTM SI-10 Standard for the Use of International
1.1 This test method covers the determination of the loga-
System of Units (SI)
rithmic viscosity number of poly(vinyl chloride) (PVC) ho-
2.2 ISO Standard:
mopolymers after compounding or processing.
1628-2 Plastics—Determination of Viscosity Number and
1.2 It is the basic assumption of this technique that the
Limiting Viscosity Number—Part 2: Poly (Vinyl Chlo-
formulation of the compounded resin is known and that any 3
ride) Resins
additives present can be separated from the resin by extraction
withdiethylether.Thisisnecessarytopermitadjustmentofthe
3. Terminology
amount of sample used in the test to give a resin concentration
3.1 Units and symbols used in this test method are those
in cyclohexanone of 0.2 6 0.002 g/100 mL.
recommended in IEEE/ASTM SI-10.
1.3 This standard does not purport to address all of the
3.2 Definitions of Terms Specific to This Standard:
safety concerns, if any, associated with its use. It is the
3.2.1 The term logarithmic viscosity number is defined by
responsibility of the user of this standard to establish appro-
the equation is 9.1.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific precau-
4. Summary of Test Method
tionary statements are given in 7.3 and 8.4.1.
4.1 The sample is pressed into a thin film and extracted to
NOTE 1—This test method and ISO 1628-2 are not equivalent.
remove the plasticizer.
4.2 The plasticizer-free film is dissolved in cyclohexanone
2. Referenced Documents
and centrifuged to remove insoluble matter.
2.1 ASTM Standards:
4.3 Theviscosityofthecyclohexanonesolutionismeasured
D445 Test Method for Kinematic Viscosity of Transparent
in accordance with Test Method D1243.
and Opaque Liquids (and Calculation of Dynamic Viscos-
ity)
5. Significance and Use
D446 Specifications and Operating Instructions for Glass
5.1 The logarithmic viscosity number provides information
Capillary Kinematic Viscometers
on the effect of compounding or processing of PVC.
D1243 Test Method for Dilute Solution Viscosity of Vinyl
Chloride Polymers
5.2 Exposure of PVC compositions to shear or to high
D2124 Test Method forAnalysis of Components in Poly(Vi-
temperatures can result in a change in the logarithmic viscosity
nyl Chloride) Compounds Using an Infrared Spectropho-
number of the resin.
tometric Technique
E1 Specification for ASTM Liquid-in-Glass Thermometers 6. Apparatus
E691 Practice for Conducting an Interlaboratory Study to
6.1 Centrifuge, capable of 2500 rpm with 100-mL sample
container.
6.2 Heated Hydraulic Press, capable of 620-kN ram force
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
and a temperature of 165°C.
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
Current edition approved Feb. 1, 2011. Published March 2011. Originally
6.3 Soxhlet Extraction Apparatus with a 150-mLflask and a
approved in 1977. Last previous edition approved in 2003 as D3591 – 97(2003).
27 by 100-mm thimble.
DOI: 10.1520/D3591-97R11.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3591 − 97 (2011)
6.4 Volumetric Flasks, 100-mL.
6.5 Viscometers.
6.6 Infrared Spectrophotometer, see 5.4 of Method D2124.
7. Reagents
7.1 Cyclohexanone, high-purity (see Annex A1).
7.2 Diethyl Ether, anhydrous, reagent grade.
7.3 (Warning—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
FIG. 1 Calibration Curve, 1 % Plasticizer in PVC Resin at 5.8 µm
620 kN. Maintain the force for 3 min, then cool while
maintaining the force.
8.2 Weigh, to 60.2 mg, approximately1gof pressed film
into a 27 by 100-mm extraction thimble.
8.3 PlacethethimbleinaSoxhletextractionapparatusfitted
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 (Warning—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-
mumof1hto 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 3100 /B (1)
~ !
where:
FIG. 2 Acceptable Residual Plasticizer,
A = weight of extracted plasticizer (7.6), and
Less than 0.05 % at 5.8 µm
B = sample weight (7.2).
8.8 Dry the film to remove all solvent.
8.9 Determine the sample size of the extracted film that will
8.8.1 Theextractedfilmmustbefreeofplasticizer.Errorsin
yield 0.02 6 0.002 g of PVC resin as follows:
excess of 10 % will result from small residual amounts of
plasticizer. Examine the extracted film by infrared spectros-
100 2 P
F 5 30.2 (2)
copy to ascertain that the plasticizer level is less than 0.05 % in
R
order to obtain satisfactory results. An example for a carbonyl
where:
containing plasticizer is shown in Fig. 1 and Fig. 2.
F = weight of extracted film, g,
P = plasticizer, %, and
Cannon Fenske No. 75 or Ubbelohde No. 1 have been found satisfactory for
R = PVC, %.
this purpose.
D3591 − 97 (2011)
8.10 Weigh a sample of extracted film as determined in 8.9 10.1.4 Efflux time of solvent, and
and transfer to a 100-mL glass-stopped volumetric flask. Take 10.1.5 Logarithmic viscosity number.
care to transfer all of the weighed sample.
TABLE 1 Logarithmic Viscosity Number (Inherent Viscosity) of
8.11 Add 50 to 70 mL of cyclohexanone to the flask. Make
Formulated PVC Com
...
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