You are on page 1of 6

::: Application Note

Single-Point Calculations of Polymer


Specific Parameters (e.g. Intrinsic
Viscosity) Using the Lovis 2000 M/ME
The intrinsic viscosity usually is the characteristic value that
specifies a polymer‘s storage stability and its quality.

With the Lovis 2000 M/ME the intrinsic viscosity can be determined
Grafik oder Bild
automatically via single-point measurements.

1 Introduction The principle of viscosity measurement of polymer


solutions is simple:
The intrinsic viscosity usually is the characteristic value
First the capillary is filled with the pure solvent and the
which specifies a polymer‘s storage stability and its quality.
runtime of the ball inside is measured. Next the capillary is
Intrinsic viscosity values changing in dependence on the
filled with the polymer solution and once again the runtime
time give information on the polymer‘s stability (aging,
of the ball inside is measured.
degradation). Constant product quality (e.g. of different
Out of the runtime of the pure solvent and the runtime of
batches) yields unchanging intrinsic viscosity values.
the polymer solution the relative viscosity is determined,
However, each determination of the intrinsic viscosity
which is the basic value for all subsequent polymer
needs sample preparation, filtration and determination of
calculations.
the running times of a series of concentrations.

A much easier method to control storage stability and 3 Polymer Specific Values Automatically
quality of the product is to perform single-point Calculated by the Lovis 2000 M/ME
measurements. Saving both time and money, single-point
measurements do not require a range of concentrations for Relative Viscosity
intrinsic viscosity determination, but only the running time
of a single concentration. (1) The relative viscosity (ηr) is the viscosity of the polymer
solution (η) at a given concentration divided by the
viscosity of the pure solvent (η0). If the solvent density and
2 Viscosity Measurement of Polymer Solutions the solution density differ by less than 0.5%, the viscosity
ratio will be given by the runtime ratio.
For viscosity measurements the polymer has to be
dissolved in an appropriate solvent. Valid combinations of  t
polymers and solvents can be looked up in particular r  
ASTM and ISO standards and literature.
 0 t0

Typical concentrations of polymer solutions are between Specific Viscosity


0.001 to 0.050 g/mL. At these concentrations the densities
of polymer solution and solvent are nearly the same and The specific viscosity is the difference in the runtime (t) of
can therefore be neglected for the further calculations. the polymer solution at a given concentration to the runtime
of the pure solvent (t0), relative to the runtime of the pure
When performing single-point calculations the solvent (t0).
concentrations should be selected in the range of possible
relative viscosities, that means the running time of the t  t0
polymer solution should be between 1.2 - 2.5 times the  sp   r  1 
t0
running time of the pure solvent (1).

C72IA017EN-A 1 www.anton-paar.com
::: Application Note

Reduced Viscosity Inherent Viscosity

The reduced viscosity also referred to viscosity number or The inherent viscosity is the logarithmic viscosity number.
Staudinger function.

 
t  t0 ln  
 red  I  VN   ln  r 
t0  c inh   0
c c

Intrinsic Viscosity
4 Performing the Polymer Evaluation with the
The intrinsic viscosity carries the same information content Lovis 2000 M/ME
as the molar mass.
The following steps will explain how to measure the solvent
There are several methods for evaluating single point
and polymer-solution at one defined angle. All
measurements:
subsequent automatically performed polymer calculations
Billmeyer are related to the measurements at one measuring angle
(one shear rate).

   0.25    r  1  3  ln ( r )  There are two different polymer methods:


 c  • Polymer (Runtime)

Using the runtime of the solvent and polymer solution for


Solomon-Ciuta the subsequent calculations; values related to this method
are marked with “RT”.
2  [ sp  ln ( r )] This method is used, if the measurement of the solvent and
   the measurement of the polymer solution are performed at
c the same angle.

Deb-Chatterjee • Polymer (Viscosity)

Using the dynamic viscosity of the solvent and polymer


3 3  ln ( r )  1.5   sp  2  3  sp solution for the subsequent calculations; values related to
   this method are marked with “VI”.
c
This method is used, if the measurement of the solvent and
the measurement of the polymer solution are performed at
The choice of evaluation method depends on the
different angles (e.g. If the runtimes of the solvent are
polymer/solvent combination.
much lower compared to the runtimes of the polymer
solution it is possible to measure the solvent at a very flat
K-Value
angle and the polymer solution at a steeper angle.)
The K-value is the average number of monomers a
polymer is composed of, it is a measure of the average (Important: for the dynamic viscosity always the density
degree of polymerization (DIN EN ISO 1628-1). value is needed!)

K  value  1000  k 4.1 Prepare the polymer solution at the required


concentration.
2 
1.5  lg  r   1  1    2  1.5  lg  r  1.5  lg  r 
c  (Choose the concentration of the polymer solution, so that
k the relative viscosity is between 1.2 and 2.5.)
150  300  c
Typical concentrations for polymer solutions are between
0.001 and 0.050 g/mL.

C72IA017EN-A 2 www.anton-paar.com
::: Application Note

4.2 Open the desired Polymer-Method


Go to “Menu > Methods > Method Settings” and open
either “Polymer (Runtime)” or “Polymer (Viscosity)”.

If your instrument is not equipped with these methods get


into contact with your Anton Paar representative and install
it according to the manual („Service > Backup Instrument
Settings“).

4.4 Define the measuring parameters


Go to “Menu > Methods > Method Settings > Polymer >
Lovis Module”.

Define the measuring parameters (Temperature Settings,


Measuring Settings and Advanced Settings) for the
subsequent measurements.

4.3 Activate the check boxes


Go to “Menu > Methods > Method Settings > Polymer >
Activate Modules/Constants”.

Depending on the application ensure that:

The check boxes Solution Concentration (RT) and Solvent


Runtime (RT) are activated for the subsequent polymer
calculations using the runtime.
OR
The check boxes Solvent Dynamic Viscosity (VI) and
Solution Concentration (VI) are activated for the
subsequent polymer calculations using the dynamic
viscosity.

Important!
When defining the “Measuring Settings” activate the check
box for using the manual angle and enter the required
angle.

C72IA017EN-A 3 www.anton-paar.com
::: Application Note

4.5 Define the polymer specific output quantities Open the group “User Functions” and choose your
polymer specific output quantities.
Go to “Menu > Methods > Method Settings > Polymer >
Result Output”.

Define the list of polymer specific output quantities for


printouts and data exports.

4.6 Define the display layout


Go to the “Main Screen” for directly changing the content
of the output fields. The changes are automatically saved
in the current polymer measuring method.
Use the drop-down box to choose the „Group“. Tap on the output field to be changed in the main screen.
Select "User Functions", "Quantity", associated "Unit" (if
applicable) and number of "Digits".
Tap <OK> to save your settings.

C72IA017EN-A 4 www.anton-paar.com
::: Application Note

4.7 Measure the runtime/dynamic viscosity of 4.8 Measure the runtime/dynamic viscosity of
the pure solvent the polymer solution
Go to the “Main Screen” for measuring the runtime of the Go to the “Main Screen” for measuring the runtime of the
pure solvent. polymer solution.
Open the “Quick Settings” and select the “S (Standard)” Open the “Quick Settings” and select the “S (Standard)”
parameter. parameter.

When measuring the runtime: When measuring the runtime:


Enter “0” for the “solvent average runtime”, the “solution
Enter the measured solvent average runtime and the
concentration” and “density”. (These values are not used
concentration of your polymer solution. Enter “0” for the
for the subsequent solvent measurement but the
“density”.
measurement cannot be started when these fields are kept
empty.) When measuring the dynamic viscosity:
When measuring the dynamic viscosity:
Enter the measured solvent dynamic viscosity, the
Enter “0” for the “solvent dynamic viscosity” and the concentration of your polymer solution and the density of
“solution concentration”. For the “density” enter the density the polymer solution.
value of the solvent.

Press <OK> and <Start> to measure the runtime/dynamic


viscosity of the solvent.

At the end of the measurement write down the average


runtime/dynamic viscosity of the solvent.

C72IA017EN-A 5 www.anton-paar.com
::: Application Note

Press <OK> and <Start> to measure the runtime/dynamic 5 Conclusion


viscosity of the polymer solution.
The Lovis 2000 M/ME Microviscometer with its many
special features is the ideal instrument for these
single-point polymer measurements:

• Due to the small capillary sizes only little sample


volume is required.

• The variable inclination angle of the measurement


allows both the variation of the shear rate and the
easy repetition of measurements.

• Due to the closed system any contamination and


evaporation can be avoided.

• The built-in Peltier thermostat provides high precision


temperature control.

• The instrument is highly modular and easily connected


to other Anton Paar instruments; it can be combined
with DMA M Density Meters for automated calculation
of dynamic viscosity.

At the end of the measurement all polymer specific values It can also be combined with an Xsample sample
are calculated automatically and shown on the display. changer for automatic filling and cleaning of the
capillary and measurements with high sample
throughput.

6 Reference

(1) Introduction based on: W.-M.Kulicke, C.Clasen,


“Viscometry of Polymers and Polyelectrolytes”, Springer
Laboratory

When measuring more than one polymer sample:

If all the polymers are dissolved in the same solvent and


measured at the same temperature, you measure the
runtime of the solvent once and continue with step 4.8.
Contact Anton Paar GmbH:

If the polymers are dissolved in different solvents or Tel: +43 316 257-0
measured at different temperatures you always have to Fax: +43 316 257 257
measure the solvent before the measurement of the info@anton-paar.com
polymer solution. www.anton-paar.com

C72IA017EN-A 6 www.anton-paar.com

You might also like