Intrinsic Viscosity as Quality Control Parameter of PET

Relevant for: Polymers, Plastics, ISO 1628, PET

PET is one of the most important polymers used for packaging materials in the world. Different
grades of PET are classified using the Intrinsic Viscosity, a parameter to calculate the polymer’s
molar mass. Lovis 2000 M with its implemented polymer software measures and calculates
polymer parameters automatically at the touch of a button.

The demand for reliable Intrinsic Viscosity

measurements is high as PET has to be characterized
in various fields:

 Research & Development, where new polymers

are synthesized and characterized
 PET suppliers, who want to control the quality
of their products
 Process plants, who want to optimize their
conditions for constant production
 Recycling facilities, that need to control the
properties of recycled PET

1 Intrinsic viscosity for quality control of PET

Dilute solution viscometry using Lovis 2000 M
One technique often used for quality control is dilute
PET(Polyethylene terephthalate) is a linear solution viscometry. Polymers are diluted in
thermoplastic with a wide range of use including appropriate solvents and the viscosity of the pure
fibers, textiles and of course as a packaging material. solvent is set in relation to the viscosity of the polymer
solution. This procedure yields the relative viscosity, a
The main indicator for the quality and the most basic parameter from which many others, including
important characteristic of PET is the value of its the Intrinsic Viscosity can be calculated.
Intrinsic Viscosity. The Intrinsic Viscosity is related to
the polymer’s molar mass and therefore reflects the The Lovis 2000 M is perfectly suited for determining
material’s melting point, crystallinity and tensile the properties of polymers using dilute solution
strength. The Intrinsic Viscosity is dependent upon the viscometry as it offers many features making
length of the polymer chains. The longer the polymer measurements easy and comfortable:
chains are, the more entanglements between chains
occur and therefore the viscosity value is higher. The
desired Intrinsic Viscosity of PET is dependent on its  Polymer software for automatic calculation of
application and classified in different grades (see all desired polymer parameters
Table 1).  Low sample/solvent consumption reducing
the contact with hazardous chemicals
 Optional combination with sample changers
PET grade Intrinsic Viscosity [dL/g]
for enhanced throughput
Fiber grade 0.40 – 0.70  High chemical resistance
Film grade 0.70 – 1.00
Bottle grade 0.70 – 0.78 This report presents Intrinsic Viscosity measurements
Water and soft drink bottle grade 0.78 – 0.85 of PET used for bottle manufacturing of softdrinks.
Measuring settings and a detailed sample preparation
Table 1: Typical Intrinsic Viscosity values of different PET grades.
is given.

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2 Samples and sample preparation Tip: Sample preparation is a critical step, as errors
made here will lead to wrong results and/or bad
The Intrinsic Viscosity [mL/g] of three different PET repeatability.
raw forms for plastic bottle production was measured.
Samples and solvents are listed in Table 2.

Sample and chemicals Chemical Description 3 Measurement

Polyethylene terephthalate (PET), three
Sample
batches This section describes the instrument set-up and the
Dichloroacetic acid (DCA), for dissolving used method settings.
Solvent 1
the polymer and cleaning
Ethanol for removing the acid from the 3.1 Instrumental set-up
Solvent 2
system before drying
Table 2: Tested samples and chemicals used For measurements, a Lovis 2000 M in flow-through
mode was used.
Batch 1 (PET 1) and 2 (PET 2) were transparent
granulates with an approximate size of 4 mm,  Capillary: 1.8 mm glass
whereas batch three (PET 3) was a white granulate  Ball material: gold coated steel
with a size of approximately 2 mm.
 O-rings: Kalrez

2.1 Sample preparation

A chemical resistance upgrade kit can be ordered,
The samples were prepared according to ISO 1628-5, including a batch of gold coated balls and Kalrez® O-
a common test-method for determining the viscosity of rings for enhanced chemical resistance.
thermoplasts.

0.250 g of the sample were weighed into a graduated

50 mL flask and the weight was noted down
(d= 0.1 mg, Table 1). A magnetic stirring bar and
approximately 25 mL of DCA were added and the
flask was closed. For dissolving, the sample was
stirred for 60 min on a hot plate – set to 100 °C – with
stirring function. After approximately 60 min still some
residues were visible and therefore the dissolving
process was extended to 120 min in total. The flask
was then removed from the hot plate and cooled to
room temperature.

Tip: Dissolving times can vary depending on polymer

types and size of the material. Always check if the
polymer solution is clear and that no residues are
Figure 1: Lovis 2000 M in flow- through filling mode
visible anymore.

After removing the stirring bar the flask was filled with
DCA to a final volume of 50 mL resulting in a final 3.2 Method settings
concentration of 0.005 g/mL. To avoid concentration
gradients the flask is shaken properly before the  Measurement mode: Polymer
measurements. The solvent blank was processed in  Temperature: 25 °C
the same way as the sample. Each of the samples  Measurement cycles: 3
was dissolved once.
 Manual angle: 30°
 Measuring distance: long
 Variation Coefficient: 0.35 %

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3.3 Measurement and results 4 Conclusion

Each polymer solution was filled and measured in

The Lovis 2000 M is the perfect solution for
triplicate with cleaning inbetween. Out of the runtimes
determining the grade of PET through Intrinsic
of the pure solvent and the polymer solution all
Viscosity measurements.
polymer parameters were automatically calculated.
For more measuring comfort an Xsample™ 340 can
be added to the measuring assembly. This one
Table 3 displays the results for the three PET batches syringe sample changer enables automatic filling and
expressed in relative and Intrinsic Viscosity [mL/g]. cleaning with up to two cleaning agents and reduces
the contact of the user with hazardous chemicals.
Relative viscosity Intrinsic Viscosity
Sample type
[Mean ± 1 σ (RSD %)] [mL/g,mean ± 1 σ (RSD %)]

PET 1 1.48 ± 0.001 (0.07) 82.1 ± 0.1 (0.12)

PET 2 1.49 ± 0.001 (0.07) 85.5 ± 0.1 (0.12)
PET 3 1.50 ± 0.001 (0.07) 85.0 ± 0.1 (0.12)
Table 3: Relative and Intrinsic Viscosity of the raw material and the
end product

To check for the measuring quality two parameters

are of interest, namely the FW/BW deviation and the
Variation Coefficient (see Table 4).

 The FW/BW deviation gives the deviation

between the runtime of a forward Figure 2: Lovis 2000 M + Xsample™ 340
measurement (e.g. +70° angle) and the
subsequent backward measurement (e.g. -70°
angle).
5 References
 The Variation Coefficient gives the runtime
repeatability in between the measurement 1. ISO 1628-5, Plastics - Determination of the
cycles. viscosity of polymers in dilute solution using glass
capillary viscometers - Part 5: Thermoplastic polyester
(TP) homopolymers and copolymers
Variation coefficient FW/BW deviation
Sample type 2. Materials Science and Engineering: Concepts,
[%] [%]
Methodologies, Tools, and Applications, 2017
PET 1 ≤ 0.08 ≤ 1.37
PET 2 ≤ 0.05 ≤ 1.37
Contact Anton Paar GmbH
PET 3 ≤ 0.02 ≤ 1.37
Table 4: Lovis Variation coefficient and FW/BW deviation as quality support-visco@anton-paar.com
indicators of measurement
support-lps@anton-paar.com

Tip: Limits for the FW/BW deviation are implemented

inside of the instrument. If they are exceeded, a
warning will appear on screen. The limit for the
Variation Coefficient can be set. Per default it is set to
0.35 % for polymer solutions.

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