Polymer Testing 33 (2014) 138144

Contents lists available at ScienceDirect

Polymer Testing
journal homepage: www.elsevier.com/locate/polytest

Test method

A novel method for the determination of steady-state torque

of polymer melts by HAAKE MiniLab
Cong Wang, Jing Wang, Chenyang Yu, Bingtian Wu, Ya Wang, Wenguang Li*
State Key Laboratory of Polymer Materials Engineering, Polymer Research Institute of Sichuan University, Chengdu, Sichuan 610065,
Peoples Republic of China

a r t i c l e i n f o

a b s t r a c t

Article history:
Received 25 October 2013
Accepted 2 December 2013

HAAKE MiniLab is an apparatus specially designed for compounding polymer material and
on-line testing of rheological properties. For the rst time, it was used to establish a dynamic speed test method for the rapid determination of steady-state torque of polymer
melts. The choices of sample feed quantity and screw rotation speed, as well as calibration
for real torque, were carefully studied before torque measurements. The repeatability and
reliability of torque data were also evaluated. Results showed that the torque could be
calibrated by subtracting the torque without samples. Also, a feed quantity of ca. 6 g with a
dynamic speed test range of 10105 r/min was suitable for the determination of steadystate torque of polyolen samples. The new method was quick, effective and reliable to
correlate the steady-state torque with rotation speed. Therefore, MiniLab would be a very
useful tool in exploring and characterizing polymer ow behavior through its torque
measurements.
2013 Elsevier Ltd. All rights reserved.

Keywords:
HAAKE MiniLab
Steady-state torque
Dynamic speed test method
Repeatability
Reliability

1. Introduction
In the polymer eld, torque refers to the hindering force
met when polymer resins or compounds are plasticized
and mixed with rotation of screws or rotors. It has been
used as an engineering indicator to learn the polymer
melting process for determining suitable processing conditions, as well as to monitor industrial extrusion production for process quality control. Steady-state torque is the
measurement of the torque at equilibrium as the plasticized material is in a stable and homogeneous melt state.
For a pure polymer in a given process, the steady-state
torque is a characteristic of the polymer, which can be
used as a rheological parameter to characterize the polymer ow behavior [14].
The torque-rheometer is the most commonly used tool
in polymer processing laboratory for torque measurements.
It can simulate a mixer and the extrusion process in nearly
* Corresponding author. Tel.: 86 028 85460817; fax: 86 028
85402465.
E-mail address: wgli2007@126.com (W. Li).
0142-9418/$ see front matter 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.polymertesting.2013.12.001

real processing conditions. Therefore, many researchers

have used it to study the processing properties and mixing
quality of polymers [512]. However, as the mixing of
polymer materials with the rotation of rotors generates
heat from viscous dissipation, the pre-set temperature always changes during the mixing process, dependent upon
material and experimental conditions such as mixing time
and rotation rate. As a result, it is almost impossible to
obtain a consistent torque for a polymer at a given temperature [13,14]. As for measuring the correlation of steadystate torque with rotation rate at a given temperature, it is
generally required to select several rotation rates and
measure separately the variation of torque with time at
each rotation rate. This is a time-consuming process with
no certainty of reliable data. Only a few researchers have
tried such experiments with no satisfactory results [1517].
For the above reasons, the application of torquerheometers for characterizing the properties of polymer
melts has been greatly restricted.
MiniLab Micro Compounder and Rheometer, devised by
HAAKE Company, Germany, is specially designed for the
compounding of small volume (7 mL only) samples.

C. Wang et al. / Polymer Testing 33 (2014) 138144

Simultaneously, the rheological properties can be recorded

to document structural changes. Its main features include
integrated torque and viscosity measurements, co- and
counter rotation twin screws and an automatic bypass
operation for circulation/extrusion with pneumatic
feeding. Therefore, MiniLab is considered as a combination
of a batch mixer, a twin-screw extruder and a rheometer.
Based on the units specications, we found that, in
addition to small usage of samples, there are two distinct
advantages in determining steady-state torque of polymer
melts by MiniLab over other torque-rheometers. First,
MiniLab has a special backow channel integrated with the
extrusion housing for circulation, which ensures a precise
and stable operating temperature, thus signifying that the
variation of polymer melt state with temperature due to
viscous dissipation can be negligible. Second, MiniLab can
perform dynamic speed measurements in a selected speed
range by a pre-set test program. We will show that in this
way the correlation of steady-state torque with rotation rate
can be quickly obtained through only a single test, making it
possible and convenient to explore the rheological properties of polymer melts with signicant time and cost savings.
Despite the prominent characteristics of MiniLab as stated
above, published research still relates to using it only as a
conventional mixer to prepare experimental samples and to
compound expensive materials such as nano-composites,
bio-polymers and pharmaceuticals [1827]. No attention
has been paid to its potential powerful function in torque
measurements. The reason may be that the reliability of
rheological measurements by MiniLab has not been evaluated. Moreover, no appropriate method has been established
for the determination of steady-state torque of polymer melts.
This situation was motivation for the current research.
This paper presents a novel method, termed dynamic speed
test method, for the determination of steady-state torque of
polymer melts by means of the MiniLabs functions. We will
introduce how to obtain repeatable, reliable torque data as
well as the correlation of steady-state torque with rotation
rate in the MiniLab test. The calibration of torque data, sample
loads and screw rotation speeds were carefully investigated
as regards the repeatability of data. The comparison of the
new method with the common xed speed method for
steady-state torque measurements was also done to
demonstrate the reliability of data. Our results show that the
dynamic speed test is a quick, effective and reliable method
for determining steady-state torque of polymer melts.

139

Table 1
Characteristics of materials used.
Material Grade
HDPE
HDPE
LDPE
iPP

Melt ow index
(g/10 min)

Supplier

6070EA 7.2 (190  C/2.16 kg) Dushanzi Petrochemical,

China
60550
7.0 (190  C/2.16 kg) Lanzhou Petrochemical,
China
18D
1.5 (190  C/2.16 kg) Daqing Petrochemical,
China
T30S
2.0 (230  C/2.16 kg) Lanzhou Petrochemical,
China

unit (2), extruder housing (3) and feeding device (5). The
control system includes the manual operating panel (4) and
the application software (1). Both the dynamic speed
measurement and the experimental data documentation
can only be performed through the software. The drive unit
offers motor motion and precisely controls experimental
conditions, such as testing temperature and rotation speed.
It also measures the motor torque from a mixer sensor. The
structure of the extruder housing with co-rotation twin
screws is displayed in Fig. 2 (the co-rotation mode was used
in this study). The lled-in sample can be extruded in a
circulation via an integrated backow channel. The backow channel is constructed as a rheological slit capillary
with two pressure sensors. While the sample is extruding
through the backow channel, the rheological information
about the viscosity of the sample can be obtained from the
two pressure sensors. Lastly, the feeding device enables
periodic sample feeding by the piston of a pneumatic
cylinder.
2.3. Dynamic speed test method
There are two stages in the dynamic speed test method.
In the rst stage, samples were dynamically plasticized and
melted under a rotation speed range predetermined according to the requirement of the experiment and the nature of the material. The number of speed points was set to
520 with equal distance logarithmic intervals (rpm)
within the speed range. At each speed, the software program measured the torque of the material, and then

2. Experimental
2.1. Materials
All the samples in this study were carefully selected
from commercial resins. These were high-density polyethylene (HDPE), low-density polyethylene (LDPE) and
isotactic polypropylene (iPP). The characteristics of the
materials were shown in Table 1.
2.2. Instrumental details
The HAAKE MiniLab, as illustrated in Fig. 1, is made up of
ve functional elements: control system (1 and 4), drive

Fig. 1. The constitution of HAAKE MiniLab: (1) and (4) control system, (2)
drive unit, (3) extruder housing, (5) feeding device.

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C. Wang et al. / Polymer Testing 33 (2014) 138144

2.7. Study on repeatability of torque data

Two polyethylenes, HDPE (6070 EA) and LDPE (18D)
with a feed quantity of 6 g, were chosen as test samples.
Plasticizing and measuring were done with a dynamic
speed range of 10105 r/min. The temperature was set at
190  C for 6070 EA and at 150  C for 18D.

2.8. Study on reliability of torque data

Fig. 2. The structure of extruder housing: (1) backow channel, (2) pressure
sensor, (3) conical twin-screw, (4) bypass valve, (5) temperature sensor, (6)
extrusion channel.

selected 20 data points that met the programs required

stability criteria. Afterwards, the instrument would automatically switch to the next speed point until the operating
program was over. In the second stage, the same program
ran again in the same way as in the rst stage. Then, the
measured data were recorded to correlate steady-state
torque with rotation speed for polymer melts at the test
temperature. Generally speaking, it only took about 15 min
to nish the whole measurement with a speed range of 10
105 r/min.

HDPE (6070 EA) was chosen as test material with a

usage of 6 g. The comparison of steady-state torque
determined by the common xed speed method was made
with that measured by the new dynamic speed test
method. In the xed speed method, the test samples were
mixed for 8 min at speeds of 30 r/min, 50 r/min, 80 r/min
and 100 r/min. The torque values from 5 min to 8 min were
averaged to obtain the steady-state torques under different
rotation speeds. For the dynamic speed test method, after
being plasticized under a dynamic speed range of 10105 r/
min, the sample was measured in the same speed range to
acquire the steady-state torques. The experimental temperature in both methods was kept at 150  C.
3. Results and discussion

2.4. Torque measurements by MiniLab

There were two main steps for the determination of
steady-state torque of the material. In the rst step, device
setup was carried out and the measuring procedure was
dened using the software. When the temperature reached
the set point, torque measurements without samples were
performed to obtain a relationship between torque and
rotation speed for calibration purposes. In the second step,
the torque measurements were done after the sample was
fed into the extruder and plasticized. The correlation of
steady-state torque with rotation speed was achieved via
calculating the data exported from the above two-step
measurements.

2.5. Choice of feed quantity

To choose a suitable feed quantity for torque measurements, iPP (T30S) and HDPE (60550) with a dosage of 47 g
were used. The test was carried out under a dynamic speed
range of 10105 r/min and the temperature was xed at
190  C.

2.6. Choice of rotation speed

HDPE (6070 EA) with 6 g was selected as the sample and
three experiments were conducted as follows. Two samples
were separately plasticized for 5 min under a xed speed of
50 r/min and 100 r/min, respectively, and another under a
dynamic speed range of 10105 r/min. All the samples were
measured in the dynamic speed range of 10105 r/min. The
temperature was set at 150  C for both plasticizing and
measurement.

3.1. Torque calibration without samples

According to the instruction manual for the HAAKE
MiniLab, before beginning the measurement, motor torque
without material but with rotating screws must be calibrated to its torque zero point. It was found that the torque
calibration in the manual worked well for a xed speed but
not for a dynamic speed test. Some torque values were not
always accurate over a wide rotation speed range. Hence in
this paper, we calibrated torque through subtraction on the
basis of the following.
Fig. 3 depicts the torque plotted against rotation speed
without samples in the MiniLab. It can be seen that there
is a linear relationship between torque and rotation speed
within a rather wide range of 5205 r/min, which can be
expressed as y 0.0018*x 0.019, where x is the rotation
speed, y is the corresponding torque value. It should be
noted that the slope or intercept of the linear line might
vary slightly with the time passed. However, our MiniLab
instrument, after many years of usage, has consistently
demonstrated this linear relationship between torque
and rotation speed. The instruments performance
was not subject to atrophy that may apply to other
instruments.
Based on the above nding, we proposed a subtraction
approach to calibrate the torque of polymer melts. That is,
the real torque value was obtained by subtracting the torque value without samples from the torque values with
samples. For any dynamic torque measurement, it was
necessary to preferentially establish the correlation of torque with rotation speed without samples before beginning
the measurement. Thus, the real torque of polymer melts
could be obtained throughout the dynamic speed test
method.

C. Wang et al. / Polymer Testing 33 (2014) 138144

141

Fig. 3. Relationship of torque-rotation speed without samples.

3.2. Effects of feed quantity on torque measurements

The torque, by denition, is obviously dependent on the
amount of material used in a measurement. For the MiniLab, the feed quantity needs to be suitable for obtaining a
consistent measuring torque value.
Fig. 4 outlines the effects of feed quantity on the steadystate torque of T30S (a) and 60550 (b). It can be seen from
Fig. 4(a) that the torque of T30S signicantly increased with
feed quantity varying from 4 g to 6 g at given rotation
speeds. When continuing to add up to 7 g, the steady-state
torque leveled off. It should be noted that the torque started
to fall with increased feed quantity from 6 g to 7 g at a
rotation speed of 105 r/min. The most probable explanation
of this trend was that the PP chains degraded with rotation
at such a high speed.
As shown in Fig. 4(b) for 60550, it was also found that
the torque increased with the increased feed quantity from
4 g to 6 g. However, unlike T30S, the steady-state torque of
60550 was constant when the feed quantity was between
6 g7 g, even at a high rotation speed of 105 r/min. This
may be due to the better chain stability of HDPE than that of
PP.
The above results indicated that loads of ca. 6 g were
suitable for obtaining consistent torque values in the
MiniLab. This is reasonable if the following calculation is
considered. As bulk densities of PP and HDPE are about
0.91 g/cm3 and 0.96 g/cm3, respectively, the volume of 6 g
sample could correspond to 6.6 mL for PP and 6.3 mL for
HDPE at room temperature. When PP or HDPE is molten,
the polymer volume will expand somewhat. Since MiniLab
has a cavity of 7 mL volume, the feeding quantity of ca. 6 g
polyolen samples should completely ll the cavity, which
leads to the maximum torque as expected. Therefore, the
experimental results are in agreement with the theoretical
calculations.
It should be mentioned that lling with 45.5 g of material, as suggested in the operating manual of MiniLab, was
not suitable for torque measurements. Since the steadystate torque of polymer melts is strongly related to feed
quantity, it is important to determine the optimum quantity for any unknown material. Only by doing that, can

Fig. 4. The relationship between steady-state torque and feed quantity to

T30S (a) and 60550 (b).

repeatable and valuable data from torque measurements in

the MiniLab be obtained.
3.3. Effects of rotation speed on torque measurements
Steady-state torque depends, to an extent, on both
plasticizing and measuring conditions, especially on the
screw rotation speed. If samples are plasticized or
measured at a very high rotation speed, polymer chains can
be easily broken down, leading to a low torque value. If
samples are measured at a very low rotation speed, the
torque may be too small to be accurately determined.
Hence, there is an optimum rotation speed range for torque
measurements, in which the measured torque can accurately represent the rheological character of the material.
Fig. 5 gives the steady-state torques of 6070 EA plasticized under three different plasticizing conditions. It was
observed that the torque-rotation speed curve of 6070 EA
plasticized at a dynamic speed range of 10105 r/min was
in accordance with that plasticized at a xed speed of 50 r/
min, revealing that two plasticizing conditions could
generate almost identical polymer melts with homogeneous and stable states. However, for the sample

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C. Wang et al. / Polymer Testing 33 (2014) 138144

Fig. 5. The steady-state torque of 6070 EA plasticized under different rotation speed.

plasticized at a xed speed of 100 r/min, the torquerotation speed curve dramatically declined with
increasing speed as compared to that of other two samples.
This trend indicates that polymer chains had been greatly
degraded under that plasticizing condition.
Thus, from the above results, a dynamic speed range of
10105 r/min was chosen for torque measurements. This
speed range was appropriate enough for the preparation of
samples with identical melt states. Therefore, the true
torque values can be obtained within a relatively wide
speed range.
3.4. Evaluating the repeatability of torque data
Repeatability of measured data must be a primary criterion of how well an instrument works. Fig. 6 shows the
torque-rotation speed curves of 6070 EA measured at
different times (on March 23, May 17 and June 6 of 2012,
respectively). It can be seen that, although there was a
small deviation of data at the speeds of above 80 r/min, the
highest standard deviation was only 2.15% (at a speed of

Fig. 6. Torque-speed curves of 6070 EA measured at different times.

Fig. 7. Torque-speed curves of 18D measured in three consecutives.

105 r/min). Therefore, the data repeatability was very good

for the same samples tested at different times. The results
also indicated that the working state of MiniLab was very
stable.
Fig. 7 shows the relationship between torque and rotation speed of 18D measured on three consecutive tests after
being plasticized at 150  C. The torque curve in the rst test
was almost completely overlaid with that in the second
test. In the third test, it started to decline slightly, probably
due to degradation of LDPE chains with time at high temperature. The results demonstrated that the data repeatability was also very good for the sample tested in the rst
two replicates after the sample was plasticized.
In general, if test temperature and dynamic speed range
are well set up to minimize the degradation of polymer
chains, we can always get repeatable torque measurements
for any sample by MiniLab.
3.5. Evaluating the reliability of torque data
Data reliability is critical for a measuring method.
Although the measurements were obtained quickly, the

Fig. 8. Torque measurements of 6070 EA under xed speed.

C. Wang et al. / Polymer Testing 33 (2014) 138144

143

Fig. 10 presents the comparison of the steady-state

torques determined by the two methods. It can be seen
that, except at high rotation speed where the torque
measured by the dynamic method was slightly higher than
that determined by the xed speed method (due to small
degradation of polymer chains), all of other torque data
results were in agreement with each other. This revealed
that these two methods for steady-state torque measurements worked very well in MiniLab. However, the dynamic
speed method had advantages over the common xed
speed method because of time and cost savings, as well as
achieving accurate data and minimum degradation of
polymer chains.
4. Conclusions
Fig. 9. Torque measurements of 6070 EA under dynamic speed.

reliability of the torque data was not compromised. Fig. 8

exhibits the variation of torque with time for 6070 EA
under the xed speed test method. It can be seen from
Fig. 8 that, after feeding the sample, the torque values
under each xed speed from 30 r/min to 100 r/min all
changed with time in the rst 5 min. Thereafter, they
reached equilibrium values up to 8 min. As expected, the
steady-state torques increased with increase of rotation
speed. It is important to note that, if the sample is added
into the extruder cavity all at once, the feed path becomes
obstructed. Thus, the sample was divided into two portions,
resulting in two peaks on the graph.
The dynamic speed test method includes plasticizing
and measuring stages. After the plasticizing stage, the
sample becomes a homogeneous and stable melt. Thus, the
torque of a sample quickly reaches an equilibrium value
when the rotation speed changes from one speed to
another. Fig. 9 describes the variation of torque with time in
the measuring stage, by which the steady-state torques
were directly measured with 10 separate rotation speeds.
Please note that only one sample was used in the method
and the steady-state torques could be obtained for 10
different rotation speeds within no more than 15 min.

Fig. 10. Comparison of two methods.

We proposed a novel method for determination of

steady-state torque of polymer melts using the features of
the MiniLab instrument. The torque was calibrated by
subtracting that without material. The optimum feed
quantity of ca. 6 g and a dynamic speed range of 10105 r/
min were determined for torque measurements of polyolen samples. The data repeatability was evaluated by
measuring the same samples separately at different times
or with sample replicates. The data reliability was
conrmed by comparing the new method with the common xed speed method for steady-state torque measurements. The results showed that the dynamic speed test
was a direct, effective and rapid method for the determination of steady-state torque of polymer melts by MiniLab.
The torque data obtained were repeatable and reliable.
Moreover, the new method had a remarkable time and cost
savings as compared to the conventional method. The
correlation of steady-state torque with rotation speed was
generally considered as a rheological curve for polymer
melts. This promises great potential in academic research
and industrial applications.
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