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• rheotalk biennial<br />
Overview<br />
Welcome to the second edition<br />
of our cumulative Biennial<br />
RheoTalk. This has been<br />
complied to provide our<br />
Australian customers and<br />
readers of RheoTalk with an<br />
easy reference and source<br />
of the product information,<br />
application articles and news<br />
from 2007 - 2008.<br />
The newsletter has been cross indexed and<br />
referenced by industry, so that each key area<br />
can identify the specific information that<br />
relates to their industry. There classifications<br />
that we have used are listed and are also<br />
colour coded:<br />
• Mining Industries<br />
• Polymer Industries<br />
• Food Industries<br />
• Surface Coatings Industries<br />
• Chemical & General Manufacturing<br />
Industries<br />
• Construction & Building Industries<br />
• Pharmaceutical, Cosmetics & Allied<br />
Industries<br />
• All Industries<br />
Additionally, the indexes have been divided<br />
into three sections covering Application<br />
Notes, News & Views, and Product News<br />
& Industry Applications. There is an index<br />
at the beginning of each of these sections,<br />
listing the contents within that section with<br />
a cross reference to the industry that it<br />
applies to.<br />
• rheotalk biennial<br />
In This Issue...<br />
• rheotalk biennial<br />
Information<br />
Request<br />
Form<br />
At the end of the cumulative issue of<br />
RheoTalk we have provided an Information<br />
Request Form for those that wish further<br />
information. The form can be printed and<br />
filled out and then either faxed or posted.<br />
Alternatively, you can send an email direct<br />
with details of the information you are<br />
seeking to info@rheologysolutions.com<br />
We trust that the Biennial RheoTalk will be<br />
beneficial to all that read and search through<br />
the issue. Any enquiries from the Biennial<br />
RheoTalk not within Australia will be<br />
forwarded to our overseas partner for their<br />
action. Happy reading<br />
biennial 07-08<br />
• rheotalk biennial<br />
Search<br />
Facility<br />
This file has been created as a PDF which<br />
therefore provides full search function. This<br />
means that searching can be conducted by<br />
any word, phrase, industry type, brand name,<br />
application or product model.<br />
Application Notes & Laboratory Reports Product News & Industry Applications<br />
Application Notes ............................ 2-31 Product Focus ........................... 56-105<br />
Laboratory Reports............................ 2-31 Product Reviews ........................ 56-105<br />
News & Views Product News ........................... 56-105<br />
Industry <strong>Solutions</strong> ............................ 32-55 Information Request Form... 106-110<br />
Company News ................................ 32-55<br />
info@rheologysolutions.com 1<br />
www.rheologysolutions.com
Application Notes<br />
& Laboratory Reports<br />
Application Notes<br />
• Experimental Influences on the Casson-Viscosity. The Casson Yield<br />
Point for Chocolate Tests ........................................................................ 6 •<br />
• How to Select the Most Suitable Sensor for Your Application ........................ 7 •<br />
• Rheological Analysis of Powder Coatings........................................................ 4 •<br />
• Rheological Characterisation of Tooth Paste ................................................ 5 •<br />
• Rheological Investigation of Three Rubbers with Different Shore Factors<br />
With Respect to their Shape Stability before Curing ........................................ 5 •<br />
• Rheological Properties of Fresh Building Materials ........................................ 6 •<br />
• Breaking Strength of Chocolate ................................................................ 8 •<br />
• A New Approach to Rheological Modelling of an Electrostatic<br />
Ash & Water Mixture – Quadratic Law ........................................................ 11 •<br />
• A New Definition in Reactor Temperature Control with the Highly Dynamic<br />
HAAKE DynaMax System ........................................................................ 10 •<br />
• A Numerical Study of Temperature & shear Flow in a Transiently<br />
Loaded Lubricant Film ................................................................................ 10 •<br />
• Characterisation of the Thixotropic Behaviour of Semi-Solid Foodstuffs ........ 13 •<br />
• Dynamic Master Curves of Polymer Modified Asphalt<br />
From Three Different Geometries ................................................................ 13 •<br />
• Online Quality Control of Polymers & Extruded Films ................................ 11 •<br />
• Rheological & Microstructural Analysis of a Model Rennet<br />
Casein Gel as Influenced by Cooling Rate ................................................ 12 •<br />
• <strong>Rheology</strong> as a Tool for Immiscible Polymer Blends<br />
Characterisation: Interfacial Tension & Compatibilisation ................................ 12 •<br />
• Thickening of Electrostatically Stabilised Latices by Ethyl<br />
Acrylate-Methacrylic Acid Copolymers with Various Molecular Weights ........ 13 •<br />
• Rheological Analysis of Powder Coatings- Paint & Resin Article ................ 30 •<br />
• Rheological Characterisation of Asphalt Binders ........................................ 16 •<br />
• Rheological Characterisation of Tooth Paste – COSSMA Article 9/2007 ........ 14 •<br />
• What Happens When Rheological Properties Change? Looking into<br />
Rheological Properties with Simultaneous Collection of Microscopic Images 16 • • • • •<br />
• New Measuring Cell for UV Assisted Thermal Curing<br />
at Elevated Temperatures ........................................................................ 19 • • • • •<br />
• QC Measurements for Liquid Food Products and Packaging ........................ 17 • •<br />
• Rheological Behaviour of Automotive Paint Systems........................................ 18 •<br />
• Rheological Methods for Determining Molecular Weight &<br />
Molecular Weight Distribution ........................................................................ 20 • • • • •<br />
• Solvent Trap & Double Cone System for Reproducible Results in<br />
Rheological Measurements of Low Viscous Volatile Fluids ........................ 9 •<br />
• The Rheological Properties of a Copper Concentrate Slurry: From<br />
Surface Chemistry to Pipeline Transport ........................................................ 17 •<br />
• Wet-Shotcrete of Refractory Castables ........................................................ 18 • •<br />
• Cellulosic Derivatives in Capillary Break-up. Influence of the<br />
MWD & Gel Particles ................................................................................ 24 •<br />
biennial 07-08<br />
2 www.rheologysolutions.com<br />
ALL INDUSTRIES<br />
POLYMER<br />
FOOD<br />
SURFACE COATINGS<br />
MINERAL<br />
CHEMICAL<br />
PHARMACEUTICAL<br />
BUILDING
Application Notes<br />
& Laboratory Reports<br />
Application Notes<br />
• Correlation of Misting During Printing with Extensional<br />
Rheological Investigation on Offset Printing Inks ........................................ 24 •<br />
• Improved Torque Sensitivity & Normal Force<br />
Resolutions for Routine Measurements ........................................................ 23 •<br />
• Overview of <strong>Rheology</strong>-Based Process Challenges<br />
for the Mineral Processing Industries ........................................................ 23 •<br />
• Slurry <strong>Rheology</strong> & Pipeline Transport Properties, an Overview ........................ 22 • •<br />
• The Influence of Thickeners on the Application Method of Automotive<br />
Coatings and Paper Coatings – Rheological Investigation ................................ 22 •<br />
• Continuous On-Line Rheometry for Industrial Slurries ................................ 29 •<br />
• Measuring Coatings ................................................................................ 29 •<br />
• Rheological Measurements in the Coatings Industries – The Last 60 Years 27 •<br />
• Rheological Properties of Bitumen Modified with<br />
Polyethylene and Polyethylene Based Blends ................................................ 28 •<br />
• Small Scale Compounders for Pharmaceutical Research ................................ 30 •<br />
• Measurement of the Irganox Content in Polypropylene Polymers<br />
During Extrusion ........................................................................................ 28 •<br />
Laboratory Reports<br />
• Test Methods for Characterisation and Optimisation of Recycling Polymers 4 •<br />
• Correlation Between Mixer Tests & The Extrusion Behaviour of PVC Dry Blends 14 •<br />
• Evaluating the Plasticisation Process of Different Soft-PVC Samples ................ 15 •<br />
• NanoComposites – Examples on Compounding of Nanoclay<br />
Blends in Twin Screw Extruders. ................................................................ 21 •<br />
• Pharma MiniLab – Small Scale Compounder for Pharmaceutical Research 21 •<br />
• Small Scale Catheter Production ................................................................ 21 •<br />
• A Collaborative Study of the Structure and Rheological Properties<br />
of EVOH/SMA Blends Produced by Reactive Extrusion ................................ 27 •<br />
• New Die Design for the Characterisation of the Extensional<br />
and Shear Properties of Polymers for Laboratory and On-Line Use ................ 28 •<br />
• Recent Developments in Bench-Top Twin-Screw Compounders ................ 25 •<br />
info@rheologysolutions.com<br />
ALL INDUSTRIES<br />
POLYMER<br />
FOOD<br />
SURFACE COATINGS<br />
MINERAL<br />
biennial 07-08<br />
CHEMICAL<br />
3<br />
PHARMACEUTICAL<br />
BUILDING
application notes & technical articles<br />
Test Methods for Characterisation<br />
and Optimisation of Recycling<br />
Polymers<br />
Polymers are used daily in thousands of tons.<br />
Recycling of the used polymers is essential to<br />
reduce the amount of waste. One of the key<br />
problems in polymer recycling is the separation of<br />
the polymers to defined sorts of polymers such as<br />
PE, PP, PVC and Polyesters etc.<br />
Even sorted materials show a wide variation of<br />
biennial 07-08<br />
polymer industries<br />
Powder coatings are a cost effective and<br />
environmentally friendly alternative to liquid<br />
coatings. Traditional coatings systems network<br />
via a thermally activated process. This usually<br />
involves placing a powder coated surface into an<br />
oven between 160°C to 200°C in temperature.<br />
The powder melts at around 80°C to 120°C and<br />
becomes an even film. At temperatures of<br />
between 110°C to 140°C the network reaction<br />
begins. The curing time typically lasts between<br />
15 and 30 minutes, depending on the<br />
temperature and reactivity of the system. New to<br />
the market place are U.V. curing powder coating<br />
systems, where the curing process takes place in<br />
a shorter amount of time, even at temperatures of<br />
below 100°C. A further advantage of the U.V.<br />
induced networking is that it works virtually<br />
independently of temperature. This opens up new<br />
flow behaviour, which eventually precents a<br />
smooth processing of the recycled polymers.<br />
The report describes various test methods to<br />
analyse the flow and processing behaviour of<br />
polymers.<br />
The test were mainly operated with a recycling<br />
granulate, made of HDPE – cosmetic bottles. The<br />
bottles were sorted, grinded and washed to clean<br />
the material and to remove the paper sticking on<br />
the polymer. After drying, the material was<br />
application possibilities for coating heat sensitive<br />
surfaces like wood or synthetics.<br />
When powder coating different substrates it is not<br />
only smooth, tough surfaces that are desired but<br />
also adhesive strength, corrosion protection and<br />
durability.<br />
The melting and curing relationship of powder<br />
coatings can be rheologically analysed using<br />
oscillation tests with an air bearing rheometer.<br />
The advantage of this method is that the<br />
structural change of the coating as a function of<br />
time or temperature can be demonstrated without<br />
disturbing the process ie. at very small oscillation<br />
amplitudes.<br />
The rheological measurements that are usually of<br />
interest are complex viscosity h*, complex<br />
modulus G*, the loss factor tan d as well as the<br />
phase displacement angle d. As many powder<br />
coatings become very hard after the complete<br />
packed in drums for further processing.<br />
The laboratory report includes an overview of the<br />
following test methods: Testing of Melt Flow Rate<br />
(MFR); Capillary <strong>Rheology</strong>; Laboratory Extruder<br />
Tests; and Laboratory Mixer Tests.<br />
A full copy of “Test Methods for<br />
Characterisation and Optimisation of<br />
Recycling Polymers” is available by quoting<br />
reference no: LR-45<br />
application notes & technical articles<br />
Rheological Analysis of Powder<br />
Coatings<br />
surface coatings<br />
industries<br />
curing process, parallel measurements using<br />
plate plate geometry PP20 with 20 mm plate<br />
diameter are recommended for the rheological<br />
tests.<br />
Rheological analysis of powder coatings takes<br />
place at temperatures of somewhere between<br />
80°C and 250°C. This range can easily be<br />
covered using the electric temperature unit<br />
TC501 with cone heating. The following outlines<br />
some recommendations of practical examples<br />
and typical measurement definitions. All<br />
measurements have been carried out using the<br />
air bearing rheometer Haake RheoStress, with the<br />
high temperature measuring unit TC501 with<br />
cone heating and the parallel plate geometry<br />
PP20 (20mm plate diameter). As a standard<br />
measurement the gap was set at 0.5 mm.<br />
A full copy of “Rheological Analysis of<br />
Powder Coatings” is available by quoting<br />
reference no: V-157<br />
4 www.rheologysolutions.com
application notes & technical articles<br />
Rheological Investigation of<br />
Three Rubbers with Different Shore<br />
Factors with Respect to their<br />
Shape Stability before Curing<br />
polymer industries<br />
A great variety of rubber parts is produced for the<br />
automotive industry. To minimise problems during<br />
the assembly of the cars and to ensure best<br />
performance, the parts have to be manufactured<br />
with the smallest possible variation in size and<br />
shape. The size can be controlled by the extrusion<br />
and injection parameters – the shrinking of the<br />
material can often be well estimated. But what<br />
What is actually in the tooth paste?<br />
Tooth pastes are viscoelastic products well known<br />
in every day life. Its main components are<br />
abrasives, moisture agents, binding agents,<br />
surfactants, sweeteners, preservatives, artificial<br />
coloring, flavors and special active ingredients.<br />
As abrasives often hydroxides, carbonates,<br />
phosphates or silicates are used which are to<br />
support the mechanical cleaning effect of the<br />
tooth brush. Moisture agents like glycerin, sorbit,<br />
lignite or polyethylenglycols prevent a drying out<br />
of the tooth paste; at the same time they increase<br />
the low temperature stability and have a texture<br />
building effect.<br />
info@rheologysolutions.com<br />
about the shape? The problem is not only the<br />
relaxation of the rubber after leaving the mold –<br />
this can be controlled by an appropriate design of<br />
the injection process. There can also be variation<br />
of the shape before entering the oven for<br />
vulcanisation, which takes typically half an hour.<br />
Due to gravitational force there can be significant<br />
changes in shape of an injected part depending<br />
on the rubber formulation used. To avoid such<br />
effects and to improve production performance, it<br />
would be highly advantageous to predict the<br />
Binding and thickening agents give the tooth<br />
paste its desired texture and prevent a phase<br />
separation between fluid and solid. Hydrocolloids<br />
like Alginate, Carrageenan, Methylcellulose or<br />
Xanthan are mainly used as binding agents. A<br />
frequently used thickening agent is high-disperse<br />
silicium dioxide or Bentonite.<br />
Surfactants decrease the surface tension thus<br />
improving the even distribution of the tooth paste<br />
in the mouth. In dental care only tasteless, nontoxic<br />
anion surfactants are suitable like e.g.<br />
sodium lauryl sulfate, or coconut aliphatic<br />
monoglyceride sulfonate.<br />
Sweeteners as well as the flavors serve as taste<br />
correctives. Preservatives are necessary as<br />
protection from microbial decomposition.<br />
Colors and pigments are finally used for the<br />
respective properties of the sample. The<br />
presentation will show, that prediction of shape<br />
stability is possible with appropriate rheological<br />
investigations.<br />
A full copy of "Rheological Investigation of<br />
Three Rubbers with Different Shore Factors<br />
with Respect to their Shape Stability before<br />
Curing" is available be quoting reference<br />
no: V-169<br />
application notes & technical articles<br />
Rheological Characterisation of<br />
Tooth Paste<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
coloring of striped tooth pastes. Besides this,<br />
there may be active ingredients as protection<br />
from caries or for the care of the gums or<br />
painsensitive teeth.<br />
How is tooth paste produced?<br />
The production of tooth paste is either done<br />
batch-wise in a vacuum mixer or in continuous<br />
production processes. In the continuous<br />
production 5 different process steps can be<br />
differentiated: gel production, metering of liquid<br />
components, metering of solids, mixing process<br />
as well as homogenization and ventilation.<br />
A full copy of “Rheological Characterisation<br />
of Tooth Paste” is available by quoting<br />
reference no: V-142<br />
biennial 07-08<br />
5
application notes & technical articles<br />
Rheological Properties of Fresh<br />
Building Materials<br />
After the introduction of the OICCC standard<br />
recently, rheological tests are a must in the<br />
industry for quality assurance of the chocolate.<br />
They include measurements at different shear<br />
rates up to 60s -1 to be performed after a defined<br />
pre-treatment of the chocolate. With the<br />
computerised rheometers available today the<br />
measuring conditions and procedures can be<br />
preset so that most of them can be carried out<br />
automatically by the push of a button. This will<br />
reduce the time effort for routine tests drastically<br />
and the saved work capacity can be used<br />
otherwise. However, even when working<br />
accurately and, on the first glance, with identical<br />
pre-treatment of the samples the results can<br />
differ considerably especially in comparison with<br />
tests performed by someone else and with<br />
different instruments. Some of these<br />
measurement-related aspects should be<br />
biennial 07-08<br />
construction &<br />
building industries<br />
The rheological behavior of building material<br />
suspensions plays a central role in the<br />
processability of cement bonded building<br />
materials and thus also in the rheological<br />
behavior of their properties in hardened state. On<br />
account of the widely spread application of very<br />
different admixtures and materials, the empirical<br />
test methods at disposal are, up to date,<br />
inadequate in their validity for assessing the<br />
rheological properties of these materials in fresh<br />
state. Investigations with the rotational rheometer<br />
– HAAKE RheoStress 600 – however, enable a<br />
comprehensive description of the rheological<br />
behavior of these materials.<br />
Different problems with the description of the<br />
rheological behavior of fresh building material<br />
suspensions will be briefly explained in this<br />
article. Finally, individual measuring methods for<br />
application notes & technical articles<br />
Experimental Influences on the<br />
Casson-Viscosity. The Casson<br />
Yield Point for Chocolate Testing<br />
food industries<br />
introduced and explained. However, the<br />
dependence of the flow properties of chocolate<br />
on their composition will not be discussed here.<br />
History<br />
From the rheological point of view chocolate is<br />
not an easy fluid: it is a suspension of cocoa,<br />
sugar and solid milk particles in a continuous fat<br />
phase. The mix of the substances and their<br />
interactions are strongly dependent on production<br />
and pre-treatment. The yield point of chocolate<br />
e.g. increases with longer tempering time since<br />
the cocoa butter is already partly crystallising (i.e.<br />
physical networks are forming which have to be<br />
broken off before a possible shearing). In order to<br />
obtain comparable results special attention has to<br />
be paid to the correct reproducibility of the pretreatment<br />
of the sample (there are tolerances<br />
even within the OICCC standard which can have<br />
their effects on the results, e.g. the cooldown/tempering<br />
times when filling the chocolate<br />
determining these properties, as well as the<br />
results that were won in the scope of an<br />
investigation program for the development of<br />
pumping-capable self-compacting light-weight<br />
concrete will be introduced.<br />
A full copy of “Rheological Properties of<br />
Fresh Building Materials” is available by<br />
quoting reference no: V-217<br />
into the rheometer). The differences occurring for<br />
thixotropic chocolate are especially dramatic:<br />
Here, the viscosity depends on the stirring time<br />
(shearing time).<br />
However, allowing sufficient time for preshearing<br />
can eliminate errors (the necessary time can be<br />
determined by test with a constant shear rate).<br />
Two successively recorded flow curves of a<br />
sample of a nougat cream available on the<br />
market (measuring time 3 min each) which also<br />
had a different history is shown. A slight decrease<br />
of the viscosity can be detected which can be the<br />
result of the small thixotropy but also of<br />
sedimentation or homogenizing effects by<br />
shearing.<br />
A full copy of “Experimental Influences on<br />
the Casson-Viscosity...” is available by<br />
quoting reference no: V-129<br />
6 www.rheologysolutions.com
application notes & technical articles<br />
How to Select the Most Suitable<br />
Sensor for your Application<br />
all industries<br />
The objective of this tech-note is to provide the<br />
information that will be very helpful in selecting<br />
which sensor is most useful for a particular<br />
material, deformation, or temperature range.<br />
Comparisons between different sensor systems<br />
give confidence to operators that they are really<br />
seeing material behavior and not some<br />
instrument artifact.<br />
Basically, three different sensor systems are<br />
compared, those sensors are: concentric cylinders<br />
(Couette system), cone and plate, and parallel<br />
plates.<br />
The utilities for a concentric cylinder sensor are:<br />
• Best for lower viscosities, η0 0.95 Good for<br />
suspension settling<br />
clean N1 impractical<br />
Cone and plate Best N1 High η: edge failure, loading difficult<br />
Best for G(τ, γ) Homogeneous Low η: inertia Evaporation<br />
β < 0.1 rad Need good alignment<br />
Parallel plates Easy to load viscous samples Nonhomogeneous: not good for<br />
Best for G’ and G” of melts, G(τ, γ) OK for G(τ) and η(γ) Edge<br />
curing Vary γ by η and Ω failure Evaporation<br />
(N 1-N 2)(γ)<br />
biennial 07-08<br />
7
application notes & technical articles<br />
Breaking Strength of Chocolate<br />
biennial 07-08<br />
food industries<br />
Chocolate appeals to all of<br />
our senses. We see the<br />
colour and the glossy<br />
surface of the bar, we smell<br />
the elusive flavours, we<br />
weigh it in our hands and<br />
feel how it melts, we hear it<br />
break and sense its<br />
resistance, and savour the<br />
taste. With so much<br />
“sensuality“, it is easy to<br />
forget how quickly the<br />
pleasure can be destroyed,<br />
if even just one of these<br />
properties is not as we<br />
expect it or are<br />
accustomed to.<br />
Even unconsciously, the breaking behaviour of<br />
chocolate plays an important role in influencing<br />
the consumer's impression. Chocolate experts<br />
can even evaluate the quality of a sample by<br />
breaking off a piece.<br />
<strong>Rheology</strong> plays an important role in several steps<br />
of chocolate production. The liquid chocolate<br />
formulation and the fats used can be<br />
characterised by their viscosities, yield stresses<br />
and solidification behaviours. These parameters<br />
are important for quality control and processing,<br />
and can be determined using rotational or<br />
oscillation measurements.<br />
Sensory properties as experienced during the<br />
melting process, or “mouth feeling“, can be<br />
described with the viscosity curves and the yield<br />
stress. However, these rheological parameters<br />
contain no information about the breaking<br />
strength of the final chocolate bar - and therefore<br />
a new method and new equipment are necessary<br />
to assess the resistance to break.<br />
The HAAKE MARS rheometer, manufactured by<br />
Thermo Scientific, features a highly sensitive<br />
normal force sensor and a very precise lift motor<br />
which allows the customer to apply controlled<br />
axial forces to the sample, pushing or pulling it,<br />
and to analyse its axial deformation.<br />
For example, with a new measuring geometry<br />
(figure 1), chocolate bars can be positioned on<br />
the rheometer and submitted to an increasing<br />
axial force until they break. The new measuring<br />
geometry consists of two parallel support bars<br />
which can be mounted onto a base plate in a<br />
variable distance from 1 to 7 cm. The sample lies<br />
on these bars and a user-defined piston can be<br />
lowered onto the sample, making possible<br />
bending, breaking and penetration tests.<br />
The new bending geometry was used to<br />
investigate the breaking behaviour of small bars<br />
of milk and dark chocolate. The distance of the<br />
support bars was fixed at 5 cm. The piston was<br />
cylindrical with a diameter of 6 mm. The piston<br />
was lowered at a rate of 1.3 mm/min.<br />
The comparison of the results in figure 2 shows a<br />
much greater deformation prior to breakage for<br />
the dark chocolate - it is more elastic than the<br />
milk chocolate. The normal force increases<br />
quickly and then falls to zero almost immediately<br />
(blue curve). This behaviour is typical for hard and<br />
brittle samples.<br />
Figure 1. Breaking test on a chocolate bar on the<br />
HAAKE MARS using the new bending geometry<br />
The milk chocolate is much “softer“, which can<br />
be seen in the moderate increase in the normal<br />
force (red curve). Only a third of the normal force<br />
required for the dark chocolate is needed to<br />
break the milk chocolate bar. The bar breaks in<br />
two steps: first it cracks to about the middle of its<br />
thickness before breaking completely.<br />
Using the new bending geometry for the HAAKE<br />
MARS rheometer, it was possible to characterise<br />
two types of chocolate with respect to their<br />
breaking behaviour. The axial deformation, the<br />
necessary normal force for breakage and the<br />
shape of the force/deformation curves can be<br />
used as evaluation parameters. With the same<br />
method, different formulations of a certain<br />
chocolate type may be analysed for an efficient<br />
product development, or the quality of different<br />
production lots can be controlled.<br />
Unlike subjective sensory tests which depend on<br />
the test person, the new method provides<br />
objective and reproducible results, independent of<br />
the analyst.<br />
Continued on page 9<br />
8 www.rheologysolutions.com
Figure 2. Breakage curves of half bitter (blue) and a mild (red) chocolate bars<br />
info@rheologysolutions.com<br />
Continued from page 8<br />
This new accessory significantly broadens the<br />
application range of the HAAKE MARS rheometer.<br />
The determination of additional relevant product<br />
properties can be performed on the same<br />
instrument used for the analysis of flow and<br />
visco-elastic behaviour of the samples - which is<br />
much more cost efficient than the purchase of a<br />
second specific instrument. The new geometry for<br />
bending and breaking tests is just one example of<br />
the wide range of application specific accessories<br />
available for the HAAKE MARS.<br />
A copy of this application note is available<br />
by quoting V-222.<br />
• application notes<br />
Solvent Trap & Double Cone System for<br />
Reproducible Results in Rheological<br />
Measurements of Low Viscous Volatile Fluids<br />
all industries<br />
Abstract<br />
Rheological measurements of low viscous volatile<br />
fluids require the control of the surrounding<br />
atmosphere of the measuring gap. The solvent<br />
trap creates a defined atmosphere around the<br />
measuring gap and the unique HAAKE double<br />
cone system provides a sealed system for low<br />
viscous samples.<br />
Introduction<br />
Low viscous water-based glues are a good<br />
example for volatile low viscous fluids. In order<br />
to get good measuring results in the low shear<br />
regime a controlled stress (CS) rheometer (HAAKE<br />
RheoStress 600) was used. To show the<br />
advantage of the solvent trap (Fig. 1) and the<br />
unique HAAKE double cone system (Fig. 2),<br />
measurements were performed with and without<br />
solvent trap and double cone system.<br />
A complete copy of this application note is<br />
available by requesting V-229<br />
biennial 07-08<br />
9
application notes & technical articles<br />
A New Definition in Reactor<br />
Temperature Control with the Highly<br />
Dynamic HAAKE DynaMax System<br />
The new DynaMax platform<br />
is designed to control the<br />
temperature in jacketed<br />
reactors more efficiently<br />
than other types of<br />
temperature control<br />
systems.<br />
DynaMax systems' “time to temperature” is the<br />
fastest in the industry. Temperature deviation<br />
control is accomplished with the help of Dynamic<br />
Heat Load Suppression (DHLS) technology. Most<br />
importantly, DynaMax systems are designed not<br />
only to increase yields, but also to safeguard<br />
equipment and the operator.<br />
Abstract<br />
biennial 07-08<br />
construction &<br />
building industries<br />
A numerical study was undertaken to provide an<br />
understanding of the influence of thermal<br />
conditions on friction build-up for a paraffinic<br />
mineral oil (PAM). Matlab 6.5 was used to<br />
perform computations for two lubricated infinite<br />
and rigid plates in relative motion, subjected to a<br />
Jacketed reactor vessels and temperature control<br />
units have been used for years to respond to and<br />
to maintain the temperatures of exothermic and<br />
endothermic reactions. These partially or fully<br />
automated systems can be found in such markets<br />
as Chemistry, Pharmaceutical, Biotechnology, and<br />
Food and Beverage. The typical uses for the<br />
jacketed reactors are:<br />
• product development<br />
• process development<br />
• process optimisation<br />
• safety investigations<br />
• scale up applications<br />
Maintaining precise temperature control is<br />
desirable to ensure the process is kept in control<br />
for repeatability and reproducibility. Both low and<br />
high pressure options are available to control<br />
double-jacketed reactor vessels. Correct selection<br />
of a temperature control unit can be difficult,<br />
transient load pulse. Two different rheological<br />
models, one nonlinear viscous and one nonlinear<br />
viscoelastic (Ree-Eyring), were used.<br />
From the friction coefficients calculated it is<br />
concluded that viscosity effects do not account<br />
for the phenomenon of decreasing friction<br />
coefficient with increasing maximum pressure of<br />
the loading pulse. It appears that an explanation<br />
for this phenomenon must be sought in the<br />
friction properties of the interface of the ruptured<br />
however, because there are many parameters<br />
that determine the heating/cooling requirements<br />
inside the reaction vessel. Here are some<br />
examples:<br />
• heat transfer efficiency of the jacketed vessel<br />
(glass, stainless steel etc)<br />
• flow rate of the heat transfer fluid through<br />
the jacketed vessel<br />
• flow state of the medium inside the reactor<br />
boiler (stirrer speed, flow resistance, etc)<br />
• temperature difference between medium<br />
inside the reaction boiler and heat transfer<br />
liquid<br />
• viscosity and thermal capacity of the heat<br />
transfer fluid<br />
Written by: Toni Kölbli, Thermo Fisher Scientific,<br />
Temperature Control, Karlsruhe, Germany<br />
A full copy of this application note is<br />
available by quoting TC06-01<br />
application notes & technical articles<br />
A Numerical Study of Temperature<br />
and Shear Flow in a Transiently<br />
Loaded Lubricant Film<br />
chemical & allied industries<br />
solidified lubricant. It is also concluded that the<br />
thermal properties of the lubricated medium<br />
present in the contact affect friction and the<br />
formation of shear bands.<br />
Keywords: EHD, TEHL, transient, viscoelastic,<br />
nonlinear, rheology, lubricant, friction,<br />
thermodynamic, heat, equation.<br />
A full copy of the paper is available by<br />
quoting reference no. RF: 180902-se-01<br />
10 www.rheologysolutions.com
application notes & technical articles<br />
A New Approach to Rheological<br />
Modeling of an Electrostatic Ash<br />
and Water Mixture - Quadratic Law<br />
Abstract<br />
mining industries<br />
In the paper a new rheological model for an<br />
electrostatic ash and water mixture flow is<br />
proposed. Fundamental equation of the<br />
rheological model was used to determine the<br />
relationship between the shear stress and the<br />
Abstract<br />
Today in modern polymer plants online quality<br />
control is done automatically and alarming the<br />
operators immediately so that the operators can<br />
react and avoid more damage to the final<br />
product. This “close loop”-concept also allows a<br />
grading of the pellet lot.<br />
The Film producers, the customers of the polymer<br />
plants, also use web inspection systems to<br />
control their final product quality, the quality of<br />
the raw materials and also their process<br />
parameters.<br />
Between both control concepts exist some<br />
interrelationships and also problems, because the<br />
environment parameters are different. This<br />
relative correlation and the impact for the polymer<br />
and film producers will be discussed with<br />
practical examples.<br />
info@rheologysolutions.com<br />
shear rate as well as the equation of a velocity<br />
profile for a flow through a straight pipe.<br />
Experimental results obtained from a capillary<br />
viscometer were used as the basis to determine<br />
the parameters for the proposed model by the<br />
nonlinear regression analysis.<br />
With the Quadratic law a numerical analysis of a<br />
mixture flow through a capillary pipe with the<br />
This paper was written and presented at the<br />
TAPPI European PLACE Conference 2007 in<br />
Athens on May 14 - 16 by:<br />
Oliver Hissmann - Dipl.-Oec., MBA (USA) ,<br />
Sales Manager<br />
OCS Optical Control Systems GmbH<br />
Email: hissmann@ocsgmbh.com<br />
A full copy of the paper is available on<br />
request by quoting OCS004<br />
finite volume method was performed. Derived<br />
equations for the velocity profile, shear stress and<br />
shear rate were validated through comparison of<br />
numerically obtained and theoretical results.<br />
Finally the comparison between the Quadratic law<br />
and Power law is presented.<br />
A full copy of the paper is available by<br />
quoting reference no. RF- 030902-SI-01<br />
application notes & technical articles<br />
Online Quality Control of Polymers<br />
and Extruded Films<br />
polymer industries<br />
High Speed Pellet Scanning System PS200C from<br />
OCS. The online pellet scan systems inspect the<br />
transparent or opaque granules on a vibrating<br />
channel or moving belt and detect discolouration<br />
and foreign particles. After inspection these<br />
defects can be sorted out into a separate<br />
container. The good material can be fed back into<br />
the process. These systems reach throughputs up<br />
to 250 kg/hr<br />
biennial 07-08<br />
11
application notes & technical articles<br />
<strong>Rheology</strong> as a Tool for Immiscible<br />
Polymer Blends Characterisation:<br />
Interfacial Tension and<br />
Compatibilisation<br />
Polymer blends have gained an increasing<br />
popularity in the field of polymer science and<br />
industry during the last thirty years. The growth in<br />
the use of polymer blends is mainly due to their<br />
ability to combine the properties of their phases<br />
in a unique product, making polymer blends<br />
broadly employed in automobile, aerospace,<br />
packing, and general goods industries. Currently,<br />
about 40% of the world polymer market is<br />
involved with the production of polymer blends,<br />
representing trades of billions of US$ a year. The<br />
final properties of polymer blends are directly<br />
related to the quality of their morphology, which in<br />
turn depends on the rheological properties of the<br />
phases of the blend, on the composition of the<br />
blend, on the processing conditions of the blend,<br />
and on the interfacial tension between the<br />
polymers forming the blend. However, most<br />
polymer blends are incompatible, resulting in<br />
materials with coarse morphology, weak adhesion<br />
among phases and poor mechanical properties. In<br />
fact, the future of polymer blends is based on<br />
biennial 07-08<br />
polymer industries<br />
methods to achieve stable morphologies, so that<br />
the enhanced and optimized properties of<br />
polymer blends do not change during the product<br />
processing due to phenomena such as<br />
coalescence and breakup. This matter still<br />
remains an industrial challenge and is the object<br />
of intense research.<br />
Interfacial tension between molten polymers has<br />
received considerable experimental and<br />
theoretical attention due to its implication in<br />
several industrial applications such as coating,<br />
composites and especially in polymer blends.<br />
Interfacial tension is the single most accessible<br />
parameter that describes the thermodynamic<br />
state and structure of an interface in polymer<br />
blends, therefore directly related to compatibility<br />
and hence morphology of polymer blends. Also,<br />
interfacial tension can be considered as a key<br />
parameter that measures the state of miscibility<br />
between incompatible polymers. The compatibility<br />
between the phases of a blend can be improved<br />
by the addition of compatibilisers which result in<br />
a finer and more stable morphology, better<br />
adhesion between the phases of the blends and<br />
consequently better properties of the final<br />
product. The exact definition of the optimum<br />
concentration of compatibiliser to be added is<br />
associated with the costs minimisation, since<br />
most compatibilisers are much more expensive<br />
than ordinary polymers.<br />
In this work, rheological measurements are<br />
shown to be a useful technique to study polymer<br />
blends. In particular, they can be used to<br />
determine the interfacial tension between<br />
immiscible polymers and define the optimum<br />
concentration of compatibiliser to be added to the<br />
blend. This study is based on the execution of<br />
small amplitude oscillatory shear (SAOS) tests in<br />
the linear viscoelasticity region of the materials.<br />
The determination of interfacial tension is related<br />
to the study of relaxation spectrum of a polymer<br />
blend, which is a result of the contribution of the<br />
phases and the interface. The definition of the<br />
concentration of compatibiliser is determined<br />
studying the applicability of time-temperature<br />
superposition (TTS) for the blend as a function of<br />
compatibiliser concentration.<br />
A full copy of the paper is available by<br />
quoting reference no. RF- 110902-br-01<br />
application notes & technical articles<br />
Rheological and Microstructural<br />
Analysis of a Model Rennet Casein<br />
Gel as Influenced by Cooling Rate<br />
food industries<br />
Cooling is a final process during process cheese<br />
production and is therefore critical when<br />
determining the texture and functional properties<br />
of the product. It is well established that a slower<br />
cooling yields a firmer cheese. However, there is a<br />
lack of quantitative description of this operation,<br />
and the mechanism behind the observation is<br />
needed to better control the cooling process. The<br />
rheological data for process cheese cooled at<br />
different rates was quantified and was consistent<br />
with the industrial observation. To illustrate<br />
physical changes during cooling, rennet casein<br />
gels were studied as our first step in<br />
understanding the cooling effects on process<br />
cheese texture and microstructure. A similar trend<br />
in storage modulus to process cheese was<br />
observed when the casein gels were cooled at<br />
different rates. To explain this behavior, a<br />
schematic illustration was used as the physical<br />
bases for microstructure of colloidal gels that can<br />
result in different rheological properties. Fractal<br />
dimension, floc size, and floc order in the protein<br />
network were treated as three possible variables.<br />
The theory developed by Shih et al. (1990) was<br />
used to determine the floc fractal dimension, and<br />
a confocal laser scanning microscope observed<br />
the floc size and order. The results showed that<br />
the floc fractal dimension and size were not<br />
significantly different when casein gels were<br />
cooled at different rates. However, the cooling did<br />
impact floc arrangement in the protein network. A<br />
higher order at a slower cooling rate resulted in a<br />
higher storage modulus, a smaller limit of linear<br />
viscoelastic range, and an increase in gelation<br />
temperature. The rheological data were consistent<br />
with the microscopic images, and the<br />
hypothesised variables sufficiently explained the<br />
physical changes in casein gels during cooling at<br />
different rates.<br />
A full copy of the paper is available by<br />
quoting reference no. RF- 200902-US-01<br />
12 www.rheologysolutions.com
application notes & technical articles<br />
Thickening of Electrostatically<br />
Stabilised Latices by Ethyl Acrylate-<br />
Methacrylic Acid Copolymers with<br />
Various Molecular Weights<br />
surface coatings industries<br />
Electrostatically stabilised lattices having various<br />
sizes were used to study the thickening of alkalissolutable<br />
ethyl acrylate-methacrylic acide<br />
copolymer (50 wt. % of the acid; MW = 0.78 x<br />
105, 4.36 x 105 and 11.6 x105). It was found<br />
that the effect increases with the molecular<br />
application notes & technical articles<br />
Dynamic Master Curves of Polymer<br />
Modified Asphalt from Three<br />
Different Geometries<br />
Abstract<br />
construction &<br />
building industries<br />
Polymer modified asphalt is highly temperature<br />
sensitive material. To obtain the master curves of<br />
dynamic material functions, for this material, one<br />
has to perform the testing over the temperature<br />
interval from -30ºC to at least 90ºC. Since the<br />
info@rheologysolutions.com<br />
weight of the copolymers and with the decreasing<br />
size of the latex particles. The pronounced<br />
tendency towards non-dredging flocculation and<br />
phase separation suggest that the thickening<br />
effect of the materials results from depletion<br />
(volume restriction) flocculation rather that<br />
depletion stabilisation. The role of the effective<br />
volume fraction of the dissolved copolymer as a<br />
variable which controls the rheological properties<br />
polymer modified asphalt undergoes the transition<br />
from a glass-like to the Newtonian-like material,<br />
in this temperature range, the benefit of using the<br />
three testing geometries is studied, here. The<br />
geometries used were: plate-plate (for the mid<br />
range temperatures); torsion bar (for the low<br />
temperatures) and bob and cup (for the high<br />
temperatures). The advantage of the combination<br />
of these three geometries is discussed. Stress<br />
and strain controlled rheometers were used to<br />
of the thickened lattices was tested<br />
experimentally.<br />
Keywords: Electrostatically stabilized lattices, Ethyl<br />
acrylate-methacrylic acid copolymers,<br />
Flocculation, Rheological properties, Thickening<br />
A full copy of the paper is available by<br />
quoting reference no. V-26<br />
conduct all dynamic experiments. Master curves<br />
obtained by these geometries cover up to 20<br />
decades of the reduced frequency.<br />
Keywords: Polymer modified asphalt, dynamic<br />
material functions, time temperature<br />
superposition, different geometries.<br />
A full copy of the paper is available by<br />
quoting reference no. RF- 110902-JO-01<br />
application notes & technical articles<br />
Characterisation of the Thixotropic<br />
Behavior of Semi-Solid Foodstuffs<br />
Abstract<br />
food industries<br />
Many food products exhibited the thixotropic<br />
behavior, in which, the apparent viscosity of<br />
material decreases with time of shearing at<br />
constant shear rate.<br />
The structural kinetic model (SKM) was used to<br />
characterise the thixotropic behavior of three<br />
different kinds of food products. Foods selected<br />
for analysis represent the fluid and semisolid food<br />
materials. They include milled sesame,<br />
concentrated yogurt and mayonnaise. The<br />
structural kinetic model postulates that the<br />
change in the rheological behavior is associated<br />
with shear-induced breakdown of the internal<br />
structure of the food product. This model for the<br />
structure decay with time at constant shear rate<br />
assumes nth order kinetics for the decay of the<br />
material structure with a rate constant, k. The<br />
dependence of the degree and the extent of<br />
thixotropy of the materials on the temperature,<br />
composition and shear history of the food product<br />
was determined.<br />
Key words: structural kinetic model, milled<br />
sesame, concentrated yogurt, mayonnaise,<br />
thixotropy.<br />
A full copy of the paper is available by<br />
quoting reference no. RF -110902-JO-01<br />
biennial 07-08<br />
13
application notes & technical articles<br />
Correlation Between Mixer Tests<br />
and the Extrusion Behaviour of<br />
PVC Dry Blends<br />
Abstract<br />
This report describes the correlation between<br />
measurements done on a laboratory mixer with<br />
PVC Dry Blends and their processing behaviour<br />
on a counter-rotating twin screw extruder.<br />
Introduction<br />
On July 1st, 2006, the EU Directive 2002/95/EG<br />
(RoHS-Directive, Restriction of Hazardous<br />
Substances“) was put into force. It restricts<br />
producing and trading of products containing i.e.<br />
lead, mercury and cadmium.<br />
Because a lot of PVC compounds still contain<br />
lead as stabilising media, there is urgency for the<br />
PVC industry to replace these stabilisers by less<br />
dangerous materials like CaZn stabilisers.<br />
Changing the formulation of a PVC compound by<br />
using a new stabiliser, always takes the risk that<br />
also the production behaviour will change. The<br />
reason behind this is the fact that stabilisers also<br />
work as a lubricant. So the change of stabilisers<br />
will influence the fusion behaviour of the PVC<br />
compound. To make sure that the PVC compound<br />
keeps its processing properties it is necessary to<br />
adapt the whole compound formulation.<br />
biennial 07-08<br />
polymer industries<br />
The most common tool to check the fusion<br />
behaviour of PVC compounds is the laboratory<br />
mixer test. It is an easy and reliable method to<br />
characterise the fusion and degradation behaviour<br />
of PVC compounds.<br />
The samples used for this investigation were<br />
three PVC Dry Blends with new lead free<br />
formulations.<br />
Materials and Methods Polymer:<br />
Three samples of a PVC Dry Blend with different<br />
CaZn-Stabilisers<br />
Test arrangements Mixer Test:<br />
• Torque-rheometer: RheoDrive 4<br />
• Double range torque CAN sensor<br />
• Analysis software PolySoft OS<br />
• Mixer Rheomix600 OS<br />
• Roller Rotors<br />
• Pneumatic feeding ram<br />
Extruder Test:<br />
• Laboratory twin screw extruder:Rheomex<br />
CTW100 OS<br />
• Extruder screws: Standard screws<br />
• Sheet die 50 x 1.0 mm<br />
• Hopper with vibrator<br />
• Melt-pressure sensors<br />
HAAKE Laboratory Mixer<br />
application articles<br />
Rheological Characteristics<br />
of Toothpaste<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
Certain product properties<br />
of toothpastes can be<br />
successfully quantified<br />
using rheology tests.<br />
In many cases it is possible to make appropriate<br />
adjustments to the rheology during the<br />
development of new products. This eliminates the<br />
need for expensive storage tests and saves costs.<br />
COSSMA is published by Health & Beauty<br />
Business Media GmbH, and in their September<br />
2009 issue the article “Rheological<br />
Characteristics of Toothpaste” written by Dr. Han-<br />
Michale Petri et al. Thermo Fisher Scientific,<br />
HAAKE Laboratory Extruder<br />
A complete copy of this application note is<br />
available by requesting LR-60<br />
Process Instruments, Karlsruhe, Germany will be<br />
published.<br />
Details on COSSMA can be viewed on their<br />
website www.cossma.com<br />
A copy of the full paper as a PDF can be<br />
obtained from <strong>Rheology</strong> <strong>Solutions</strong> as<br />
a PDF by quoting HA042.<br />
14 www.rheologysolutions.com
application notes & technical articles<br />
Evaluating the Plasticisation Process<br />
of Different Soft-PVC Samples<br />
polymer industries<br />
Abstract<br />
A HAAKE PolyLab OS torque rheometer, equipped<br />
with a Mixer was used to test four different soft<br />
PVC samples. The type and amount of plasticizer<br />
was varied. The corresponding torque curves<br />
helped to differentiate the formulas. The PolySoft<br />
Mixer data evaluation is explained in detail in this<br />
application note, and valuable hints are given for<br />
substituting PVC blend ingredients, e.g.<br />
plasticisers, stabilisers.<br />
Introduction<br />
PVC blends are complex mixtures of PVC<br />
particles, fillers, lubricants,stabilisers and<br />
plasticizers. They are used to provide unique<br />
properties to a wide range of end products.<br />
However, manufacturers are often forced to<br />
modify these complex recipes due to<br />
technological advances, cost pressures or<br />
regulatory requirements. For example, two EU<br />
directives came into force, 2002/95/EG (RoHS)<br />
restricting hazardous lead stabilizers in the waste.<br />
CaZn systems now are well investigated, also in<br />
Mixers tests. Another example is the<br />
precautionary EU regulation on phthalate<br />
plasticizers in children’s toys which was widely<br />
discussed in the press.<br />
Plasticisers are used in the PVC industry to soften<br />
the product.<br />
Approximately 100 different plasticizers are in<br />
use, which represents an estimated 7 billion EUR<br />
market. The type and amount of plasticizer have a<br />
major influence on the melt and processing<br />
behaviour when investigating alternate blends. In<br />
addition to tests on the final product, small-scale<br />
tests in a mixer are advisable before starting<br />
production. The mixer test is used for quality<br />
control during production.<br />
The HAAKE Rheomix system offers a quick<br />
method to characterize the influence of<br />
plasticizers on the plasticization and flow process<br />
of PVC dry blends. Using HAAKE Polysoft OS<br />
Software for mixer tests, the evaluation<br />
and comparison of different samples is quite<br />
quick and easy. Different routines are available,<br />
and it is also possible to create customised<br />
evaluation methods. Maxima, minima, points of<br />
inflection, thresholds and slopes can easily be<br />
calculated from all measurement data curves.<br />
info@rheologysolutions.com<br />
HAAKE PolyLab OS Torque Rheometer<br />
A complete copy of this application note is available by requesting LR-59<br />
biennial 07-08<br />
15
application notes & technical articles<br />
What Happens When Rheological<br />
Properties Change?<br />
Looking into rheological properties with simultaneous<br />
collection of microscopic images<br />
To gain information about the<br />
reasons for certain changes in<br />
rheological properties, a new<br />
special module for the HAAKE<br />
MARS has been developed.<br />
biennial 07-08<br />
polymer industries<br />
food industries<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
chemical & allied industries<br />
surface coatings industries<br />
It combines a temperature control unit for<br />
cone/plate- and plate/plategeometries<br />
with a state-of the- art microscope. The<br />
RheoScope module is presented and example<br />
data from different applications is shown.<br />
<strong>Rheology</strong> is a”macroscopic“method, which tells<br />
us how a material behaves under given conditions<br />
but never tells us why. For an understanding<br />
about the reasons why a certain behaviour<br />
occurs, we need to combine rheology with a<br />
“microscopic method“ able to look into the<br />
structure of the material.<br />
Examples for such techniques complementing<br />
rheological measurements are GPC, thermal<br />
analysis, (FT)IR or microscopy. Running two<br />
independent measurements on different<br />
instruments, however, doubles instrument time<br />
application notes & technical articles<br />
Rheological Characterisation<br />
of Asphalt Binders<br />
construction &<br />
building industries<br />
The bitumen binders used in<br />
asphalt are playing a crucial<br />
role for the performance of the<br />
asphalt.<br />
Today, 25% of the binders are polymer modified<br />
bitumen (PmB), providing a more sophisticated<br />
performance and a wider temperature range than<br />
pure bitumen does. The future share of PmB is<br />
likely to grow due to environmental regulations,<br />
due to a higher quote of recycling asphalt and<br />
due to requests for lower temperature processing<br />
e.g. for air port run ways.<br />
A first world-wide applied standard for asphalt<br />
binders was determined in the US Strategic<br />
Highway Research Program (SHRP) which was<br />
started in 1987. The results were published in<br />
1993, standardizing for rheological testing a<br />
Dynamic Shear Rheometer (DSR) to investigate<br />
and predict the fatigue behaviour (4°C and 40°C)<br />
and the behaviour at elevated temperatures<br />
(46°C and 82°C) with a steady state stepped<br />
temperature profile with steps of 6 degrees –<br />
corresponding to the performance grades.<br />
Moreover, the processability of the binders is<br />
tested at 135°C with a rotational viscometer or<br />
rheometer.<br />
In order to achieve the standard compliant<br />
temperature accuracy of ± 0.1 deg<br />
or better, particular SHRP temperature control<br />
and measuring time and often leaves a bit of a<br />
doubt whether the sample and its treatment<br />
before measuring have been exactly the same.<br />
The double effort of time and resources can be<br />
avoided by running two different methods on the<br />
same sample simultaneously, testing its<br />
macroscopic and its microscopic properties. The<br />
two resulting data sets can easily be correlated<br />
since they have been collected at the same time<br />
on the same sample.<br />
A complete copy of this application note is<br />
available by requesting V-228<br />
units were designed in the 1990s (Fig.2). Today,<br />
more and more measurements are made with<br />
Peltier temperature control units, e.g. for the<br />
screening of differently modified PmBs. The<br />
Peltier temperature control units provide a wider<br />
temperature range – also facilitating the relevant<br />
sub ambient temperatures.<br />
When bitumen or PmB is subjected to cooling, it<br />
shows exceptionally strong shrinkage leading to<br />
higher forces than the already high forces that<br />
are brought about by shrinking thermoplastics.<br />
The shrinkage of asphalt binders may lead to<br />
quality issues and it is therefore of interest to<br />
determine the occurring normal force and the<br />
shrinkage in micrometers.<br />
A complete copy of this application note is<br />
available by requesting V-225<br />
16 www.rheologysolutions.com
• application notes & technical articles<br />
QC Measurements for Liquid Food<br />
Products and Packaging<br />
polymer industries<br />
food industries<br />
Abstract<br />
Production quality and uniformity in food<br />
processing and its subsequent packaging is<br />
closely related to good quality control (QC) during<br />
the manufacturing process. In order to achieve<br />
high quality merchandise with minimal production<br />
losses, good process control and monitoring is<br />
critical. This is true for production of both the food<br />
product itself, the packaging, and of course for<br />
putting the former inside the latter efficiently.<br />
Laboratory and on-line systems are capable of<br />
delivering solutions for QC monitoring, and in<br />
cases where extra information (related sometimes<br />
to product development, and not to QC) about the<br />
flow properties are unnecessary, an online option<br />
can be the most useful.<br />
On-line systems often provide streamlined data,<br />
showing changes in more limited criteria for the<br />
product during the process. In this way corrective<br />
action can be quickly taken, minimising potential<br />
for waste and reprocessing. Laboratory<br />
instruments, designed for quick data collection<br />
(only a few seconds or minutes) and intuitive<br />
understanding of the data can also be useful in<br />
this respect where no proven online alternative<br />
exists. On-line monitoring of shear viscosity is<br />
widely accepted for many kinds of materials<br />
including for liquid foods, and molten polymer<br />
packaging. In pipe or in-tank probes can closely<br />
monitor the shear viscosity of the material in-situ,<br />
allowing operators and engineers to take<br />
appropriate action to maintain the specifications of<br />
the food product. These probes can also be<br />
mounted at the die end of an extruder, to monitor<br />
the viscosity of molten polymer before the<br />
moulding of packaging. Post-extrusion, the quality<br />
of the packaging material can be monitored<br />
optically to detect, catalogue and notify when user<br />
defined flaws exist in the packaging material (eg<br />
fish eyes, pinholes, dark/light spots etc). For filling<br />
a liquid food into a package (by pouring, squirting,<br />
spraying etc), extensional viscosity often<br />
dominates the process. Unfortunately, there is no<br />
proven on-line method for monitoring the<br />
extensional viscosity of foods as they are<br />
dispensed from above into their packaging.<br />
Fortunately a novel, simple and quick laboratory<br />
technique has been developed for exactly this<br />
purpose – measuring the relative impact of the<br />
extensional properties of a liquid. In this way the<br />
product and the packaging can be monitored<br />
on-line right through the process, until the product<br />
has safely been deposited in its packaging<br />
Introduction<br />
Several products exist today for testing in the<br />
laboratory, both for QA and for product development.<br />
Laboratory testing for product quality in the<br />
food industry can include rheometers and<br />
viscometers, to measure liquid flow properties<br />
such as yield stress, viscosity and elasticity under<br />
different shear flow conditions. These instruments<br />
can also measure the flow properties of packaging<br />
materials, eg molten plastics etc, to ensure that<br />
they can be properly moulded etc. Testing of solid<br />
like properties in the laboratory is possible for both<br />
foods and their packaging with uniaxial testing.<br />
Miniature uniaxial testers – texture analysers –<br />
can be used to objectively quantify textural<br />
properties of a food, while units with larger<br />
capacities can also be used to investigate the<br />
tearing, stretching, crushing etc of the finished<br />
packaging product. Often, during filling, a liquid is<br />
poured, squirted, sprayed or otherwise dispensed<br />
into the package.<br />
For some materials ‘stringy’ strands hang from the<br />
nozzle and soil the packaging, necessitating an<br />
extra process step to clean the packaging. This<br />
stranding is related to the extensional viscosity of<br />
the material (completely different to the shear<br />
viscosity measured by rotational viscometers).<br />
Recently developed techniques now enable these<br />
extensional properties to be properly measured in<br />
the laboratory using extensional rheometers.<br />
Laboratory analyses are good solutions for<br />
material characterisation and in many cases can<br />
not be otherwise replicated online. However,<br />
during production it is sometimes preferable to<br />
have an on-line system for QC, so that any<br />
deficiencies in the product or its packaging can be<br />
detected as quickly as possible. This technical<br />
note seeks to explore and to explain on-line<br />
viscosity monitoring, online quality control for<br />
packaging film and ingredients and a novel<br />
laboratory technique for monitoring the extensional<br />
properties of liquids to diagnose excessive<br />
stranding.<br />
A complete copy of this article is available on<br />
request by quoting Rheo051.<br />
• application notes & technical articles<br />
The Rheological Properties of a Copper<br />
Concentrate Slurry: From Surface Chemistry<br />
to Pipeline Transport<br />
mining industries<br />
The rheological properties of a copper concentrate<br />
slurry produced from a real mining operation have<br />
been investigated. In particular, the yield stress<br />
and viscosity of the slurry was measured after<br />
various chemical treatments were used to alter the<br />
surface chemistry and thus, interactions between<br />
info@rheologysolutions.com<br />
the particles within the slurry. These chemical<br />
treatments are: (1) the addition of acid and (2) the<br />
addition of polyphosphate or naphthalene<br />
suffocate formaldehyde condensate (dispersants).<br />
The changes in surface chemistry of the slurry<br />
under the various chemical treatments were<br />
investigated by X-ray photoelectron spectroscopy<br />
(XPS) and used to describe the changes in the<br />
observed rheological properties. The rheological<br />
data collected was then utilised to calculate the<br />
energy required to pump the slurry down a<br />
pipeline under the various different chemical<br />
regimes. Finally, a simple analysis of the reagent<br />
cost against energy price was used to compare<br />
the financial viability of each scheme.<br />
A complete copy of this article is available on<br />
request by quoting RF-3000702-AU-01.<br />
biennial 07-08<br />
17
• application notes & technical articles<br />
Wet-Shotcrete of Refractory Castables<br />
construction & building<br />
industries<br />
mining industries<br />
In recent years, the refractory<br />
industry has focused much<br />
effort on discovering novel<br />
techniques for castable<br />
installation that combine<br />
high placing rate and low cost<br />
while maintaining final material<br />
properties.<br />
The use of versatile and automated placing<br />
methods such as pumping of self-flowing<br />
castables and shotcrete has been encouraged to<br />
replace the traditional vibration moulding<br />
technique.<br />
Based on these aspects, wet shotcrete is highly<br />
interesting from a technological standpoint,<br />
particularly for the lining of large areas and/or for<br />
the repair of damaged surfaces.<br />
The technique consists of pumping the castable<br />
from the miser to the pipeline nozzle, where<br />
high-pressure compressed air is injected so as to<br />
project the pumped castable onto the surface to<br />
• application notes & technical articles<br />
Rheological Behaviour of Automotive<br />
Paint Systems<br />
surface coatings industries<br />
Modern Characterisation<br />
Methods Show Good<br />
Correlations to Observable<br />
Effects<br />
biennial 07-08<br />
be covered. This promotes a spray flow that<br />
ensures a high installation rate and the formation<br />
of a thick layer.<br />
The difficulties involved in the shotcrete technique<br />
relate mainly to the bonding of the material on the<br />
area to be lined. The primary condition for a<br />
successful operation is that the projected material<br />
does not flow over the back lining refractory<br />
surface, and this requires a sudden loss of the<br />
castable’s fluidity. Traditionally, this effect is<br />
achieved by the controlled use of cement settling<br />
accelerators, which are also injected into the<br />
nozzle.<br />
Although they ensure the material’s cohesion,<br />
conventional accelerators such as sodium silicate<br />
and aluminium sulfate usually deteriorate the<br />
mechanical properties of castables at high<br />
temperatures. Therefore, proposals have been<br />
made for novel additives based on distinct<br />
concepts to promote the rapid reduction of<br />
castable fluidity.<br />
In most bases, material waste is generated during<br />
shotcrete application due to the so-called rebound<br />
effect. This wastage occurs when a portion of the<br />
sprayed castables, which may amount to as much<br />
as 30%, fails to adhere to the applied surface. The<br />
rebound effect, which is also enhanced by the use<br />
of accelerators, can be minimised by selecting<br />
additives that simultaneously impart adhesive and<br />
In this paper the most important measuring<br />
methods for studying the rheological behaviour of<br />
modern paint systems (oscillation tests,<br />
determination of low yield points) are described.<br />
These methods were at first used to describe the<br />
rheological/physical properties of model<br />
polyurethane micro gels. The measured values for<br />
storage modulus, phase shift and yield point in<br />
waterborne Pearle scent/coloured pigment<br />
systems were compared with flop-index values.<br />
The results show good correlations between the<br />
plastic characteristics to the castable, resulting in<br />
homogeneous and cohesive linings, even when<br />
successive layers are applied<br />
In addition to the intrinsically complex pumping<br />
operation, wet-shotcrete applications must also<br />
take into account: (a) an abrupt increase in the<br />
castable shearing rate and the injection of<br />
additives, controlled by the air rate supplied in the<br />
nozzle, and (b) the material’s adhesion and<br />
consolidation on the surface.<br />
The conventional testing techniques, however do<br />
not properly evaluate shotcrete castables, given<br />
the rheological behaviour of these castables under<br />
similar shearing conditions during their installation<br />
is not analysed. The traditional approaches focus<br />
mainly on the influence of additives on the<br />
castable’s consistency (fluidity measurements) and<br />
on post-setting properties.<br />
The main objective of the present study was to<br />
develop a novel shotcrete characterisation<br />
technique based on castable rheometry that<br />
simulates the material’s application. Commercial<br />
wet-shotcrete additives and other compounds with<br />
a high potential for this application were also<br />
evaluated using the new testing procedure.<br />
A complete copy of this article is available on<br />
request by quoting Rf-290802-BR-02.<br />
observable effect and the rheological parameters<br />
of the liquid paint.<br />
Also measurements of powder and electrode<br />
position coatings and clear coats with the<br />
oscillation technique to determine the viscositytemperature<br />
behaviour correlate well with<br />
technical properties of the final films.<br />
A complete copy of this article is available on<br />
request by quoting Rheo008TP.<br />
18 www.rheologysolutions.com
• application notes<br />
New Measuring Cell for UV Assisted<br />
Thermal Curing at Elevated Temperatures<br />
polymer industries<br />
food industries<br />
surface coatings industries<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
chemical & allied industries<br />
Introduction<br />
In industry thermal curing is used in a wide range<br />
of applications like powder coating, adhesives,<br />
sealants, soldering materials, inks, etc. Recently<br />
there is an increased interest in replacing thermal<br />
curing by UV assisted thermal curing in an effort to<br />
improve product properties, increase productivity<br />
and reduce production costs, for example by<br />
reducing the amount of energy needed for<br />
initiating the curing reaction, at the same time.<br />
For the development of, and measurements on,<br />
such kind of samples a new high temperature UV<br />
curing tool was developed for the HAAKE MARS<br />
rheometer.<br />
The new UV curing tool for the CTC oven as well<br />
as selected results of measurements on different<br />
adhesives are presented.<br />
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info@rheologysolutions.com<br />
Instrumentation<br />
Rheometer<br />
Rheological properties (G’, G” etc.) were measured<br />
using the HAAKE MARS rheometer in combination<br />
with CTC environmental test chamber for the<br />
temperature control.<br />
UV curing tool<br />
The new UV curing tool is a modular extension for<br />
the existing CTC test chamber (temperature range<br />
-150°C up 600°C.)<br />
The UV curing tool consists of a hollow lower shaft<br />
with a removable light guide. The light guide can<br />
be connected to any suitable commercially<br />
available light source. Mounted on top of the light<br />
guide a removable and disposable quartz glass<br />
plate forms the lower part of the measuring<br />
geometry. The upper plate consists of a disposable<br />
aluminium plate mounted on a special shaft.<br />
Figure 3a: UV Curing cell integrated<br />
UV curing tool<br />
UV light<br />
biennial 07-08<br />
Rheometer<br />
drive shaft<br />
CTC shell<br />
19<br />
Disposable upper<br />
aluminium<br />
Sample<br />
Disposable lower<br />
quartz glass plate<br />
Hollow lower shaft<br />
UV light guide<br />
Figure 2: Schematic drawing of UV curing cell<br />
The UV light source can switched on/off by means<br />
of a trigger signal from the rheometer which is<br />
controlled by the rheometer software. By<br />
programming an automatic measuring routine the<br />
sample can first be pre-cured by the UV light and<br />
then thermally cured using the CTC oven.<br />
continued on page 20
• application notes<br />
Rheological Methods for Determining<br />
Molecular Weight & Molecular Weight<br />
Distribution<br />
polymer industries<br />
food industries<br />
surface coatings industries<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
chemical & allied industries<br />
Figure 4a: Detailed view of the in CTC new UV<br />
curing cell<br />
New Measuring Cell<br />
for UV Assisted Curing<br />
continued from page 19<br />
Results<br />
Curing behaviour of an<br />
acrylic resin adhesive<br />
Figure 4 shows the UV curing process of an acrylic<br />
resin adhesive, which is used in the production flat<br />
panel displays, at a temperature of 20°C. UV light<br />
with a wave length of 360 nm and a light intensity<br />
of 500 mJ/cm 2 was applied to the sample for a<br />
duration of 4 min. The measurements were<br />
performed using a 10 mm diameter parallel plate<br />
measuring geometry. For this application no post<br />
heat treatment was necessary.<br />
biennial 07-08<br />
Abstract<br />
The molecular weight and molecular weight<br />
distribution (MWD) of linear polymers can be<br />
derived by using rheological methods. The<br />
mechanical excitation of polymers leads to a<br />
characteristic response of the material depending<br />
on its macromolecular structure. Using the HAAKE<br />
RheoWin software with optional tools like TTS<br />
(Time Temperature Superposition), Spectra and<br />
MWD (Molecular Weight Distribution) master<br />
curves, relaxation time spectra and molecular<br />
weight distributions can be easily generated out of<br />
dynamic tests (Oscillation frequency sweeps).<br />
Practical results are presented and discussed in<br />
this application report.<br />
A complete copy of this application note is available by requesting V-230<br />
Figure 4: UV curing behaviour of an acrylic resin<br />
adhesive without thermal curing<br />
After a waiting time of 15 min (in which the<br />
temperature was increased to 35°C) the glass<br />
transition temperature Tg of the cured sample<br />
was determined by gradually increasing the<br />
temperature from 35°C to 95°C. The Tg was<br />
found to be 74.5°C.<br />
Curing behaviour of an epoxy<br />
resin adhesive<br />
Figure 5 shows the UV and thermal curing<br />
behaviour of an epoxy resin adhesive which is also<br />
used in the production of flat panel displays. In this<br />
case UV light with a wave length of 360 nm and a<br />
light intensity of 500 mJ/cm 2 was applied to the<br />
sample for a duration of 7 min. A post heat<br />
treatment was used to improve the product<br />
properties in respect of adhesion and stiffness.<br />
Introduction<br />
A well-established method to measure the<br />
molecular weight distribution is the gel permeation<br />
chromatography. This conventional method<br />
however has some disadvantages, which are e.g.<br />
solubility of the polymer, expensive instruments,<br />
time-consuming procedure and less sensitivity for<br />
high molecular components. Accordingly<br />
rheological methods are an interesting alternative.<br />
The theoretical relationships between the<br />
molecular weight distribution and material<br />
functions that can be determined through rheology<br />
are well investigated. Powerful numerical methods<br />
have been developed, which together with PC<br />
technology provide a means to determine MWD<br />
from rheological measurements.<br />
Figure 5: UV curing behaviour of an epoxy resin<br />
adhesive with post thermal curing<br />
The measured normal force signal (up to 50 N<br />
with a 10 mm diameter plate!) shows that this<br />
sample under goes a rather large volume<br />
expansion with increasing temperature. This is<br />
something that should be accounted for during<br />
the production process.<br />
Conclusions<br />
The measurement result shows that modern<br />
rheometry is a versatile tool for analysing the<br />
properties of materials during UV curing and<br />
subsequent thermal curing. The curing behaviour<br />
of the sample and the mechanical properties of<br />
the final cured product could be determined in<br />
one continuous measuring job.<br />
A complete copy of this application note is<br />
available by requesting HA-047<br />
20 www.rheologysolutions.com
• application notes<br />
Small Scale Catheter Production<br />
polymer industries<br />
Abstract<br />
Catheters were produced of Polystyrene (PS) and<br />
Polycaprolactone (PCL). A PolyDrive extruder<br />
system, as stand alone extruder was used with the<br />
catheter die. For stable extrusion it was necessary<br />
to use a water bath and the take off system. By<br />
Pharma MiniLab – Small Scale<br />
Compounder for Pharmaceutical Research<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
Abstract<br />
Hot melt extrusion and continuous process leads<br />
to cost efficient production.<br />
In development of new drug/ excipients small<br />
scale extrusion systems reduce time to market<br />
and use comparable processes to production.<br />
Applications and products for development with<br />
the HAAKE Pharma MiniLab are described.<br />
Nanocomposities – Examples on<br />
Compounding of Nanoclay Blends<br />
in Twin Screw Extruders<br />
polymer industries<br />
Abstract<br />
This report describes practical examples of<br />
nanoclay – polymer compounds processed<br />
successful in the Karlsruhe PI Demo centre<br />
during 2006. Nanoclay was compounded with<br />
commercially available resins such as PP, PA<br />
info@rheologysolutions.com<br />
varying take off speed and output different sizes of<br />
the catheter were obtained..<br />
Introduction<br />
Catheters are widely used for medical applications,<br />
new developments focus on biodegradable<br />
materials and compounding of contrast media for<br />
x-ray depiction. Though the commercial products<br />
are highly sophisticated and produced on<br />
Introduction<br />
The pharmaceutical industry involves numerous<br />
batch processes. Recently a trend to continuous<br />
processes is visible as continuous processing has<br />
a couple of advantages. Especially the hot melt<br />
extrusion can produce more efficiently and with<br />
higher output. Furthermore allows the extrusion<br />
process the monitoring of processing parameter.<br />
As compounding takes place directly in the molten<br />
stage, aqueous solutions are avoided. Reduced or<br />
removed drying steps help to save energy.<br />
Extrusion is a predominant technique in polymer<br />
and ABS. Test setup and instrument parameters<br />
are given as a guide line.<br />
Introduction<br />
Nanomaterials enter the consumer market. The<br />
focus shifts from science to standard applications.<br />
For polymer based Nanocomposites the research<br />
is often driven by the automotive industry<br />
searching alternatives to bulk materials. Especially<br />
nanoclaypolymer blends are known to improve<br />
“pharma“ extrusion lines, proof of concept studies<br />
and first developments can be run on a standard<br />
PolyDrive single screw extruder. Obviously, in the<br />
same way a Poly-Lab OS with single screw<br />
extruder 19/25 OS can run the same application.<br />
A complete copy of this application note is<br />
available by requesting LR-58<br />
processing. Profiles, sheets and bags are<br />
produced as end products, compounds as<br />
intermediate products. Even in the huge<br />
installation of a petrochemical plant we see<br />
extruders producing LDPE, PP resins with an<br />
output of 40 t per hour. In pharmaceutical<br />
technology the extrusion is known for more than<br />
35 years. Developed in industries for products far<br />
less expensive on a kilogram basis the extrusion<br />
gives a key to survival under growing cost<br />
constraints.<br />
A complete copy of this application note is<br />
available by requesting LR-53<br />
nanoclaypolymer blends are known to improve<br />
material characteristics such as flame resistance,<br />
barrier properties or toughness. Decreasing prices,<br />
high availability, readymade Masterbatch, vast<br />
research work, make nanoclay compounds perfect<br />
systems to start development or assess a<br />
machines performance.<br />
A complete copy of this application note is<br />
available by requesting LR-62<br />
biennial 07-08<br />
21
• application notes & technical articles<br />
The influence of thickeners on the application<br />
method of automotive coatings and paper<br />
coatings – rheological investigations<br />
surface coatings industries<br />
Spraying automotive coatings<br />
and the application of paper<br />
coatings are industrial<br />
processes, in which<br />
elongational flows play an<br />
important role.<br />
As a result, the application behaviour of these<br />
fluids often cannot be sufficiently characterised<br />
with traditional shear experiments. Products with<br />
similar shear viscosities can have very different<br />
elongation properties.<br />
With the Thermo Scientific HAAKE CaBER 1<br />
extensional rheometer, a liquid filament is created<br />
that is stretched under the influence of surface<br />
tension. Using the decrease in the filament<br />
diameter as a function of time and the life of the<br />
filament, it is possible to characterise the<br />
elongational behaviour of low viscosity to pasty<br />
liquids in a simple way. The rheological properties<br />
of typical water-based automotive coatings and<br />
paper coatings are determined by the thickeners<br />
used and their interactions with the other recipe<br />
components. In the CaBER 1 experiment, different<br />
types of thickener display a characteristic<br />
decrease in the filament diameter as a function<br />
of time. Different break-up times are desirable,<br />
depending on the application.<br />
When automotive coatings are sprayed, short<br />
break-up times are advantageous in order to<br />
obtain the finest possible drop distribution.<br />
When paper coatings are applied with rollers,<br />
spraying and „misting“ should be prevented as<br />
much as possible, which means that formulations<br />
with long break-up times are advantageous.<br />
A full copy of the application note is available on<br />
request by quoting V-206.<br />
• application notes & technical articles<br />
Slurry rheology and pipeline transport<br />
properties, an overview<br />
surface coatings industries<br />
Slurry transport in the mining<br />
industry is a commonly used<br />
technique for moving partially<br />
and fully processed materials,<br />
and waste.<br />
Often this type of treatment is more economical<br />
and rapid than other transportation methods, such<br />
as those involving conveyor systems or haulage.<br />
Additionally, the materials on a mine-site are often<br />
slurried for processing, and pipeline transport is<br />
necessary.<br />
However frequently utilised, efficient slurry<br />
transport still poses serious engineering problems<br />
through the properties of the slurry. These<br />
include, but are not limited to, particle settling,<br />
attrition, pipe/fitting/impeller wear, degradation of<br />
flocculated or friable solids, and the pumpability of<br />
the slurry. In addition, the effects of these<br />
challenges can be exacerbated, or reduced by<br />
biennial 07-08<br />
process or environmental variables, such as<br />
temperature, pH or solids loading.<br />
In-transit particle settling leads to stratified flow,<br />
which in turn can cause uneven and excessive<br />
wear in the transport system, and in extreme<br />
cases, pipeline blockage due to solids build-up<br />
around fittings or inclined sections. Particle<br />
attrition has several drawbacks. Firstly, the<br />
product before the pump and pipe is not identical<br />
to that afterwards if the particles are friable, this<br />
may be a QC matter both for disposal and<br />
in-process. Secondly, changes in particle size<br />
distribution may affect the ability of the particles to<br />
remain suspended in the carrier fluid. Problems<br />
with the pumpability of slurries potentially include<br />
the fact that they often behave as a solid, e.g.<br />
when at rest, making it expensive to initiate<br />
pumping. Many fluids, including slurries have flow<br />
properties which depend on the ‘rate of deformation’<br />
(analogous to their flow-rate).<br />
Rheological techniques can help the engineer or<br />
technician to design for and manipulate<br />
processes. A range of instruments is available<br />
which measure the effects of solids loading,<br />
carrier fluid, particle size distribution and viscosity<br />
or pH modifiers on the propensity of particulate<br />
matter to flocculate, be suspended, settle etc.<br />
through a knowledge of the characteristic flow<br />
properties of the slurry. These rheometers and<br />
viscometers allow the engineer to directly measure<br />
and assess the causes and effects listed above.<br />
Physical quantities such as yield stress (the<br />
minimum force required for a slurry to flow),<br />
plastic viscosity (how ‘runny’ a slurry will be at a<br />
given laminar flow-rate), hysteresis (the changes<br />
in plastic viscosity and/or yield stress which are<br />
due, usually, to particle attrition or settling) can be<br />
better predicted with the appropriate equipment.<br />
Sensitive, high precision versatile equipment is<br />
available for repeatable and reliable measurement<br />
of all flow properties in the laboratory, and durable,<br />
precise, robust units for in the field use are also<br />
commercially available. These units have been<br />
shown to be of value for both QC and product<br />
development.<br />
A full copy of the application note is available on<br />
request by quoting Rheo013<br />
22 www.rheologysolutions.com
• application notes & technical articles<br />
Overview of rheology-based process<br />
challenges for the mineral processing<br />
industries<br />
surface coatings industries<br />
Mineral processing involves the<br />
transportation and processing<br />
of large quantities of materials.<br />
Mineral processing involves the transportation and<br />
processing of large quantities of materials.<br />
Combining solid materials with a carrier fluid<br />
(usually water) to create a slurry has long been<br />
popular in the industry, principally due to the<br />
increased efficiency and alacrity of mineral<br />
processing steps through use of a slurry, since the<br />
finely ground particles afford greater surface area<br />
exposure to the extracting medium. Also, the ease<br />
with which the particulate matter can be<br />
processed in this form is important for unit<br />
processes including grinding, classification,<br />
separation processes (settling, thickening,<br />
screening, filtration) and transport processes like<br />
pump/gravity flow through pipes and launders,<br />
mixing, etc.<br />
Slurry characteristics pose many engineering<br />
challenges. These characteristics include particle<br />
settling, pH, bulk/carrier fluid viscosity, particulate<br />
flocculation or dispersion, attrition,<br />
pipe/fitting/impeller wear, degradation of<br />
flocculated or friable solids and the pumpability of<br />
the slurry. The effects of these challenges can be<br />
further altered by process or environmental<br />
variables such as temperature or solids loading.<br />
Wet communition and classification can be<br />
effected by viscosity, particle size distribution, fines<br />
concentration etc. For example, hydrocyclone<br />
classification is effected by the presence of a yield<br />
stress (the minimum force required for a slurry to<br />
flow). Often, cut point increases and efficiency<br />
decreases with increasing yield stress. Separation<br />
processes are influenced by inter-particle<br />
attraction and viscosity (how easily the fluid flows<br />
once it is in motion). These variables may be<br />
manipulated through the addition of modifying<br />
agents to the slurry. The key effects of these<br />
additions should be monitored through changes in<br />
the rheological parameters of the slurry, which are<br />
directly related to process performance. In-transit<br />
particle settling causes uneven and excessive<br />
wear or complete blockage in the transport<br />
system. Particle attrition may be a QC matter both<br />
for disposal and in-process and, changes in<br />
particle size distribution may affect the ability of<br />
the particles to remain suspended. Problems with<br />
the pumpability of slurries include the high cost of<br />
initiating and continuing pumping of fluids with<br />
high yield stresses or viscosities.<br />
Rheological techniques can help assess process<br />
design and manipulation processes. A range of<br />
instruments is available to measure the rheological<br />
effects, through knowledge of the characteristic<br />
flow properties of the slurry. These rheometers<br />
allow the engineer to directly measure and assess<br />
the causes and effects listed above. Physical<br />
quantities such as yield stress, plastic viscosity<br />
and hysteresis (the changes in plastic viscosity<br />
and/or yield stress which are due, usually, to<br />
particle attrition or settling) can be quantified and<br />
predicted with the appropriate equipment.<br />
Sensitive, precise equipment is available for<br />
repeatable and reliable measurement of flow<br />
properties in the laboratory, and durable, robust<br />
units for in-the-field use are also available. These<br />
units are of value for both QC and product<br />
development.<br />
A full copy of the application note is available on<br />
request by quoting Rheo014<br />
• application notes & technical articles<br />
Improved torque sensitivity and normal<br />
force resolutions for routine measurements<br />
all industries<br />
The new HAAKE RheoStress<br />
6000 benefits from the latest<br />
MARS technology<br />
developments.<br />
The improved specifications are regarding two<br />
components, improved air bearing specifications<br />
and the change of the normal force sensor<br />
technology.<br />
The normal force sensor of the HAAKE RheoStress<br />
6000 is based on temperature-compensated<br />
info@rheologysolutions.com<br />
strain gauge technology and enables normal force<br />
measurements in the range of 0.01 to 50 N in<br />
both positive and negative direction.<br />
This technology offers the possibility to perform<br />
sensitive normal force measurements even on<br />
samples with low viscoelasticity.<br />
In addition the new sensor enables to control the<br />
normal force in the sample to compensate for<br />
sample shrinkage and expansion when measuring<br />
semisolids.<br />
The patented 4th generation air bearing in the<br />
HAAKE RheoStress 6000 is the result of more then<br />
25 years of experience with the design and<br />
manufacturing of porous carbon air bearings.<br />
The air bearing consists of three individual air<br />
bearings:<br />
• One axial air bearing that supports the motor<br />
shaft in the vertical (axial) direction and is<br />
responsible for excellent axial stiffness.<br />
• Two widely spaced radial air bearings that<br />
support the motor shaft in the radial direction<br />
and prevent the shaft from tilting.<br />
A full copy of the application note is available on<br />
request by quoting V-231.<br />
biennial 07-08<br />
23
• application notes & technical articles<br />
Correlation of misting during printing with<br />
extensional rheological investigations on<br />
offset printing inks<br />
surface coatings industries<br />
The tendency for misting<br />
on offset printing inks was<br />
examined on two samples<br />
using the rotational rheometer<br />
Thermo Scientific HAAKE<br />
RheoStress 600 and the<br />
extensional rheometer Thermo<br />
Scientific HAAKE CaBER 1.<br />
The results for the amplitude and frequency curve,<br />
the creep and recovery test and the flow curve<br />
measurement with the rotational rheometer do not<br />
correlate with misting during printing.<br />
With the rotational rheometer, it was possible with<br />
the aid of the filament break-up time to easily and<br />
quickly draw distinctions between different<br />
tendencies for misting with offset printing inks.<br />
A full copy of the application note is available on<br />
request by quoting V-208.<br />
• application notes & technical articles<br />
Cellulosic derivatives in capillary break-up.<br />
Influence of the MWD and gel particles<br />
Thermo Scientific HAAKE<br />
CaBER 1 extensional rheometer<br />
is able to detect slight differences<br />
in the MWD (molecular<br />
weight distribution) of blended<br />
polystyrene standards.<br />
biennial 07-08<br />
polymer industries<br />
However, the question remains if these results<br />
obtained on a standard system can be transferred<br />
to more complex polymers in solution like<br />
cellulosic derivatives?<br />
In order to control the adaptability of this method,<br />
commercially available, blended methylhydroxy<br />
ethyl celluloses (MHEC, e.g. used as thickener<br />
agent in construction materials) were<br />
characterised by uniaxial elongation in capillary<br />
break-up experiments with the CaBER 1<br />
extensional rheometer. The determined break-up<br />
and relaxation times t resp. τ were then<br />
correlated with the blending composition of the<br />
methylhydroxyethyl celluloses and hence with the<br />
high molar mass fraction of the sample.<br />
A full copy of the application note is available on<br />
request by quoting V-219.<br />
24 www.rheologysolutions.com
• feature article<br />
Recent developments in bench-top<br />
twin-screw compounders<br />
polymer industries<br />
Abstract<br />
Twin-screw compounders are widely used for<br />
dispersion of pigments and additives in the<br />
manufacture of masterbatch. This paper describes<br />
the availability small-scale twin-screw extruders<br />
together with a range of ancillary equipment, to<br />
assist the masterbatch producer in sample<br />
preparation, and testing of the product. It also<br />
describes the key element of heat transfer in<br />
scale-up from laboratory extruders to production<br />
plant.<br />
Introduction<br />
There are many new materials available for the<br />
formulator of Masterbatches, but how can these<br />
be investigated and new products developed in<br />
readiness for the eventual up-turn in the market?<br />
Before putting a new material into full-scale<br />
production, different formulations need to be<br />
tested and sample quantities made for customer<br />
evaluation.<br />
The presentation will describe some of these test<br />
methods, and in particular a new technique using<br />
an Optical System to evaluate dispersion in<br />
polymer films. It will also outline other test and<br />
sample preparation equipment that can be used<br />
directly on the end of the extruder.<br />
These include a simple blown film system;<br />
extrusion dies for sheet and ribbon, a screen life<br />
pressure filter test, and alternative pelletising<br />
methods.<br />
A simple PLC based data logging will be described<br />
that can be used to monitor results, and with links<br />
to a PC can be used for analysis and archiving of<br />
sample data.<br />
Finally, operation of small laboratory extruders,<br />
and what are the critical factors for a reliable<br />
scale-up to production plant will be discussed.<br />
Twin-Screw Mixing<br />
The melting and mixing process in a twin-screw<br />
compounder is a rapid process. The polymer is<br />
melted by the mechanical shear energy of the<br />
intermeshing screws. The narrow distribution of<br />
residence time in a twin screw means that all the<br />
material is subjected to a similar thermal history,<br />
giving very uniform product.<br />
info@rheologysolutions.com<br />
Filter Test<br />
The Thermo Scientific PRISM twin-screw Filter test<br />
system was described at Masterbatch 2002. The<br />
filter test technique will soon become a recognised<br />
standard in quality control. To apply this to the<br />
twin-screw compounder, a simple screen changer<br />
is bolted onto the extruder, and through the plc<br />
control and data logging, pressure increase over<br />
time is monitored, and using a computer can be<br />
matched to standards for evaluation.<br />
Film Equipment<br />
For the film producer, a blown film die with cooling<br />
tower and wind-up can be fitted to the extruder<br />
allowing direct preparation of blown film samples.<br />
A recent application of this equipment has been<br />
particularly useful in evaluating the film blowing<br />
properties of a biodegradable polymer, manufactured<br />
from renewable, natural raw materials.<br />
If the laboratory needs a thicker sheet of rigid or<br />
flexible film, different sheet dies can be fitted onto<br />
the EUROLAB to extrude sheets up to 170mm<br />
wide with thickness from 0.5 to 2.0mm.<br />
Dedicated cooling rolls are used to calibrate and<br />
cool the sheet with either a cutting table for rigid<br />
sheets or a wind-up spool for flexible films.<br />
Optical Quality Testing<br />
The Optical Quality Testing System measures the<br />
transparency of a film or sheet, and counts the<br />
number of embedded inhomogeneous particles<br />
continued on page 26 <br />
biennial 07-08<br />
25
continued from page 25<br />
and other impurities. By measuring the transmitted<br />
light through a polymer film, the CCD camera<br />
processes the image and identifies discontinuities<br />
in the film.<br />
The camera scans an area of 400 mm2 at a rate<br />
of 4 pictures per second, with a resolution to 60 μ<br />
m. There are options for higher resolution on a<br />
smaller area or scanning a larger area at a lower<br />
resolution.<br />
The results can be displayed and analysed on<br />
different formats. This first display logs the counts<br />
of different particle sizes over time.<br />
This analysis gives the distribution of particle sizes<br />
over the test.<br />
Finally this analysis shows the distribution of<br />
particles by size and frequency.<br />
Other applications of the twin-screw use the<br />
dedicated ancillary equipment that designed to<br />
make up the EUROLAB System.<br />
biennial 07-08<br />
Pelletising<br />
When samples are required in pellet form, then a<br />
strand die and traditional cooling bath and<br />
pelletiser are used. This system includes a variable<br />
length pelletiser, where the pellet length can be<br />
selected from 1mm to 3mm in 0.5mm steps. If<br />
mini-pellets are needed for micro-moulding, them<br />
a combination of high draw-down with high cutter<br />
rotation will give 1mm X 1mm pellets.<br />
When working with highly filled compounds, or<br />
water sensitive products, an air quench, face cut<br />
system is available. Here the product is cut on the<br />
face of the die, propelled into an air stream and<br />
conveyed to a cyclone for collection. This method<br />
is also very useful for new water sensitive,<br />
biodegradable polymers being studied today.<br />
Data Logging<br />
When many different materials need sampling, it is<br />
very useful to be able to record operating<br />
conditions so that reproducible samples can be<br />
prepared. This can be even more reliable if the key<br />
operating conditions can be recorded and stored<br />
as a recipe for future use. The touch screen<br />
interface and PLC control allow this to be done<br />
simply, with added security of password<br />
protection.<br />
Scale-up<br />
In any laboratory system, the operator is always<br />
concerned with scale-up to larger production scale<br />
equipment. Form our experience the most critical<br />
element in this scale-up, is heat transfer capability.<br />
Most twin-screw extruders are variable speed, and<br />
so shear rates can be matched between laboratory<br />
and production extruders. Residence time in the<br />
extruder depends on a combination of product<br />
feed rate and screw speeds. Because generally<br />
output is determined by the motor power installed,<br />
and that is usually scaled to the volume of the<br />
extruder, which again gives a good scale up.<br />
However, heat transfer in dependent on the<br />
surface area to volume ratio. This means that the<br />
ratio of surface area to volume is inversely<br />
proportional to the barrel diameter. i.e. if you<br />
double the diameter of the screws, then volume<br />
(and hence output) will increase by 8 times while<br />
surface area, and (hence heat transfer capability)<br />
will increase only 4 times.<br />
Surface Area, Free Volume<br />
relationships<br />
Conclusion<br />
In a modern masterbatch plant, quality control and<br />
product sampling are key factors in the efficient<br />
operation. By using small-scale extruders, fitted<br />
with suitable ancillaries, and with reliability in<br />
scale-up, the operator can have confidence in<br />
developing new materials and formulations. This<br />
paper has shown availability of such equipment.<br />
A copy of this article is available on request by<br />
quoting LR-51<br />
26 www.rheologysolutions.com
• application notes & technical articles<br />
Rheological measurements in the coatings<br />
industries – the last 60 years<br />
surface coatings industries<br />
Abstract.<br />
<strong>Rheology</strong> is the science of studying and predicting<br />
flow and deformation of matter. It has long been<br />
an important technique for verification of design,<br />
manufacture, storage, application and cure of<br />
coatings. As coatings formulations have increased<br />
in complexity, meeting diverse customer needs, so<br />
discriminatory testing techniques allowing different<br />
materials to be compared for all conditions has<br />
become crucial.<br />
For sixty years the industry has gradually moved<br />
from reliance on qualitative ‘guesstimates’ based<br />
on operator experience, to quantitative measurements.<br />
These quantitative techniques have<br />
included Ford and Zahn cups, still used in the field<br />
Published in Pure & Applied<br />
Chemistry. Vol. 68, No. 8, pp.<br />
1665-1682, 1996.<br />
© 1996 IUPAC<br />
Synopsis<br />
Blends of ethylene-vinyl alcohol copolymer (EVOH)<br />
and styrene-maleic anhydride copolymer (SMA)<br />
have been produced by reactive extrusion and<br />
characterised in terms of their rheology, phase<br />
morphology and the degree of covalent bonding<br />
interaction (ester linkages) between phases, as<br />
determined by FTIR.<br />
today, but which have been shown to be little more<br />
than rough estimates for the performance of<br />
rheologically complex materials, though they may<br />
still work well for Newtonian or near-Newtonian<br />
coatings. Simple Hoeppler (falling ball) or<br />
mechanically driven rotational devices such as the<br />
Krebbs or Stormer viscometers, and later<br />
Brookfield viscometers emerged, reducing much<br />
of the inaccuracy associated with cup-type<br />
measurements. They have proven themselves<br />
useful but there remains the problem that, if the<br />
material is non-Newtonian the measurements are<br />
not absolute, and data from the different<br />
instruments cannot be compared (the units of<br />
measurement are Krebbs Units, Brookfield Units,<br />
HAAKE Units etc).<br />
The ICI or “Cone & Plate” viscometers were the<br />
first to utilise a finite gap and viscometric<br />
geometry to measure absolute viscosity, but had<br />
the limitation of rotating at a fixed rpm, restricting<br />
the output of the viscometer to high shear<br />
applications only. Now that the science is maturing<br />
and high speed computing, combined with<br />
inexpensive electronics and manufacturing costs,<br />
have made low-cost rheometers and viscometers<br />
available. They are capable of providing reproducible<br />
data for all aspects of manufacture, use and<br />
performance of coatings (including cure), in<br />
absolute (SI) units, allowing direct comparison of<br />
different materials and processing conditions. The<br />
current state of the art includes measurement of<br />
materials in extension, quantifying the likelihood of<br />
spatter, stranding and misting.<br />
A full copy of this paper is available on request by<br />
quoting Rheo-050<br />
• application notes & technical articles<br />
A collaborative study of the structure and<br />
rheological properties of EVOH/SMA* blends<br />
produced by reactive extrusion (Technical Report)<br />
polymer industries<br />
info@rheologysolutions.com<br />
Strongly synergistic behaviour in terms of viscosity<br />
and melt elasticity was seen in all blends, for low<br />
frequency dynamic and low shear rate capillary<br />
tests, the largest increases occurring in blends<br />
containing 50-60% EVOH. Finely dispersed droplet<br />
phase morphologies were seen in most of the<br />
blends, the minor phase forming the dispersed<br />
phase. However the blends containing 50-60%<br />
EVOH were co-continuous or partly co-continuous;<br />
it was also notable that the blends containing 60%<br />
EVOH exhibited a surprisingly low value of Melt<br />
Index. Evidence of covalent bonding was apparent<br />
in all blends, the highest interaction levels again<br />
being seen for the 50-60% EVOH blends, despite<br />
a very low anhydride/alcohol molar ratio (only<br />
0.05). Increased mixer speed and vacuum venting<br />
during processing also improved reaction levels.<br />
These findings suggest that the availability of<br />
reactive groups is restricted by the phase<br />
morphology of the blend during production.<br />
As a result, more reaction occurs at or near<br />
co-continuous phase compositions, where the<br />
surface area is maximised. The synergistic<br />
behaviour in viscosity and elasticity can be seen<br />
as consistent with the observed increased<br />
bonding levels, which causes more efficient<br />
stress transfer into the dispersed phase.<br />
*EVOH = ethylene-vinyl alcohol copolymer; SMA =<br />
styrene-maleic anhydride copolymer<br />
A full copy of this technical report is available by<br />
requesting LR-42<br />
biennial 07-08<br />
27
• application notes & technical articles<br />
Rheological properties of bitumen modified with<br />
polyethylene and polyethylene based blends<br />
Introduction.<br />
construction &<br />
building industries<br />
Nowadays a very large majority of the roads are<br />
constructed using a mixture of bitumen (5 wt. %)<br />
and mineral aggregates. Notwithstanding this low<br />
bitumen content, the performance of the road<br />
pavement is determined by the properties of the<br />
bitumen, as bitumen is the continuous phase and<br />
the only deformable component. On the other<br />
hand, from a technological point of view, the<br />
The rheological properties of<br />
polymers in shear as well as in<br />
extensional flow are essential<br />
for their processing.<br />
continuously increasing traffic load on road<br />
pavements has resulted in tightening of binder<br />
specifications in order to obtain higher mechanical<br />
stability of asphalt roads. However, the limit of<br />
increasing pavement performance with conventional<br />
pure bitumen seems to have been reached.<br />
To achieve this improvement, it is necessary the<br />
addition of natural or synthetic polymers to the<br />
bitumen. The aim of this project is to obtain<br />
modified bitumens, using several synthetic<br />
polymers, like polyolefins or rubbers. The<br />
optimisation of composition and processing<br />
conditions will be carried out by taking into<br />
account the stability and rheological properties of<br />
bitumens for road paving under extreme<br />
conditions, which should be processed with<br />
conventional or slightly modified machinery.<br />
Keywords.<br />
EPDM/PE blends; Polyolefin modified bitumens;<br />
Bitumen rheology; Polymer/bitumen blends<br />
A full copy of this paper is available on request by<br />
quoting RF-190902-ES-01<br />
• application notes & technical articles<br />
Measurement of the Irganox content in<br />
polypropylene polymers during extrusion<br />
Abstract.<br />
Near infrared spectroscopy was used as an in-line<br />
control system for the measurement of polypropylene<br />
filled with different amounts of Irganox<br />
additives. For this purpose transmission probes<br />
were installed in an extruder. The probes can<br />
• application notes & technical articles<br />
New die design for the characterisation of the<br />
extensional and shear properties of polymers<br />
for laboratory and on-line use<br />
biennial 07-08<br />
polymer industries<br />
polymer industries<br />
withstand temperatures up to 300oC and<br />
pressures up to 60 MPa. Transmission spectra of<br />
polypropylene mixed with Irganox with a coefficient<br />
of models were generated with partial least square<br />
regression which resulted in a model which<br />
estimated Irganox with a coefficient of determination<br />
of 0.984 and root square error of prediction of<br />
0.098%. Furthermore the possibilities for<br />
controlling process conditions by measuring<br />
transmission at a specific wavelength were shown.<br />
Unfortunately their complete characterisation in<br />
the laboratory requires the complementary use<br />
of sophisticated techniques which are time<br />
consuming and need great expertise.<br />
Therefore quality control is mainly limited to<br />
the measurement of a melt flow index, a shear<br />
viscosity and eventually a melt strength test to<br />
assess extensional properties. The on-line<br />
monitoring of material parameters would be very<br />
helpful but is today mostly restricted, whenever<br />
performed, to MFI or a capillary shear viscosity<br />
measurement.<br />
Keywords.<br />
polymer, irganox, extrusion, in-/on-line<br />
Reference: W. Becker and N. Eisenreich, J. Near<br />
Infrared Spectroscopy. 13, 147 – 154 (2005).<br />
© NIR Publications. www.impublications.com<br />
The HAAKE X-die has been developed to cover<br />
the need for a quick characterization in shear<br />
and extension, with little or even no operator<br />
intervention. It can be mounted on a traditional<br />
capillary rheometer or directly on-line with a melt<br />
pump feeding it. Data obtained by this die with a<br />
standard LDPE already tested in round robin tests,<br />
are presented and confirm the validity of this new<br />
approach.<br />
A full copy of the laboratory report is available on<br />
request by quoting LR-39<br />
28 www.rheologysolutions.com
• application notes & technical articles<br />
Measuring coatings<br />
surface coatings industries<br />
Published in Polymers Paint<br />
Colour Journal, May 2006,<br />
pp: 50 – 53.<br />
www.coatingsgroup.com<br />
A wide range of measurements with viscometers<br />
and rheometers is used to characterise the<br />
rheological properties of coatings such as inks,<br />
varnishes, dip coatings, paints, dispersions,<br />
paper coatings, printing ink, security printing<br />
pastes and powder coatings.<br />
This paper is intended to give a brief overview<br />
of which properties can be measured with which<br />
tests and which instrumentation is required.<br />
Besides the well-established shear flow testing<br />
in rotation, creep and oscillation, the benefits of<br />
extensional testing are discussed for viscoelastic<br />
fluids.<br />
• application notes & technical articles<br />
Continuous online rheometry<br />
for industrial slurries<br />
Abstract<br />
mining industries<br />
Mineral solids are usually processed, produced<br />
or handled in the form of two-phase slurries.<br />
Accurate and reliable measurements of the<br />
rheological properties of settling slurries using<br />
conventional viscometric instruments can be<br />
difficult, if not impossible, since the solid particles<br />
settle rapidly under the influence of gravity. In this<br />
paper we report on the development of an on-line<br />
flow rheometer specially designed and constructed<br />
for characterising the rheological behaviour of<br />
info@rheologysolutions.com<br />
In order to keep the quality of coatings on a high<br />
level, continuous quality control is required as well<br />
as sound knowledge of raw materials, processing<br />
steps, storage conditions and application<br />
procedures.<br />
<strong>Rheology</strong> plays a crucial role in each of the steps<br />
which a coating undergoes: After development of<br />
the formulation, production starts with quality<br />
control of raw materials like binders, solvents,<br />
pigments, fillers and additives. For processing,<br />
the components require the ability of mixing,<br />
dispersing, pumping, stirring, homogenising and<br />
stabilising. A good coating shows stability during<br />
shelf life and transportation without sedimentation,<br />
flocculation, agglomeration and coagulation.<br />
Rheological measurements help to select proper<br />
dimensions of pipelines, pumps and stirring<br />
vessels as well as filling machines.<br />
A variety of application processes uses high shear<br />
rates or high extensional rates – eg painting,<br />
settling slurries. The instrument design is based<br />
on the principles of helical flow, which is the<br />
combination of tangential Couette and axial<br />
Poiseuille flows. The data reduction procedure<br />
developed is firmly based on the theory of helical<br />
flow and has been extensively tested and validated<br />
with fluids of different rheological behaviour. Good<br />
results have been obtained using the rheometer<br />
for various Newtonian liquids, pseudoplastic<br />
polymeric solutions and mineral slurries.<br />
Keywords<br />
Flow rheometer, on-line viscometer, mineral slurry,<br />
rheological characterisation, helical flow<br />
spraying, printing, dipping which is followed<br />
usually by gravity-driven steps – for example by<br />
levelling in order to obtain a homogeneous film<br />
with good properties in texture, appearance and<br />
protection of the coated substrate.<br />
While stability during shelf like and properties like<br />
levelling or sagging are best characterised by a<br />
controlled stress (CS) measurement, the various<br />
shear rates of stirring, pumping, filling, painting<br />
are well represented in controlled rate (CR)<br />
measurements. Creep testing is performed in<br />
CS mode. Gelation, cross linking and curing are<br />
best recorded with oscillatory measurements in<br />
controlled deformation (CD) mode while amplitude<br />
sweeps as well as frequency or time sweeps can<br />
be performed in CS as well as CD oscillatory<br />
mode.<br />
In order to understand the extensional processes<br />
in printing and roll coating as well as in dies for<br />
filling, spraying or spray dying, the extensional<br />
properties require experimental determination.<br />
A full copy of this paper is available on request<br />
by quoting HA-030<br />
Introduction<br />
The control of the rheology of settling suspension<br />
is of great importance to the mineral industry as it<br />
is a critical factor in optimising plant life cycle<br />
costs. Many processes involve handling particles<br />
of diverse sizes, usually in the form of rapid<br />
settling (unstable) slurries and it is the slurry<br />
viscosity not the solids concentration that effects<br />
the energy consumption and many of the design<br />
factors of mineral processing units. It is therefore<br />
essential that the rheological properties of these<br />
slurries be determined accurately under conditions<br />
that resemble closely those found in the actual<br />
processes.<br />
A full copy of the paper is available on request by<br />
quoting RF-200902-AU-01.<br />
biennial 07-08<br />
29
• application notes & technical articles<br />
Small scale compounders<br />
for pharmaceutical research<br />
pharmaceutical, cosmetics<br />
& allied industries<br />
Abstract<br />
Hot melt extrusion and continuous granulation<br />
provide for rapid product and process design,<br />
flexible manufacturing, a well controlled process<br />
and cost-efficient pharmaceutical production. In<br />
the development of new drugs/excipients, small<br />
scale continuous extrusion systems reduce time<br />
to market, reduce consumption of expensive<br />
ingredients, and use processes comparable to<br />
production. Applications and products for<br />
development with small scale twin-screw<br />
compounders are discussed.<br />
Introduction<br />
Manufacturing of clinical and commercial scale<br />
pharmaceuticals is traditionally accomplished<br />
using batch processes. Recently, because of its<br />
many advantages, a trend toward continuous<br />
processing is becoming more prevalent. For<br />
example, hot melt extrusion can deliver increased<br />
efficiency and higher throughput, when compared<br />
with a classical batch process. Continuous<br />
processing also allows for the real-time monitoring<br />
news & views<br />
Rheological Analysis of<br />
Powder Coatings<br />
surface coatings industries<br />
Powder coatings are a<br />
cost effective and an<br />
environmentally friendly<br />
alternative to liquid coatings.<br />
Traditional coating systems form networks via a<br />
thermally activated process. This usually involves<br />
placing a powder coated surface into an oven at<br />
temperatures between 160°C and 200°C. The<br />
powder melts at around 80°C to 120°C and<br />
becomes an even film. At temperatures<br />
between 110°C and 140°C the cross linking<br />
reaction starts. The curing time typically lasts<br />
between 15 and 30 minutes, depending on the<br />
temperature and reactivity of the system.<br />
UV curing powder coating systems have been<br />
established, where the curing process takes place<br />
biennial 07-08<br />
in a shorter amount of time, even at temperatures<br />
below 100°C. A further advantage of the UV<br />
induced network formation is that it works virtually<br />
independently of temperature. This opens up new<br />
application possibilities for coating of heat<br />
sensitive surfaces like wood or synthetics.<br />
The melting and curing relationship of powder<br />
coatings can be rheologically analysed via<br />
oscillatory tests with an air-bearing rheometer.<br />
The advantage of this method is that the<br />
structural change of the coating as a function of<br />
time or temperature can be monitored without<br />
disturbing the process i.e. at very small oscillation<br />
amplitudes. The rheological measurements that<br />
are usually of interest are complex viscosity η)*,<br />
complex modulus G*, the loss factor tan δ<br />
as well as the phase displacement angle δ.<br />
As many powder coatings become very rigid after<br />
the complete curing process, parallel<br />
continued on page 31 <br />
of processing parameters and in-process material<br />
properties. Extrusion is an established technique in<br />
polymer processing, and is particularly important<br />
for PAT. With real-time monitoring and process<br />
understanding, a continuous process can more<br />
easily be controlled to yield the highest quality<br />
product in the most efficient way. In addition, as<br />
compounding takes place directly in the molten<br />
stage, aqueous solutions are avoided, reducing or<br />
removing drying steps which helps to save energy.<br />
In pharmaceutical technology, extrusion has been<br />
studied and deployed for more than 35 years [1] .<br />
gives a The following article is discussing the<br />
smallest scale of extrusion with an output of<br />
several grams to 150 grams per hour leading to<br />
development and production scale extruders with<br />
outputs in the 10 to 20 kilogram per hour range.<br />
A full copy of this paper is available on request by<br />
quoting PRISM 004<br />
30 www.rheologysolutions.com
continued from page 30<br />
measurements using a plate/plate geometry PP20<br />
with 20 mm plate diameter are recommended for<br />
these rheological tests. Rheological analysis of<br />
powder coatings take place at temperatures of<br />
somewhere between 80°C and 250°C. Below are<br />
experimental results which can be measured with<br />
an air-bearing rheometer such as the HAAKE<br />
Mars (see photo). The temperature range can be<br />
easily covered using an electric temperature<br />
control unit consisting of a lower and an upper<br />
heating system.<br />
The following outlines some recommendations of<br />
practical examples and typical measurement<br />
methods. A disposable plate/plate measuring<br />
geometry made of aluminium with a diameter of<br />
20 mm and a measuring gap of 1 or 0.5mm is<br />
recommended.<br />
1. Analysis of the curing process of powder<br />
coatings at a constant temperature<br />
The change in complex viscosity η* was analysed<br />
as a function of time at a constant oscillatory<br />
frequency. As the sample cures while measuring,<br />
the oscillatory amplitude τ had to be gradually<br />
increased in order to maintain a constant sample<br />
deformation γ.<br />
A desired deformation γ is assigned to the sample<br />
(typically γ=0.5% ), the rheometer then controls<br />
the recommended amplitude τ.<br />
It is important for the reproducibility of the<br />
measurement results to maintain the same<br />
conditions for powder filling and for setting the<br />
start of the test. In Fig. 1 an oscillation time curve<br />
of a powder coating is illustrated. The<br />
measurement was carried out at 200°C with a<br />
frequency of 1 Hz. A deformation of 0.5% was<br />
chosen. 200 data points per segment were taken.<br />
Fig. 1: Curing of a powder coating at 200°C<br />
(f=1 Hz, γ = 0.5 %)<br />
Each oscillation was only carried out once<br />
(number of repeats 1, no waiting time) so that the<br />
time dependent changes of the sample could be<br />
info@rheologysolutions.com<br />
monitored. The complex viscosity η* and the<br />
phase shift angle b are shown as a function<br />
of time in the diagram. Analysis of the same<br />
powder coating at two different temperatures<br />
under the same conditions, establishes that the<br />
curing process is clearly slower at 150°C than at<br />
200°C (Fig. 2). At lower temperatures the curing<br />
process is slower and therefore the complex<br />
viscosity of the sample has a lower value. While<br />
the plateau value of the complex viscosity is<br />
reached after around 10 minutes of measuring<br />
time at 200°C, η* still increases at 150°C after<br />
16 minutes measuring time. For the latter<br />
measurement, no plateau value was reached after<br />
a measuring time of 16 minutes. A prediction<br />
as to whether the same end value would be<br />
achieved as at 200°C and after what time, is not<br />
possible from the available results.<br />
Fig. 2: Oszillation time curves at two temperatures<br />
(f=1 Hz, γ = 0.5 %, 150 and 200°C)<br />
2. Analysis of the melting and curing<br />
process as a function of temperature<br />
The examination of changes in complex viscosity<br />
as a function of temperature is interesting given<br />
that two influences, namely temperature and time<br />
are tracked simultaneously.<br />
Firstly the powder is melted and the complex<br />
viscosity drops to a minimum and then increases<br />
for the curing process. The position of the<br />
minimum and also the value of viscosity at the<br />
minimum are dependent on the substance<br />
itself as well as on the chosen heating rate.<br />
Fig. 3 shows η* in relation to temperature at a<br />
heating rate of 6 K/min for two different powder<br />
coatings. Powder A reaches a minimum viscosity<br />
at around 180°C, while the minimum viscosity of<br />
sample B is reached at 160°C.<br />
Examination of the minimum viscosity values in<br />
the curves however, yield a much lower value for<br />
sample A than for sample B (120 Pas compared<br />
to 400Pas).<br />
For processing purposes coating A should result<br />
in a more even coating as the lower viscosity<br />
Fig. 3: Comparison of two powder coatings<br />
(f=1 Hz, γ = 0.5 %, heating rate 6 K/min)<br />
should give a better development (film formation)<br />
on the surface. In Fig. 4 a powder coating sample<br />
analysis at three different heating rates is shown.<br />
At a lower heating rate (1 K/min) the complex<br />
viscosity runs at a minimum at 110°C after<br />
around 30 minutes. Afterwards it increases again<br />
and reaches a plateau value after around 80<br />
minutes. After this the networking formation is<br />
virtually complete. At higher heating rates the<br />
viscosity minimum shifts to a higher temperature.<br />
The effects of the two influences can be seen: the<br />
viscosity decreases with increasing temperature,<br />
the system simultaneously cross-links and the<br />
viscosity rises again. At higher heating rates the<br />
decrease of the viscosity predominates<br />
momentarily because the curing process develops<br />
more slowly.<br />
Therefore at the highest heating rate (10K/min)<br />
the viscosity at the curve minimum is somewhere<br />
around 10 times lower than at the lowest heating<br />
rate (1 K/min). The minimum viscosity at the<br />
highest heating rate is achieved after around 7<br />
minutes, at the mid-rate (5 K/min), after around<br />
11 minutes. In Fig. 4 the three curves are shown<br />
only as a function of temperature, not as a<br />
function of time. This explains why the complete<br />
cross-linking process is only recognisable at one<br />
point on the graph.<br />
This report was published in Paint & Resin,<br />
Issue 3 - 2007<br />
Fig. 4: Influence of the heating rate on the<br />
Process η* (f=1 Hz, γ = 0.5 %)<br />
biennial 07-08<br />
31
News & Views<br />
Industry <strong>Solutions</strong><br />
• Feature Story- Qenos Install A Pellet Size & Shape Distribution (PSSD) System 33 •<br />
• CoolTech Application Story – Rehau Pty Ltd ................................................ 42 •<br />
• Feature Story – Uncompromising Eyes ........................................................ 43 • • • •<br />
• Sensor System to Measure Viscosity of Tailings from Marimex ........................ 41 •<br />
• Customer Installation - Plantic Technologies Ltd in Altona Victoria recently<br />
purchased a HAAKE PolyLab with <strong>Rheology</strong> Dies ........................................ 47 •<br />
• High Quality Pharmaceutical Film –<br />
Customer Story Klockner Pentaplast, Germany ........................................ 48 • •<br />
• Industry Overview – Material Characterisation <strong>Solutions</strong> ................................ 49 • • • • •<br />
• Feature Article - OnLine Close-Loop Monitors Four Cast Film Extruders<br />
During Production ........................................................................................ 51 •<br />
• Food Industry Feature & Product Focus ........................................................ 54 •<br />
• How to Measure Series for Mining Slurries ................................................ 43 •<br />
Company News<br />
• A Brand New Year – A Brand New Look! ........................................................ 35 •<br />
• Australian Food Engineering Association<br />
– Technical Meeting – September 2006 ........................................................ 38 •<br />
• Conferences & Exhibitions in 2007 – 29th Australian<br />
Polymer Society Conference & Exhibition........................................................ 36 •<br />
• Conferences & Exhibitions in 2007 – 8th Joint Conference of Australian<br />
Society of Cosmetic Chemists........................................................................ 36 •<br />
• Conferences & Exhibitions in 2007- Paste & Thickened Tailings- A Guide 2007 36 •<br />
• How to Series of Workshops– Calls for Expressions of Interest ........................ 39 •<br />
• New Addition to our <strong>Rheology</strong> Team ........................................................ 35 •<br />
• New Website Additions – Biennial Rheotalk ................................................ 40 •<br />
• New Website Additions – Interactive Dictionary ........................................ 40 •<br />
• Polymers Extrusion & Compounding Workshops<br />
– Calls for Expressions of Interest ................................................................ 33 •<br />
• New Website Now Online! – www.TemperatureControlBaths.com ................ 37 •<br />
• Staff Update ................................................................................................ 38 •<br />
• Update on Paste & Thickened Tailings Conference ........................................ 42 •<br />
• Workshop – High Temperature Micro-<strong>Rheology</strong> ........................................ 41 • • • •<br />
• Staff Update ................................................................................................ 46 •<br />
• Staffing Changes - Administration Manager ................................................ 35 •<br />
• The Mayonnaise Jar & Two Cups of Coffee ................................................ 48 •<br />
• Service Department Update ........................................................................ 50 •<br />
• <strong>Rheology</strong> <strong>Solutions</strong> – 10th Anniversary ........................................................ 39 •<br />
• Staff Update ................................................................................................ 50 •<br />
• Company News – Home of a New High Technology Facility ........................ 55 •<br />
• Exhibitions - 30 APS Australian Polymer Symposium ................................ 36 •<br />
• Exhibitions - Ausplas 2008 ........................................................................ 43 •<br />
• Exhibitions - FoodPro 2008 ........................................................................ 66 •<br />
biennial 07-08<br />
32 www.rheologysolutions.com<br />
ALL INDUSTRIES<br />
POLYMER<br />
FOOD<br />
SURFACE COATINGS<br />
MINERAL<br />
CHEMICAL<br />
PHARMACEUTICAL<br />
BUILDING
feature story – customer installation<br />
Qenos install a Pellet Size Shape<br />
& Distribution (PSSD) System<br />
polymer industries<br />
Qenos in Altona has taken<br />
delivery of an Optical<br />
Control Systems (OCS),<br />
Pellet Size, Shape and<br />
Distribution (PSSD) System<br />
in December 2006.<br />
all industries<br />
During 2005, <strong>Rheology</strong> <strong>Solutions</strong> in conjunction<br />
with Thermo Electron Stone ran a series of<br />
workshops using the PRISM EuroLab 16 mm Twin<br />
Screw Extruder. The inaugural workshop was well<br />
attended by over 75 people during a 7 day<br />
timeframe. Based on the success and interest in<br />
the 2005 workshop, <strong>Rheology</strong> <strong>Solutions</strong> is<br />
planning on running the series in 2007.<br />
Equipment planned for the workshop includes:<br />
info@rheologysolutions.com<br />
The decision to purchase the PSSD system was<br />
based on a rigorous process of evaluation,<br />
testing, trials and discussions between the Qenos<br />
Technical Centre personnel, <strong>Rheology</strong> <strong>Solutions</strong><br />
and Optical Control Systems. The process of<br />
discussion and trials commenced prior to Ausplas<br />
in 2005 and resulted in Qenos bringing samples<br />
(natural and pigmented polyethylene pellets) to<br />
the exhibition to run them on the OCS PSSD<br />
system to obtain bench mark results on pellet<br />
geometry. Further samples were then sent to OCS<br />
in Witten in Germany for geometry testing. The<br />
objective was to compare and correlate the<br />
current manual testing conducted at Qenos with<br />
optical inspection results from the PSSD.<br />
In early July, <strong>Rheology</strong> <strong>Solutions</strong> in conjunction<br />
• PRISM EuroLab 16 mm Twin Screw Extruder<br />
• Water Bath & Palletiser<br />
• Extrusion Dies, Chill roll system and filter test<br />
equipment.<br />
The workshop will be half day in duration and run<br />
as either private or public sessions where<br />
attendees can run their own samples.<br />
The workshop is of interest to all those in the<br />
polymer industry including:<br />
• Previous attendees at the 2005 workshop<br />
• R&D personnel • Universities<br />
• Raw material & end product manufacturers<br />
with OCS conducted a workshop for the polymer<br />
industry where customers could bring their pellet<br />
and powder samples for testing. Qenos attended<br />
a private workshop session and discussed their<br />
final system requirements. These requirements<br />
and specifications were then taken back to OCS<br />
where their program development team<br />
incorporated these additional requirements into<br />
their software and tailored the software to report<br />
and show the specific results in the format that<br />
they needed to allow them to determine the<br />
quality and consistency of their pellet geometry.<br />
The software configuration was modified to meet<br />
all the Qenos reporting requirements and further<br />
samples were run at OCS to compare the results<br />
Continued on page 33<br />
news & views - call for expressions of interest...<br />
Polymer Extrusion & Compounding<br />
Workshops<br />
Interested? Contact <strong>Rheology</strong> <strong>Solutions</strong><br />
to register your interest in the series.<br />
Each workshop will be limited to 6 – 9 attendees<br />
to ensure that each attendee will have maximum<br />
opportunity for hands on training and operation of<br />
the PRISM EuroLab 16mm Twin Screw Extruder<br />
and ancillary equipment and adequate discussion<br />
with Dr Tim Kealy during the workshop.<br />
Further information on the PRISM range of<br />
Twin Screw Extruders can be obtained from<br />
http://www.rheologysolutions.com/prodtwin.<br />
html<br />
biennial 07-08<br />
33
Tracey Boseley replacing the lid for sample feed<br />
to the PSD.<br />
Continued from page 32<br />
Qenos install a Pellet Size Shape<br />
& Distribution (PSSD) System<br />
of the sample from the PSSD to their manual<br />
testing results. The results from the comparison<br />
on the same sample were positive and an order<br />
for the PSSD unit was placed with <strong>Rheology</strong><br />
<strong>Solutions</strong> in November 2006.<br />
The PSSD will be used at Qenos as a quality<br />
management tool for pellet geometry. The system<br />
has been installed in the Physical Laboratory<br />
within the Technical Centre. The unit will be used<br />
for rapid and reliable characterisation of Qenos<br />
polyethylene’s, replacing the intensive manual and<br />
time consuming techniques that had been<br />
previously employed within the Technical Centre.<br />
The use of the PSSD will be complementary to but<br />
not replace the in-plant quality control pellet<br />
geometry tests.<br />
biennial 07-08<br />
Tim Kealy setting up the OCS software before<br />
running a sample on the PSSD.<br />
Qenos use Australian oil and gas feedstocks from<br />
Bass Strait and the Moomba Basin. Qenos employ<br />
approximately 800 people and their plants<br />
produce olefins and a full range of polyethylene<br />
products, including high density polyethylene<br />
(HDPE), low density polyethylene (LDPE), linear low<br />
density polyethylene (LLDPE) and medium density<br />
polyethylene (MDPE). This makes Qenos a vital<br />
link in the Australian manufacturing chain,<br />
supplying industries that employ hundreds of<br />
people. Polyethylene is manufactured at Qenos<br />
plants in Botany and Altona with the capacity in<br />
the order of 200,000 tonnes HDPE, 90,000<br />
tonnes LDPE and 125,000 tonnes of LLDPE.<br />
The Australian market for virgin polyethylene is<br />
approximately 450 kt and of this, nearly 65% is<br />
used in the packaging industry. The rigids market<br />
is made up predominantly of bottles and<br />
containers for milk, juice, household and industrial<br />
chemicals, plus caps and closures. The flexibles<br />
market is made up primarily of films for food<br />
packaging including frozen foods, bread and fresh<br />
produce; shopping bags; sling and shrink wraps;<br />
industrial films and extrusion coating applications<br />
such as liquid paper board.<br />
In addition to its use in the packaging market,<br />
some of Qenos’ end products are used for water<br />
management activities such as polyethylene<br />
piping and rotational moulded water tanks.<br />
Polyethylene is used for pipes and fitting; in wire<br />
and cable applications; in the automotive<br />
components sector for tanks and storage; in<br />
household goods and in construction.<br />
The breadth and depth of the applications and<br />
uses for the polyethylene is immense. The<br />
addition of the OCS PSSD system will further<br />
ensure that Qenos continues to provide products<br />
of consistent quality.<br />
Full training and commissioning of the PSSD<br />
system will be undertaken in January 2007 for<br />
the Technical Centre staff at Qenos. The training<br />
will be provided by OCS and will include an<br />
intensive two days of hands on training for all<br />
staff. The training will also be supported by Dr Tim<br />
Kealy – Technical Manager and Mr Richard<br />
Donaldson – Service Engineer from <strong>Rheology</strong><br />
<strong>Solutions</strong>.<br />
34 www.rheologysolutions.com
note from the editor<br />
A Brand New Year<br />
- A Brand New Look!<br />
all industries<br />
<strong>Rheology</strong> <strong>Solutions</strong> is<br />
pleased to provide you with<br />
a new look RheoTalk for<br />
their first issue in 2007.<br />
RheoTalk will continue to be published three<br />
times per year and be available as a printed full<br />
colour newsletter or electronically as a PDF.<br />
The newsletter has been expanded to reference<br />
each article in the newsletter to specific industry<br />
<strong>Rheology</strong> <strong>Solutions</strong> is<br />
pleased to introduce Evie,<br />
the newest team member.<br />
Evie joined <strong>Rheology</strong> <strong>Solutions</strong> on Thursday, 23<br />
November 2006 at the young age of 5 weeks<br />
and 4 days. Evie, is a Border Collie and was born<br />
on 15 October, 2006 to Maggie and Sam.<br />
info@rheologysolutions.com<br />
classifications. An industry quick reference guide<br />
can also be found on page 1. This will guide you<br />
to the contents that may be of most interest to<br />
you. The cross referencing by industry<br />
classification was also introduced in the electronic<br />
version of the Biennial RheoTalk for 2005 – 2006<br />
which is available on our website.<br />
We welcome your comments, feedback and<br />
suggestions on what you would like to see<br />
included in future issues of RheoTalk. We trust<br />
that 2007 is a successful year for each of you<br />
and we look forward to working with you during<br />
the coming year. Cheers and happy reading.<br />
rheology solutions news<br />
New Addition to our<br />
<strong>Rheology</strong> Team<br />
Evie comes to work every day along with her<br />
older canine friend, Mal who is an Alaskan<br />
Malamute of 101 /2 years old. Mal has been<br />
coming to work for over 81 /2 years and has<br />
welcomed the newest team member to assist<br />
him in his day to day activities.<br />
Mal and Evie look forward to greeting you when<br />
you next visit <strong>Rheology</strong> <strong>Solutions</strong>.<br />
Mal and Evie relaxing before they get<br />
back into their days work.<br />
news & views<br />
Staffing<br />
Changes –<br />
Administration<br />
Manager<br />
Administration Manager Jackie Wrigglesworth<br />
all industries<br />
For the past four years, Jackie Wrigglesworth has<br />
been employed as the Marketing Assistant. From<br />
1 July, 2007 her position in the company has<br />
expanded to incorporate office administration as<br />
well as her marketing support role on a full time<br />
basis in the position of Administration Manager.<br />
This now places Jackie as the first point of contact<br />
for all enquiries across; general information;<br />
product information; updating contact information;<br />
status of delivery for current orders; scheduling of<br />
service, repairs and calibrations (either on site or<br />
off site); accounts receivable and payable.<br />
Please assist us in welcoming Jackie into her<br />
expanded role with <strong>Rheology</strong> <strong>Solutions</strong>.<br />
biennial 07-08<br />
35
news & views<br />
Conferences & Exhibitions in 2007<br />
During 2007, <strong>Rheology</strong><br />
<strong>Solutions</strong> will be attending<br />
the following national<br />
conferences and exhibitions.<br />
• 29th Australian Polymer Society<br />
Conference & Exhibition<br />
11-15 February, 2007, Hobart, Tasmania<br />
www.29aps.org<br />
<strong>Rheology</strong> <strong>Solutions</strong> will be exhibiting a range of<br />
materials characterisation products from Thermo<br />
Fisher Scientific specifically to meet the<br />
requirements of the polymer industry in R&D,<br />
QA/QC and production applications. The products<br />
will include:<br />
• HAAKE MARS – Modular High<br />
Temperature/High Pressure R&D Rheometer<br />
available with interchangeable temperature<br />
control units, and application oriented<br />
measuring systems.<br />
• HAAKE MiniLab – Co- and counter-rotating<br />
twin screw extruder with integrated viscosity<br />
measurement for compounding sample<br />
volumes up to 7 ml.<br />
• HAAKE MiniJet – Injection moulding machine<br />
for sample preparation system to produce test<br />
specimens from 5 gm of material from<br />
powders, pellets or melts.<br />
biennial 07-08<br />
polymer industries<br />
• PRISM Twin Screw Extruder – Segmented<br />
barrel with lift off top half for easy access to<br />
screws. Available with ancillary equipment<br />
including pre-mixers, screen changers, chill<br />
rolls, strand pelletising lines, air-cooled facecut<br />
system and cast sheet or blown film lines.<br />
The conference will be attended by Dr Tim Kealy<br />
and Mr Patrick Griffin and both will be available<br />
on the <strong>Rheology</strong> <strong>Solutions</strong> stand number 5 to<br />
discuss your materials characterisation and<br />
rheology requirements.<br />
mining industries<br />
• Paste and Thickened Tailings<br />
– A Guide 07<br />
13-15 March 2007, Perth, WA<br />
www.acg.uwa.edu.au<br />
<strong>Rheology</strong> <strong>Solutions</strong> will be exhibiting during the<br />
Paste 2007 Seminar. On display at the exhibition<br />
will be the HAAKE ViscoTester 550 which is<br />
widely accepted and used within the mining<br />
industry.<br />
The HAAKE ViscoTester 550 will be fully<br />
operational and demonstrated during the<br />
exhibition. In addition, <strong>Rheology</strong> <strong>Solutions</strong> will<br />
have a range of information kits specifically<br />
developed and produced for the mining industry.<br />
These kits will be made available on request and<br />
cover: Contract Testing Capabilities for Mining<br />
• exhibitions<br />
Australian Polymer Symposium<br />
polymer industries<br />
The Australian Polymer Symposium, is being held<br />
in Melbourne from 30 November – 4 December,<br />
2008 and <strong>Rheology</strong> <strong>Solutions</strong> will be participating<br />
in the exhibition on stand number 13.<br />
The stand will be showcasing the HAAKE PolyLab<br />
QC with Rheomix 600 - from Thermo Scientific.<br />
The HAAKE PolyLab QC with Rheomix 600 is a<br />
modular torque rheometer with measuring mixer.<br />
Matthias Jährling, Senior Application Specialist,<br />
Manager MC Application Laboratories, Process<br />
Instruments from Thermo Fisher Scientific in<br />
Germany will be joining <strong>Rheology</strong> <strong>Solutions</strong> on<br />
the stand.=<br />
Slurries; <strong>Solutions</strong> for Mining Slurries; Tim's Top<br />
Tips - How to Measure Thixotropy, How to<br />
Measure Yield Stress, How to Measure Flow &<br />
Viscosity Curves. The series of Tim's Top Tips<br />
have been specifically written for the HAAKE<br />
ViscoTester 550 which has been established over<br />
the last 10 years as the mining slurries industry<br />
standard and choice for viscosity & flow curves,<br />
yield stress and thixotropy testing.<br />
For further information on the HAAKE ViscoTester<br />
VT550 visit www.rheologysolutions.com/<br />
viscotester550_techs.html<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
• 8th Joint Conference of Australian<br />
Society of Cosmetic Chemists<br />
22-25 March 2007, Wollongong, NSW<br />
www.ascc.com.au/news/conferences<br />
Dr Tim Kealy from <strong>Rheology</strong> <strong>Solutions</strong> will be<br />
presenting a paper titled “Measurements of the<br />
viscoelastic properties of cosmetic foam products<br />
using a vane sensor“. The paper was co-authored<br />
by Alby Abram and Richard Buchta from<br />
Connectics Australia and Dr Tim Kealy from<br />
<strong>Rheology</strong> <strong>Solutions</strong>. Tim will be available for<br />
questions regarding application, contract testing<br />
facilities, instrument evaluation for materials<br />
characterisation and rheology applications.•<br />
36 www.rheologysolutions.com
news & views<br />
NEW Website - Now Online!<br />
all industries<br />
temperaturecontrolbaths.com<br />
offers the best selection of<br />
temperature control<br />
products within Australia<br />
Our range covers solutions for heating and<br />
cooling applications for industries including:<br />
• biological • environmental<br />
• laboratories • manufacturing<br />
• packaging • printing<br />
• process • raw materials<br />
• research • universities<br />
Some 100 products are itemised on this website<br />
across 12 category types (Accessories/Options,<br />
Baths, Cryostats, Fogging Tester, Heating Bath<br />
Circulators, Immersion Circulators, Laboratory<br />
BUY ONLINE<br />
CoolTech 320<br />
Refrigerated circulator<br />
Temperature range<br />
-28ºC to +100ºC<br />
AUS $3,999<br />
excluding GST<br />
& local delivery<br />
>> more information<br />
info@rheologysolutions.com<br />
Chillers, Open Bath Circulators, Process Chillers,<br />
Refrigerated Bath Circulators, Shaking Water<br />
Baths, Temperature Control Systems) and each<br />
product has full technical specifications.<br />
The range and diversity of the temperature<br />
control baths available has been established to<br />
meet the control requirements across the depth<br />
and breadth of temperature control applications.<br />
Currently, there are two products which can be<br />
purchased on-line (CoolTech 320 and HeatTech<br />
26L) and this will expand to meet the needs and<br />
requirements of the customer enquiries over the<br />
coming months.<br />
Buy on-line with delivery ex-stock ready to<br />
despatch within 48 hours (or two full working<br />
days) from receipt of official company purchase<br />
order.<br />
TemperatureControlBaths.com is owned and<br />
operated by <strong>Rheology</strong> <strong>Solutions</strong> Pty Ltd and is a<br />
privately owned company based in Victoria.<br />
The diversity of applications, industries and extent<br />
of the product range instigated the creation of<br />
this dedicated website for<br />
TemperatureControlBaths.com<br />
<strong>Rheology</strong> <strong>Solutions</strong> was established in April 1998<br />
to service the requirements of the materials<br />
science market in Australia by providing the<br />
world's leading products and supporting sales<br />
and distribution with service, technical support<br />
BUY ONLINE<br />
HeatTech 26L<br />
Heating circulator<br />
Temperature range<br />
ambient to +100ºC<br />
AUS $2,399<br />
excluding GST<br />
& local delivery<br />
>> more information<br />
and education. The vision is to recognise the<br />
importance of specialisation and dedication to a<br />
specific science and provide full technical support<br />
and service throughout Australia. The Company<br />
goal is to integrate industry experience and<br />
materials characterisation techniques to provide<br />
practical solutions for customers.<br />
Building on the underlying vision that dedication<br />
and specialisation is key to providing customers<br />
with the right solution through knowledge,<br />
experience and support,<br />
TemperatureControlBaths.com was created.<br />
The goal of the TemperatureControlBaths.com<br />
website is to provide service, support and meet<br />
the needs and application requirements within the<br />
area of temperature control and offer the best<br />
selection of products from recognised world<br />
leading manufacturers.<br />
We look forward to working with you and to<br />
providing you with the best products, service and<br />
support for temperature control products.<br />
We welcome your feedback and will actively work<br />
to provide the highest level of efficiency, customer<br />
support and service.<br />
for more information visit:<br />
temperaturecontrolbaths.com<br />
all email enquiries welcome:<br />
info@temperaturecontrolbaths.com<br />
biennial 07-08<br />
37
news & views<br />
Staff<br />
Update<br />
Mal takes a break with a bit of shut eye outside<br />
biennial 07-08<br />
all industries<br />
Another day at the office for Evie which comprises<br />
sleeping, greeting delivery people, a run and game<br />
in the car park outside the office or a game with<br />
some of the toys at work.<br />
Mal, however prefers to spend the day outside<br />
resting and relaxing – just visiting from time to<br />
time to have a drink of water or join us for lunch.<br />
He knows when it is lunch time and always is on<br />
hand to assist us with our food.<br />
It is tough at work and often a break from sitting<br />
under the desk and sleeping away the hours is<br />
needed – a game of fetch and catch is a favourite<br />
pastime – then, it’s back to sleep under the desk<br />
for the next while.<br />
Sometimes however, Evie likes to serenade us all<br />
– by squeaking her purple and pink football in her<br />
mouth and howling at the top of her voice – most<br />
entertaining except when you are on the phone to<br />
a customer – which has happened on a few<br />
occasions.<br />
Evie with her favourite purple and pink football<br />
news & views<br />
Australian Food<br />
Engineering Association<br />
Technical Meeting -<br />
September 2006<br />
food industries<br />
<strong>Rheology</strong> <strong>Solutions</strong> and<br />
The Australian Food<br />
Engineering Association,<br />
(AFEA) present a seminar<br />
for the food industry in<br />
Melbourne.<br />
The paper was presented by Dr Tim Kealy -<br />
Technical Manager, <strong>Rheology</strong> <strong>Solutions</strong> Pty Ltd.<br />
“Some theory and techniques for<br />
rheological measurements for food<br />
and beverages”<br />
Rheological characterisation for product design<br />
and process control is becoming increasingly<br />
common in the food industry, as understanding of<br />
the power of these measurement techniques and<br />
instruments improves amongst professional food<br />
engineers and scientists. In September 2006,<br />
<strong>Rheology</strong> <strong>Solutions</strong> and the AFEA collaborated to<br />
bring the AFEA members a brief introductory<br />
seminar on rheology and rheological techniques<br />
applied to the food industry as the first part of a<br />
two-part series of seminars.<br />
The seminar was held at the Institute of Engineers<br />
Australia buildings in Parkville, Melbourne, with<br />
about thirty or so Food Professionals – Engineers,<br />
Chemists and Food Scientists – in attendance.<br />
Obtaining a good understanding of the rheology of<br />
a food product is critical for situations as diverse<br />
as lifecycle assessment, QC and customer<br />
satisfaction. It is the rheology of the product<br />
which, in large part, dictates its processability, its<br />
structural stability and its texture. Rheological<br />
measurements can therefore provide a valuable<br />
insight into how a material will behave during<br />
processing, during storage, and when the<br />
customer finally consumes it.<br />
New applications for foods – usually improved<br />
products with increased functionality – are being<br />
developed and marketed almost weekly. These<br />
new functionalities usually result from a small<br />
change in the ingredients making up the food<br />
recipe. These small changes in formulation can<br />
often have a startling impact on the food as it is<br />
processed, filled into containers, stored and<br />
eaten. Rheological analyses can evaluate the<br />
extent of these impacts and help predict their<br />
effect.<br />
So, intelligent food design must involve some<br />
rheological measurements and understanding to<br />
ensure success. Without understanding the<br />
consequences of changes in the process,<br />
ingredients, storage conditions and so on, we<br />
cannot hope to reliably manufacture a food<br />
product to meet with the full approval of the<br />
consumer.<br />
The seminar consisted of explanations and<br />
examples of how some of the most common<br />
rheological measurement techniques including<br />
extensional properties, yield stress, flow curves<br />
and viscosity curves can be conducted, and what<br />
the data can tell us. Along the way, introductions<br />
to and explanations of the technical jargon and<br />
concepts encountered in rheology were made,<br />
and the measurement principles of different<br />
rheometers, viscometers and measurement<br />
geometries were introduced, in particular<br />
rotational and extensional instruments for liquids<br />
and uniaxial testers (“texture analysers”) for solids<br />
and semi-solids. The concepts were illustrated<br />
using real examples and data from the food<br />
industries. The seminar was interactive with an<br />
excellent question and answer session at the<br />
close when the attendees had an opportunity to<br />
discuss their specific queries.<br />
38 www.rheologysolutions.com
news & views - call for expressions of interest...<br />
How to Series of Workshops<br />
all industries<br />
<strong>Rheology</strong> <strong>Solutions</strong> is planning to run a series of<br />
workshops based on the Tim’s Top Tips series<br />
covering rheology across:<br />
• How to Measure Thixotropy<br />
• How to Measure Yield Stress<br />
• How to Measure Flow Viscosity Curves<br />
The workshops will be half day in duration and<br />
provide all attendees with hands-on training using<br />
the HAAKE ViscoTester VT550 running their own<br />
samples. The concept of the workshop will be to<br />
provide attendees with a clear understanding of<br />
what tests should be conducted, what the results<br />
mean based on real data and real results, how to<br />
use the results to improve the process or the<br />
product.<br />
The session will include a round table discussion<br />
to determine each attendee’s objective and what<br />
is important for them to have at the end of the<br />
workshop. A brief theoretical overview will be<br />
info@rheologysolutions.com<br />
provided to cover the theory of each of the<br />
measurements being conducted and how to use<br />
the data once the results have been obtained.<br />
Each attendee will be provided with an induction<br />
on the HAAKE ViscoTester VT550, hard copy of<br />
the full method and procedures for each<br />
measurement conducted, copies of their results,<br />
and an information folder including the theory of<br />
rheology, dictionary definitions, copies of the Tim’s<br />
Top Tips – How To series for their specific<br />
industry and relevant product information.<br />
At the conclusion of the testing of customer<br />
samples, a wrap up session will be conducted to<br />
cover questions and review of the data and<br />
results.<br />
Each half day workshop will be industry specific<br />
and conducted either as public or private<br />
sessions.<br />
This series of workshops is of particular interest<br />
to all QA/QC, process engineers, production and<br />
laboratory staff across the following industries:<br />
• Food Industries<br />
• Pharmaceutical, Cosmetics & Allied Industries<br />
• Surface Coatings Industries<br />
• Mineral Slurries<br />
• Construction and Building Materials Industries<br />
• Chemical & General Manufacturing<br />
Interested? Contact <strong>Rheology</strong> <strong>Solutions</strong><br />
to register your interest in the series.<br />
Each workshop will be limited to 6 – 9 attendees<br />
to ensure that each attendee will have maximum<br />
opportunity for hands on training and operation of<br />
the HAAKE ViscoTester VT550 and adequate<br />
discussion with Dr Tim Kealy during the<br />
workshop.<br />
Further information on the HAAKE<br />
ViscoTester VT550 can be obtained from<br />
www.rheologysolutions.com/viscotester550_<br />
techs.html<br />
news & views<br />
<strong>Rheology</strong> <strong>Solutions</strong> 10th Anniversary<br />
all industries<br />
On Wednesday 30 April, 2008,<br />
<strong>Rheology</strong> <strong>Solutions</strong> turned 10.<br />
There have been a lot of changes over the 10<br />
years since <strong>Rheology</strong> <strong>Solutions</strong> was formed, with<br />
the business starting out of a home office in rural<br />
Victoria. Four years ago, the office moved to<br />
facilitate the growing business needs some 15<br />
kms closer to Melbourne in Bacchus Marsh. The<br />
move has meant that the local staff that we<br />
employ also moved with us.<br />
<strong>Rheology</strong> <strong>Solutions</strong> was established by Pat &<br />
Kaye Griffin and both are still full time and active<br />
in the business. I think that there is the hope that<br />
long service leave may apply at some point in the<br />
near future for both of them.<br />
Jackie joined us just over six years ago as a<br />
Marketing Assistant working part time, and now<br />
has the diverse role of Administration Manager<br />
and works full time.<br />
Richard has always had an involvement with the<br />
business, and has been with us since Pat & Kaye<br />
relocated back to Victoria after a four year stay in<br />
Sydney over 10 years ago. Richard’s role is<br />
National Service Engineer across the entire<br />
product range we offer – it certainly keeps him<br />
on his toes and ensures that his frequent flyer<br />
points continue to rack up.<br />
<strong>Rheology</strong> <strong>Solutions</strong> will continue to offer the world<br />
leading products in temperature control, polymer,<br />
rubber, optical scanning systems, rheology and<br />
viscometry instruments and equipment and are<br />
committed to maintaining their specialisation<br />
and dedication to the science of materials<br />
characterisation.<br />
Our vision is to recognise the importance of<br />
specialisation and dedication to a specific science<br />
and to provide full technical support and service<br />
throughout Australia. Our company goal is to<br />
integrate industry experience and materials<br />
characterisation techniques to provide practical<br />
solutions for customers.<br />
All of us at <strong>Rheology</strong> <strong>Solutions</strong> thank you for your<br />
business over the last ten years and we look<br />
forward to being of continued service to you. <br />
biennial 07-08<br />
39
news & views<br />
New Web Site Additions<br />
During 2007 a number<br />
of new features and<br />
functions will be made<br />
available on the <strong>Rheology</strong><br />
<strong>Solutions</strong> website<br />
www.rheologysolutions.com<br />
Biennial RheoTalk – Now available<br />
as a PDF on line<br />
This inaugural cumulative Biennial RheoTalk issue<br />
has been compiled to provide our Australian<br />
customers and readers of RheoTalk with an easy<br />
reference and source of the product information,<br />
application articles and news from 2005 – 2006.<br />
The newsletter has been cross indexed and<br />
referenced by industry, so that each key industry<br />
area can identify the specific information that<br />
relates to their industry. The industry<br />
classifications that we have used are colour<br />
coded and cover:<br />
• Mineral Slurries<br />
• Polymer Industries<br />
• Food Industries<br />
• Surface Coatings Industries<br />
• Chemical & General Manufacturing Industries<br />
• Construction & Building Industries<br />
• Pharmaceutical, Cosmetics & Allied Industries<br />
Additionally, the indexes have been divided into<br />
three sections covering Application Notes, News &<br />
Views, and Product News & Industry Applications.<br />
There is an index at the beginning of each of<br />
these sections, listing the contents within that<br />
section with a cross reference to the industry that<br />
it applies to.<br />
The PDF enables the reader to utilise the search<br />
facility with the software. This means that<br />
searching can be conducted by any word, phrase,<br />
industry type, brand name, application or product<br />
model.<br />
At the end of the cumulative issue of RheoTalk an<br />
information request form has been provided for<br />
those that require further information. The form<br />
can be printed and filled out and then either faxed<br />
or posted. Alternatively, requests can be sent by<br />
biennial 07-08<br />
all industries<br />
email direct to info@rheologysolutions.com with<br />
details of the information requested.<br />
We trust that the Biennial RheoTalk will be a<br />
useful and easy source to access industry<br />
specific rheology and materials characterisation<br />
information that we have provided during 2005 –<br />
2006.<br />
Interactive Dictionary… Coming soon<br />
As a continuation of our commitment to providing<br />
education, knowledge and resources to industry,<br />
<strong>Rheology</strong> <strong>Solutions</strong> has developed an extensive<br />
materials characterisation dictionary covering<br />
seven key industry areas. The dictionary explains<br />
both rheological and industry specific terminology<br />
and relates it to measurement techniques and<br />
instrumentation.<br />
The interactive dictionary will be available on line<br />
as a PDF which can be searched according to<br />
industry type (Food, Chemical, Pharmaceutical,<br />
Cosmetics, Construction, Building, Surface<br />
Coatings, Polymer, and or Mineral), term, and<br />
product brand.<br />
The dictionary will have links to a summary page<br />
specific to each industry classification which will<br />
detail all the available information for that<br />
industry. This information can then be requested<br />
and will be supplied as hard copy.<br />
The interactive dictionary has been developed to<br />
provide industry with a reference source that<br />
relates their terminology to the governing<br />
properties and measurement information for<br />
material characterisation solutions. The benefit of<br />
this dictionary is that it has been created from the<br />
industry perspective using their process terms<br />
and providing an overview of how to identify,<br />
measure, and apply testing protocols.<br />
40 www.rheologysolutions.com
new & views<br />
Sensor System to Measure<br />
Viscosity of Tailings from Marimex<br />
mining industries<br />
A new sensor style from<br />
Marimex Industries Corp.<br />
now extends its application<br />
base into the mining<br />
industry.<br />
This sensor is based on a standard Marimex<br />
design but employs a special coating to inhibit<br />
the abrasive conditions often found in the mining<br />
industry. Previously such sensors have already<br />
been used without coating in similar industries<br />
like cement and concrete applications, where<br />
abrasion is also very high. The use of this special<br />
coating is expected to extend the lifetime of the<br />
sensor.<br />
As environmental impacts are being felt around<br />
the world, it is also felt in the mining industry<br />
especially as it applies to water usage. In many<br />
areas water has become a precious resource and<br />
steps need to be taken to limit use of water.<br />
Viscosity measurement can assist in determining<br />
and limiting such water usage as an example in<br />
tailings streams. Already a relatively small<br />
additional amount of water to a tailings stream<br />
will lower the viscosity of the stream by an<br />
info@rheologysolutions.com<br />
amount measurable with a Marimex viscometer.<br />
Marimex viscometer sensors provide a high<br />
resolution measurement in process and yet are<br />
rugged for the application. Different styles are<br />
available to cover a wide range of measurement.<br />
Every system is factory calibrated and capable to<br />
measure over multiple decades of viscosity.<br />
Systems can be easily field configured to<br />
measure 1% of the calibrated range as a full<br />
range yet again with the resolution still being 1%<br />
of the configured range. No change or physical<br />
modification to the sensor is required. A<br />
configuration change on the transmitter is all that<br />
is required.<br />
Together with the introduction of this new sensor<br />
Marimex is also introducing new electronics.<br />
Based on the proven technology of the model VS-<br />
4450 the new model VS-D250 reduces both the<br />
size and the price of the transmitter. This has<br />
been achieved by repacking the electronics and<br />
leaving off a few capabilities, which are often not<br />
required in some applications. The model VS-<br />
D250 is housed in a DIN rail housing and can<br />
easily be mounted in a back panel rather than<br />
taking up front panel space. It is capable to carry<br />
two output cards which are available as 4 to 20<br />
mA analog outputs or RS485 and RS232 serial<br />
outputs. An additional RS232 output is available<br />
on the front plate as well and can be used for all<br />
included Modbus capabilities including<br />
configuration via a computer. Power supply for<br />
this transmitter is 24 VDC, which makes it easy to<br />
be connected to a non-interruptible 24 VDC<br />
power supply. A model VS-C250 with the similar<br />
capabilities as the model VS-D250 is also<br />
available. This model is for insertion directly into a<br />
sensor. however due to the mounting inside the<br />
sensor, this electronics can only be configured via<br />
a computer, whilst the model VS-D250 can also<br />
be configured by hand via three push buttons.<br />
workshop<br />
High Temperature Micro-<strong>Rheology</strong><br />
food industries<br />
polymer industries<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
chemical & allied industries<br />
High temperature rheology and simultaneous<br />
microscopy on polymer melts is now achievable.<br />
Thermo Scientific have developed the HAAKE<br />
MARS with RheoScope module to meet the<br />
customer requirements for high temperature<br />
rheology and microscopy applications.<br />
<strong>Rheology</strong> <strong>Solutions</strong> will conduct an applications<br />
workshop with the equipment in Victoria where<br />
customers can bring their own samples for<br />
testing.<br />
This product will be of interest to R&D, Research<br />
Organisations, Universities, Food, Polymer,<br />
Pharmaceutical, Cosmetic & Allied Industries and<br />
Chemical Industries.<br />
If you are interested in purchasing this equipment<br />
to meet your application requirements, let us<br />
know now. We will then coordinate the<br />
workshop with the support of Thermo Scientific<br />
and advise you of the planned date.<br />
Send an email with details of your<br />
application and any questions that you have<br />
to kayegriffin@rheologysolutions.com <br />
biennial 07-08<br />
41
news & views<br />
CoolTech Application Story<br />
Recently <strong>Rheology</strong> <strong>Solutions</strong><br />
sold a CoolTech 320<br />
refrigerated circulator to<br />
REHAU Pty Ltd for use<br />
in a display at a recent<br />
exhibition in Melbourne.<br />
The application where the<br />
CoolTech was used was<br />
quite unusual and outside<br />
of the 'square'.<br />
biennial 07-08<br />
all industries<br />
At the DESIGNEX expo held at the Melbourne<br />
convention centre 19 - 21st April, 2007, REHAU<br />
used the Thermo Scientific CoolTech 320<br />
refrigerated circulator unit and 16mm RAUPINK<br />
under floor heating pipe to set up an ice bar<br />
along side their 'Under floor heating display'. The<br />
aim of which was to provide a visual indicator to<br />
their customers and show them the conductive<br />
nature of their RAUPINK pipe.<br />
The pipe was set up in a snail formation within a<br />
stainless tray. The CoolTech 320 was set up at<br />
-8ºC for the duration of the three day expo.<br />
Customers were able to physically see and touch<br />
the ice, which was then used to serve shots of<br />
CoolTech 320 installed RAUPINK under floor heating pipe Afternoon tea<br />
In March 2007 <strong>Rheology</strong><br />
<strong>Solutions</strong> attended the<br />
conference in WA and<br />
exhibited the HAAKE<br />
Viscotester VT550 and took<br />
over 150 copies of Tim's<br />
Top Tips “How to Measure<br />
Series” for the mining<br />
industry.<br />
The response from the attendees to the HAAKE<br />
ViscoTester VT550 was positive with 10 HAAKE<br />
ViscoTester VT550 Slurry Packages being sold<br />
during the exhibition. The copies of the “How to<br />
Measure Series” for the mining industry was also<br />
schnapps to them at the afternoon tea break.<br />
According to REHAU the project was a great<br />
success and proved to be very popular with their<br />
customers.<br />
REHAU is an independent and privately owned<br />
company with over 120 branches, 44 plants and<br />
12 training academies across 53 countries,<br />
REHAU is one of the world's leading polymer<br />
solutions providers. Their products are found in a<br />
wide range of applications from energy efficient<br />
uPVC windows and automotive bumper systems<br />
to life-preserving medical components for the<br />
healthcare industry. www.rehau.com.au<br />
news & views<br />
Update on Paste and Thickened<br />
Tailings Conference<br />
mining industries<br />
of great interest - especially the booklet covering<br />
'Yield Stress'. Almost all the copies were gone by<br />
the middle of the second day of the conference,<br />
and before the end of the conference there were<br />
no copies left.<br />
If you missed out on the 'How To Series'<br />
for mining industries and would like copies,<br />
complete the information request form<br />
and we will send them to you.<br />
42 www.rheologysolutions.com
feature story<br />
Uncompromising Eyes<br />
polymer industries<br />
chemical & allied industries<br />
food industries<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
Film Inspection. Online<br />
inspection systems are an<br />
established part of high-quality<br />
film production today. A<br />
manufacturer of PE laminating<br />
and surface protection films is<br />
used to illustrate the<br />
incorporation of an integrated<br />
quality concept with the aid of<br />
practical examples<br />
info@rheologysolutions.com<br />
By Gerd Finn - Orbita Film<br />
Oliver Hissmann - Optical Control Systems<br />
PE surface protection, interlayer, label and<br />
laminating films have to meet very high quality<br />
requirements. In particular, these films must<br />
have the lowest possible number of fish-eyes,<br />
which are unavoidable in PE films. Fish-eyes are<br />
small film homogeneities characterised by their<br />
area (size in transmitted light) and protrusion<br />
above the film surface. The fish-eye count is to<br />
some extent an inherent film property. Film<br />
manufacturers and users therefore try to<br />
minimise the fish-eye count and fish-eye size to<br />
a level where the fish-eyes pose no problem for<br />
the particular film converting process and<br />
intended application. See Figure 1.<br />
Continued on page 44<br />
• news & views<br />
How to measure series for mining slurries<br />
mining industries<br />
Three “How to Measure” tips<br />
have been written for mining<br />
slurries and are available on<br />
request. The series provides a<br />
booklet which details tips on<br />
measuring thixotropy, flow &<br />
viscosity curves, and yield<br />
stress.<br />
Thixotropy is a relative measurement and as such<br />
depends on the experimental conditions and<br />
technique used to measure it. There are several<br />
such techniques, the simplest being modified flow<br />
curves, or constant shear rate or shear stress<br />
measurements. A more complicated, but perhaps<br />
more intuitively understood method is the shear<br />
and recovery method.<br />
In order to attain repeatability the most appropriate<br />
technique should be selected and the sample<br />
handling and experimental procedures defined<br />
fully. These should be unchanged for all tests, so<br />
that thixotropy for different materials can be<br />
properly compared.<br />
Thixotropy is a relative measure of the extent and<br />
seed of recovery of the internal structure of a<br />
material during and after shear. It is useful<br />
because it allows and estimate of the effects of<br />
agitation, pumping etc for prolonged periods, and<br />
also the effects of ceasing the agitation etc (i.e.<br />
how quickly the structure will rebuild, and how<br />
difficult it will be to restart the process as a result).<br />
Flow & Viscosity Curves. A flow curve is used to<br />
define the interdependency of the shear rate and<br />
shear stress for a material. To generate a flow<br />
curve either a range of shear rates or of shear<br />
stresses can be imposed on the material, and the<br />
other of the pair – the response of the material –<br />
is measured. A viscosity curve shows the viscosity<br />
of a material at each shear rate from the flow<br />
curve. Flow and viscosity curves can be presented<br />
either on logarithmic or linear axes. They describe<br />
the flow behaviours at a variety of shear rates, so<br />
that pump, pipe, impeller, etc sizing can be<br />
correctly achieved. They are also important<br />
because they define the type of flow behaviour<br />
one can expect from a material – Newtonian,<br />
• exhibitions<br />
Ausplas 2008<br />
polymer industries<br />
<strong>Rheology</strong> <strong>Solutions</strong> will be participating<br />
in this exhibition (booth number 100) in<br />
Melbourne from 7 – 10 October 2008<br />
showcasing a range of equipment and<br />
instruments specifically for the polymer<br />
industry.<br />
pseudoplastic (shear thinning), dilatant (shear<br />
thickening) etc.<br />
Yield Stress has an impact on the mining industry<br />
in a variety of ways. In pumping and mixing at<br />
start-up, it must be overcome so that the impellers<br />
can turn. In pipeline transport yield stress<br />
influences the velocity profile of the material, and<br />
under some circumstances can cause the material<br />
to flow as a solid plug carried by a lubricating<br />
liquid layer at the wall where shear stresses are<br />
high. The yield stress of a material dictates<br />
whether or not a solid fraction will settle to the<br />
bottom of a tank, pipe or other container, and also<br />
whether gaseous materials can rise through it.<br />
Disposal of mining waste is an important issue<br />
and the yield stress influences the slope of<br />
beaches in disposal areas, the ability of high solids<br />
pastes to be compressed and to flow after<br />
disposal and so on.<br />
Note: Each Tip includes working definitions.<br />
Copies of How to Measure … Yield Stress,<br />
Thixotropy, Flow & Viscosity Curves are available<br />
on request. <br />
biennial 07-08<br />
43
Feature Story<br />
Uncompromising Eyes<br />
Continued from page 43<br />
Figure 1. Film with foreign contaminant<br />
Causes of Fish-eyes<br />
In higher-molecular-weight constituents from the<br />
polymeristaion process or foreign polymeric<br />
materials do not completely melt, they form fisheyes.<br />
Contaminants such as dust from bulk<br />
containers, abraded particles in material transfer<br />
lines and foreign materials, e.g. from poorly<br />
cleaned silos, can also cause fish-eyes. During<br />
the transfer of PE pellets in pipelines, some of the<br />
PE pellets melt and smear on the walls of the<br />
pipelines due to abrasion and form ribbon-like<br />
streamers (angle hair) that gradually flake off into<br />
the pellet stream. While the streamers are still<br />
adhering to the pipeline walls, their large surface<br />
area comes into prolonged contact with<br />
atmospheric oxygen. This gives rise to reactive<br />
molecular groups, which form fish-eyes. Deposits<br />
on the inside wall of the extruder or excessively<br />
long thermal exposure during a stoppage can<br />
lead to fish-eyes with characteristic brownish<br />
occlusions. Poorly homogenised additives such as<br />
pigments, antiblocking agents, etc. act as nuclei<br />
around which polymer accumulates to form fisheyes.<br />
See figures 2 & 3.<br />
Figure 2. Fish-eye in a coextruded centre layer<br />
biennial 07-08<br />
Figure 3a & Figure 3b. 3-D view of a fish eye<br />
Problems with<br />
Contaminants<br />
Surface protection films are coated with adhesive<br />
and bonded to high-gloss metal surfaces<br />
(aluminium sheet, stainless steel sheet) or<br />
scratch-sensitive plastic surfaces (PMMA, PC,<br />
PVC) to protect these vulnerable surfaces during<br />
further processing and transport. In<br />
thermoforming - for example into headlamp<br />
reflectors or kitchen sinks - excessively large fisheyes<br />
press slightly into the surface and leave<br />
behind noticeable imperfections, which are not<br />
accepted in final quality control inspection.<br />
The same effect can occur with interlayer films<br />
wound up in aluminium coils to protect the<br />
aluminium layers from each other. As a result of<br />
the winding pressure, marks can be left.<br />
Fish-eye mark in an aluminium sheet<br />
Labeling films and special laminating film are<br />
printed with sophisticated motifs. The fish-eyes<br />
give rise to blank unprinted dots, which show up<br />
particularly in large plain-coloured areas. In<br />
addition, in the laminating process, the fish-eyes<br />
can be pressed into the film. This results in<br />
indentations that are many times larger and<br />
therefore much easier to see that the fish-eyes<br />
that produced them. In the subsequent printing<br />
operation, no link is deposited in these<br />
indentations and once again, there is a “halo”<br />
around the fish-eye. See figure 4.<br />
Figure 4. Black fish-eye with halo in a film<br />
laminated to aluminium<br />
PE Laminating films are bonded to other materials<br />
(e.g. PET, PP, PA, aluminium) with adhesive. If<br />
there are fish-eyes present in the film, a “halo” is<br />
again formed around the fish-eye, rather like an<br />
air-filled bubble, which is far larger than its origin<br />
and therefore much easier to detect as a flaw.<br />
The most critical flaws are brownish or black fisheyes<br />
from extruder deposits, which are<br />
interpreted as contamination. Such defects are<br />
absolutely impermissible in the pharmaceutical<br />
and food packaging industries. In film composites<br />
with aluminium foil, large fish-eyes can even<br />
impair barrier properties in the worst case<br />
scenario.<br />
Film Inspection<br />
Modern-day inspection systems have a data rate<br />
of up to 160MHz per camera (see Figure 5)<br />
Continued on page 45<br />
44 www.rheologysolutions.com
Continued from page 44<br />
because of the “embedded PC” concept. This<br />
concept permits the storage and transfer of all<br />
measurement data via the Ethernet to a server.<br />
According to the application, CCF line cameras<br />
with 2,048, 4,096, 6,144 or 8,192 pixels can be<br />
used. These achieve image acquisitions rates<br />
ranging from 72,000/s at 2,048 pixels to<br />
18,000/s at 8,192 pixels. So even at very high<br />
web speeds, high resolution in the web direction<br />
is obtained. Through the use of special lenses<br />
and the further development of CCF sensors, the<br />
reproduction quality of long CCD lines (e.g. 8,192<br />
pixels) is just as sensitive as for shorter CCD lines<br />
(e.g. 2,048 pixels). This means equally good<br />
inspection results for considerably lower<br />
investment costs.<br />
Figure 5. Inspection system for a blown film line<br />
A simple example will serve to illustrate the<br />
advantages of using long CCD sensors. A blown<br />
film line with a width of 2,600mm and maximum<br />
web speed of 120mm/min is to be inspected with<br />
a resolution of 200μm in both the web travel and<br />
transverse directions. To achieve this resolution,<br />
either four cameras with 4,096 pixels each or two<br />
cameras with 8,192 pixel cameras, a better<br />
price/performance ratio is obtained with equally<br />
good inspection results because of the lower<br />
purchase, maintenance and operating costs.<br />
The systems detect and distinguish defects such<br />
as fish-eyes, gel particles, scorch marks, black<br />
specs, streaks, lines and insects. Depending on<br />
its configuration, the inspection system can warn<br />
the operator of critical individual defects (e.g. a<br />
fly), defect trends (e.g. more than 10 gel particles<br />
in a diameter between 200 and 300 m/m2) or<br />
film rolls that are off-spec. Online, production<br />
trends can be mapped over extended periods of<br />
time, e.g. the last twelve hours. Offline, whole<br />
runs can be compared and analysed in order to<br />
info@rheologysolutions.com<br />
assess, for example, the fish-eye count obtained<br />
with different raw material batches on specific<br />
extruders. See Figure 6.<br />
Figure 6. Fish-eye count plotted against time<br />
Self-learning Systems<br />
By using the so-called easy-teach-in-function, the<br />
operator can identify defects with the aid of<br />
defect pictures and sort them into classes. The<br />
classifier then automatically specifies the<br />
inspection parameters for the individual defects.<br />
Since these systems work with fuzzy algorithms,<br />
they are able, for example, to differentiate flies<br />
from black specs. This differentiation is crucially<br />
important, since the cause of the defect may lie<br />
in either the clean room environment or the<br />
production process. Similarly, fluff attracted by<br />
static charges is classified as such and therefore<br />
not identified as a defect. See Figure 7.<br />
Figure 7. Topographical representation (rolling<br />
map) of the fish-eyes with photos of defects<br />
Lighting Technology<br />
The use of the right lighting technology is vitally<br />
important for film inspection. The standard<br />
lighting normally comprises fast-pulse fluorescent<br />
tubes. But fibre-optic or LED lighting is also<br />
employed. The lighting may be used as reflected<br />
or transmitted light. If possible, transmitted light is<br />
preferred because it enables both sides of the<br />
film to be inspected. On the other hand, physical<br />
irregularities, such as scratches, in opaque<br />
surfaces can be more reliably detected in<br />
reflected light. Another bonus of film surface<br />
inspection is that the absolute and relative opacity<br />
of transparent and translucent materials can be<br />
determined.<br />
Integrated Quality<br />
Concept<br />
For quality control of PE films, even today, film<br />
samples are still sometimes taken from the end<br />
of the roll and visually inspected by employees.<br />
The results of such an inspection are very<br />
subjective and relate to only a tiny product<br />
quantity. In other words, they are not statistically<br />
meaningful. Counting the fish-eyes is a more<br />
objective method but very time-consuming. But<br />
here again, only a small random sample is taken<br />
and the assessment of fish-eyes is also<br />
subjective. Counting the fish-eyes on the running<br />
machine by manual assessment is even less<br />
objective because of the film movement. In the<br />
random sample inspection at the end of the roll,<br />
defects are not identified until some hours after<br />
production. If the film is faulty, considerable<br />
amounts of material are wasted in this way and<br />
production times are squandered.<br />
To ensure continuous monitoring of the<br />
production process, the subjective assessment of<br />
quality must be replaced by an objective method.<br />
For this purpose surface inspection systems like<br />
the FSP600 film quality inspection system from<br />
OCS GmbH, Witten, Germany, can be used. At<br />
Orbita-Film GmbH, Weißandt-Gölzau, Germany,<br />
several such inspection systems have been<br />
installed since 1994. Some systems operate with<br />
one camera and scan widths of 300mm or<br />
700mm. One system is equipped with three<br />
cameras and monitors a film width of 3,000mm.<br />
The systems operate in transmitted light for<br />
transparent, translucent and opaque films up to a<br />
certain degree of opacity.<br />
Most equipment does not inspect the whole film<br />
width but only a section. With this philosophy,<br />
only the homogeneously distributed defects are<br />
statistically detected. Depending on the film<br />
width, 30 to 70% of the entire film width is<br />
scanned in contrast to the maximum of 0.005%<br />
with manual inspection.<br />
In transmitted light, only the optically effective<br />
surface of the fish-eyes in the plane of the film is<br />
Continued on page 46<br />
biennial 07-08<br />
45
Continued from page 45<br />
detected. The fish-eyes that are actually<br />
detrimental, i.e. those which protrude significantly<br />
above the film surface, are far fewer in number<br />
than the measured and displayed fish-eye count.<br />
Because of the difficulty of picking out these<br />
“projecting” fish-eyes from the rest, the total fisheye<br />
count is generally recognised as an index for<br />
the level of fish-eyes. The principal advantages of<br />
these systems are objective, reproducible<br />
inspection of surface quality and the possibility of<br />
reacting immediately to changes in the fish-eye<br />
level.<br />
The systems are integrated in the company's<br />
internal network. With each roll change, the<br />
inspection data for the particular roll are<br />
automatically stored on an internal server by roll<br />
number and production data.<br />
Application Examples<br />
An example of the successful use of fibre-optic<br />
lighting by Orbita is the inspection of black and<br />
white surface protection films for stainless steel<br />
in transmitted light. Each fish-eye causes an<br />
optical dint in the stainless steel. This<br />
phenomenon is intensified by a thermoforming<br />
process. Because of its high opacity, the film is<br />
very difficult to inspect in transmitted light but<br />
double-sided inspection in reflected light is very<br />
costly and technically complex to achieve.<br />
news & views<br />
Staff Update<br />
Evie has grown<br />
considerably since her first<br />
photo début in RheoTalk<br />
(January - April 07 issue).<br />
She turned 6 months on April 15 and is nearly<br />
full grown at just under 17 kg in weight, which is<br />
still a long way from Mal's weight of 43 kgs. Mal<br />
celebrated his 11th birthday on March 19 and is<br />
biennial 07-08<br />
Inspection systems with a camera are used in the<br />
blown film lines. Only a section of the films are<br />
inspected with resolutions up to 100μm. This<br />
statistically monitoring is sufficient to guarantee<br />
fish-eye-free film quality.<br />
The cast film lines for self-adhesive film with<br />
widths of up to 2,600mm are 100% inspected. In<br />
this case, a very high resolution is achieved to<br />
detect even the smallest defect. The 100%<br />
inspection also enables optimum setting of both<br />
the extruder and the die.<br />
In the adhesive coating zone, Orbita also monitors<br />
the complete web. Here a wide variety of defects<br />
in the film are detected as defects of adhesive<br />
application. In this way, the coating process is<br />
optimised and absolute quality control achieved.<br />
Conclusion<br />
The use of online inspection systems for surface<br />
inspection of PE films has proved successful in<br />
practice and permitted faster, more efficient<br />
detection of surface defects in recent years. As a<br />
result, it has been possible to reduce the number<br />
of rejects and complaints. With these systems, it<br />
is possible to meet continually increasing product<br />
quality requirements, while ensuring efficient<br />
production.<br />
finding that keeping up with a young Border<br />
Collie is challenging. Mal has the strength to play<br />
for a long time - but Evie certainly has the turn of<br />
speed when needed.<br />
Being at work for them is part of their daily<br />
routine - as soon as the car keys are picked up<br />
they are at the door and ready to leave - this is<br />
regardless of whether it is time to come to work<br />
or time to leave. A trip in the car anywhere is<br />
always a happy outing for them both.<br />
About the Authors<br />
Dipl-Phys. Gerd Finn, born 1943, is Quality<br />
Control Manager at Orbita-Film GmbH, Weißandt-<br />
Gölzau<br />
Dipl-Oec. Oliver Hissmann, born in 1970, is Sales<br />
Manager at OCS Optical Control Systems, Witten<br />
Poli-Film Group<br />
As a subsidiary of the globally active Poli-Film<br />
Group, Orbita-Film GmbH is a leading German<br />
manufacture of polyethylene films. Films ranging<br />
in thickness from 7 to 500μm are produced in<br />
widths from 50 - 18mm at this manufacturing<br />
facility, which has a built area covering 51,000m 2<br />
and total area of 210,000m 2 . The company's site<br />
at Weißandt-Gölzau is home not only to Orbita-<br />
Film but also to its sister companies Orbita-Cast<br />
and Poli-Coat, which offer a similarly wide range<br />
of products. The films are used in the packaging,<br />
construction, agricultural and horticultural sectors<br />
as well as in industry and the retails trade.<br />
At Orbita-Film, some 50 blown film machines are<br />
installed in total. At Orbita-Cast (stretch film<br />
producer) and Poli-Coat (manufacturer of surface<br />
protection films), the products are extruded using<br />
the cast film method. www.orbita-film.de<br />
A full copy of the paper is available on<br />
request by quoting OCS005<br />
46 www.rheologysolutions.com
news & views<br />
Customer Installation<br />
polymer industries<br />
Plantic Technologies Ltd in<br />
Altona Victoria recently<br />
purchased a HAAKE PolyLab<br />
with rheology dies.<br />
The system that was purchased included the<br />
HAAKE Rheocord torque rheometer drive unit with<br />
mixer (with Banbury, sigma and roller rotors) and<br />
single screw extruder (with an adjustable lip film<br />
die, and slit and capillary rheology dies).<br />
Plantic Technologies Limited is a world leading<br />
innovator in bioplastics, with a track record of<br />
science and industry awards, an international<br />
network of corporate customers and distributors,<br />
and a growing list of premium quality<br />
info@rheologysolutions.com<br />
multinational research and development partners.<br />
Plantic Technologies is based in Australia, where<br />
its head office, principal manufacturing and R&D<br />
facility is located. The company also has sales<br />
offices in German and the United Kingdom, and<br />
employs approximately 40 people internationally.<br />
A New Approach to Plastic<br />
Plantic has achieved a unique place in the world<br />
market for bioplastics through proprietary<br />
technology that delivers a completely<br />
biodegradable and organic alternative to<br />
conventional plastics based on corn; which is not<br />
genetically modified. The entire process integrates<br />
the science of organic innovation with commercial<br />
and industrial productivity in a new way. The<br />
result is both a broad range of immediate<br />
performance and cost advantages, and long-term<br />
environmental and sustainability benefits.<br />
Plantic's single-minded commitment is to provide<br />
bioresponsible materials solutions for the world<br />
market that deliver all the functionality of<br />
conventional petrochemically derived plastics in<br />
an economical and ecosensitive way.<br />
The torque rheometer will be used to measure<br />
the relative processing properties of various<br />
thermoplastic starch (TPS) blends and resins in<br />
R&D. The sheet die will be used to mimic larger<br />
scale processes, to optimise screw<br />
configuration & processing conditions for the<br />
different TPS grades in R&D. The rheology (slit<br />
and capillary) dies will help to characterise the<br />
TPS grades for efficient processing.<br />
Rod capillary die at Plantic Technologies is<br />
used for rheological characterisation of polymeric<br />
materials.<br />
biennial 07-08<br />
47
news & views<br />
The Mayonnaise Jar<br />
& Two Cups of Coffee<br />
This article discusses defects<br />
that may possibly occur during<br />
production of film on<br />
calendaring equipment as well<br />
as the sources of black spots,<br />
their detection, evaluation and<br />
possible means of prevention.<br />
The article was written by Andreas Schnabel<br />
(works in the filed of metrology and process<br />
biennial 07-08<br />
all industries<br />
When things in your life seem<br />
almost too much to handle,<br />
when 24 hours in a day are<br />
not enough, remember the<br />
mayonnaise jar and the<br />
2 cups of coffee.<br />
A professor stood before his philosophy class and<br />
had some items in front of him. When the class<br />
began, he wordlessly picked up a very large and<br />
empty mayonnaise jar and proceeded to fill it with<br />
golf balls. He then asked the students if the jar<br />
was full. They agreed that it was.<br />
The professor then picked up a box of small<br />
pebbles and poured them into the jar. He shook<br />
the jar lightly. The pebbles rolled into the open<br />
areas between the golf balls. He then asked the<br />
news & views<br />
High-Quality Pharmaceutical Film –<br />
Customer story Klockner Pentaplast, Germany.<br />
polymer industries<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
students again if the jar was full. They agreed that<br />
it was.<br />
The professor next picked up a box of sand and<br />
poured it into the jar. Of course, the sand filled up<br />
everything else. He asked once more if the jar<br />
was full. The students all responded with a<br />
unanimous "YES".<br />
The professor then produced two cups of coffee<br />
from under the table and poured the entire<br />
contents into the jar effectively filling the empty<br />
space between the sand. The students laughed.<br />
"Now", said the professor as the laughter<br />
subsided, "I want you to recognise that this jar<br />
represents your life. The golf balls are the<br />
important things--your family, your children, your<br />
health, your friends and your favourite passions -<br />
and if everything else was lost and only they<br />
remained, your life would still be full".<br />
"The pebbles are the other things that matter, like<br />
your job, your house and your car".<br />
technology at Klochner Pentaplast GmbH & Co<br />
KG, Montabaur, Germany; and Oliver Hissmann<br />
(employed by OCS GmbH, Witten, Germany).<br />
Pharmaceutical products are packaged in plastic<br />
blister packs around the world. Every customer<br />
expects that the film used satisfies increasingly<br />
stringent requirements. In addition to economy,<br />
hygiene, protection in different climates and<br />
atmospheres, this also means a guarantee of<br />
maximum safety for the product packaged in<br />
compliance with new and ever more demanding<br />
requirements.<br />
The monolayer film that is produced primarily on<br />
calendaring equipment is converted into blister<br />
packs or serves as the substrate for high-quality<br />
"The sand is everything else - the small stuff".<br />
"If you put the sand into the jar first" he<br />
continued, "there is no room for the pebbles or<br />
the golf balls. The same goes for life. If you spend<br />
all your time and energy on the small stuff you<br />
will never have room for the things that are<br />
important to you".<br />
"Pay attention to the things that are critical to<br />
your happiness. Play with your children, look after<br />
your health, take your spouse out to dinner. Play<br />
another 18 holes. There will always be time to<br />
clean the house and fix the car. Take care of the<br />
golf balls first--the things that really matter. Set<br />
your priorities. The rest is just sand".<br />
One of the students raised her hand and inquired<br />
what the coffee represented. The professor<br />
smiled, "I'm glad you asked". "It just goes to<br />
show you that no matter how full your life may<br />
seem, there's always room for a couple of cups<br />
of coffee with a friend".<br />
coatings and laminates. These calendered<br />
monolayer films are plasticizer-free rigid PVC<br />
films that are manufactured in various<br />
thicknesses and colours. They can be classified<br />
into three product groups: With their good<br />
thermoforming characteristics and their good<br />
chemical resistance, homopolymer films are wellsuited<br />
for production of standard blister packs.<br />
For demanding blister geometries or maximum<br />
processing speeds, copolymer and high<br />
copolymer films offer greatly improved flow<br />
characteristics.<br />
A reprint of the paper from Kunstoffe<br />
international 7/2007, is available on<br />
request from <strong>Rheology</strong> <strong>Solutions</strong> by quoting<br />
OCS-007<br />
48 www.rheologysolutions.com
industry overview<br />
Material Characterisation <strong>Solutions</strong><br />
food industries<br />
surface coatings industries<br />
polymer industries<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
chemical & allied industries<br />
Thermo Fisher Scientific<br />
offers a comprehensive range<br />
of material characterisation<br />
products that analyse and<br />
process material for<br />
rheological and thermal<br />
properties.<br />
These instruments analyse and measure viscosity,<br />
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mechanical changes of plastics, foods, adhesives,<br />
coatings, and a wide variety of liquids or solids.<br />
A brief overview of innovative solutions across a<br />
number of industries for R&D, Process, and QC<br />
applications follows:<br />
Ceramics<br />
Rheological measurement data relating to<br />
dispersability and flow characteristics of ceramic<br />
injection moulding compounds and pastes provide<br />
the ceramics industry with valuable information to<br />
optimise products. To do this, a flexible, modular<br />
rheometer platform is needed to evaluate product<br />
processes used for manufacturing ceramics and<br />
suspensions for porcelain and/or ceramics.<br />
Food<br />
Innovative recipe development, comprehensive<br />
reproduction simulation, and reliable quality<br />
assurance require a powerful rheometer platform<br />
in conjunction with pioneering measurement<br />
extruders and mixers.<br />
info@rheologysolutions.com<br />
Paints, Dyes & Powder Coatings<br />
Innovative paints and dyes demand extensive and<br />
precise rheological measurements. This begins<br />
with reliable quality control of raw materials and<br />
products and continues in the research and<br />
development of new formulations. Stability, time<br />
dependence, process characteristics when<br />
spraying or coating, and structural properties of<br />
these products must be derived in the early<br />
stages of development.<br />
Petrochemistry<br />
In the petrochemical industry simulation of pump<br />
characteristics and measurements for oils and<br />
drilling fluids under pressure is vital.<br />
Pharmaceutical & Cosmetics<br />
Understanding the processability, consistency,<br />
time- and temperaturedependent properties of<br />
raw materials and end products in order to<br />
develop innovative and successful products is<br />
critical.<br />
Polymers<br />
Processing-related data such as melt<br />
characteristics, the effect of additives,<br />
temperature, shear stability and dynamic viscosity<br />
during shear are of great significance to the<br />
development of innovative polymers. Process<br />
simulation in compounding and extrusion of rods,<br />
profiles or films, combined with rheological or<br />
visual measurements, help the plastics industry to<br />
optimise procedural parameters, to create<br />
inspection bodies for tests or to perform quality<br />
checks at incoming and outgoing goods for<br />
viscosity, dispersion or plastifying characteristics.<br />
Rubber<br />
The impact of carbon black on the cross-linking<br />
characteristics of a rubber compound and the<br />
dispersion or vulcanisation and flow properties of<br />
rubber are key to product quality. Furthermore,<br />
optimised end product mixing times are important<br />
not only to ensure efficient use of production<br />
plants, but also to successfully launch competitive<br />
products onto the market.<br />
Further information on your application<br />
requirements is available by requesting<br />
detailed information specific to your<br />
industry.<br />
biennial 07-08<br />
49
• news & views<br />
Staff Update<br />
Mal & Evie just getting ready to start a game in the<br />
office - it starts with a gentle torment and then<br />
fires up to tumbling and chasing<br />
At last there has been some well needed rain in<br />
Bacchus Marsh, not enough to do more than just<br />
wet the ground, but every drop counts.<br />
With the colder weather now approaching, both<br />
Mal & Evie spend more time in the office keeping<br />
warm.<br />
A game of chase in the office is often on the cards<br />
– it certainly breaks the routine of the day for<br />
them, and also for all of us. When the game is<br />
over, they are happy to lie back and catch up on a<br />
bit of shut eye. It doesn’t seem to matter to them<br />
where they lay down, they are happy for us to walk<br />
around them or over them – once they are settled<br />
they are down for the count – happy to rest and<br />
recuperate.<br />
biennial 07-08<br />
all industries<br />
• news & views<br />
Service Department Update<br />
all industries<br />
Recently, our service engineer<br />
Richard Donaldson has been<br />
travelled around Australia<br />
conducting installations<br />
and calibrations on a variety<br />
of the HAAKE Viscometers<br />
and Rheometers.<br />
Additionally, there were installations during this<br />
period for Optical Control Systems products.<br />
During an eight week period he has carried out<br />
calibrations on the HAAKE Viscotester VT550,<br />
HAAKE RheoStress, HAAKE RheoStress 600,<br />
HAAKE RheoStress 100 and HAAKE RotoVisco<br />
RV1. A total of 28 viscometers and rheometers<br />
have now been calibrated across, Queensland,<br />
Victoria, South Australia, Western Australia and<br />
New South Wales. His frequent flyer miles by now<br />
will be adding up to a sizable amount and well<br />
deserved.<br />
Just to ensure that he was kept fully occupied, he<br />
has also been involved in the installation of three<br />
HAAKE PolyLab's –one in Victoria and two in<br />
Queensland, and one PRISM EuroLab 16 mm twin<br />
screw extruder in Victoria.<br />
But the installations didn’t stop with the<br />
rheological instruments; there were also a<br />
number of Optical Control Systems (OCS) units<br />
installed during this same eight week period both<br />
into Victoria into separate companies. The<br />
systems installed were the OCS Surface<br />
Inspection system for the laboratory - FSA100,<br />
and the modular surface inspection system for<br />
in use in production - FSP600.<br />
Calibration overview<br />
The ability of a measurement device to accurately<br />
measure a physical quantity changes with a<br />
number of factors. Time in service, temperature,<br />
humidity, environmental exposure, and abuse can<br />
all affect your measurement accuracy of your<br />
instrument.<br />
Calibration quantifies this change in measurement<br />
accuracy and, when required, adjusts the device's<br />
measurement capability to decrease error.<br />
Whether your calibration needs are driven by<br />
ISO-9000 requirements, by company mandates, or<br />
by Good Laboratory Practice, <strong>Rheology</strong> <strong>Solutions</strong><br />
Pty Ltd can tailor our service to suit your needs.<br />
Why Re-Calibrate?<br />
The accuracy of the electronic components used<br />
in all instruments drifts over time. The effects of<br />
time in service as well as environmental conditions<br />
add to this drift. As time progresses, changes in<br />
component values cause greater uncertainty in<br />
your measurements. At some point in time, the<br />
drift causes the instrument's uncertainty to<br />
become undefined, meaning the manufacturer can<br />
no longer predict the uncertainty and guarantee<br />
measurement results. To resolve this issue<br />
instruments must be calibrated at regular intervals<br />
as defined by the manufacturer.<br />
Richard Donaldson, Service Engineer<br />
Calibration is the comparison of an instrument's<br />
performance to a standard of known accuracy.<br />
The result of a calibration may be documentation<br />
showing the deviation of a measurement from the<br />
known standard or it may also include adjusting<br />
the instrument's measurement capability to<br />
improve measurement accuracy.<br />
The goal of calibration is to quantify and improve<br />
the measurement accuracy of your instrument.<br />
The benefits of maintaining properly calibrated<br />
equipment include:<br />
• Reduced measurement errors<br />
• Consistency between measurements<br />
• Increases in production yields<br />
• Assurance you are making accurate<br />
measurements<br />
We recommend that you periodically calibrate your<br />
hardware to ensure measurement accuracy and to<br />
keep your devices operating in peak precision.<br />
If you have any queries regarding the timing<br />
or arranging for your HAAKE viscometer or<br />
rheometer to be calibrated, contact Jackie by<br />
email jackiew@rheologysolutions.com.<br />
50 www.rheologysolutions.com
• feature article<br />
Online Close-Loop Monitors<br />
Four Cast Film Extruders<br />
During Production<br />
polymer industries<br />
Applying the close-loop<br />
concept, a raw material<br />
producer’s off-line laboratory<br />
can perform continuous online<br />
metering, making optimisation<br />
of the process achievable.<br />
Following the principle of the close-loop concept,<br />
the conventional off-line laboratory is connected<br />
to the production process right on line, so the<br />
producer can control process and quality.<br />
info@rheologysolutions.com<br />
Small quantities of raw material are taken during<br />
processing, to obtain representative information<br />
to oversee the entire production. Before the<br />
introduction of the close-loop concept, data on<br />
the quality of production could take an entire<br />
shift before it was available.<br />
Online quality control<br />
Online quality control comprises two areas:<br />
measurement of the granules and measurement<br />
of the extruded cast or blown flim.<br />
Measuring the granules produces information on<br />
LAB colour value, Melt Index (MI), pellet size<br />
distribution (pellet size and shape distribution<br />
Online close-loop monitoring four<br />
production lines (cast film extruders).<br />
systems) as well as dust/abrasion and<br />
contamination (pellet scan systems).<br />
Yet, measuring the extruded film online makes<br />
statements on bittiness (gel count), additive<br />
content and physical properties (IR spectroscopy),<br />
brilliance (glossmeter) and/or the value of turbidity<br />
(hazemeter).<br />
Online pellet analysis<br />
Conducting pellet analysis online, a sampler<br />
withdraws the granules from the flow of<br />
continued on page 52<br />
biennial 07-08<br />
51
OnLine Close-Loop<br />
Monitors<br />
continued from page 51<br />
production. The system then automatically takes<br />
them to the measuring system, examines and<br />
sorts them. Those granules that meet the specified<br />
demands, are returned to the process.<br />
For the purpose of measuring the colour, the<br />
pellets are transported into a cuvette, where LAB<br />
values, yellowness index and several other colour<br />
values are determined.<br />
The Online Pellet Scan System, on a vibrating<br />
table or swivel plate, passes the transparent or<br />
opaque granules below a colour matrix camera.<br />
The pellets are examined as to colour soiling or<br />
foreign particles, and rejected if necessary.<br />
The Pellet Shape and Shape Distribution analysis<br />
examines the granules during free fall. It uses a<br />
line scan camera to check granule size<br />
distribution, sphericity, angel hair, dust/wear,<br />
doubles and triples.<br />
All of these systems mentioned can be connected<br />
right in series and be controlled by an integrated<br />
software solution, using an interface such as<br />
Modbus; they are linked to the Production Data<br />
Acquisition (PDA) system. In case of deviation, the<br />
operator is alerted automatically.<br />
At-line rheology<br />
The rheometer of the newly patented OCS<br />
technology is a hybrid between measurement of<br />
granules and extruded films. Highly precise off-line<br />
laboratory measurement following ASTM 1283<br />
and ISO 1133 is carried out continuously as well<br />
as right “at-line” next to the production facility,<br />
biennial 07-08<br />
giving the operator parameters crucial for reactor<br />
control (Fig. 1). This is done by continuously taking<br />
specimens out of the granule flow, heating them<br />
up and submitting them to high pressure to<br />
compress them carefully. This process causes only<br />
relatively slight changes in molecule structure,<br />
reaching reproducible accuracies of 0.5% which is<br />
better than off-line laboratory equipment. At the<br />
same time, metering without screw shear does not<br />
change the polymer structure and maintains better<br />
correlation with the ASTM/ISO methods.<br />
Measuring extruded<br />
sheets online<br />
The analysis methods mentioned above, however,<br />
fails to provide any information on the granules’<br />
speck content and their actual quality. To enable<br />
this measurement, a narrow film is extruded, in<br />
parallel, while regular extrusion takes place, and<br />
its speck content determined continuously. It is of<br />
major significance here, to seize the utmost<br />
number of small specimens, in order to safeguard<br />
continuous process control. A gel shower, for<br />
instance, may last five to 10 minutes, then<br />
disappear. Therefore, it is recommended that<br />
cycles should comprise at least 50 specimens<br />
per hour.<br />
Following cast or blown film extrusion, the sheet<br />
passes below a line scan camera and is wound<br />
without a tube on a pneumatic mandrel (Fig. 2).<br />
The winding unit is suspended at one side (godet<br />
structure) and comprises several servo drives.<br />
These provide for the film guidance to be<br />
absolutely stable and they avoid fluttering.<br />
Sheet guidance is just as essential as a clean<br />
environment (up to a clean room), since granules<br />
Fig. 2. Online Close-Loop concept<br />
(blow moulding plant)<br />
for applications such as high-voltage cables have<br />
resolutions of down to 5 μm, which must be<br />
inspected. For downmarket raw materials such<br />
as polyethylene, standard resolutions are 50μm<br />
to 25μm.<br />
The process has been optimised for raw material<br />
control and it works almost autonomously. Other<br />
measurements, e.g. of haze according to ASTM<br />
1003, of additive density and composition (IR<br />
spectroscopy), of brilliance or thickness can easily<br />
be integrated into the winding unit and software.<br />
The Web Browser supports remote control and<br />
maintenance of the plant. The systems are<br />
inter-linked internally with an OPC server, and<br />
connected externally to the customer’s PDA<br />
system.<br />
Quality concept for<br />
a polymer plant<br />
A world-scale raw material supplier has integrated<br />
into their polymer plant a standardised online<br />
close-loop concept. In order to minimise problems<br />
resulting from granule transport, such as<br />
generation of dust or abrasion, a container was<br />
placed right next to the extruders, suited to<br />
perform clean room measurements. (Fig. 3).<br />
Analytical software is integrated into the PDA<br />
system with a Modbus, Profibus, Ethernet OPC<br />
interface etc. enabling the operator to control the<br />
plant from the control room. From here, the raw<br />
material specimens can be automatically allocated<br />
to the individual measuring systems.<br />
Pellet analysis systems sort out contaminated<br />
granules, camera systems evaluate speck content,<br />
IR spectroscopy determines additive content and<br />
composition. In case of a problem, the plant<br />
continued on page 53 <br />
Fig. 1. At-Line rheometer<br />
52 www.rheologysolutions.com
OnLine Close-Loop<br />
Monitors<br />
continued from page 52<br />
operator is alerted immediately and the<br />
contaminated material is diverted into a different<br />
silo. Simultaneously, the system significantly<br />
reduces changeover times, anticipates<br />
maintenance and optimises maintenance intervals.<br />
Inspection of extruded<br />
films during production<br />
Producers of high-quality sheets today use sheet<br />
inspection systems, which monitor 100% of<br />
outputs. These systems detect flaws such as<br />
specks, brands, fish eyes, streaks, flow lines or<br />
insects, mark them and alert the operator<br />
immediately. This monitors the process itself,<br />
the raw material and the final product.<br />
The system raises an alarm in case it detects e.g.<br />
a critical individual flaw (a fly for instance), flaw<br />
trends (more than 10 gels of 200 to 300 mm<br />
diameter per square meter), or if there is a roll or<br />
use error, that is not specified. The data is stored<br />
in the system and can be accessed at any time.<br />
Production tendencies can be presented online<br />
for relatively long periods of time (12 hours). In an<br />
off-line mode, entire campaigns can be compared<br />
to each other and evaluated, enabling the<br />
engineer, e.g. to evaluate the bittiness of a raw<br />
material charge applied on a certain extruder.<br />
The system provides protocols of roll pressures,<br />
tailored to the individual manufacturer’s<br />
requirements.<br />
Inspection technology<br />
Today’s inspection systems reach pixel frequencies<br />
up to 160 MHz per camera, being processed<br />
by an Embedded PC right beside the camera.<br />
info@rheologysolutions.com<br />
A single camera can buffer up to 1,800 photos of<br />
flaws a second. All measured data is transmitted,<br />
via Ethernet, to a server, visualised and stored.<br />
Analysis is conducted in real time, alerting the<br />
operators, in case of irregularities.<br />
Subject to the individual application, CCD line<br />
cameras can be used with either 2,048; 4,096;<br />
6,144 or 8,192 pixels. The scan rates achieved<br />
range from 72,000 per second with 2,048 pixels,<br />
up to 18,000 per second with 8,192 pixels.<br />
This way, solutions are high in web direction, even<br />
with very high web speeds. While using special<br />
objectives and technological development in CCD<br />
sensors, the image quality of long CCD lines (e.g.<br />
8,192 pixels) today is reproduced just as<br />
sensitively as with short CCD lines (e.g. 2,048<br />
pixels). For the sheet manufacturer, this means<br />
that findings from inspections remain good while<br />
investment costs are significantly lower, since the<br />
price of a CCD camera for long lines is only<br />
slightly higher.<br />
With standard sheet processing, control is<br />
performed on speeds achieving up to 600 or even<br />
800 m/min (roll slitting machine, coating) and<br />
widths reaching up to 10 m (biaxial stretching unit)<br />
(Fig. 4). Solution is 50 μm, in optical films, while<br />
ranging between 200 and 300 μm in thermo<br />
formed high-barrier films. In laminated sheets, the<br />
value is between 100 and 200 μm, while ranging<br />
from 300 to 400 μm in diaper films. Generally, the<br />
solution is determined by the end customers’<br />
specifications as well as the production process.<br />
Examples of practical<br />
application<br />
While producing surface-protecting films, the<br />
causes of specks were examined. Having<br />
evaluated the situations of alert, engineers found<br />
Fig. 3.Container designed for online<br />
Close-Loop measuring<br />
out the following: 40% of all specks are caused by<br />
dust and abrasions during raw material transport.<br />
This comprises silos and silo tankers, as well as<br />
pellet conveying systems in the factory to transport<br />
the material from the silo to the extruder. Specks<br />
caused by the raw material itself, e.g. by<br />
inter-linkage or insufficient shearing, make up<br />
25%. The extrusion plant causes 20% of the<br />
specks, due to dissatisfactory screw geometry or<br />
dead zones, while 15% are attributed to the<br />
production process, for instance screen changes<br />
or wrong temperature parameters.<br />
An enterprise producing sanitary film also<br />
compounds the blends it requires. In the<br />
compounding sector, each charge is submitted to<br />
continuous examination on a laboratory extruder<br />
that includes units designed for winding, as well<br />
as gel count. Using an interface, the data is<br />
transmitted to the PDA system. The information<br />
serves as a basis for producing the film according<br />
to the customer’s quality specifications. On the<br />
cast film extruder, 100% film inspection is carried<br />
out, while the film is 2,000 mm wide and speed is<br />
100 m/min. The data obtained from the two<br />
inspection systems is evaluated by the same<br />
off-line analysis software, which also relates them<br />
to each other.<br />
Fig. 4. System to inspect films in a stretching<br />
unit online<br />
Conclusion<br />
Close-Loop today is a standard concept applied in<br />
raw material production. Not only does it monitor<br />
qualities; it controls and optimises the production<br />
process.<br />
Author. Oliver Hissmann, DIPL.-PEC., MBA. Sales<br />
Manger, Optical Control Systems, Witten,<br />
Germany.<br />
A copy of this article is available on request by<br />
quoting OCS-008.<br />
biennial 07-08<br />
53
• rheotalk special issue<br />
Food Industry feature<br />
<strong>Rheology</strong> <strong>Solutions</strong> offer<br />
material characterisation<br />
solutions to measure, monitor<br />
and provide reproducible data<br />
for quality control, development<br />
and production applications<br />
that will improve performance<br />
within the food industries.<br />
Services<br />
An extensive range of technical articles have been<br />
produced specific to the challenges found within<br />
the food industry, these include:<br />
• Food and Beverage Material Characterisation<br />
- Introduction to the influences of rheological<br />
and process parameters. Rheo 025TP<br />
• Comparison of Rheological Techniques for<br />
the Characterisation of Semi-Solid Foods.<br />
(Rheo 027TP)<br />
biennial 07-08<br />
food industries<br />
• Application of Liquid and Solid Rheological<br />
Technologies to the Textural Characterisation<br />
of Semi-Solid Foods. (Rheo049)<br />
• QC Measurements for Liquid Food Products<br />
and Packaging. (Rheo051)<br />
• Tim's Top Tips - Explanation & Evaluation<br />
of Mouthfeel. (Rheo253)<br />
• Tim's Top Tips - Explanation & Evaluation<br />
of Shelf Life. (Rheo254)<br />
• Tim's Top Tips - Explanation & Evaluation<br />
of Processability. (Rheo255)<br />
• Tim's Top Tips - Explanation & Evaluation<br />
of Cohesiveness, Cohesion Strength and<br />
Cohesive Quality. (Rheo256)<br />
• Tim’s Top Tips – How to Measure Flow<br />
& Viscosity. (Rheo358)<br />
• Tim’s Top Tips – How to Measure Thixotropy.<br />
(Rheo360)<br />
• Tim’s Top Tips – How to Measure Yield Stress.<br />
(Rheo362)<br />
Additionally, an information kit – <strong>Rheology</strong><br />
<strong>Solutions</strong> for the Food Industry is available. Copies<br />
of the technical papers and the solutions kit are<br />
available on request from <strong>Rheology</strong> <strong>Solutions</strong>.<br />
special issue<br />
Products<br />
Rheological parameters are reliable pointers for<br />
food performance and are critical factors for<br />
processability and product quality.<br />
Measuring these parameters will improve process<br />
and product performance within the food<br />
industries.<br />
There are a range of instruments and measurements<br />
that can be used to quantify rheology<br />
related challenges (processes or consumption)<br />
some of which may be described by the following<br />
terms:<br />
• adhesion • build<br />
• cohesion • cover<br />
• crispiness • elasticity<br />
• mouthfeel • spread<br />
• stringiness • viscosity<br />
• and many more<br />
<strong>Rheology</strong> <strong>Solutions</strong> will be exhibiting at Foopro<br />
(stand no. 6084) in Sydney in July 2008, and<br />
following is an overview of the products and<br />
services that will be available at the stand and<br />
fully operational during the exhibition.<br />
54 www.rheologysolutions.com
• company news<br />
Bacchus Marsh – Home of a<br />
new high technology facility<br />
all industries<br />
<strong>Rheology</strong> <strong>Solutions</strong> based in<br />
Bacchus Marsh Victoria has<br />
signed a license agreement<br />
with CSIRO to develop and<br />
manufacture a novel process<br />
control instrument known as<br />
the On-Line Rheometer (OLR).<br />
Mr Pat Griffin, Managing Director of <strong>Rheology</strong><br />
<strong>Solutions</strong> announced that after a long period of<br />
discussion and negotiation, agreement with CSIRO<br />
had been reached for taking on the license for the<br />
OLR. CSIRO initially released an Expression of<br />
Interest (EOI) in early 2007 to seven international<br />
companies that were known to have expertise in<br />
the appropriate markets, and we are pleased to be<br />
the successful partner.<br />
The OLR will be developed by <strong>Rheology</strong> <strong>Solutions</strong><br />
and will be taken to the world market. A world<br />
class manufacturing facility will be established in<br />
Bacchus Marsh employing 20 highly skilled<br />
technical and engineering staff adding to the<br />
region’s skill base. This is a significant development<br />
for the region with the establishment of a<br />
purpose built manufacturing facility.<br />
info@rheologysolutions.com<br />
Mr Dennis Silvers of CSIRO stated that: “The<br />
initiative brought to the table a viable offer that<br />
otherwise would not have occurred, which will<br />
result in about $2 million in royalties and a small<br />
manufacturing and distribution facility to be built in<br />
Bacchus Marsh, a town west of Melbourne, that<br />
will employ between 15 and 20 people and bring<br />
in more than $16 million to the local community”.<br />
“The Moorabool Shire Council and the Victorian<br />
State Government have given much support to the<br />
project in terms of assisting to finalise the<br />
agreement with CSIRO”, said Mr Griffin. “We will<br />
be seeking on-going financial assistance from the<br />
Local and Federal Government as we progress the<br />
development of the instrument. This project will<br />
inject significant revenues into the region and will<br />
also increase employment.”<br />
What is the On-Line<br />
Rheometer?<br />
Developed by CSIRO Industrial Physics, this novel<br />
instrument delivers fast, accurate results with a<br />
single measurement over a range of frequencies.<br />
The OLR reduces wastage, saving time and money<br />
with potential environmental benefits. Its simple<br />
design and stainless steel construction makes it<br />
easy to use and clean.<br />
To date, when more detailed knowledge of the<br />
viscoelastic properties of the fluid is required test<br />
volumes must be removed from the process<br />
stream and measured using an off-line laboratory<br />
rheometer. This is a time consuming procedure<br />
that may require the process line to be shut down<br />
until the results are available to confirm, or<br />
otherwise, the quality of the product. Alternatively,<br />
the process flow may continue with the potential<br />
loss of product. In some cases, the volume of lost<br />
product could be large and this could be<br />
particularly problematic when processing high<br />
value materials (such as pharmaceuticals),<br />
products that cannot be reprocessed or products<br />
that incur a disposal cost (such as, an environmental<br />
levy). Thus a genuine process control<br />
rheometer which can be operated in an in-line or<br />
on-line configuration and measure the viscoelastic<br />
properties of a process fluid in real time, has the<br />
potential to improve product quality and reduce<br />
processing costs.<br />
The CSIRO designed On-Line Rheometer (OLR)<br />
is such an instrument, and uses a patented<br />
multi-frequency squeezing flow technique that<br />
allows the viscoelastic flow properties of a<br />
material to be measured in a very short time.<br />
The measured rheological parameters can be<br />
used as process controls in a feedback system<br />
to control the process, and hence the quality,<br />
of the final product.<br />
Above: (from left) Bruce Fox (CSIRO), Pat Griffin<br />
(<strong>Rheology</strong> <strong>Solutions</strong>), Dennis Silvers (CSIRO),<br />
and Jennifer Labourne (<strong>Rheology</strong> <strong>Solutions</strong>)<br />
at the signing of the License Agreement.<br />
Left: Mr Pat Griffin (right), Managing Director of<br />
<strong>Rheology</strong> <strong>Solutions</strong> Pty Ltd and Mr Bruce Fox (left)<br />
of CSIRO with the phototype of the New On-Line<br />
Rheometer.<br />
biennial 07-08<br />
55
Product News<br />
& Industry Applications<br />
Product Focus<br />
• HAAKE MARS RheoScope Module ................................................................ 61 •<br />
• NESLAB ThermoFlex Recirculating Chillers ................................................ 64 •<br />
• New Heating Circulator ................................................................................ 60 •<br />
• New Cooling Circulator ................................................................................ 59 •<br />
• Disposable Plate/Plate – Measuring Geometry for the<br />
Controlled Temperature Chamber (CTC) ........................................................ 72 •<br />
• Marimex ViscoScope In Line Torsional Viscometer ........................................ 73 • • • •<br />
• Optical Analysis and <strong>Rheology</strong> ................................................................ 71 • • • •<br />
• Schleibinger presents a New probe for SCC Mortar for the Viskomat NT ........ 67 •<br />
• Cooling Recirculators ................................................................................ 76 •<br />
• HAAKE MiniLab Compounder & Reactor ........................................................ 81 •<br />
• Heating Recirculators ................................................................................ 74 •<br />
• High Speed Pellet Scan System throughput up to 250kg / hr ........................ 77 •<br />
• Higher Instrument Precision & Reliable Quality Control<br />
– Hand Held Viscometer – HAAKE Viscotester 1 Plus & 2 Plus ........................ 80 •<br />
• Nano-Composites ........................................................................................ 74 •<br />
• NanoLab Compounder Package ................................................................ 80 • • • •<br />
• New NESLAB ThermoFlex 2500 Recirculating Chiller ................................ 75 •<br />
• Twin-Screw Extrusion at a Lab Scale ........................................................ 76 •<br />
• HAAKE MARS with CTC ................................................................................ 67 •<br />
• HAAKE PolyLab QC ................................................................................ 83 •<br />
• HAAKE RheoStress 6000 – The Universal Rheometer ................................ 87 •<br />
• Heating & Cooling Recirculators ................................................................ 63 •<br />
• The OP5 Online Rheometer ........................................................................ 86 •<br />
• New Device for Rheological Measurements.<br />
A Measuring Device for Special Mortars ........................................................ 91 •<br />
• New Product – Circulator to Heat &<br />
Cool External Applications from -10ºC to 80ºC................................................ 68 •<br />
• Rheological Measurement with Optical Analysis<br />
– High Temperature Version Extends Testing up to 300ºC ........................ 69 • • • • •<br />
• The Industry Choice for Viscosity Measurements of<br />
Mineral Slurries and Suspensions HAAKE Viscotester 550 ........................ 92 •<br />
• Extended Product Range - Recirculating Chillers ........................................ 101 •<br />
• Using a Refrigerated Circulator with a Rotary Evaporator<br />
– Environmentally Friendly Solution................................................................ 98 •<br />
Industry Applications<br />
• Continuous Granulation for the Pharmaceutical Industry ................................ 65 •<br />
• CR-Mode – Low Shear Rates ........................................................................ 70 •<br />
• Tim’s Top Tips – How to Measure Series ................................................ 59 •<br />
biennial 07-08<br />
56 www.rheologysolutions.com<br />
ALL INDUSTRIES<br />
POLYMER<br />
FOOD<br />
SURFACE COATINGS<br />
MINERAL<br />
CHEMICAL<br />
PHARMACEUTICAL<br />
BUILDING
Product News<br />
& Industry Applications<br />
Industry Applications<br />
• Food Industry Feature & Product Focus- Extensional Rheometer<br />
HAAKE CaBER1 ........................................................................................ 95 •<br />
• Food Industry Feature & Product Focus<br />
- Heating Bath Circulator Thermo HeatTech 26L ........................................ 96 •<br />
• Food Industry Feature & Product Focus<br />
- Process Viscometer Marimex ViscoScope ................................................ 94 •<br />
• Food Industry Feature & Product Focus<br />
- Rotational Viscometer HAAKE Viscotester 6L plus......................................... 94 •<br />
• Food Industry Feature & Product Focus<br />
- Refrigerated Bath Circulator Thermo CoolTech 320 ................................ 96 •<br />
• Food Industry Feature & Product Focus<br />
- Recirculating Chiller NESLAB ThermoFlex 900 ........................................ 95 •<br />
• Polymer Industry Feature & Product Focus<br />
- Modular Torque Rheometer with Measuring Mixer........................................ 103 •<br />
• Polymer Industry Feature & Product Focus<br />
- Modular Torque Rheometer with Twin-Screw Extruders ................................ 103 •<br />
• Polymer Industry Feature & Product Focus<br />
- Modular Torque Rheometer with Single-Screw Extruder................................ 104 •<br />
• Polymer Industry Feature & Product Focus<br />
- Modular Twin-Screw Extruder PRISM EuroLab ........................................ 104 •<br />
• Polymer Industry Feature & Product Focus – Pellet Scanner PS-25C................ 105 •<br />
• Polymer Industry Feature & Product Focus – Web Inspection System FSP600 105 •<br />
Product News<br />
• Accessories for HAAKE MARS –<br />
- Cone/Plate-Exchangeable Measuring Geometries ........................................ 62 •<br />
- Measuring Cell for <strong>Rheology</strong> of Building Materials ........................................ 62 •<br />
- Sample Loading Tool ................................................................................ 61 •<br />
- Trimming Tool ........................................................................................ 62 •<br />
- Solids Clamp ........................................................................................ 62 •<br />
- CD Mode Curing Measurement. ................................................................ 78 • •<br />
- Standard Liquids. ................................................................................ 79 •<br />
- Sample Fixture for Bending & Breaking Tests ........................................ 78 • • • •<br />
- Support Fixture for the Analysis of Textile Samples. ................................ 78 • •<br />
- Tool For Checking the Optical Quality of the RheoScope Module ................ 79 • • • • •<br />
- (SER)Extensional <strong>Rheology</strong> System ........................................................ 100 •<br />
- Universal Container Holder for HAAKE MARS and RheoStress 6000. ........ 99 •<br />
• Process Viscometer – Software Options. ........................................................ 82 • • • • •<br />
info@rheologysolutions.com<br />
ALL INDUSTRIES<br />
POLYMER<br />
FOOD<br />
SURFACE COATINGS<br />
MINERAL<br />
biennial 07-08<br />
CHEMICAL<br />
57<br />
PHARMACEUTICAL<br />
BUILDING
Product News<br />
& Industry Applications<br />
Product News<br />
• New Product Brochure –<br />
- HAAKE PolyLab OS Docking Station ........................................................ 71 • •<br />
- PolyLab OS Torque Rheometer RD4 Application Packages ........................ 71 • •<br />
- HAAKE PolyLab OS Open System. Measuring Mixer Extruder System<br />
from Thermo Fisher. ................................................................................ 90 •<br />
- Micro Compounder for Small Sample Amounts ........................................ 66 • •<br />
- Sample Specimen preparation Instrument. ................................................ 66 • •<br />
- Food Industry Feature & Product Focus........................................................ 97 •<br />
- Comprehensive Material Characterisation for Polymers ................................ 97 •<br />
- Extrusion & Material Characterisation for Drug Development & Production 97 •<br />
• HAAKE Viscometers ................................................................................ 89 •<br />
• Polymer Industry Feature & Product Focus ................................................ 102 •<br />
• Accessories for HAAKE Viscotester 7Plus –<br />
- Thermal Printer ........................................................................................ 70 •<br />
- Adapters for HAAKE Viscotester models 6 and 7 plus for measuring<br />
range extension and sample temperature measurement (optional) ................ 99 •<br />
• Product Accessories - UV Curing Cell for an individual<br />
arrangement of optical components ........................................................ 99 •<br />
• Bath Recirculators - NESLAB RTE & EX Series ................................................ 97 •<br />
• Product Accessories - Vane Rotors for HAAKE MARS & HAAKE<br />
RheoStress 6000 ........................................................................................ 100 •<br />
• Product Accessories - Tribology Cell for HAAKE RheoStress 6000 ................ 100 •<br />
biennial 07-08<br />
58 www.rheologysolutions.com<br />
ALL INDUSTRIES<br />
POLYMER<br />
FOOD<br />
SURFACE COATINGS<br />
MINERAL<br />
CHEMICAL<br />
PHARMACEUTICAL<br />
BUILDING
news & views<br />
NEW Cooling Circulator<br />
all industries<br />
CoolTech 3320 Specifications<br />
Temperature Range -28°C to +100°C<br />
Temperature Accuracy +/- .02K<br />
Heater Capacity (230V) 2.0 kW<br />
Cooling Capacity at 20°C 320 W<br />
at 0°C 205 W<br />
at -20°C 75 W<br />
Pump Pressure (Maximum) 300 mbar<br />
Pump Flow Rate (Maximum) 12.5 lpm<br />
Bath Opening (W x L x D) 13cm x 10cm x 15cm<br />
Bath Volume 4.5 L<br />
Overall Dimensions 23cm x 46cm x 58cm<br />
Unit Weight 29.8 kg<br />
Order number 230V/50Hz 426-2601<br />
CoolTech 320 Features & Benefits:<br />
• Rapid cool down and heat up times<br />
• Powerful pump accommodates the bath plus<br />
connections to external applications<br />
• Front access drain for easy cleaning<br />
• Safety for temperature & fluid level<br />
• CFC-free refrigeration system<br />
The series has now been expanded to cover<br />
seven key industries, and each industry has a<br />
series of three How to measure … notes for<br />
three key characterisation techniques, which are:<br />
• How to Measure Thixotropy<br />
info@rheologysolutions.com<br />
$3999<br />
EXCLUDING GST<br />
CoolTech 320 Applications:<br />
• Condensers • Rotary Evaporators<br />
• Catalyst Reactions • Electrophoresis<br />
• Bioreactors • Instrument Calibration<br />
• Refractometers • Spectrophotometers<br />
• Sample Preparation<br />
ORDER TODAY<br />
DELIVERY EX STOCK!<br />
Cool Down – Time to Temperature<br />
Pumping Capacity<br />
Place your order now for despatch within 24 hours of order receipt.<br />
Fax your purchase order to <strong>Rheology</strong> <strong>Solutions</strong> Pty Ltd on 03 5367 6477<br />
or email your purchase order to info@rheologysolutons.com<br />
industry applications<br />
Tim’s Top Tips - How to Measure...<br />
all industries<br />
• How to Measure Yield Stress<br />
• How to Measure Flow & Viscosity Curves<br />
The new industry application areas now covered<br />
are: Food; Pharmaceutical, Cosmetic & Allied<br />
Industries; Surface Coatings; Chemical & General<br />
Manufacturing; Building & Construction<br />
Industries; and Polymer Industries. The series was<br />
introduced last year with the first industry covered<br />
by the How to measure … series was for<br />
Mineral Slurries<br />
<strong>Rheology</strong> <strong>Solutions</strong> is planning a series of<br />
workshops based on the “How To Measure”<br />
Series” - please see page 10 for more<br />
information.<br />
biennial 07-08<br />
59
news & views<br />
NEW Heating Circulator<br />
biennial 07-08<br />
all industries<br />
HeatTech 26L Specifications<br />
Temperature Range Ambient +8°C to +100°C<br />
Temperature Accuracy +/- 0.02K<br />
Heater Capacity (230V) 2.0 kW<br />
Pump Pressure (Max) 300 mbar<br />
Pump Flow Rate (Max) 12.5 lpm<br />
Bath Opening (W x L x D) 30 x 35 x 20cm<br />
Bath Volume 26 L<br />
Overall Dimensions 34 x 56 x 40cm<br />
Unit Weight 10.9 kg<br />
Order number 230V/50Hz 426-2261<br />
HeatTech 26L Features & Benefits:<br />
• Large bath area accommodates more samples<br />
• Quiet system ensures pleasant environment<br />
• Powerful pump accommodates the bath plus<br />
connections to external applications<br />
• Safety for temperature & fluid level<br />
• Front access drain for easy cleaning<br />
$2399<br />
EXCLUDING GST<br />
HeatTech 26L Applications:<br />
• Fecal Coliform Testing • Enzyme Assays<br />
• Quality Control Testing • Tissue Baths<br />
• Instrument Calibration • Viscosity Testing<br />
• Sample Preparation • DNA Melting Curves<br />
ORDER TODAY<br />
DELIVERY EX STOCK!<br />
Heat-Up – Time to Temperature Curve<br />
Pumping Capacity<br />
60 www.rheologysolutions.com
product news & industry applications<br />
HAAKE MARS Rheoscope Module<br />
all industries<br />
The HAAKE MARS<br />
is a modular high<br />
temperature/high pressure<br />
R&D rheometer that was<br />
designed for flexibility with<br />
an architecture that permits<br />
customer modules to be<br />
integrated into the system.<br />
A RheoScope Module was developed for the<br />
HAAKE MARS system that combines high<br />
resolution microscopy and advanced rheometery<br />
technology. With this module the connection<br />
between a sample’s microscopic structures and<br />
rheological properties can be monitored<br />
simultaneously, and the rheological and optical<br />
data can be saved in the same file. Visible<br />
textures and structures in solutions, suspensions,<br />
thixotropy, emulsification, coalescence,<br />
aggregation, gelification, dissolution and<br />
flocculation. Together with the user-friendly<br />
info@rheologysolutions.com<br />
HAAKE RheoWin 3 measuring and evaluation<br />
software, all functions of the microscope and<br />
camera can be controlled in addition to the<br />
rheometer. The rheological and optical data can<br />
be monitored online during the measurement as<br />
well as saved and exported in different formats<br />
for further analysis.<br />
Specifications<br />
Microscope Servo motor-driven, focus and<br />
position adjustment controlled<br />
with software<br />
Lenses Magnification: 5x, 10x, 20x<br />
and 50x<br />
Light source 150 W, 12 V, wave length<br />
range: 380 - 750<br />
Resolution 1 um (20x lenses)<br />
Field depth 5 um (20x lenses)<br />
Contrast improvement Polariser servo motor-driven<br />
Data acquisition Maximum 15 images / second<br />
and storage with standard image format<br />
(eg: TIFF) or video acquisitions<br />
with user-definable data<br />
compression<br />
Image analysis Option for the determination of<br />
software the particle size and its<br />
distribution<br />
Measuring geometries Polished plates and cones with<br />
different diameters<br />
product news & industry applications<br />
NEW Accessories for HAAKE MARS<br />
all industries<br />
Sample loading tool for measurements<br />
on pellets and powders using a<br />
plate/plate- or cone/plate- measuring<br />
geometry<br />
In most cases rheological investigations on<br />
polymers were performed using a rheometer with<br />
plate/plate- or cone/plate- measuring geometry.<br />
Too much or too little sample volume can result in<br />
an experimental error of up to 20% for the<br />
viscosity or the modulus.<br />
In order to get reliable experimental data with a<br />
high reproducibility a suitable sample preparation<br />
is necessary, e.g. production of specimen using an<br />
injection moulding machine. The feed material can<br />
be modified due to the fact that the sample<br />
preparation is carried out at the processing<br />
temperature of the polymer.<br />
A sample loading tool was designed for<br />
measurements using the feed material in form of<br />
pellets or powder. This tool consists of a forming<br />
tool for measuring geometries with different<br />
diameters (20, 25 and 35 mm), a tool to check the<br />
forming as well as a set of disposable strips made<br />
of stainless steel.<br />
HAAKE MARS Rheoscope Module<br />
The strips have a thickness of 0.2 mm. Using a<br />
moulding tool these strips can be shaped into<br />
loops with diameters corresponding with the lower<br />
plates of our cone/plate or plate/plate geometries.<br />
Having this border around the lower plate, the<br />
geometry can easily be filled with pellets or<br />
powders. Afterwards, the automatic lift, controlled<br />
by HAAKE RheoWin, will move the upper geometry<br />
into the measuring position and the metal strip<br />
can be opened and taken away.<br />
This procedure leads to an optimum filling of the<br />
geometry with a correct sample volume and no air<br />
bubbles. Continued on page<br />
biennial 07-08<br />
61
Sample loading tool for cone/plate – measuring<br />
geometries consisting of forming tool (left), tool<br />
to check the geometry (middle) and strips out<br />
of stainless steel (in the front); measuring plate<br />
cover with sample loading tool (right)<br />
The filling procedure should be carried out at the<br />
measuring temperature in order to eliminate a<br />
thermal modification of the sample.<br />
Trimming tool to remove overfilling<br />
in a plate/plate-and cone/plate<br />
measuring geometry<br />
In order to get reliable measuring data with a<br />
high reproducibility an optimised gap filling is<br />
necessary: using an underfilling the measured<br />
value for the viscosity is too low, whereas an<br />
overfilling results in a too high viscosity value.<br />
The fringe effect depends on the diameter of the<br />
measuring geometry: the effect increases with<br />
decreasing diameter.<br />
For samples with a medium and higher viscosity<br />
a special trimming tool is available as an optional<br />
accessory to remove the overfilling.<br />
Plate/Plate – measuring geometry with measuring<br />
plate cover (MPC) for optimized gap filling<br />
This tool is made out of stainless steel, robust<br />
and ergonomically designed to remove surplus<br />
material easily and without residue.<br />
For all plate/plate – and cone/plate – measuring<br />
geometries measuring plate covers are available<br />
biennial 07-08<br />
with standard diameters of 8, 20, 35 and 60 mm.<br />
These measuring plate covers are designed with<br />
a plateau, in which surplus material can be<br />
collected automatically.<br />
Trimming tool to remove surplus material for<br />
medium and high viscous samples<br />
New solids clamps for measurements<br />
on (semi)-solids<br />
For the controlled test chamber (CTC) a new<br />
solids clamping tool according to DIN/ISO 7621-1<br />
has been designed. It consists of an upper and a<br />
lower holder. Each is equipped with two moving<br />
jaws, which guarantee an automatic centering of<br />
the sample relative to the rheometers axis.<br />
The automatic clamping force adaptation for the<br />
sample as well as a very simple semi-automatic<br />
gap adjustment for a wide range of sample<br />
thicknesses with just one fixture allow the user to<br />
measure over a wide range of temperatures in<br />
one go without ever loosing the grip on the<br />
sample.<br />
The jaws are easily removable for cleaning. Also<br />
jaws with various profiles for different sample<br />
types (soft, medium, hard) are available.<br />
The sample can be 5.0 – 12.7 mm wide, 0.15 –<br />
4.0 mm thick and have a maximum length of 68<br />
mm.<br />
Solids clamps set (left) and a sample held by the<br />
clamps (right)<br />
The bottom clamp can be adjusted in height.<br />
Samples of different lengths can all be fixed with<br />
their middle part being close to the centre of the<br />
CTC. Thus all samples of different lengths are<br />
exposed to the same extremely low temperature<br />
gradient. Using a flexible temperature sensor the<br />
temperature is measured very close to the<br />
sample.<br />
Cone/plate-exchangeable measuring<br />
geometries for maximum flexibility<br />
For the temperature control chamber (CTC) a new<br />
design for cone/plate- measuring geometries<br />
have been developed, in order to fulfill individual<br />
customer requirements without restrictions.<br />
The exchangeable measuring geometry consists<br />
of an upper and a lower holder with integrated<br />
temperature sensor. Both holders are equipped<br />
with an adapter for a plate or a cone.<br />
Selection of different exchangeable geometries<br />
(right)<br />
Plates and cones made of stainless steel with<br />
different diameters (8, 20, 25 and 35 mm) and<br />
cone angles are available. The lower plate is<br />
designed to collect surplus material.<br />
Geometries made of aluminum with diameters 20<br />
and 25 mm are available as reusable plates. For<br />
this kind of geometry a collection device is<br />
recommended, in order to protect the<br />
temperature chamber against fouling.<br />
Thanks to the modular design individual<br />
requirements for material (e.g. Titanium,<br />
Hastelloy), special surfaces (e.g. profiles) and<br />
diameters can easily be realized. They are<br />
available on request.<br />
New measuring cell for rheology<br />
of building materials<br />
In order to carry out measurements on samples<br />
with medium and large particles, a special<br />
measuring geometry is often the only way to get<br />
meaningful data with a high reproducibility.<br />
For measurements on building materials a new<br />
measuring cell has been developed, which can be<br />
Continued on page 63<br />
62 www.rheologysolutions.com
NEW Accessories for HAAKE MARS<br />
Continued from page 62<br />
used for HAAKE MARS as well as rheometers of<br />
the HAAKE RheoStress series.<br />
This measuring cell is characterized by its variable<br />
profile. For all existing coaxial cylinders the profile<br />
is fixed and can not be changed. The profile of the<br />
new measuring cell is exchangeable: for each<br />
lamella the profile depth can be individually<br />
chosen.<br />
Lamellas with a profile depth of 2mm are included<br />
in the standard delivery. Lamellas with 1 mm is<br />
available as an option, whereas other profile<br />
depths are available on request.<br />
Specially shaped vane rotors are included in the<br />
price list with 26 and 29,5 mm diameters.<br />
info@rheologysolutions.com<br />
The measuring cell is made of stainless steel in a<br />
very robust design. The surface with an optimized<br />
structure guarantees an easy cleaning.<br />
Using the cell for construction materials in<br />
combination with a HAAKE MARS rheometer the<br />
temperature can be controlled; a suitable<br />
circulator is required. The temperature control unit<br />
is mounted on an adapter plate, in an overhung<br />
position and centered by the measuring cell. Using<br />
a temperature sensor the temperature can be<br />
measured within the sample. With a swingmechanism<br />
the temperature sensor can be<br />
positioned automatically and on a reproducible<br />
position.<br />
A measuring cell cover is available as an optional<br />
accessory.<br />
• product information<br />
Heating & Cooling Recirculators<br />
all industries<br />
In Stock – Despatched within<br />
48 hours from receipt of order.<br />
CoolTech 320 HeatTech 26L<br />
Refrigerated circulator Heating circulator<br />
Temperature range Temperature range<br />
-28ºC to +100ºC ambient to = 100ºC<br />
$3,999 $2,399<br />
All prices quoted exclude GST and local delivery<br />
Full product information is available on line<br />
for these products plus an extensive range<br />
of temperature control baths to meet the<br />
application requirements of diverse industries.<br />
For full product information and technical<br />
specifications please visit our dedicated website<br />
for temperature control products:<br />
www.temperaturecontrolbaths.com<br />
Cross-section of the measuring cell for buidling<br />
materials with adapter plate,<br />
temperature control unit incl. vane rotor<br />
www.temperaturecontrolbaths.com<br />
The website covers the entire range of temperature control baths currently available across<br />
the diverse product range and depth.<br />
biennial 07-08<br />
63
product news & industry applications<br />
Neslab ThermoFlex Recirculating<br />
Chillers<br />
biennial 07-08<br />
all industries<br />
Reliable, easy-to-use chillers<br />
optimised for the most<br />
demanding applications<br />
NESLAB ThermoFlex Recirculating Chillers deliver<br />
a continuous cooling capacity up to 1400 watts.<br />
These units are reliable, easy-to-use chillers<br />
optimised for the most demanding applications.<br />
These units are ideal for diverse applications<br />
within the following markets:<br />
• Laser • Packaging<br />
• University • Research<br />
• Analytical instrumentation<br />
• Medical equipment<br />
High Reliability<br />
You can expect years of operation from the<br />
NESLAB ThermoFlex 900 and 1400 recirculating<br />
chiller. The unit features a robust refrigeration<br />
system designed for continuous use in a variety<br />
of environments. The recirculation system<br />
incorporates highly reliable plumbing connections<br />
to eliminate leaks. Integrated air and fluid filters<br />
minimise wear to mechanical parts, which lowers<br />
lifetime maintenance costs and improves system<br />
reliability.<br />
NESLAB ThermoFlex 900<br />
Recirculating Chiller<br />
Setpoint Temp. Range 5°C - 40°C<br />
Ambient Temp. Range 10°C - 40°C<br />
Temperature Stability +/- 0.1°C<br />
Setpoint Cooling 60 Hz 900W (3072 BTU)<br />
Capacity at 20°C 50 Hz 750W (2560 BTU)<br />
(see graph below for cooling curves)<br />
Reservoir Volume 7.6 Liters<br />
Dimensions (HxWxD) 69.6 x 36.1 x 62.7cm<br />
Unit Weight 57.2kg<br />
Pumps (see graph below for performance curves)<br />
PD 1 - Positive 60 Hz 2.1 gpm @ 60 psi<br />
Displacement 50 Hz 1.7 gpm @ 60 psi<br />
PD 2 - Positive 60 Hz 4.1 gpm @ 60 psi<br />
Displacement 50 Hz 3.3 gpm @ 60 psi<br />
Compliance NRTL Certified to CSA and<br />
UL Standards; CE-Marked<br />
Cooling Capacity<br />
Pumping Capacity<br />
NESLAB ThermoFlex 1400<br />
Recirculating Chiller<br />
Setpoint Temp. Range 5°C - 40°C<br />
Ambient Temp. Range 10°C - 40°C<br />
Temperature Stability +/- 0.1°C<br />
Setpoint Cooling 60 Hz 1400W (4778 BTU)<br />
Capacity at 20°C 50 Hz 1170W (3995 BTU)<br />
(see graph below for cooling curves)<br />
Reservoir Volume 7.6 Liters<br />
Dimensions (HxWxD) 69.6 x 36.1 x 62.7cm<br />
Unit Weight 57.2kg<br />
Pumps (see graph below for performance curves)<br />
PD 1 - Positive 60 Hz 2.1 gpm @ 60 psi<br />
Displacement 50 Hz 1.7 gpm @ 60 psi<br />
PD 2 - Positive 60 Hz 4.1 gpm @ 60 psi<br />
Displacement 50 Hz 3.3 gpm @ 60 psi<br />
Compliance NRTL Certified to CSA and<br />
UL Standards; CE-Marked<br />
Cooling Capacity<br />
Pumping Capacity<br />
Specifications obtained at sea level using water as the recirculating fluid, at a 20°C process setpoint, 25°C ambient condition,<br />
at nominal operating voltage. Other fluids, fluid temperatures, ambient temperatures, altitude or operating voltages will affect<br />
performance. Thermo Electron reserves the right to change specifications without notice. Pump performance results obtained<br />
with no restrictions on return to the system.<br />
64 www.rheologysolutions.com
product news & industry applications<br />
Continuous Granulation for the<br />
Pharmaceutical Industry<br />
pharmaceutical, cosmetic<br />
& allied industries PRISM PHARMALAB 16<br />
Granulator with feeder<br />
The pharmaceutical<br />
industry needs consistent,<br />
continuous, small scale<br />
production capabilities<br />
and easy cleaning. The<br />
system needs to provide<br />
flexibility for new product<br />
development, with reliable<br />
and repeatable operating<br />
conditions, plus accurate<br />
process data for product<br />
audit.<br />
The PRISM Pharmalab 16 Extruder system meets<br />
the needs of the pharmaceutical industry with:<br />
• Small-scale twin screw continuous granulation<br />
• Crevice-fee design with opening barrel and<br />
ancillaries<br />
• Flexible screw and barrel configurations<br />
• Programmable recipe storage<br />
• Integrated data logging and analysis<br />
The benefits of the PRISM Twin screw systems for<br />
the pharmaceutical industry is:<br />
• Continuous granulation delivering consistent<br />
quality on small scale production<br />
• Opening barrel and easily dismantled product<br />
contact parts ensure reliable clean down<br />
• Modular design of screws and barrel gives<br />
flexibility for new product development<br />
• Recipe storage delivers reliable and repeatable<br />
operating conditions<br />
• Integrated data logging provides accurate<br />
process data for product audit<br />
info@rheologysolutions.com<br />
and dosing pump.<br />
PRISM PHARMALAB 16 Extruder showing all<br />
contact sections removed for cleaning<br />
PRISM PHARMALAB 16 Granulator showing<br />
discharge area<br />
PRISM PHARMALAB 16 Granulator showing<br />
hopper stirrer<br />
PRISM PHARMALAB 16 Granulator showing<br />
product discharge<br />
biennial 07-08<br />
65
• new product brochure<br />
A micro compounder for<br />
small sample amounts<br />
polymer industries<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
The Thermo Scientific HAAKE<br />
MiniLab II needs a sample<br />
amount of only 5 g.<br />
Compounding expensive or small scale materials<br />
such as nano-composities, bio-polymers or<br />
pharmaceutical is no longer a problem.<br />
Simultaneously, the rheological properties can<br />
be recorded to document structural changes.<br />
By using the optional force feeder, continuos<br />
extrusion with very small flows is possible.<br />
Main features:<br />
• Co –rotating twin screws (option: counter-<br />
rotating twin screws)<br />
• Integrated viscosity measurement<br />
• Automatic bypass operation for<br />
circulation/extrusion<br />
• Pneumatic feeding<br />
• LCD screen for graphical data display<br />
• Manual or computer control<br />
• Easy to clean due to exit in split barrel<br />
• Fits into laboratory fume hood=<br />
• new product brochure<br />
Sample specimen<br />
preparation instrument<br />
polymer industries<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
The Thermo Scientific<br />
HAAKE MiniJet II optimised<br />
the development process,<br />
enabling the testing of the<br />
mechanical properties of<br />
specimens as small as 5 g.<br />
The need to produce various sample geometries<br />
coupled with common reality of limited material<br />
quantities can often create a challenge during<br />
product development.<br />
Main features:<br />
• Small sample volume<br />
• Quick & easy to use<br />
• Interchangeable moulds<br />
• Test samples can be produced from<br />
powders, pellets or melts<br />
• A control and design concept that provides<br />
simplistic handling with consistent,<br />
reproducible results<br />
Applications:<br />
• Sample preparation for<br />
- Rheometry<br />
- Optical testing<br />
- Mechanical testing<br />
• Preparation of special specimen<br />
for pharmaceutical testing=<br />
FoodPro - the trade event for the food and beverage industry<br />
Visit <strong>Rheology</strong> <strong>Solutions</strong> on stand no: 6084<br />
Sydney Convention & Exhibition Centre • www.foodproexh.com • 21-24 July 2008<br />
biennial 07-08<br />
66 www.rheologysolutions.com
• product information<br />
HAAKE<br />
MARS<br />
with CTC<br />
Developed specifically for the HAAKE MARS<br />
platform, the Controlled Temperature Chamber<br />
(CTC) moves smoothly on guide rails. The CTC<br />
consists of two halves that allow convenient<br />
handling and optimal access to the sample. They<br />
can be moved independently backwards and<br />
sidewards, and can be opened and closed easily<br />
by hand. No special tools are needed. The two<br />
halves automatically center themselves around the<br />
sample automatically when closed. Each chamber<br />
half is equipped with a window to observe the<br />
sample during measurement.<br />
A unique feature is the "parking" position, which<br />
allows another temperature control unit to be<br />
attached without removing the CTC.<br />
Above: HAAKE MARS with CTC<br />
info@rheologysolutions.com<br />
news & views<br />
Schleibinger Presents<br />
a New Probe for<br />
SCC-mortar for the<br />
Viskomat NT<br />
construction &<br />
building industries<br />
At the 16 Conference on<br />
“<strong>Rheology</strong> of Building<br />
Materials” at the University<br />
for Applied Science<br />
Regensburg Germany,<br />
March 2007, Schleibinger<br />
presented a new probe for<br />
measuring SCC mortars.<br />
The conference has been<br />
running for 16 years and is<br />
organised by Schleibinger<br />
and was attended by some<br />
80 participants from Europe.<br />
The new design developed by Professor R. Vogel,<br />
Weimar Germany, in cooperation with Schleibinger<br />
is called a “Basket-Probe” for measuring SCC<br />
(Self-Consolidating Concrete) mortars.<br />
It has a flat double gap standard geometry, so you<br />
can get real rheological parameters but in<br />
opposite to other standard systems it minimises<br />
Professor Vogel (left) in discussion with some<br />
conference participants<br />
the wall slippage effects. The cylinder is like a<br />
gasket or a basket so strong cohesion effects<br />
between the materials dominates above the weak<br />
adhesive forces.<br />
The probe works best with very fluid but stable<br />
pastes and mortars used for groups, SCC or Self-<br />
Leveling compounds. Patent pending.<br />
The Viskomat NT is a versatile rotational<br />
viscometer for determining the workabilty of finegrained<br />
building materials such as cement paste,<br />
mortar, fine concrete, plaster etc. with a maximum<br />
particle size of 2 mm. With the Viskomat NT, you<br />
can obtain information on:<br />
1. flow curves and rheological parameters<br />
2. temperature dependent workability properties<br />
3. stiffening behaviour as a function of time an<br />
stirring speed<br />
4. effects of concrete admixtures and mineral<br />
blending agents on workability<br />
Schematic drawing of the Basket-Probe for use<br />
with the Viskomat NT viscometer<br />
biennial 07-08<br />
67
• new product<br />
Circulator to heat & cool external<br />
applications from -10ºC to +80ºC<br />
all industries<br />
The Thermo Scientific HAAKE<br />
EZ Cool 80 circulator is a versatile<br />
and economical option for<br />
laboratory cooling and heating<br />
needs from -10ºC to +80ºC.<br />
Its bathless design minimises the evaporation of<br />
temperature fluid during daily use. The stainlesssteel<br />
circulator is both quiet and robust, making it<br />
well suited for laboratory use.<br />
The HAAKE EZ Cool 80 supports diverse<br />
applications that include cooling and temperature<br />
control of analytical instruments. It can also be<br />
used as an economical chiller with heating options<br />
to replace tap water cooling in small laboratory<br />
applications.<br />
Applications:<br />
• Analytical instrumentation control<br />
• Bioreactors • Catalyst reactions<br />
• Chemical reactors • Closed-loop systems<br />
• Condensers • Electrophoresis<br />
• Instrument calibration • Refractometers<br />
• Rotary evaporators • Spectrophotometers<br />
Features & Benefits<br />
• Rapid cool down and heat up times<br />
• 4 pre-set temperatures<br />
• Real temperature adjustment for display<br />
of external temperature<br />
• Limits for customised high & low<br />
temperatures<br />
• Powerful pump accommodates connections<br />
to external applications<br />
• Front access drain for easy cleaning<br />
• Variable over temperature protection<br />
• Fault identification system<br />
• CFC-free refrigeration system <br />
Product Specifications<br />
Temperature Range -10°C to +80°C<br />
Temperature Accuracy +/- 0.1K<br />
Heater Capacity (230V) 1.5 kW<br />
Cooling Capacity 20°C 220 W<br />
0°C 60 W<br />
Pump Pressure (Maximum) 250 mbar<br />
Pump Flow Rate (Maximum) 12 lpm<br />
Internal tank volume 3.5 L<br />
Overall Dimensions (WxLxH) 26x50x40cm<br />
Unit Weight 30 kg<br />
Order number 230V/50Hz 426-1621<br />
biennial 07-08<br />
Left: The HAAKE EZ Cool 80 is ideal to control temperatures within a variety of laboratory applications<br />
including: Pharmaceutical, Biotechnology, Academic Research, Food and Beverage, Chemical, Petrochemical<br />
Right: Front panel showing display panel and control for temperature settings<br />
Pumping Capacity<br />
Pressure (mbar)<br />
400<br />
300<br />
200<br />
100<br />
10 20 30<br />
Flow (LPM)<br />
Cool-Down – Time to Temperature Curve<br />
Temperature (ºC)<br />
100<br />
20<br />
15<br />
10<br />
5<br />
0<br />
-5<br />
-10<br />
Heat-Up – Time to Temperature Curve<br />
Temperature (ºC)<br />
90<br />
80<br />
70<br />
60<br />
50<br />
40<br />
30<br />
20<br />
10<br />
Time (Minutes)<br />
2 4 6 8 10 12<br />
Time (Minutes)<br />
Bath Liquid: Ethanol<br />
-15<br />
0 10<br />
20 30 40 50 60<br />
68 www.rheologysolutions.com
• product news<br />
Rheological measurement with optical<br />
analysis - high temperature version extends<br />
testing up to 300ºC<br />
food industries<br />
polymer industries<br />
surface coatings industries<br />
pharmaceutical, cosmetics<br />
& allied industries<br />
chemical & allied industries<br />
<strong>Rheology</strong> and Microscopy<br />
The Thermo Scientific RheoScope module for<br />
HAAKE MARS Rheometer simultaneously records<br />
rheological properties and changes in the<br />
microscopic structure of the tested sample at a<br />
macroscopic level. Understanding micro structures<br />
enables researchers to characterise a product’s<br />
mechanical properties. The module is comprised<br />
of an optical microscope, digital video camera and<br />
temperature control unit that is used in conjunction<br />
with the HAAKE MARS rheometer platform.<br />
The HAAKE RheoWin software used to control the<br />
rheometer also positions and focuses the scope<br />
and polarisation filter. Rheological data and images<br />
(video sequences) can be viewed on line next to<br />
each other. In addition, the data and images can<br />
be stored in various formats for further evaluation<br />
and export. The RheoScope’s architecture allows<br />
the module to be adapted quickly for customised<br />
user configurations. The RheoScope module is<br />
available in two versions. The temperature range<br />
of the standard version is -5 to 120°C. In the<br />
high-temperature version the temperature is<br />
extended to 300°C.<br />
Simultaneously measures rheological properties<br />
and changes in the microscopic structure of the<br />
tested sample. The results allow researchers to<br />
speed formulation development, process<br />
optimisation and product processability.<br />
Applications / Examples<br />
• Food: fat, starch<br />
• Polymer: solution, melt<br />
• Pharma/Cosmetic: cream, lotion<br />
• Paint/Inks: printing paste, thickening agents<br />
• Petrochemical: crude oil, drilling fluid<br />
• Others: medical<br />
Formulations<br />
• Gels • Suspensions<br />
• Emulsions/Dispersions • <strong>Solutions</strong><br />
• Foam • Melts<br />
Rheological phenomena and structural changes<br />
that can be observed:<br />
• Shear thinning • Dilatancy<br />
• Thixotropy • Aging<br />
• Emulsification • Gelification<br />
• Disaggregation • Flocculation<br />
• Homogeneity • Orientation<br />
• Melting behaviour • Mixing<br />
Benefits:<br />
• Compact and full integration in the HAAKE<br />
MARS rheometer platform<br />
• All measuring modes including normal force<br />
measurement available with simultaneous<br />
recording of microscopic properties<br />
• Camera and microscope control with software<br />
• Simultaneous rheological and optical<br />
measurements<br />
• Visualisation of data and images in one<br />
software package<br />
• Analysis of structural changes under shear<br />
• Image analysis software for determination of<br />
particle sizes, particle size distribution and<br />
structure analysis <br />
Temperature ramp measured on potato wild type starch in water Thermo Scientific RheoScope module for the HAAKE Mars Rheometer<br />
info@rheologysolutions.com<br />
biennial 07-08<br />
69
product news & industry applications<br />
Accessories for HAAKE<br />
Viscotester 7 plus - Thermal Printer<br />
Thermal printer for HAAKE<br />
Viscotester 7 plus for<br />
recording and logging<br />
measured data.<br />
The rotational viscometer HAAKE Viscotester 7<br />
plus in combination with the thermal printer, is a<br />
set-up for routine measurements conforming to<br />
the ISO 2555 standard and fulfils the requirement<br />
for recording and logging measured data.<br />
The HAAKE Viscotester 7 plus is designed for<br />
measurements compliant with the standard ISO<br />
2555. Each rotational viscometer which fulfils the<br />
requirements of this standard is conforming to<br />
the Brookfield method and the measurement data<br />
of such viscometers are fully comparable with<br />
one another as long as the same viscometer type<br />
(L or R), same spindle and same rotational speed<br />
is used.<br />
Operating of the HAAKE Viscotester 7 plus can be<br />
either manual or computer controlled via the<br />
biennial 07-08<br />
all industries<br />
Figure 1. Rotational viscometer HAAKE Viscotester 7 plus (left), thermal printer (centre), Loading of a<br />
new paper roll (right).<br />
user-friendly HAAKE RheoWin 3 software<br />
(additional options: DFA 21 CFR Part 11 Tool).<br />
In the manual operation mode, the parameters;<br />
viscosity, percentage of maximum torque,<br />
rotational speed, spindle number, maximum<br />
viscosity and temperature are displayed. For<br />
recording and logging measure results, the<br />
thermal printer can be connected via the RS232<br />
port on the viscometer. At the end of a<br />
product news & industry applications<br />
CR-Mode - Low Shear Rates<br />
all industries<br />
Applying (very) low<br />
shear rates<br />
Most (very) low shear rate measurements are<br />
performed in CS Mode, because most real live<br />
applications in which (very) low shear rates are<br />
important are driven by a constant stress.<br />
Examples are sagging, sedimentation, shelf live,<br />
phase separation, all phenomena that are driven<br />
by a constant force i.e. gravitation. These<br />
processes are simulated in a rheometer by<br />
applying a constant stress. However, under<br />
certain circumstances applying a (very) low<br />
shear-rate might be required, for example when<br />
the flow of material which is slowly stirred in a<br />
large container needs to be simulated<br />
(measured). The measurement data below shows<br />
that the HAAKE MARS is very capable of applying<br />
very low rotational speed, i.e. very low shear<br />
rates.<br />
Reliable data down to n = 10 -5 rpm<br />
The graphs below show the result of an<br />
experiment in which the rotational speed was<br />
stepwise increased from 10 -5 rpm to 10 -2 rpm.<br />
Even at a very low rotational speed (and a very<br />
low torque) the measured viscosity is within 5%<br />
from the specified value.<br />
A full copy is available by quoting<br />
PS002-e<br />
measurement the displayed data, as well as date<br />
and time, can be printed out at the push of a<br />
button. Moreover, the print-out has a filed for the<br />
signature for the operator. Thus the measured<br />
data is ready for archival storage.<br />
Ordering number: 999-0118. Thermal<br />
printer for HAAKE Viscotester 7 plus<br />
(including connecting cable for HAAKE<br />
Viscotester 7 plus).<br />
Instrument: HAAKE MARS, UTC Peltier, PP35, gap<br />
= 0.5 mm. Sample: Newtonian Oil, η = 175 Pas<br />
70 www.rheologysolutions.com
product news & industry applications<br />
Optical Analysis and <strong>Rheology</strong><br />
food industries<br />
polymer industries<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
chemical & allied industries<br />
Simultaneously measure<br />
rheological properties and<br />
microscopic structure of<br />
your tested sample.<br />
HAAKE PolyLab OS Torque<br />
Rheometer RD4 Application<br />
Packages<br />
RD4 application packages for the Thermo<br />
Scientific torque rheometer HAAKE PolyLab OS<br />
are dedicated to serving the polymer processing<br />
and polymer formulation laboratory. These<br />
application packages incorporate batch mixers<br />
and single-screw extruders to form test samples<br />
required for polymer melts and ceramic slurries.<br />
The typical combination for the characterisation of<br />
these types of materials is:<br />
• PolyLab OS Mixer Package<br />
• PolyLab OS Extruder Package<br />
• PolyLab OS Upgrade Packages<br />
info@rheologysolutions.com<br />
Gain insight in to rheological phenomena like:<br />
• Shear thinning • Dilatancy<br />
• Thixotropy • Gelification<br />
• Aging • Emulsification<br />
The Thermo Scientific HAAKE MARS Rheometer<br />
with RheoScope module combines rheology with<br />
microscopy allowing you to speed formulation<br />
development and process optimisation.<br />
Benefits include:<br />
• Camera and optical control with HAAKE<br />
RheoWin Software<br />
• Observation of data and images in one<br />
software package<br />
product news & industry applications<br />
New Product Brochures<br />
polymer industries<br />
chemical & allied industries<br />
HAAKE PolyLab OS<br />
Docking Station<br />
Mobile bench for measuring mixers and<br />
measuring extruders. When existing measuring<br />
mixers and extruders need to be upgraded with<br />
newer torque rheometer drives and software, the<br />
modular Thermo Scientific HAAKE Docking Station<br />
OS is the right accessory to use.<br />
Applications:<br />
• Mobile bench for Rheocord mixer 600 and<br />
Rheocord miser 3000<br />
• Docking station for existing single-screw<br />
extruders<br />
• Adapter bench for CTW 100 conical twin<br />
screw extruder<br />
• Modular bench to integrate mixers and<br />
extruders of different brands<br />
Product brochures are available on<br />
request by completing the information<br />
request form<br />
• All measuring modes including normal force<br />
measurement available with simultaneous<br />
recording of microscopic properties<br />
• mage analysis software SPIP for the<br />
determination of particle size, particle<br />
distribution and for structural analysis.<br />
Formulations: Gels, suspensions, solutions, foam,<br />
dispersion/emulsion<br />
An application note on the Image<br />
analysis software SPIP is available by<br />
quoting P009-e<br />
biennial 07-08<br />
71
product news & industry applications<br />
Disposable plate/plate-measuring<br />
geometry for the controlled<br />
temperature chamber (CTC).<br />
For the controlled<br />
temperature chamber (CTC)<br />
a new plate/plate measuring<br />
geometry has been<br />
developed.<br />
The set consists of an upper shaft and a lower<br />
shaft with an integrated temperature sensor.<br />
By using the supplied press tool an exact<br />
perpendicular alignment and reproducible<br />
mounting of the disposable plates on the shafts is<br />
guaranteed (Fig.1).<br />
The standard aluminium plates have a diameter<br />
of 20 mm. Plates with other diameters are<br />
available on request.<br />
It is recommended to use the optionally available<br />
sample collection ring (below the lower plate); in<br />
order to protect the temperature chamber against<br />
spilled sample material.<br />
After a measurement the disposable plates are<br />
easily removed from the holders by using the<br />
supplied removal tool (Fig. 2).<br />
A copy of this is available by quoting<br />
P010-e<br />
biennial 07-08<br />
all industries Handling information:<br />
Figure 1 Mounting of a disposable plate on a shaft: press tool, upper shaft and disposable plate (left).<br />
Mounting of a disposable plate on a shaft (middle). Disposable measuring geometry consisting of upper<br />
an lower shaft with sample collection ring build into a HAAKE MARS (right)<br />
Figure. 2 Removing of a disposable plate from a shaft: removal tool positioned on the lower shaft (left).<br />
Handling of the removal tool (middle). Disassembled disposable geometry (left)<br />
Order information:<br />
222-1808 Disposable plate/plate-measuring geometry consisting of a lower and an upper shaft, incl.<br />
press tool for mounting the disposable plates on the shafts and removal tool to remove<br />
the disposable plates from the shaft<br />
Necessary accessories:<br />
222-1769 Temperature sensor for lower shaft<br />
222-1295 Disposable aluminium plates PP20E, diameter = 20 mm (100 pieces)<br />
Plates with other dimensions are available on request, e.g.:<br />
603-0021 Disposable aluminium plates PP35E, diameter = 35 mm (100 pieces)<br />
Recommended accessories:<br />
222-1778 Sample collection ring (5 pieces), stainless steel for plates PP20E<br />
If you have an application and interest in high temperature rheology<br />
& simultaneous microscopy and would like to be a part of a workshop<br />
where you can run your own samples, refer to the information on page 4.<br />
72 www.rheologysolutions.com
product news & industry applications<br />
Marimex - In Line Torsional<br />
Viscometers<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
chemical & allied industries<br />
polymer industries<br />
mining industries<br />
ViscoScope viscosity<br />
analysers from Marimex<br />
have been applied in many<br />
different industries. Whether<br />
it is ambient temperature<br />
applications in the<br />
pharmaceutical industry like<br />
herbal ointments or a high<br />
temperature application in<br />
the polymer industry like<br />
phosphorous pentasulfide.<br />
If you have an application as yet unsolved, send<br />
us details of the application and we will work with<br />
Marimex to provide you with a constructive<br />
solution.<br />
Following are some examples of ViscoScope<br />
applications and their related specifications:<br />
The ViscoScope process viscometer measures the<br />
viscosity of liquids continually and precisely inline.<br />
The measurement system consists of a sensor,<br />
transmitter and the transmission cable. Safety<br />
barriers are added, if the sensor is being used in<br />
a hazardous area.<br />
The sensor does not employ any moving parts<br />
and it is maintenance free. To measure the<br />
viscosity, the viscometer utilises the torsional<br />
oscillation principle. The power required, to<br />
maintain the small amplitude at the resonance<br />
frequency of the sensor, is a measure for the<br />
viscosity (mPa.s x gr/cm3 / η x ρ)<br />
info@rheologysolutions.com<br />
Marimex ViscoScope Sensor with model caption.<br />
Application Instrument Used & Conditions<br />
Herbal Ointment VA-300M with VS-4550 or VS-B450<br />
Ambient temperature, pressure
product news & industry applications<br />
Nano Composites<br />
biennial 07-08<br />
polymer industries<br />
Nano compounds are often prepared in solid form<br />
using the traditional and available mixing and<br />
extrusion devices. Now you can optimise these<br />
sensitive processes.<br />
Nanotechnology – typical applications:<br />
• Improving mechanical properties<br />
• Increasing the electrical conductivity<br />
• Increasing thermal conductivity<br />
• Biocide / antibacterial<br />
• UV absorption<br />
Dispersive and distributive mixing:<br />
• For nearly all mixing applications a well<br />
dispersed and well distributed mixture is<br />
required<br />
• Distributive mixing can be achieved by<br />
splitting and reorienting the flow repeatedly<br />
• Dispersive mixing can be achieved by<br />
passing the mixture through small regions of<br />
intense deformation<br />
• Mixing and composites, M. Kontopoulous<br />
Chee18.2. p390 presentation Queens<br />
University.<br />
A copy of the PowerPoint presentation is<br />
available on request by quoting<br />
Nano Composites 2007.<br />
In Stock – Despatched<br />
within 48 hours from receipt<br />
of purchase order.<br />
HeatTech 26L heating circulator – temperature<br />
range ambient to +100ºC. $2,399 excluding GST<br />
and local delivery<br />
...Feed ports...<br />
...Screw design...<br />
Maximum flexibility is available with twin screw extruders for HAAKE PolyLab OS<br />
product information<br />
Heating Recirculators<br />
all industries<br />
Full product information is available on line plus<br />
an extensive range of temperature control baths<br />
to meet the application requirements of diverse<br />
industries.<br />
Visit www.temperaturecontrolbaths.com<br />
for full product information and technical<br />
specifications<br />
...Length...<br />
...Split Barrel<br />
Poorly distributed - Poorly dispersed Well distributed - Poorly dispersed<br />
Poorly distributed - Well dispersed Well distributed - Well dispersed<br />
HeatTech 26L<br />
74 www.rheologysolutions.com
product news<br />
New NESLAB ThermoFlex 2500 –<br />
Recirculating Chiller<br />
all industries<br />
This is the third configuration<br />
of the ThermoFlex platform<br />
released by Thermo<br />
Fisher Scientific.<br />
Suitable for a diverse range of applications<br />
and industries:<br />
• Semiconductor<br />
• Packaging<br />
• Analytical instrumentation<br />
• Laser<br />
• Research<br />
• Medical equipment<br />
Key Options Include:<br />
Auto refill Allows for self-filling of the chiller to<br />
ensure that the proper level in reservoir is<br />
maintained, saving valuable time.<br />
Anti-drainback Ensures reservoir does not<br />
overflow when chiller is shut down. This allows<br />
the chiller to be installed more than 24 ft. below<br />
the application.<br />
DI resistivity internal DI filtration internal to the<br />
chiller is used to maintain the resistivity level<br />
below 3 Mohm, with an alarm at 1 Mohm. This<br />
minimises footprint and eliminates downtime<br />
needed to change the filter, while ensuring<br />
constant quality of DI water to your application.<br />
Pressure relief Easily adjustable pressure relief<br />
valve allows for control of the outlet pressure<br />
from the chiller to be regulated, ensuring your<br />
process performance requirements are met.<br />
Flow Control Utilizes a 3-way valve that allows<br />
you to control the amount of flow to the<br />
application. The process flow is measured on the<br />
return to the unit, ensuring the appropriate<br />
amount of flow is provided to the application.<br />
Pressure/Flow Control Allows you to control the<br />
pressure as well as the flow in your application.<br />
Utilises a pressure relief valve and monitors the<br />
flow through the process return and displays the<br />
reading on the controller.<br />
info@rheologysolutions.com<br />
The NESLAB ThermoFlex 2500 is a reliable, easyto-use<br />
chiller optimised for the most demanding<br />
applications. Delivers continuous cooling capacity<br />
up to 2500 watts.<br />
Water-Cooled Uses facility water to cool the<br />
system, minimizing heat dissipation into the<br />
environment.<br />
Key Accessories Include:<br />
Installation Kit Supply and return plumbing<br />
available in 25 and 50 ft lengths, suitable for<br />
temperatures up to +80°C.<br />
Fluid Quality Kit Complete fluid quality system<br />
includes algaecide and corrosion inhibitor to<br />
ensure your process has optimal fluid quality.<br />
Ethylene Glycol Laboratory-grade ethylene glycol<br />
allows circulation to temperatures down to -20°C<br />
in a 50/50 mixture with water. Available in a 5<br />
gallon container.<br />
Propylene Glycol Laboratory-grade propylene<br />
glycol allows circulation to temperatures down to<br />
-20°C in a 50/50 mixture with water. Available in<br />
a 5 gallon container.<br />
Maintenance Kit Includes condenser air filters and<br />
in-line fluid filters for ease of maintenance.<br />
A dedicated website for temperature control has been established<br />
by <strong>Rheology</strong> <strong>Solutions</strong> …www.temperaturecontrolbaths.com<br />
The website covers the entire range of temperature control baths<br />
currently available to meet the diverse needs of industry applications<br />
across QA/QC, R&D and Production areas<br />
biennial 07-08<br />
75
Product Specifications<br />
Setpoint Temperature Range 5°C - 40°C<br />
Ambient Temperature Range 10°C - 40°C<br />
Temperature Stability +/- 0.1°C<br />
Setpoint Cooling Capacity at 20°C<br />
(see graph above for cooling curves)<br />
60 Hz 2500W (8538 BTU)<br />
50 Hz 2200W (7513 BTU)<br />
Reservoir Volume Litres 7.2<br />
Footprint or dimensions<br />
(HxWxD) cm 73.8 x 43.5 x 65.2<br />
Unit Weight kg 80.3<br />
Pumps<br />
(see graph above for performance curves)<br />
PD 1 - Positive Displacement<br />
50 Hz 1.7 gpm @ 60 psi<br />
PD 2 - Positive Displacement<br />
50 Hz 3.3 gpm @ 60 psi<br />
Power options 230V/50Hz/1 Phase<br />
16A Circuit<br />
Compliance NRTL Certified<br />
to CSA and UL<br />
Standards;<br />
CE-Marked<br />
Specifications obtained at sea level using water as the<br />
recirculating fluid, at a 20°C process setpoint, 25°C ambient<br />
condition, at nominal operating voltage. Other fluids, fluid<br />
temperatures, ambient temperatures, altitude or operating<br />
voltages will affect performance. Thermo Fisher Scientific<br />
reserves the right to change specifications without notice.<br />
biennial 07-08<br />
product information<br />
Twin-Screw Extrusion<br />
at a Lab Scale<br />
all industries<br />
PRISM small scale extruders and ancillaries allow<br />
research and development at a laboratory scale.<br />
The twin screw extruders from 16mm to 36mm<br />
diameters are supplemented by purpose built<br />
PRISM 16 mm EuroLab twin screw extruder<br />
ancillaries including bench-top blenders,<br />
pelletisers and sheet and film take-off units.<br />
For complete details and product<br />
information, complete the information<br />
request form or send an email detailing<br />
your application requirements.<br />
product information<br />
Cooling Recirculators<br />
all industries<br />
In Stock – Despatched<br />
within 48 hours from receipt<br />
of purchase order.<br />
CoolTech 320 refrigerated circulator -<br />
temperature range -28ºC to +100ºC. $3,999<br />
excluding GST and local delivery<br />
Full product information is available on line plus<br />
an extensive range of temperature control baths<br />
to meet the application requirements of diverse<br />
industries.<br />
Visit www.temperaturecontrolbaths.com<br />
for full product information and technical<br />
specifications<br />
CoolTech 320<br />
76 www.rheologysolutions.com
product focus<br />
High Speed Pellet Scan System –<br />
Throughput up to 250 kg/hr<br />
polymer industries<br />
The PS200C inspection<br />
system from Optical Control<br />
Systems is used to analyse<br />
transparent and opaque<br />
pellets.<br />
The pellets are inspected with a high-resolution<br />
3-Chip CCD colour camera for impurities, foreign<br />
bodies, or colour deviations as well. The testing<br />
material is fed into the appliance through a<br />
hopper. The pellets are conveyed separately over<br />
the inspection zone. After the optical evaluation<br />
the contaminated pellets can be separated into a<br />
different container (sorting unit option).<br />
Measuring errors are eliminated by use of<br />
numerous additional optical components.<br />
There is no colour dependency as with many<br />
other optoelectronic appliances.<br />
A high level of efficiency is achieved by powerful<br />
image processing software. The synchronisation<br />
of the transport system with the image<br />
processing offers a major contribution to the<br />
reproducibility of the measurement results.<br />
Installation in the bypass guarantees production<br />
monitoring and rapid reaction to any occurrences.<br />
The system provides a variety of individual<br />
configurations, which guarantee an improved<br />
adaptation to specific requirements.<br />
The measurement data are stored in a test report<br />
to enable future analysis. The recorded images<br />
and measured data can be observed on a screen<br />
during the measuring process. The results can be<br />
shown and printed in tables or graphs.<br />
Along with a pure inspection of pellets the system<br />
can also be used to record, file and document.<br />
Each defined deviation is recorded in the<br />
measurement protocol via a multidimensional<br />
characteristics vector with an error map.<br />
The system can be adapted exactly to the<br />
respective requirements with the<br />
help of the extensive software packages.<br />
info@rheologysolutions.com<br />
High Speed Pellet Scan System PS200C<br />
Applications<br />
• Opaque pellets<br />
• Coloured pellets<br />
• Transparent pellets<br />
• Material throughput up to 250 kg/hr<br />
Technical Data<br />
Camera 3 Chip CCD colour matrix camera<br />
Lighting High frequency synchronised<br />
fluorescent lamp. White light<br />
spectrum<br />
Computer Industrial CPU: Intel Pentium 4,<br />
up-to-date technology<br />
Interfaces Ethernet 10/100 M Base-T,<br />
Digital and analogue I/O, USB,<br />
MODBUS, PROFIBUS, RS232,<br />
BDE, SAP interface or SQL<br />
Remote Extender max. 100 m Service<br />
Control Remote control<br />
Software Operating System Windows XP<br />
Size Dimensions (l x w x h)<br />
650 x 770 x 770 mm<br />
Weight approx. 100 kg<br />
Connection Power supply 230 V<br />
values AC / 115 V AC<br />
Temperature 10ºC to 45ºC<br />
Benefits<br />
• Optimising the production process through<br />
detailed characteristics specifications<br />
• 24 hour online production surveillance trend<br />
analysis parallel to production<br />
VisConfig software for easy configuration of all<br />
parameters<br />
Pellet conveyor line<br />
biennial 07-08<br />
77
product news & industry applications<br />
New Product Brochures<br />
& Information Sheets<br />
CD-Mode Curing Measurement<br />
– HAAKE MARS<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
chemical & allied industries<br />
The HAAKE MARS is equipped with a self-learning<br />
deformation control loop based on neural network<br />
technology for controlled deformation (CD)<br />
oscillation measurements.<br />
The HAAKE MARS rheometer is now available<br />
with a support fixture for the comparative analysis<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
chemical & allied industries<br />
The HAAKE MARS rheometer is equipped with a<br />
highly sensitive normal force sensor and a very<br />
biennial 07-08<br />
In CD-Mode the deformation sine wave is<br />
continuously controlled, this enables the control<br />
loop to react almost instantaneously to changes in<br />
the material. A quick reaction to material changes<br />
is required when the mechanical properties of a<br />
material are measured, during a curing reaction,<br />
using constant strain oscillation.<br />
The brochure provides an example of curing<br />
of a dental material. A copy is available by<br />
requesting PS001-e<br />
Support fixture for the analysis of<br />
textile samples - Accessories for<br />
HAAKE MARS<br />
polymer industries<br />
chemical & allied industries<br />
polymer industries<br />
food industries<br />
of elasticity and sensoric (haptic) properties of<br />
textile samples.<br />
The brochure provides full details on the<br />
fixture, tests recommended and ordering<br />
information. A copy is available by requesting<br />
P012-e<br />
Sample fixture for bending and<br />
breaking tests – Accessories for<br />
HAAKE MARS<br />
precise lift motor which allows applying controlled<br />
axial forces to the sample, pushing or pulling the<br />
material.<br />
A new sample fixture has been developed to<br />
investigate the bending and breaking behaviour of<br />
a wide range of materials.<br />
The brochure provides details on the tool,<br />
and adapting it to the HAAKE MARS, plus full<br />
ordering information. A copy is available by<br />
requesting P014-e<br />
78 www.rheologysolutions.com
product news & industry applications<br />
New Product Brochures<br />
& Information Sheets<br />
Tool for checking the optical<br />
quality of the RheoScope module<br />
– HAAKE MARS<br />
polymer industries<br />
food industries<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
chemical & allied industries<br />
surface coatings industries<br />
Standard Liquids<br />
all industries<br />
The functionality and/or calibration of any<br />
measuring instrument should be checked<br />
regularly. Checking a rheometer or viscometer is<br />
usually and most easily done by measuring a<br />
standard liquid with a certified viscosity value.<br />
A standard liquid is a Newtonian fluid for which<br />
the viscosity value is certified for one or several<br />
temperature values.<br />
A wide range of standard liquids with different<br />
viscosity values and uncertainties as well as<br />
different reference temperatures and chemical<br />
structures (mineral oils, synthetic oils) are<br />
available.<br />
Standard liquids from Thermo Fisher Scientific are<br />
delivered with a certified viscosity at 20°C and an<br />
uncertainty of ±2% (±4% for E7). Standard<br />
liquids with viscosity values between 5 mPas and<br />
40000 mPas are available in 100ml or 500 ml<br />
containers.<br />
Standard liquids with other viscosity values or<br />
other reference temperatures as well as the<br />
info@rheologysolutions.com<br />
A new tool for checking the quality of images<br />
acquired with the RheoScope module for the<br />
HAAKE MARS has been developed.<br />
This tool consists of a closed cell with a reflective<br />
upper plate and a lower glass plate, containing a<br />
watery solution with standard particles with<br />
diameters of 1.5, 4, 8 and 20 μm.<br />
Full information is available in the brochure<br />
and a copy is available by<br />
requesting P016-d<br />
delivery in other containers (e.g. 1.0 l) are<br />
available on request.<br />
Standard liquids with a lower uncertainty of the<br />
viscosity (±0.4%) and/or certified viscosity values<br />
at other temperatures between 20°C and 100°C<br />
are available from the German Calibration Service<br />
(DKD – Deutscher Kalibrierdienst) amongst<br />
others.<br />
Because of their lower viscosity - temperature<br />
dependence silicon oils are often used for<br />
checking simple viscometers which do not<br />
provide any means of temperature control. For<br />
this application the slight shear thinning<br />
behaviour of silicone oils (decreasing of the<br />
viscosity with increasing shear rate) should be<br />
neglected.<br />
For checking a specific viscometer or rheometer<br />
configuration it is important to use a standard<br />
liquid that matches the parameters (temperature,<br />
viscosity, etc.) of the routine measurements<br />
normally run on that instrument.<br />
When comparing the measured viscosity value<br />
with the standard liquid's certified value it is<br />
important to take the instruments uncertainty into<br />
account also.<br />
An information sheet is available covering<br />
the above text and also includes full<br />
ordering information. A copy is available on<br />
request by quoting P-015-e<br />
biennial 07-08<br />
79
product news<br />
Higher Instrument<br />
Precision and Reliable<br />
Quality Control<br />
HAAKE Viscotester 1 plus and 2 plus<br />
Higher instrument precision<br />
is now requested for basic<br />
rheology measurement with<br />
handheld instruments.<br />
The VT 2 plus allows the 1% calibration accuracy<br />
needed to fulfil this requirement.<br />
The entire VT 1 plus and VT 2 plus series is<br />
the standard in quality control and combines ease<br />
of use with exact and reliable measurements.<br />
The HAAKE Viscotester 1 plus & 2 plus are quick,<br />
exact and reliable rotational viscometers with a<br />
one button operation which can be operated<br />
hand-held or on a stand. A digital display delivers<br />
clear results. Battery powered, these units do not<br />
biennial 07-08<br />
all industries<br />
require external power. These Viscotester models<br />
are delivered in a sturdy carrying case as a<br />
complete ready-to-use package with 3 measuring<br />
systems.<br />
During the past decades HAAKE Viscotesters have<br />
successfully proven their value wherever quick<br />
and reliable tests and comparative measurements<br />
are part of daily routine work. They have also<br />
been established as standard instruments for<br />
quality control. The new generation – HAAKE<br />
Viscotester 1 plus & 2 plus – continues this<br />
tradition and fulfils the highest demands<br />
regarding design and convenience.<br />
Main features:<br />
• Quick, exact and reliable<br />
• One button operation<br />
• LCD display<br />
• No mains supply needed (battery-operated)<br />
HAAKE Viscotester 1 / 2 plus<br />
Typical application fields:<br />
• Quick viscosity tests, e.g. for process<br />
optimization or machine adjustment<br />
• Batch control in production<br />
• production in control<br />
Typical samples:<br />
• Printing inks, paints, inks<br />
• Shampoos, creams, lotions<br />
• Oils, greases, pastes, lubricants<br />
• Sauces, thickeners<br />
product news<br />
NanoLab Compounder Package<br />
polymer industries<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
chemical & allied industries<br />
surface coatings industries<br />
The Thermo Scientific<br />
NanoLab compounder<br />
package contains the tools<br />
to mix or compound Nano<br />
particles (Nano tubes) in a<br />
base polymer.<br />
Based on recommendations from users in the<br />
industry and Universities it is recommended to:<br />
• use the standard Thermo Scientific HAAKE<br />
MiniLab micro compounder for temperatures<br />
up to 350°C<br />
• use the control panel for quick test runs,<br />
trials and the cleaning<br />
• employ the application software to run<br />
defined and reproducible tests<br />
• compound Nano particles and do rheometry<br />
with counter-rotating screws<br />
• use the co-rotating screws for applications<br />
with additives requiring less shear force<br />
A copy of this product information brochure<br />
is available by request.<br />
HAAKE MiniLab II compounder with co- and<br />
counter-rotating screws<br />
80 www.rheologysolutions.com
product information<br />
HAAKE MiniLab –<br />
Compounder & Reactor<br />
polymer industries<br />
The use of a conical twin<br />
screw extruder with backflow<br />
channel combines aspects of<br />
mixing and extrusion in a<br />
batch process.<br />
Tests and results of the new MiniLab micro<br />
compounder are discussed in the following paper.<br />
With a total filling volume of 7 ml and a built in<br />
slit capillary die the applications focus on<br />
compounding and reactions of small amounts of<br />
polymers in molten stage.<br />
Selecting the screw types: Co- or counter<br />
rotating?<br />
In order to open up an even wider spectrum of<br />
applications for the customer, the MiniLab works<br />
as co-rotating or as counter-rotating doublescrew<br />
extruder. This results in different types of<br />
screws.<br />
Simply exchanging two gear wheels in the<br />
gearbox changes the rotating direction of the<br />
screws. Figure 2 shows the co-rotating pair of<br />
screws. It also shows a faster compounding of<br />
the master batch in comparison to Figure 4.<br />
In the following table further characteristics of<br />
the used screws are summarised.<br />
Table 2 Characteristics of the screw types<br />
Co- Counter<br />
rotating rotating<br />
Resident time distribution wide narrow<br />
Forced extrusion - +<br />
Cleaning + -<br />
Extruder amount + 0<br />
Blending of sensitive products ++ 0<br />
High shear rates, dispersing - ++<br />
Rheological measurements 0 ++<br />
Required duration of blending ++ +<br />
info@rheologysolutions.com<br />
HAAKE MiniLab II Complete System<br />
Fig. 2: Co-rotating screws: a) PE melt, b) Asaclean (PS cleaning compound) + Remafin orange duration<br />
of the test t = 90 s, test conditions like in Figure 4.<br />
A number of topics and applications have been<br />
presented on the HAAKE MiniLab in a combined<br />
product information flyer. The topics included are:<br />
• Toughness enhancements in poly (methyl<br />
methacrylate) by addition of oriented<br />
multiwall carbon nanotubes<br />
• The effect of processing variables on the<br />
structure and rheological properties of<br />
polymer/clay nanocomposites: Nylon 6/clay<br />
• Improving polymer blend dispersions in minimixers<br />
HAAKE MiniLab II Barrel Section<br />
A copy of this product information is<br />
available by request and includes the<br />
above mentioned topics.<br />
biennial 07-08<br />
81
product information<br />
Process Viscometers –<br />
Software Options<br />
Marimex ViscoScope process<br />
viscometers measure the<br />
viscosity of liquids continually<br />
and precisely in-line.<br />
ViscoScope sensors do not have any moving<br />
parts and are maintenance free. A constant<br />
amplitude torsional oscillation principle is utilised<br />
to measure the viscosity. Various ViscoScope<br />
sensors and transmitters are available. All sensors<br />
work with all transmitters.<br />
All transmitters are delivered with VisConfig<br />
configuration software to simplify the start-up<br />
process. Optionally ViscoView software for PC<br />
compatible computers and a touch panel display<br />
are available as a graphical interface.<br />
ViscoView Software – Optional Software<br />
Collected data is stored in a tab delimited ASCII<br />
format. The file is being closed after each data<br />
collection, this enables the file to be copied into a<br />
different directory at any time. The data collection<br />
rate can be adjusted between 10 and 600<br />
seconds. The file can be imported into a<br />
spreadsheet like Excel, where additional<br />
calculations and graphical manipulations can be<br />
accomplished. The following parameters can be<br />
collected:<br />
• Viscosity (all available)<br />
• Process Temperature<br />
• Coil Temperature (transducer dependent)<br />
• Resonance Frequency (transmitter dependent)<br />
• External Input (transmitter dependent)<br />
• Date and Time<br />
biennial 07-08<br />
food industries<br />
surface coatings industries<br />
mining industries<br />
pharmaceutical, cosmetic<br />
& allied industries<br />
chemical & allied industries<br />
ViscoView® data collection software for ViscoScope viscometer systems<br />
VisConfig software for easy configuration of all parameters<br />
VisConfig Software<br />
The VisConfig Software provides an easy interface<br />
for the configuration of all customer accessible<br />
parameters via a PC compatible computer.<br />
VisConfig has been configured to work with the<br />
ViscoScope firmware version MMX1.011. Special<br />
issues are available to interface to others<br />
firmware versions. VisConfig also provides a tool<br />
to check all ViscoScope Modbus addresses<br />
and instrument types connected to the PC. A<br />
single Modbus address can be reconfigured in<br />
the first screen. A functionality check is available<br />
to check the function of the sensor in air after the<br />
zero procedure. The result will show if the sensor<br />
works within known parameters. VisConfig also<br />
does a one time check of all measurement<br />
parameters and can be used to continuously<br />
sample selected measurement parameters –<br />
the last 20 samples can be observed.<br />
82 www.rheologysolutions.com
• new product<br />
HAAKE PolyLab QC<br />
polymer industries<br />
The HAAKE PolyLab QC<br />
is a new measuring mixer<br />
& extruder system that meets<br />
todays and future quality<br />
control (QC) needs.<br />
The modular torque rheometer<br />
can be connected to an<br />
interchangeable mixer,<br />
single-screw extruder, or<br />
conical twin-screw extruder.<br />
info@rheologysolutions.com<br />
Concept<br />
• Modular torque rheometer with<br />
interchangeable mixer, single-screw extruder,<br />
conical twin-screw extruder<br />
• Bench or floor model<br />
• Control via HAAKE PolySoft software<br />
Backwards Compatibility<br />
• Hardware compatible with old mixers,<br />
extruders<br />
• Existing accessories can still be used<br />
• Data compatibility (importing of old data)<br />
Specifications<br />
• Torque range: 0 - 300Nm<br />
• Speed range: 0 - 200 rpm<br />
• Temperature control zones: 5<br />
• Temperature reading channels: 4<br />
Interfaces/Communication<br />
• CAN open control communication with<br />
temperature, motor controller<br />
• CAN open data communication for pressure<br />
and remote signals<br />
• USB interface to host computer (LAN as<br />
option)<br />
HAAKE PolyLab QC<br />
Measuring Mixers<br />
A typical mixer test is run at a defined rotor speed<br />
(shear rate). The material’s response to the shear<br />
is recorded as torque and displayed versus time.<br />
As a material’s properties are very sensitive to<br />
temperature, the mixer chamber is separated into<br />
continued on page 84 <br />
biennial 07-08<br />
83
Haake PolyLab QC<br />
continued from page 83<br />
As a material’s properties are very sensitive to<br />
temperature, the mixer chamber is separated into<br />
different sections. These are individually<br />
temperature-controlled by the HAAKE PolyLab QC.<br />
Optimum temperature control quality can be<br />
achieved by an automated recognition of the<br />
connected mixer.<br />
Although the temperature of the mixing chamber<br />
is constantly controlled, the material’s melt<br />
temperature during a test may rise due to the<br />
shear introduced. The melt temperature is also<br />
recorded during the test by a separate<br />
thermocouple. The recorded “Rheogram” (torque<br />
and melt temperature vs. time at constant speed)<br />
is characteristic for different material types and<br />
HAAKE PolyLab QC mixer - Intelligent measuring<br />
mixers simplify your quality control<br />
blends. It can be used as a fingerprint in quality<br />
control for outgoing and incoming product<br />
inspections. As changes in torque are related to<br />
structural changes in the material, a Rheogram<br />
can be used to investigate and verify reactions of<br />
different additive types or concentrations on the<br />
sample’s melting behaviour.<br />
Typical Investigations<br />
• Testing the melting and degradation behaviour<br />
of polymer melts<br />
• Quantifying viscosity when adding nano<br />
particles or other additives<br />
• Testing gelation and plastification behaviour<br />
of PVC dry-blends<br />
• Measuring the flow and curing behaviour<br />
of thermosetting plastics<br />
• Characterizing the influence of different<br />
additives such as carbon black, fillers<br />
lubricants, accelerators and sulphur for<br />
rubber mixtures<br />
• Recording the masticating and vulcanizing<br />
behaviour of elastomers<br />
biennial 07-08<br />
• Measuring oil absorption of carbon black<br />
• Quantifying the absorption of DOP for PVC<br />
dry-blends<br />
• Measuring the stable torque in regard to<br />
individual and combined influences of fillers<br />
and additives such as stabilizers, lubricants<br />
and colour pigments<br />
• Testing high performance plastics to check<br />
processability<br />
• Performing electric conductivity<br />
measurements for rubber mixtures.<br />
Due to the backwards compatibility of the<br />
mechanical and electrical interfaces of the HAAKE<br />
PolyLab QC, existing mixing equipment can be<br />
used with a state-of-the-art torque rheometer that<br />
is equipped with reliable digital controls and<br />
operated using the modern, user-friendly Thermo<br />
Scientific HAAKE PolySoft software package.<br />
]<br />
m<br />
N<br />
[<br />
M<br />
55<br />
50<br />
45<br />
40<br />
35<br />
30<br />
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20<br />
15<br />
10<br />
5<br />
0<br />
A<br />
B C<br />
0 0,8 1,6 2,4<br />
t [min]<br />
F F<br />
3,2<br />
F<br />
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Mixer Software<br />
Small laboratory mixers are traditionally used to<br />
mix and/or measure the viscosity of a 40-70 g<br />
mixture as a function of time and temperature with<br />
different shaped rotors. Typical examples are PVC<br />
dry blend mixing, PVC degradation test,<br />
rubber/carbon black mastification, cross linking of<br />
polymers, curing of resins and thermosetting<br />
properties.<br />
HAAKE PolyLab QC Single<br />
& Twin Screw Extruders<br />
Single-screw extruder<br />
The most common methods in processing<br />
polymers are screw plastification and injection<br />
moulding. For testing quality and processability of<br />
those materials, the single-screw laboratory<br />
extruder 19/25 QC-B is a proven tool. With over<br />
35 years of expertise, we’ve developed a wide<br />
variety of different screw designs that are<br />
guaranteed to provide the best performance.<br />
Special solutions such as chemical or wear<br />
resistance are also available to extrude harsh<br />
materials. To shape a polymer for further<br />
processes and tests, different dies can be adapted<br />
to the extruder. Rod dies and water bath for strand<br />
extrusion, sheet and ribbon dies in various<br />
dimensions to produce bands or cast films, and<br />
blown film dies and take off tower complete the<br />
testing equipment. Besides the standardised filter<br />
test (EN 13900-5), comprehensive rheological<br />
studies can be conducted.<br />
Applications<br />
• Testing of the plasticizing behaviour<br />
• Testing the performance of additives<br />
and fillers<br />
• Measuring of the melt temperature and<br />
pressure along the barrel to optimize process<br />
parameters<br />
• Provide a homogeneous and constant flow<br />
melt<br />
• Production of strands, sheets, cast and blown<br />
films<br />
PVC_Sample A M = f(t)<br />
PVC_Sample B M = f(t)<br />
PVC_Sample C M = f(t)<br />
• Extrusion of ceramics and feed stock<br />
• Melt rheology<br />
Conical twin-screw extruder<br />
For continuous compounding and plasticising, the<br />
Thermo Scientific HAAKE CTW 100 QC is the ideal<br />
extruder in the HAAKE PolyLab QC system. This is<br />
a counter rotating conical twin-screw compounder,<br />
with intermeshing screws, that will give<br />
well-defined residence time for faultless<br />
production of process-critical polymers are ideal to<br />
mix additives and pigments. Dies and downstream<br />
ancillaries are compatible with the 19/25 QC-D<br />
single-screw extruder.<br />
Applications<br />
• Extrusion of thermally critical materials such<br />
as PVC<br />
• Compounding of fillers and reinforcing<br />
materials<br />
• Blending of polymers<br />
• Pilot plant production of master batches<br />
• Continuous mixing of recycling materials<br />
• Mixing of nano clays and carbons<br />
• Discharge for further process states<br />
continued on page 85 <br />
84 www.rheologysolutions.com
Haake PolyLab QC<br />
continued from page 84<br />
Compatibility of existing<br />
extruders<br />
Single-screw extruders and conical twin-screw<br />
extruders that are operated with the driving unit<br />
HAAKE Rheocord 90 or 9000, HAAKE RheoDrive<br />
5000 or System 40 are compatible to the HAAKE<br />
PolyLab QC. Laboratory extruders from other<br />
manufacturers can be adapted, too.<br />
HAAKE PolyLab QC Extruder - Powerful extruders<br />
continuously control your quality<br />
Measuring options provided<br />
by the HAAKE PolyLab QC<br />
Mixing, Kneading,<br />
Compounding & Plasticising<br />
In conjunction with measuring mixers, the HAAKE<br />
PolyLab QC offers a wide range of different<br />
applications. A typical mixer test is run at a<br />
defined speed (shear rate) versus time, and the<br />
material’s response is recorded as torque. This<br />
"Mixer-Rheogram" (torque, melt temperature vs.<br />
time at constant speed) is characteristic for<br />
different materials or blends and is often used as<br />
a "fingerprint" in quality control for incoming or<br />
outgoing product inspection.<br />
info@rheologysolutions.com<br />
Typical Investigations<br />
• Testing the melting and degradation behaviour<br />
of polymer melts<br />
• Quantifying viscosity when adding nano-<br />
particles and other additives<br />
• Testing the gelation and plasticizing behaviour,<br />
and the thermal stability of PVC dry-blends<br />
• Measuring the flow and curing behaviour of<br />
thermosetting compounds<br />
• Recording the masticating and vulcanizing<br />
behaviour of elastomers<br />
• Performing electric conductivity<br />
measurements during the mixing process<br />
]<br />
m<br />
N<br />
(<br />
]<br />
r<br />
a<br />
b<br />
[<br />
M<br />
p<br />
400<br />
350<br />
300<br />
250<br />
200<br />
150<br />
100<br />
50<br />
0<br />
2,5% Nanoclay no filler<br />
5% Nanoclay<br />
t_res: 30sec.<br />
140 150 160 170<br />
t [min]<br />
180 190<br />
Melting, Conveying,<br />
Compressing, Compounding<br />
Extruders are melting, conveying and<br />
compounding polymers under temperature,<br />
pressure and shear. The extruded polymer is<br />
pressed through a die to form a solid material<br />
such as a profile, sheet, film, strand or fibre. The<br />
extrusion process is characterized by monitoring<br />
processing power (torque), temperature, pressure<br />
and throughput. Special rheological dies (slit, rod)<br />
allow the determination of shear viscosity at<br />
defined shear rates.<br />
HAAKE PolyLab QC Measurements - Measuring<br />
options provided by the HAAKE PolyLab QC<br />
y<br />
t<br />
i<br />
s<br />
o<br />
c<br />
s<br />
i<br />
V<br />
10000<br />
1000<br />
100<br />
Oscaillation (RS Rheometer)<br />
Typical Measurements<br />
• Simulation of production processes like blown<br />
film, wire coating, profile extrusion<br />
• Testing individual and combined influences of<br />
additives (stabilizer, lubricant) and functional<br />
additives (antioxidation, UV-stabilizers,<br />
pigments and fillers)<br />
• Investigating the extrudability of newly<br />
developed materials<br />
• Manufacturing films, sheets, strands and<br />
profiles for optical, mechanical and<br />
weathering tests<br />
• Small scale production<br />
Data File<br />
M = f(t)<br />
n = f(t)<br />
p1 = f(t)<br />
TM9 = f(t)<br />
• Measuring rheological behaviour (dynamic<br />
viscosity)<br />
• Compounding and blending of polymers, fillers<br />
and additives<br />
• Dispersion and exfoliation of nano-fillers in<br />
a polymer matrix<br />
Flow curve LLPDE<br />
Online capillary rheology with HAAKE PolyLab QC<br />
is performed using a well defined die geometry<br />
(slit or capillary) on an extruder. The shear stress is<br />
derived from the pressure drop in the die (CAN<br />
pressure transducer signals) and the shear rate<br />
from the weight of the extrudate in a defined<br />
period of time.<br />
Slit-Capillary (Rheocord)<br />
Rod Capillary (Rheocord)<br />
10<br />
0,01 0,1 1 10 100 1000 10000 100000<br />
Shear rate<br />
biennial 07-08<br />
85
• new product<br />
The OP5 Online Rheometer<br />
polymer industries<br />
A system for plant optimisation<br />
and improved product quality.<br />
The function of the OP5 from Optical Control<br />
Systems (OCS) is to make certified measurements<br />
of the Melt Index and/or Polydispersity of small<br />
solid polymer samples. The primary duty of these<br />
measurements is overall control of many types of<br />
polymerisation processes. This ensures that the<br />
product can be made to specific formulations. The<br />
secondary duty is Quality Control in final product<br />
selling specification and in batch control. The OP5<br />
is logically situated in the plant analysis laboratory,<br />
which ensures best reliability and maintainability<br />
for these calibrated, precision measurements.<br />
Representative samples are therefore transported<br />
from various locations of the polymer<br />
manufacturing plant at the call of each analyser.<br />
Process Control and QC are full time activities,<br />
which require, as a minimum, one sampling point<br />
for each analyser.<br />
Representative samples are extracted from each<br />
reactor stage and from the finished product. In<br />
simple plant configurations, such as LDPE, PS,<br />
PET and Nylon this usually means one OP5 but in<br />
complex plants such as PP, HDPE and LLDPE two<br />
or more OP5 analysers would be required. The<br />
complex plants have powder samplers, which have<br />
degassing and catalyst deactivation stages close<br />
the analyser. At the plant end, these samplers can<br />
extract at the main discharge valve(s) of the<br />
reactor or at the primary de-gassing vessel, etc.<br />
according to the plant configuration. In the case of<br />
the pellet samples, these would normally be<br />
supplied from central (OCS) source, and in such<br />
cases the supply to the rheometers carries a<br />
priority to minimise the sampling delay time.<br />
biennial 07-08<br />
Melt flow measurements are performed after the<br />
solid sample is melted and conditioned to the<br />
appropriate test temperature. In the OP5 the<br />
melting process minimises any changes to the<br />
structure of the polymer but making a very rapid<br />
transition from solid to liquid, which substantially<br />
obviates shear damage, cross-linking, thermal<br />
degradation and other degradation processes. This<br />
sample preparation removes the last traces of any<br />
trapped air or gas and overall makes an important<br />
contribution to making the sample at the point of<br />
measurement fully representative of the process.<br />
In this unique way the OP5 makes control through<br />
rheology as reality.<br />
The melt flow is regulated by a sealed gear pump,<br />
which transports a metered quantity through a<br />
shaped die which has the normal MI die L/D. The<br />
shaping of the die is to minimise the delay in the<br />
slow moving polymer near the walls, without<br />
deviating the actual rheology relationships too far<br />
from the standard MI die.<br />
Measurements of pressure and flow rate are used<br />
to derive the standard Melt Index. Many features<br />
of the apparatus for measurements are covered in<br />
the patents. The patent, Melt Flow determination in<br />
Polymer process, has the following grants, EU 989<br />
45440, GB 233 4958 and US 09/622558. These<br />
patents also have integrated process control<br />
application. Systematic correlations are applied to<br />
compensate for the relationship between the OP5<br />
die and the lab test die (both ASTM D1283 and<br />
ISO 1133 tests use the same die form). The<br />
corrections derived from these correlations are<br />
specific to the actual polymer process and the<br />
local test methodology used to make the test. This<br />
is because each plant produces subtly different<br />
polymer structures and the manual test method<br />
result varies with operator and procedures. Once<br />
established the corrections<br />
continued on page 87 <br />
Performance Features<br />
• Controls - Menu-driven Windows interface<br />
and easy customisation<br />
• Access - Password protected to 5 levels<br />
• Optimum location - Use of laboratory<br />
environment to ensure high run time and<br />
accessibility for calibration and any<br />
maintenance<br />
• Low delay time - Fast sampling, sample<br />
preparation and measurement results in delay<br />
time more than adequate for control<br />
• Accuracy - Calibration is established by<br />
Porpoise Transfer Standard Optional<br />
full-time statistical process control packages<br />
• Full-time calibration - A statistical calibration<br />
system that conforms OP5 to the ISO 1133 or<br />
ASTM D1283 standards full time<br />
• Tables - Tabular display according to<br />
individual cycle measurements of<br />
temperatures, Pressure, flow rate, consumed<br />
weight of material, test results<br />
• Set points - Tabular display of all set points<br />
• Real time display - Continuous trend display<br />
of MI with tramlines and product name<br />
overlays. Additional trend displays,<br />
temperatures, pressures, mass flow, total<br />
mass flow<br />
• Recipe control of cycle and conditions -<br />
Operator control via menu of parameters,<br />
sequences and user Product Names<br />
• Sample size control - Adaptive sample sizing<br />
to minimise delay of measurement<br />
• Statistical analysis packages - User friendly<br />
calculations of averages, standard deviation,<br />
Cpk and other process variables. Export<br />
facilities<br />
• Alarms - External alarm interface<br />
• Open database - All records can be converted<br />
into any standard file format<br />
Scope Of Application<br />
• Powder or pellets from polymer processes<br />
• Powder ex-reaction<br />
• Pellets post extrusion<br />
• Samples transported to Laboratory via<br />
OCS-Porpoise systems<br />
Benefits<br />
• Integrated process control through Porpoise<br />
measurement technology<br />
• Improvement of process efficiency<br />
• Improvement of quality at source – All product<br />
made to recipe<br />
• Improvement of quality selection facility<br />
• Measurements certified to ISO 1133 or ASTM<br />
D1283 standards<br />
• High availability, high reliability<br />
• Low maintenance budget, low time to repair<br />
• Third party certification of product via SGS<br />
• Elimination of customer complaints<br />
• Fast return of investment<br />
• Perfect for all polymer processes<br />
86 www.rheologysolutions.com
The OP5 Online<br />
Rheometer<br />
continued from page 86<br />
do require regular verification, which is supplied<br />
through the OP5 operating software. The IPR of<br />
the operations are described in the EU CTM,<br />
Registration Certificate No 002729309. The<br />
methodology of calibration and measurement<br />
gives the OP5 class leading accuracy, which can<br />
be used to certify the finished product and thus<br />
completely replace routine testing using the Lab<br />
Melt Indexers. It is normal to certify these<br />
calibrations through a third party specialist. SGS,<br />
who are respected globally for such duties, have<br />
contract approval with major polymer producers<br />
for such onerous tasks.<br />
The OP5 measurement of Melt Index is performed<br />
in a batch process, termed a cycle. The MI result<br />
is based on a tiny part of the sample, which gives<br />
the OP5 a pin point accuracy. The result shows<br />
every small variation in the polymer product and<br />
which can be used to steer polymer reactions in a<br />
way not possible by long term averaging or less<br />
than adequate sample preparation. The MI result<br />
can of course be used for Quality Control but the<br />
finely resolved and accurate measurements will<br />
bring a better precision and thus maximise the<br />
added value of the production.<br />
Typically the OP5 samples every 5 minutes to fit in<br />
with the cleaning – measurement-sequence. The<br />
delay of measurement is slightly greater than cycle<br />
time of the sequence. Although the cycle has been<br />
optimised for accuracy but by using the necessary<br />
cleaning part of the cycle, the delay is made nearly<br />
independent of sample MI value. The real time<br />
delay (7-15mins) between the reaction and the<br />
measurement, which includes any sampling and<br />
sample preparation delay, is comfortably below<br />
process requirements whether it is used for<br />
reaction control and QC. In fact provided the delay<br />
is adequate, process control and QC places a very<br />
strong requirement on full-time calibration and<br />
best accuracy.<br />
The unique features of the OP5 equipment open<br />
up the huge opportunity of process control through<br />
rheology.<br />
info@rheologysolutions.com<br />
• new product<br />
HAAKE RheoStress 6000 –<br />
The Universal Rheometer<br />
all industries<br />
The HAAKE RheoStress 6000<br />
is the new generation of the<br />
Thermo Scientific HAAKE<br />
RheoStress series that is<br />
focused on standard<br />
application in R&D and QC.<br />
The HAAKE RheoStress 6000 is fully compatible<br />
with existing accessories of previous RheoStress<br />
models including temperature control units,<br />
measuring geometries and application oriented<br />
measuring cells.<br />
A variety of temperature control units is available<br />
to reliability and accurately handle temperatures<br />
ranging from -80ºC up to 500ºC<br />
A variety of temperature control units is available<br />
to reliability and accurately handle temperatures<br />
ranging from -80ºC up to 500ºC<br />
Peltier, electrical or liquid temperature control unit<br />
for coaxial cylinders, plate/plate and cone/plate as<br />
well as special measuring geometries.<br />
A number of application oriented accessories are<br />
available:<br />
• Pressure cell for use in crude all, drilling<br />
fluids, food<br />
• UV cell for use in coatings, dental material,<br />
contact lenses<br />
• Measuring cell for construction materials for<br />
use with cementitious pastes and mortars and<br />
samples with large particles<br />
• Double cone geometry for use with low<br />
viscous material where a small quantity is only<br />
available or where there is a tendency of<br />
evaporation<br />
• Disposal measuring geometries for samples<br />
which are difficult to remove such as<br />
cross-linking and curing material<br />
• Universal holder for individual containers for<br />
paints, inks and food<br />
• 3 point bending tool for food<br />
The HAAKE RheoStress 6000 offers:<br />
• CR (controlled rate) mode: Optimised speed<br />
control loop and a low motor inertia (I=10<br />
_Nms2) for fast speed steps within few<br />
milliseconds without significant overshoot<br />
• CS (controlled stress) mode: Advanced<br />
patented air-bearing technology plus accurate<br />
torque correction (MSC = Micro Stress<br />
Control) for measurements at low torque limit<br />
• CD (controlled deformation) mode: Self-<br />
learning deformation control loop based on<br />
neural network technology for fast parameter<br />
adaptations<br />
• Combinations of measuring modes: Flexible<br />
software and firmware for creative job<br />
definitions<br />
• Normal force measurements: Robust and very<br />
sensitive normal force sensor based on<br />
extremely sensitive and robust strain gauges<br />
for measurements between – 50 N and<br />
+ 50 N<br />
biennial 07-08<br />
87
HAAKE<br />
RheoStress<br />
6000<br />
Optional display/control<br />
unit. Monitoring data<br />
online even without a PC.<br />
The display/control unit of the<br />
HAAKE RheoStress 6000<br />
facilitates manual operation of lift<br />
movement and gap setting as<br />
well as starting measuring and<br />
evaluation jobs with or without<br />
PC. The colour display monitors<br />
rheological and instrument-<br />
specifi c data online.<br />
Glass plate with high<br />
resistance against chemicals<br />
for easy cleaning<br />
* DE 10 2004 050 753 A1; US 7,181,956 B2<br />
Thermo Scientific HAAKE RheoStress 6000 Specifications<br />
Min. torque rotation CS 200 nNm<br />
Min. torque rotation CR 200 nNm<br />
Min. torque oscillation CS 200 nNm<br />
Min. torque oscillation CD 200 nNm<br />
Max. torque 200 mNm<br />
Torque resolution 0.5(a) nNm<br />
Motor inertia 10 μNms2 Angular resolution 12(b) nrad<br />
biennial 07-08<br />
Min. angular velocity CS 10 -7 min -1<br />
Min. angular velocity CR 10 -5 min -1<br />
Max. angular velocity 1500, 4500(c) min -1<br />
Min. oscillation frequence 10-5 Hz<br />
Max. oscillation frequence 100 Hz<br />
Min. Normal force 0.01 N<br />
Max. Normal force 50(d)N<br />
Fixed measuring head<br />
consisting of:<br />
• Drag cup motor with the<br />
lowest available inertia<br />
(10μNms 2 )<br />
• High resolution optical<br />
encoder (12 nrad)<br />
• Patented 4th generation air<br />
bearing system*<br />
• Temperature compensated<br />
normal force sensor based<br />
on strain-gauge technology<br />
for positive and negative<br />
normal force measurements<br />
Adapter for upper<br />
measuring geometries<br />
Recepient of temperature<br />
control units and application<br />
oriented measuring cells<br />
Compact design by one<br />
column aluminum frame<br />
with integrated control<br />
and power electronics<br />
Normal force resolution 0.001 N<br />
Min. lift speed 0.2 μm/s<br />
Max. lift speed 7 mm/s<br />
Lift positioning accuracy 0.5 μm<br />
Temperature range -80 to +500(e) °C<br />
Dimensions (W x D x H) 400 x 400 x 780 mm<br />
Weight 42 kg<br />
(a) at the lowest torque (b) internal resolution (c) high shear option<br />
(d) in both positive and negative direction (e) depending on temperature control unit<br />
88 www.rheologysolutions.com
• new product brochures<br />
HAAKE Viscometers<br />
all industries<br />
Basic principles in rheology,<br />
selecting a viscometer<br />
Viscometry<br />
Measuring instruments for the determination of<br />
the flow behaviour of fluids are called viscometers.<br />
Viscosity is a material property which is dependent<br />
on different parameters such as mechanical stress<br />
and strain, time as well as temperature and other<br />
ambient conditions.<br />
Flow behaviour<br />
In rheology we differentiate between so-called<br />
Newtonian and non- Newtonian materials.<br />
Newtonian materials are characterized by a<br />
viscosity which may depend on temperature but is<br />
independent of the shear rate (and shear stress).<br />
In contrast, the viscosity of non- Newtonian<br />
materials depends on the shear rate. For most<br />
non- Newtonian materials the viscosity decreases<br />
with increasing shear rate. This behaviour is called<br />
shear thinning, or pseudoplastic. A material which<br />
viscosity increases at increasing shear rates is<br />
called shear-thickening or dilatant.<br />
Materials that do not flow until the applied shear<br />
stress surpasses a certain value are said to have<br />
a yield-stress.<br />
Rotational viscometers<br />
Using a rotational viscometer, the viscosity is<br />
calculated from the measured torque and<br />
rotational speed as well as the dimensions of the<br />
measuring geometry. If the measuring geometry<br />
fulfils certain requirements (e.g. small gap), which<br />
is the case for coaxial cylinder, plate/plate and<br />
cone/plate measuring geometries (DIN 53018, DIN<br />
53019...), the absolute value of the viscosity can<br />
be calculated.<br />
If the dimensions of the measuring geometry are<br />
not well defined, only a relative value for the<br />
viscosity can be determined. In this case, the<br />
measured viscosity value not only depends on the<br />
ambient conditions, but also on the test method,<br />
i.e. the measuring geometry.<br />
Falling ball viscometers<br />
The falling ball viscometer is a conventional and<br />
highly accurate instrument for the determination of<br />
the absolute value of the viscosity of a Newtonian<br />
material. The viscosity can be calculated from the<br />
falling time of the ball, the density of the ball as<br />
well as the diameter of the tube and the ball.<br />
Shear Rate<br />
The brochure provides full product specifications, accessories and measuring sensor systems available.<br />
A full copy of the Viscometer brochure is available on request.<br />
info@rheologysolutions.com<br />
Overview of HAAKE<br />
Viscometers<br />
Model HAAKE Viscotester<br />
1 plus & 2 plus<br />
Measurement Relative<br />
Standards -<br />
Viscosity Viscometer 1 plus: low<br />
Viscotester 2 plus: medium<br />
Model HAAKE Viscotester<br />
6 plus & 7 plus<br />
Measurement Relative<br />
Standards ISO 2555<br />
Viscosity L – Version: Low to medium<br />
R – Version: medium to high<br />
Model HAAKE Falling Ball<br />
Viscometer type C<br />
Measurement Absolute*<br />
Standards Din 53015, ISO 12058<br />
Viscosity Low to high<br />
Model HAAKE Viscotester VT550<br />
Measurement Absolute**<br />
Standards DIN 53018 / 53019,<br />
ISO 3219<br />
Viscosity Low to high<br />
*For Newtonian substances<br />
**Using absolute measuring geometries<br />
biennial 07-08<br />
89
• new product brochures<br />
HAAKE PolyLab OS<br />
- Open System<br />
polymer industries<br />
Measuring Mixer and Extruder<br />
System from Thermo Scientific<br />
The HAAKE PolyLab OS provides process relevant<br />
material data including:<br />
• Melting behaviour<br />
• Influence of additives<br />
• Shear stability<br />
• Temperature stability<br />
• Melt viscosity<br />
The torque rheometer supports process modelling<br />
activities such as:<br />
• Compounding polymers with additives to<br />
reduce flammability, viscosity, etc.<br />
• Scale-up extrusion processes by using<br />
different L/D ratios to extrapolate to your<br />
master process line.<br />
• Simulating master processes using only as<br />
little as 50 g of material to optimise extrusion<br />
or mixing in respect to temperature and shear<br />
profile<br />
• Extrusion of strands, profiles or films in<br />
combination with rheological or optical<br />
measurements<br />
HAAKE POLYLAB OS-SYSTEM<br />
Controller<br />
PC / Software<br />
biennial 07-08<br />
Mixer<br />
Single-Screw<br />
Extruder<br />
This allows you to optimise your process<br />
parameters, create test specimens or perform<br />
quality control on incoming and outgoing goods for<br />
viscosity, dispersion or plasticising behaviour.<br />
The brochure provides full product specifications,<br />
accessories and measuring sensor systems<br />
available. A full copy of the HAAKE PolyLab OS<br />
brochure is available on request.<br />
Twin-Screw<br />
Extruder<br />
Additional Analyzing<br />
Sensors<br />
Feeding<br />
Rotors<br />
Systems<br />
Screws Dies Postex<br />
HAAKE PolyLab OS<br />
– Measuring Mixer<br />
Typical Investigations<br />
• Testing the melting and degradation<br />
behavior of polymer melts<br />
• Quantifying viscosity when adding<br />
nano-particles or other additives<br />
• Testing the gelation- and plasticizing behavior<br />
of PVC dry-blends<br />
• Measuring the fl ow- and curing behavior of<br />
thermosetting plastics<br />
• Characterizing the infl uences of different<br />
additives such as carbon black, fi llers,<br />
lubricants, accelerators or sulphur for rubber<br />
mixtures<br />
• Recording the masticating and vulcanizing<br />
behavior of elastomers<br />
• Measuring the oil absorption of carbon black<br />
• Quantifying the absorption of DOP for PVC<br />
dry-blends<br />
• Measuring the stable torque in regard to<br />
individual and combined infl uences of fi llers<br />
and additives such as stabilizers, lubricants<br />
and color pigments<br />
• Testing high performance plastics to check<br />
processability<br />
• Performing electric conductivity<br />
measurements for rubber mixtures<br />
90 www.rheologysolutions.com
• product news & industry applications<br />
New device for rheological measurements -<br />
A measuring cell for special mortars<br />
Reproduced with the permission of BFT International – Concrete Plant & Forecast<br />
Technology (P 552, 01/08). www.bft-online.info<br />
construction &<br />
building industries<br />
Both quality and quantity of<br />
rheological tests are mainly<br />
determined by the available<br />
range of measuring cells.<br />
In this field, unmet needs exist<br />
especially with respect to<br />
building materials testing.<br />
This article describes one of<br />
these cells that are suitable<br />
for highly flowable mortars.<br />
This so-called basket cell<br />
enables fluid-in-fluid shear,<br />
and thus suppresses wall<br />
shear effects. The basket cell<br />
has been designed as a double<br />
annular gap cell ensuring high<br />
performance at low yield<br />
stresses.<br />
Working principle<br />
Under the assumption that solids of revolution can<br />
be used to create an appropriate shear area (see<br />
DIN 53018 or 53019), it must be observed, as a<br />
restrictive condition, that aqueous fluid may<br />
segregate at the interfaces when subjected to<br />
compression and/or shear. From a processing<br />
point of view, this is often a useful characteristic of<br />
mortars. However, this behavior results in the<br />
well-documented wall shear in the measuring cells<br />
referred to above, and thus leads to a distortion of<br />
measurement results. This effect may be limited<br />
by providing the measuring cells with a special<br />
surface texture, such as a ribbed pattern. Another<br />
possible solution could be to replace the adhesive<br />
fluid-wall bond with a cohesive bond. When<br />
pursuing this idea further, at least the critical cell<br />
walls would have to be replaced with fluid walls.<br />
Following a large number of various experiments<br />
to create such cell walls, i.e. a “fluid-in-fluid<br />
shear” using external fields of force and the<br />
correspondingly high effort, the experience gained<br />
has been used to identify an easy-to-implement<br />
compromise solution. The setup comes very close<br />
info@rheologysolutions.com<br />
to fluid-in-fluid shear if the intended fluid wall is<br />
established by means of a filigree framework. If a<br />
cylindrical framework is chosen – which would<br />
inevitably create an inner and outer fluid wall leaf,<br />
it would appear logical to also look for a solution<br />
similar to a double annular gap cell.<br />
Measuring cell design<br />
The double annular gap geometry is a favorable<br />
design not only on the basis of the considerations<br />
outlined above. It is also a suitable option because<br />
of the anticipated low limit yield stresses that<br />
result from the stability criterion [1] for<br />
self-compacting mortars (SCM).<br />
Mitnehmer-Nut<br />
D 1<br />
D 4<br />
‹berlauf-Tasse<br />
Co-axial double gap measuring cells are not a new<br />
invention. For example, DIN 54453 recommends<br />
the use of such a cell to determine the dynamic<br />
viscosity of anaerobic adhesives. While the cell's<br />
basic design is retained, its inner cylinder forming<br />
the double gap is replaced with the framework<br />
referred to above. As a result, the new measuring<br />
cell consists of an annular gap vessel – as shown<br />
in Fig. 1 – and the basket-like framework forming<br />
the sensor (Fig. 2). The framework is enclosed by<br />
a disc-shaped keyseat at the top and stiffened by<br />
an annular insert at the bottom. Following the infill<br />
of mortar into the annular gap vessel, the sensor<br />
will be moved coaxially, at low speed, to its<br />
measurement position. The fluid displaced during<br />
immersion can run off through the leveling<br />
openings of the sensor to fill the overflow<br />
receptacle of the annular gap vessel. The effective<br />
shear height L is determined by the immersion<br />
depth of the basket into the “fluid bath” in the<br />
annular gap space.<br />
This cell setup has been subjected to numerous<br />
tests, in particular with respect to determining<br />
relative gap widths and framework designs. In<br />
order to ensure a sufficiently stable bottom flow in<br />
the gap against the impact of inertial forces, an<br />
instrument drive similar to the Hatschek device<br />
was used.<br />
Above Left: (Fig.1) Section of the fluid-filled annular gap vessel of the measuring cell.<br />
Above Right: (Fig. 2) Photo of the measuring cell sensor (1) Coupling adapter (2) Mesh lining<br />
(3) Openings for fluid leveling<br />
L<br />
On this basis, diamond-shaped framework mesh<br />
structures were found to be particularly<br />
well-suited. These also allow for particle<br />
incorporation while ensuring a strong bond<br />
between the inner and outer fluid interface of the<br />
mortar attached on both sides.<br />
D 3<br />
For mortars with a maximum particle size (mesh<br />
aperture) of 2 mm and a permissible oversize of<br />
up to 2.5 mm, tests involving various wall<br />
distances in the range 32≤ (4Δ ≈ D4 - D1) ≤8dK,max<br />
demonstrated extreme measuring fluctuations, up<br />
to a total standstill of the cell, only at the lowest<br />
distances. This effect was caused by a more or<br />
continued on page 92<br />
biennial 07-08<br />
91<br />
1<br />
2<br />
3<br />
L
New service<br />
for rheological<br />
measurements<br />
continued from page 91<br />
less significant wedging of the natural particles<br />
used. The wall distance ultimately chosen to<br />
determine the main dimensions equals<br />
Δ ≈ 3dK,max, and is usable only in conjunction with<br />
the framework design shown in Fig. 2.<br />
Further design features were determined on the<br />
basis of a rather pragmatic approach. These<br />
include the position and design of the overflow<br />
receptacle and the minimization of the total weight<br />
of the annular gap vessel. These features also<br />
include the sensor immersion depth, which was<br />
determined at T [mNm] =τ [Pa] on a preliminary<br />
basis to enable a quick overview in the course<br />
of individual measurements.<br />
Prior to its use, the measuring cell must be<br />
calibrated. It is always advisable to calibrate the<br />
cell together with the other instruments available.<br />
Findings and outlook<br />
According to the experimental results obtained to<br />
date, the basket cell is suitable for all highly<br />
flowable fluids that are characterised by several<br />
phases, such as self-compacting mortars, grouting<br />
mortars, float finishes and fillers, as well as<br />
cementitious binder glues, ceramic slips, slurries<br />
of all types, and paints. <strong>Solutions</strong> can also be<br />
subjected to testing. As a prerequisite to any<br />
rheological materials testing, the object to be<br />
tested must be stable. This is also required for the<br />
setup described in this article.<br />
The experience gained in the course of<br />
development, testing and application enables<br />
continuous improvement of the basket cell<br />
depending on the specific requirements.<br />
This includes both the main dimensions of the<br />
measuring cell determined by varying maximum<br />
particle sizes and the adjustment of the framework<br />
structure to special modes of application.<br />
Prof. Dr.-Ing. habil. Ruprecht Vogel<br />
Malerstieg 6<br />
99425 Weimar / Germany<br />
r.vogel@vogel-labor.de<br />
References and<br />
further information<br />
[1] Vogel, R. Ein Stabilitätskriterium für Selbstverdichtenden<br />
Beton, BFT Betonwerk+Fertigteil-Technik 12 (2005), S.42<br />
bis 49 .<br />
[2] Vogel, R.; Riedel, M. Untersuchungen mit dem<br />
Rotationsviskosimeter RHEOTEST 2 zur Abgrenzung des<br />
Einsatzbereiches ,Silikattechnik 41 (1990), Heft 2,<br />
S.59...64<br />
[3] Vogel, R. Stabilität und Fließverhalten von Selbstverdichtendem<br />
Beton, Vortrag Ibausil Weimar Sept. 2006, Druck Bd.2,<br />
S.1047...1058<br />
[4] Vogel, R. Fließen von Selbstverdichtenden Beton – Das<br />
Fließgesetz; www.vogel-labor.de (Mitteilung 04/6)<br />
biennial 07-08<br />
• product highlight – industry application<br />
The industry choice for<br />
viscosity measurements<br />
of mineral slurries &<br />
suspensions<br />
mining industries<br />
The Thermo Scientific HAAKE<br />
Viscotester model VT550<br />
viscometer is suitable for<br />
viscosity measurements of<br />
particular suspensions using<br />
standard sensors to provide<br />
relative or absolute results<br />
which are highly reproducible.<br />
The HAAKE VT550 viscometer:<br />
• Provides the data to allow accurate<br />
calculations for pumping slurries and<br />
suspensions<br />
• Can be operated manually by the key pad<br />
or PC controlled<br />
• Measures yield points using Controlled<br />
Deformation (CD) mode<br />
• Measures inhomogeneous materials with<br />
particles in mm size<br />
• Records flow curves automatically to monitor<br />
the flow behaviour of a liquid or paste<br />
• Has interchangeable rotors to extend the<br />
measuring range and application<br />
• Can be upgraded to a coaxial- or cone and<br />
plate viscometer.<br />
The HAAKE VT550 provides results on viscosity<br />
and yield point which allows you to:<br />
• Correctly size pumps<br />
• Minimise wear in pipes & fittings<br />
• Identify start-up energy requirements for<br />
pumping<br />
• Predict the longevity of hydraulic transport<br />
equipment<br />
• Design better disposal systems<br />
HAAKE ViscoTester VT550<br />
92 www.rheologysolutions.com
• rheotalk special issue<br />
Food Industry feature<br />
food industries<br />
<strong>Rheology</strong> <strong>Solutions</strong> offer<br />
material characterisation<br />
solutions to measure, monitor<br />
and provide reproducible data<br />
for quality control, development<br />
and production applications<br />
that will improve performance<br />
within the food industries.<br />
Services<br />
An extensive range of technical articles have been<br />
produced specific to the challenges found within<br />
the food industry, these include:<br />
• Food and Beverage Material Characterisation<br />
- Introduction to the influences of rheological<br />
and process parameters. Rheo 025TP<br />
• Comparison of Rheological Techniques for<br />
the Characterisation of Semi-Solid Foods.<br />
(Rheo 027TP)<br />
info@rheologysolutions.com<br />
• Application of Liquid and Solid Rheological<br />
Technologies to the Textural Characterisation<br />
of Semi-Solid Foods. (Rheo049)<br />
• QC Measurements for Liquid Food Products<br />
and Packaging. (Rheo051)<br />
• Tim's Top Tips - Explanation & Evaluation<br />
of Mouthfeel. (Rheo253)<br />
• Tim's Top Tips - Explanation & Evaluation<br />
of Shelf Life. (Rheo254)<br />
• Tim's Top Tips - Explanation & Evaluation<br />
of Processability. (Rheo255)<br />
• Tim's Top Tips - Explanation & Evaluation<br />
of Cohesiveness, Cohesion Strength and<br />
Cohesive Quality. (Rheo256)<br />
• Tim’s Top Tips – How to Measure Flow<br />
& Viscosity. (Rheo358)<br />
• Tim’s Top Tips – How to Measure Thixotropy.<br />
(Rheo360)<br />
• Tim’s Top Tips – How to Measure Yield Stress.<br />
(Rheo362)<br />
Additionally, an information kit – <strong>Rheology</strong><br />
<strong>Solutions</strong> for the Food Industry is available. Copies<br />
of the technical papers and the solutions kit are<br />
available on request from <strong>Rheology</strong> <strong>Solutions</strong>.<br />
special issue<br />
Products<br />
Rheological parameters are reliable pointers for<br />
food performance and are critical factors for<br />
processability and product quality.<br />
Measuring these parameters will improve process<br />
and product performance within the food<br />
industries.<br />
There are a range of instruments and measurements<br />
that can be used to quantify rheology<br />
related challenges (processes or consumption)<br />
some of which may be described by the following<br />
terms:<br />
• adhesion • build<br />
• cohesion • cover<br />
• crispiness • elasticity<br />
• mouthfeel • spread<br />
• stringiness • viscosity<br />
• and many more<br />
<strong>Rheology</strong> <strong>Solutions</strong> will be exhibiting at Foopro<br />
(stand no. 6084) in Sydney in July 2008, and<br />
following is an overview of the products and<br />
services that will be available at the stand and<br />
fully operational during the exhibition.<br />
biennial 07-08<br />
93
• product focus<br />
Process Viscometer<br />
The Marimex range of<br />
ViscoScope process<br />
viscometers measures the<br />
viscosity of liquids continually<br />
and precisely in-line.<br />
The ViscoScope provides continuous measurements<br />
during food processing to ensure<br />
manufacturing is always monitored and<br />
adjustments are able to be made to keep the<br />
product within its viscosity specification range,<br />
eliminating waste and out of specification<br />
products.<br />
The Marimex range of ViscoScope systems<br />
provide maintenance free viscosity<br />
measurement for in-line applications within<br />
the food industry. Installations in the food<br />
industry currently include: Chocolate, Dairy,<br />
Gelatin, Pectin, Pipeline monitoring, Slurries,<br />
Spray dryers and the Sugar industry.<br />
Features include:<br />
• Smooth rugged sensor<br />
• Virtually no moving parts<br />
• High precision, no operator required<br />
biennial 07-08<br />
food industries<br />
• Factory calibrated with NIST traceable oils –<br />
in house calibration not required<br />
• Flexible mounting – works in any direction<br />
• High temperature capability to 450°C<br />
• High pressure capability to 5,000 Psig/350 bar<br />
• Flow rate fluctuations do not have any<br />
influence on accuracy of data<br />
• LAN diagnostic systems control<br />
The Thermo Scientific HAAKE<br />
Viscotester series provide<br />
accurate viscosity results for<br />
QA/QC in the laboratory ensuring<br />
quality control throughout<br />
the manufacturing process.<br />
The HAAKE Viscotester 6L plus is a classic<br />
rotational viscometer for QA/QC applications and<br />
provides fast determination of viscosity as defined<br />
in ISO 2555 and many ASTM standards.<br />
The Viscotester VT6L plus is one in the range of<br />
HAAKE viscometers suitable for viscosity testing<br />
applications within the food industry.<br />
ViscoScope viscometers manufactured by<br />
Marimex Industries (Germany) are available for<br />
process applications up to 450ºC and 350 bar.<br />
The sensor has torsional oscillation rotation<br />
and is constructed without any moving parts<br />
avoiding any cross contamination with the<br />
material being measured.<br />
The sensor can be mounted in any orientation in<br />
reactors, vessels and pipes for measuring in batch<br />
and continuous processes.<br />
All measurements are precise, reliable and<br />
reproducible making the ViscoScope ideal for all<br />
applications within the food industry.<br />
Marimex ViscoScope in-line measurement system<br />
provides continuous viscosity results and has been designed<br />
for maintenance free operation in process applications<br />
• product focus<br />
Rotational Viscometer<br />
food industries<br />
Model Viscotester 6L plus<br />
Viscosity range 3 – 6,000,000 mPas<br />
Accuracy +/- 1% full scale<br />
Reproducibility +/- 0.2%<br />
Standards ISO 2555 (+ others)<br />
ASTM 115, 789, 1076<br />
Features<br />
• RS232 interface for data transfer to a PC<br />
for evaluation<br />
• Digital display with viscosity, torque, speed<br />
and spindle readout<br />
• Supplied complete with spindles, stand<br />
& carry case<br />
Options<br />
• Model VT6R plus which differs in the torque<br />
by a factor of 6, i.e.: 20 - 40 000 000 mPas<br />
The VT6L plus offers great value for money, high accuracy,<br />
ease of use, good design and software options<br />
94 www.rheologysolutions.com
• product focus<br />
Extensional Rheometer<br />
food industries<br />
The Thermo Scientific HAAKE<br />
CaBER 1 is a Capillary Breakup<br />
Extensional Rheometer which<br />
measures the extensional<br />
properties of samples to<br />
optimise filling and spatter<br />
behaviour during filling<br />
processes.<br />
Knowledge of the elongational behaviour of fluids<br />
is important for both industrial and basic research<br />
purposes. Complex flows that contain strong<br />
extensional components occur in many industrial<br />
processes and applications. Some examples are<br />
extrusion flows, coating flows, contraction flows<br />
and fibre spinning flows. Most materials exhibit<br />
very different responses in an extensional flow<br />
compared to a shearing flow. The thinning and<br />
breakup of a fluid filament that is analysed with<br />
the HAAKE CaBER 1 instrument provides valuable<br />
information about the materials physical properties<br />
that rotational rheometers simply can not provide.<br />
Model CaBER 1<br />
Hencky Strains: up to 0 = 10<br />
Strain Rate Range: Imposed strain rate<br />
0.01 < 0 < 300 s-1 Fluid strain rate<br />
10-5< 0 < 10 S-1 Shear Viscosity Range: 10 - 106 mPas<br />
Plate Diameter: 4 < Dplate < 8 mm,<br />
standard = 6mm<br />
Temperature Range: 0 - 80ºC<br />
Diameter Resolution: 8 μm<br />
System Response Time: 10 ms<br />
Features<br />
• Computer controlled<br />
• Class 1 laser micrometer<br />
• Easy to operate and easy to load samples<br />
and clean<br />
• Linear motor drive with variable speed<br />
• Closed temperature-controlled sample<br />
chamber<br />
• Automatic repeated testing<br />
• Exchangeable geometries<br />
• User defined strains<br />
• Sample volume
• product focus<br />
Heating Bath Circulator<br />
food industries<br />
Thermo Fisher HeatTech 26L<br />
heating bath circulator operates<br />
from ambient to +100ºC.<br />
It is a reliable and economical unit that provides<br />
flexibility to laboratories as either a fluid bath or<br />
circulator.<br />
Features<br />
• Large bath area accommodates more<br />
samples<br />
• Quiet system<br />
• Powerful pump accommodates the bath plus<br />
connections to external applications<br />
• Safety level for fluid and temperature<br />
• Front access drain for easy cleaning<br />
• product focus<br />
Refrigerated Bath Circulator<br />
food industries<br />
Thermo Fisher CoolTech 320<br />
refrigerator bath and circulator<br />
operates at -28ºC to +100ºC.<br />
A versatile and economical<br />
option for laboratory cooling.<br />
Features<br />
• Rapid cool down and heat up times<br />
• Powerful pump accommodates the bath plus<br />
connections to external applications<br />
• CFC-free refrigerant system<br />
• Safety level for fluid and temperature<br />
• Front access drain for easy cleaning<br />
Model HeatTech 26L<br />
Temperature Range Ambient to +100ºC<br />
Temperature Accuracy +/- 0.02ºC<br />
Heater Capacity (230V) 2.0 kW<br />
Pump Pressure (max) 300 mbar<br />
Pump Flow Rate (max) 12.5 lpm<br />
Bath Volume 26 L<br />
Order Today -<br />
delivery ex stock<br />
$2,399<br />
excluding GST and local delivery<br />
Model CoolTech 320<br />
Temperature Range -28ºC to +100ºC<br />
Temperature Accuracy +/- 0.02ºC<br />
Heater Capacity 2.0 kW<br />
Cooling Capacity @ 20ºC 320W<br />
Pump Pressure (max) 300 mbar<br />
Pump Flow Rate (max) 12.5 lpm<br />
Bath Volume 4.5 L<br />
Order Today - delivery ex stock<br />
$3,999<br />
excluding GST and local delivery<br />
A versatile and economical option for laboratory cooling<br />
A reliable and economical unit that provides flexibility to laboratories as either a fluid bath or circulator<br />
biennial 07-08<br />
96 www.rheologysolutions.com
• new product brochure<br />
Food industry<br />
feature &<br />
product focus<br />
food industries<br />
<strong>Rheology</strong> <strong>Solutions</strong> offer material characterisation<br />
solutions to measure, monitor and provide<br />
reproducible data for quality control, development<br />
and product applications that will improve<br />
performance with the food industries.<br />
A four page overview of products and services<br />
specifically available for food industry applications<br />
has been produced.<br />
• new product brochure<br />
Bath<br />
recirculators<br />
all industries<br />
The Thermo Scientific NESLAB RTE and EX Series<br />
of bath circulators brochure have been updated to<br />
incorporate more product and technical information.<br />
The NESLAB RTE Series of bath circulators cool<br />
and heat from -25ºC to +200ºC and the NESLAB<br />
EX Series of bath circulators heat from ambient to<br />
+200ºC.<br />
info@rheologysolutions.com<br />
• new product brochure<br />
Material<br />
characterisation<br />
for polymers<br />
No matter what stage of the polymer’s life cycle,<br />
eliminating waste and keeping production levels at<br />
peak capacity are crucial to ensuring profitability<br />
in today’s highly competitive environment.<br />
This brochure from Thermo Scientific provides a<br />
comprehensive overview of products to cover:<br />
• R&D of new polymers<br />
• Lab scale process, pilot plant and small<br />
scale production<br />
• Quality control<br />
• new product brochure<br />
Extrusion & material<br />
characterisation for drug<br />
development & production<br />
pharmaceutical, cosmetics<br />
& allied industries<br />
In material characterisation rheological properties<br />
are of the utmost importance for the determination<br />
of the best drug format. The ability to analyse and<br />
describe the material’s mechanical or formulation<br />
properties can have a direct impact on precise<br />
polymer industries<br />
dosing and optimisation of the manufacturing<br />
process.<br />
This brochure from Thermo Scientific provides a<br />
comprehensive overview of products to cover:<br />
• Extrusion technology<br />
• Material characterisation<br />
biennial 07-08<br />
97
• product news & industry applications<br />
Using Refrigerated Circulators with Rotary<br />
Evaporators – Environmentally Friendly Solution<br />
chemical & allied industries<br />
Rotary Evaporators are widely<br />
used in various R&D and QC<br />
laboratories and also in<br />
academia.<br />
The main use of rotary evaporators is solvent<br />
recovery from various mixtures by single step<br />
distillation and they are sometimes used for<br />
organic chemistry syntheses under controlled<br />
temperature and vacuum.<br />
The basis of this procedure is the evaporation and<br />
condensation of solvents using a rotary evaporating<br />
flask under vacuum. Distilling products under<br />
vacuum increases the performance and helps to<br />
protect the products. Condensers are cooled using<br />
tap water circulation or alternatively by cooling<br />
recirculators.<br />
To achieve optimal distillation conditions, the<br />
distillation energy supply by the heating bath must<br />
be removed by the condenser. To ensure this,<br />
operate the instrument according to the following<br />
rule of thumb:<br />
Cooling water: max. 20ºC<br />
Vapour: 40ºC<br />
Bath: 60ºC<br />
This rule can also be applied to lower bath<br />
temperatures, for example:<br />
Cooling water: max. 0ºC<br />
Vapour: 20ºC<br />
Bath: 40ºC<br />
This is achieved by:<br />
• Setting the bath temperature<br />
• Setting the cooling water temperature. When<br />
the cooling water is tap water, the temperature<br />
is sometimes (especially in summer)<br />
above 20ºC. With the Thermo Scientific EZ<br />
Cool 80 refrigerated recirculating bath<br />
connected to the system it is easy to set the<br />
cooling medium temperature to the desired<br />
value between -10ºC to +20ºC.<br />
• Allowing cooling tap water to flow through the<br />
condenser at approximately 40 – 50 l/h. With<br />
the EZ Cool 80, the recirculator flow is 720<br />
l/hr (without loosing the cooling medium),<br />
providing a better, stable and efficient heat<br />
transfer.<br />
biennial 07-08<br />
• Defining the operating vacuum in such a way<br />
that at the vacuum, the boiling point of the<br />
solvent equals the vapour temperature. Refer<br />
to the solvent tables provided in the rotary<br />
evaporator manual.<br />
Advantages associated with bath temperatures of<br />
60ºC and below:<br />
• The evaporating flask can be replaced without<br />
risk of burns<br />
• The evaporation rate of the water from the<br />
heating bath is low (low energy loss)<br />
• The heating bath energy is used at a good<br />
degree of efficiency<br />
Other Advantages using the EZ Cool 80:<br />
• Environmentally friendly working conditions<br />
since no waste of tap water at 40 – 50 l/h<br />
• Four pre-set temperatures enables the<br />
practical switch of solvents which evaporate<br />
at significantly different temperatures<br />
• Ability to distil solvents with boiling points<br />
under room temperature, provided that the<br />
receiving flask is also thermostated in a<br />
cooling bath<br />
• The spiral of the condenser is always clean<br />
Ono 426-1624<br />
$3,450<br />
excluding GST and local delivery<br />
Thermo Scientific EZ Cool 80, recommended for<br />
Rotary Evaporators –the environmentally friendly<br />
solutions<br />
Prepared by: Onur Cebeci, Chemist, Anamed &<br />
Analitik Group, Chemistry Technologies Department,<br />
Turkey. References were taken from the<br />
Rotavapor Operation manual, Buchi Labortechnik<br />
AG, Swtzerland.<br />
98 www.rheologysolutions.com
• product news & industry applications - product accessories<br />
Universal container holder for HAAKE MARS<br />
and RheoStress 6000<br />
all industries<br />
A universal holder for sample containers which<br />
can be used for the HAAKE MARS and the<br />
RheoStress 6000 (as well as all of its predecessors)<br />
has been developed. Thanks to the three<br />
individually adjustable clamps, sample containers<br />
like glass jars, cans, beakers, cups, etc., can be<br />
mounted solidly onto the rheometer. This allows for<br />
the insertion of a (vane) measuring geometry into<br />
the sample without comprising its structure.<br />
A copy of this brochure is available by requesting<br />
P018e<br />
The rotational viscometers HAAKE Viscotester 6 &<br />
7 plus are described in the standard ISO 2555. In<br />
comparison to the HAAKE Viscotester 6, the<br />
HAAKE Viscotester 7 is equipped with a temperature<br />
sensor and a serial interface. Both models are<br />
available in two versions: whereas the ‘’L’’-version<br />
is suitable for measurements on low and medium<br />
Fig. 1 (above): Universal container holder with<br />
three adjustable clamps (left),<br />
Fig. 2 (right): Universal clamp holder with a peanut<br />
butter glass jar mounted on the HAAKE MARS<br />
with a vane rotor FL22 (right)<br />
• product news & industry applications - product accessories<br />
Adapters for HAAKE Viscotester models 6<br />
and 7 plus for measuring range extension<br />
and sample temperature measurement (optional)<br />
all industries<br />
viscose samples (3 up to 6.000.000 mPas) the<br />
‘’R’’-version can be used for medium and higher<br />
viscose materials (20 up to 40.000.000 mPas).<br />
Using a low viscosity adapter (UL) the lower<br />
viscosity limit can be extended. Reproducible<br />
viscosity measurements can be performed down<br />
to 1.0 mPas using the L-version respectively 6.4m<br />
Pas for the R-version. It has to be taken into<br />
account that high rotational speeds are needed for<br />
measurements of very low viscosities and Taylor<br />
vortices cause hereby can have a negative<br />
influence on the experimental results.<br />
For samples, which are available in small amounts<br />
only, a small sample adapter can be used.<br />
Depending on the Viscotester version used<br />
different sets of cylindrical spindles are available<br />
which have to be ordered separately.<br />
A copy of this brochure is available by requesting<br />
P020-e<br />
• product news & industry applications - product accessories<br />
UV curing cell for an individual arrangement<br />
of optical components<br />
all industries<br />
In order to measure a given sample’s rheological<br />
properties before, during and after controlled<br />
exposure to UV radiation, a cylindrical UV curing<br />
cell has been developed for the HAAKE MARS,<br />
HAAKE RheoStress 6000 rheometers and the<br />
respective predecessor models.<br />
info@rheologysolutions.com<br />
The cylindrical UV curing cell has an outer<br />
diameter of 48 mm and fits into fluid or electrically<br />
controlled cylindrical temperature control units.<br />
Any UV light source can be connected via light<br />
guide (outer diameter 24.5 mm). The<br />
UV light source should be capable of providing<br />
different intensities in order to measure the<br />
dependence of the curing behaviour as a function<br />
of the light intensity applied. Moreover, the light<br />
source should be equipped with a timer, a manual<br />
control switch or a foot-operated switch as well as<br />
a trigger input facilitating control of the light<br />
source via the rheometer’s measuring software.<br />
A copy of this brochure is available by requesting<br />
P-022e<br />
biennial 07-08<br />
99
• product news & industry applications - product accessories<br />
Vane rotors for pressure cells for HAAKE MARS<br />
and HAAKE RheoStress 6000<br />
all industries<br />
Different vane rotors have been developed for<br />
pressure dependent measurements on samples<br />
containing particles. Each rotor consists of 4<br />
blades mounted around a shaft, which is equipped<br />
with two sapphire bearings.<br />
With these bearings the rotors can be precisely<br />
centred on two steel pins inside the pressure cell.<br />
The vane rotors differ in the size of the blades. The<br />
• SER – Extensional rheology system<br />
for HAAKE MARS<br />
all industries<br />
The SER system is a new accessory for the HAAKE<br />
MARS with CTC oven which transforms a<br />
(rotational) shear rheometer in an extensional<br />
rheometer for melts and semi-solids.<br />
The measuring principle of the SER system, which<br />
was developed by Dr. Martin Sentmanat (Xpansion<br />
Instruments), is based on clamping the sample on<br />
two counter rotating windup drums. With the SER<br />
system a truly uniform extensional deformation in<br />
the sample is achieved. In additional to the uniaxial<br />
extension, the SER tool can be used for solid<br />
tensile testing, pear and peel testing, as well as<br />
friction testing.<br />
biggest vane rotor FL 25/90 has a diameter of 25<br />
mm and a blade height of 90 mm. This rotor is<br />
particularly suitable for measurements on low<br />
viscous samples.<br />
For measurements on samples with higher<br />
viscosities vane rotors with a blade height of 8.8<br />
mm are recommended. For choosing the suitable<br />
rotor the diameters of the suspended particles<br />
have to be taken into account. As a rule of thumb<br />
the minimum width of the gap between the rotor<br />
blades and the inner wall of the pressure cell<br />
The operating temperature range of the SER tool<br />
covers 0ºC to +250ºC.<br />
The combination of convection and radiant heating<br />
in the CTC guarantees fast temperature changes<br />
and an even temperature distribution within the<br />
sample.<br />
The SER system is fully integrated in the HAAKE<br />
RheoWin measuring and evaluation software.<br />
Measurements can be made in both controlled<br />
extensional rate and controlled tensile stress<br />
mode. The extensional properties of the sample<br />
are calculated automatically and presented directly<br />
in the software.<br />
A copy of this brochure is available by requesting<br />
P-019e<br />
• Tribology cell for HAAKE Rheometers<br />
For the rheometers HAAKE MARS, RheoStress<br />
6000 and predecessor models identical in<br />
construction and equipped with a normal force<br />
sensor, a measuring cell has been developed for<br />
testing the tribological behaviour of bearing<br />
materials.<br />
The tribology cell described here consists of a<br />
lower and an upper part. Both are made of<br />
stainless steel. The lower measuring geometry is<br />
biennial 07-08<br />
all industries<br />
designed as a reservoir.<br />
Measurement of the friction of bearing materials<br />
with and without lubricant can be performed. To<br />
measure the influence of a lubricant the reservoir<br />
can be filled with the lubricant to be tested.<br />
The upper measuring geometry is equipped with<br />
a flexible shaft, which ensures the concentric<br />
position of a ball with a diameter of ½” in the<br />
measuring cell. Usually steel bearing balls are<br />
used but other materials like e.g. ceramic are<br />
also possible.<br />
should be 3 times larger than the biggest<br />
suspended particles.<br />
The inner diameter of the pressure cell D100/200<br />
is 40 mm. For example, using a FL36/8.8 vane<br />
rotor the measuring gap between the rotor and the<br />
inner side of the pressure cell is 2 mm. Therefore<br />
a suspension with particles with a maximum size<br />
of 0.6 mm can be measured. For bigger particles<br />
a rotor with a smaller diameter has to be selected.<br />
A copy of this brochure is available by requesting<br />
P-021e<br />
Fig. 1 (left): SER tool integrated in Controlled<br />
est Chamber<br />
Fig. 2 (right): Schematic setup of the SER tool<br />
Replacing the ball is easily and quickly done,<br />
to perform every test with a fresh ball as<br />
recommended. For temperature dependent tests<br />
between - 40°C and +200°C the lower measuring<br />
geometry can be adapted on a modified<br />
measuring plate cover for a Peltier temperature<br />
control unit. Also the measuring cell can be<br />
integrated into the Control Test Chamber by<br />
adapting the lower measuring geometry onto<br />
a suitable holder.<br />
A copy of this brochure is available by requesting<br />
P-023e<br />
100 www.rheologysolutions.com
• product news & industry applications<br />
Extended product range - recirculating chillers<br />
all industries<br />
Two models have been added to<br />
the Thermo Scientific NESLAB<br />
ThermoFlex range. The range now<br />
extends to 3500 W and 5000 W<br />
cooling capacity at 20ºC.<br />
The NESLAB ThermoFlex range is reliable, easy to<br />
use chiller and is suitable for diverse applications<br />
across all industry areas within QA/QC, R&D and<br />
production applications.<br />
The range offers 1400W, 2500W, 3500W and<br />
5000W of cooling capacity and is the ideal chiller<br />
for demanding cooling applications within the<br />
polymer industry.<br />
Options - Fluid Recirculation<br />
• Pressure Relief – Allows for regulation of the<br />
chiller’s outlet pressure and is available as an<br />
internal or external option.<br />
Thermo Scientific NESLAB ThermoFlex range<br />
• Flow Control with Flow Readout – Controls flow<br />
to the application and displays on the controller.<br />
• Pressure Relief with Flow Readout – Pressure<br />
relief valve allows for regulation of the chiller’s<br />
outlet pressure and displays on the controller.<br />
• Auto Refill – Allows for automatic refilling to<br />
Cooling Capacity for NESLAB ThermoFlex 900/1400/2500 Cooling Capacity for NESLAB ThermoFlex 3500/5000<br />
cooling capacity<br />
12000<br />
10000<br />
8000<br />
6000<br />
4000<br />
2000<br />
3500<br />
3000<br />
2500<br />
2000<br />
1500<br />
1000<br />
500<br />
2500 @ 60 Hz<br />
2500 @ 50 Hz<br />
1400 @ 60 Hz<br />
1400 @ 50 Hz<br />
900 @ 60 Hz<br />
900 @ 50 Hz<br />
BTU/Hr Watts<br />
°C<br />
10 20 30 40<br />
°F 40 50 60 70 80 90 100<br />
temperature setpoint<br />
cooling capacity<br />
24000<br />
20000<br />
16000<br />
12000<br />
7000<br />
6000<br />
5000<br />
4000<br />
3000<br />
8000<br />
2000<br />
4000 1000<br />
5000 @ 60 Hz<br />
5000 @ 50 Hz<br />
3500 @ 60 Hz<br />
BTU/Hr Watts<br />
3500 @ 50 Hz<br />
°C<br />
10 20 30 40<br />
°F 40 50 60 70 80 90 100<br />
temperature setpoint<br />
ensure the proper fluid level is maintained.<br />
• Anti Drainback – Prevents the reservoir from<br />
overflowing when a chiller is installed below<br />
the application.<br />
• DI Water – Maintains fluid resistivity and is<br />
available as an internal or external option.<br />
ThermoFlex 900 ThermoFlex 1400 ThermoFlex 2500 ThermoFlex 3500 ThermoFlex 5000<br />
Setpoint Temperature Range +5°C to +40°C +5°C to +40°C +5°C to +40°C +5°C to +40°C +5°C to +40°C<br />
Ambient Temperature Range +10°C to +40°C +10°C to +40°C +10°C to +40°C +10°C to +40°C +10°C to +40°C<br />
Temperature Stability ±0.1°C ±0.1°C ±0.1°C ±0.1°C ±0.1°C<br />
Setpoint Cooling Capacity 50 Hz at +20°C 750 W / 2561 BTU 1170 W / 3996 BTU 2200W / 7513 BTU 3050 W / 10416 BTU 4400 W / 15027 BTU<br />
Reservoir Volume 7.2 liters 7.2 liters 7.2 liters 7.2 liters 7.2 liters<br />
Physical Dimensions 69.4 x 36.0 x 62.4 cm 69.4 x 36.0 x 62.4 cm 74.1 x 43.8 x 67.6 cm 101.6 x 49.4 x 79.0 cm 101.6 x 49.4 x 79.0 cm<br />
P1 - Positive Displacement Pump 50 Hz 1.7 gpm @ 60 psid 1.7 gpm @ 60 psid 1.7 gpm @ 60 psid 1.7 gpm @ 60 psid -<br />
P2 - Positive Displacement Pump 50 Hz 3.3 gpm @ 60 psid 3.3 gpm @ 60 psid 3.3 gpm @ 60 psid 3.3 gpm @ 60 psid 3.3 gpm @ 60 psid<br />
P3 - Centrifugal Pump 50 Hz 10 gpm @ 20 psid 10 gpm @ 20 psid<br />
P4 - Centrifugal Pump 50 Hz - - - 15 gpm @ 34 psid 15 gpm @ 34 psid<br />
info@rheologysolutions.com<br />
biennial 07-08<br />
101
• rheotalk special issue<br />
Polymer Industry feature<br />
<strong>Rheology</strong> <strong>Solutions</strong> offer<br />
material characterisation<br />
solutions to measure, monitor<br />
and provide reproducible data<br />
for quality control, development<br />
and production applications<br />
that will improve performance<br />
within the polymer industries.<br />
Services<br />
An extensive range of technical articles have been<br />
produced specific to the challenges found within<br />
the polymer industry, these include:<br />
• Quality Control in the Polymer Industry.<br />
Introduction to cutting edge technologies and<br />
their application in the polymer industry.<br />
Rheo 023<br />
• <strong>Rheology</strong> for the Rubber and Elastomer<br />
Industries. Introduction to the influences of<br />
rheological and process parameters and<br />
methods for their measurement. Rheo 024<br />
• Tim’s Top Tips – Explanation and Evaluation<br />
of Compounding. Rheo 289<br />
biennial 07-08<br />
polymer industries<br />
• Tim’s Top Tips – Explanation and Evaluation<br />
of Processability. Rheo 290<br />
• Tim’s Top Tips – Explanation and Evaluation<br />
of Shark Skin. Rheo 291<br />
• Tim’s Top Tips – Explanation and Evaluation<br />
of Die Swell. Rheo 292<br />
• Tim’s Top Tips – How to Measure Flow<br />
and Viscosity Curves. Rheo 364<br />
• Tim’s Top Tips – How to Measure Thixotropy.<br />
Rheo 366<br />
• Tim’s Top Tips - How to Measure Yield Stress.<br />
Rheo 368<br />
Additionally, an information kit – <strong>Rheology</strong><br />
<strong>Solutions</strong> for the Polymer Industries is available.<br />
Copies of the technical papers and the solutions<br />
kits are available on request from <strong>Rheology</strong><br />
<strong>Solutions</strong>.<br />
Products<br />
Polymer processing includes unit operations such<br />
as compression, injection and blow moulding and<br />
extrusion through a variety of dies. Specifically for<br />
the polymer industries, materials characterisation<br />
is of critical importance (including fluid related<br />
issues like sedimentation, time related structural<br />
decay or build-up and post-cure issues like<br />
strength of compression or extension) for<br />
prediction and management of sharkskin, melt<br />
special issue<br />
fracture, calendering, die swell, melt homogeneity<br />
and short- and long-term dimensional stability of<br />
extrudates or moulded parts. These processes<br />
depend on fluid rheological parameters such as<br />
viscosity, viscoelasticity, creep and recovery, and<br />
solid material properties such as behaviour under<br />
various compressive and extensional loafing<br />
conditions. Extensional flow properties dominate<br />
processes where stranding occurs and influences<br />
time, quality and energy requirements.<br />
Material characterisation parameters are reliable<br />
pointers for polymer performance and are critical<br />
factors for processability and product quality.<br />
Measuring these parameters will improve process<br />
and product performance within the polymer<br />
industries.<br />
<strong>Rheology</strong> <strong>Solutions</strong> exclusively offers a range of<br />
instruments and equipment that can be used to<br />
quantify rheology related challenges specific for<br />
polymer applications.<br />
<strong>Rheology</strong> <strong>Solutions</strong> will be exhibiting at Ausplas<br />
2008 (stand no: 100) in Melbourne during October<br />
2008, and also at 30 APS (stand no: 13) in<br />
Melbourne during November 2008, and following<br />
is an overview of the products that will be<br />
available at the stand and operational.<br />
102 www.rheologysolutions.com
• product focus<br />
Modular Torque Rheometer<br />
with Measuring Mixer<br />
polymer industries<br />
The Thermo Scientific HAAKE<br />
PolyLab QC with Rheomix 600<br />
will be shown for the first time<br />
in Australia in October.<br />
The HAAKE PolyLab QC is a new modular torque<br />
rheometer which can be connected to an<br />
interchangeable measuring mixer, single screw<br />
extruder or conical twin-screw extruder.<br />
A typical mixer test is run at a defined rotor speed<br />
(shear rate). The material’s response to the shear<br />
is recorded as torque and displayed versus time.<br />
Although the temperature of the mixing<br />
chamber is constantly controlled, the material’s<br />
melt temperature during a test may rise due to<br />
the shear introduced. The recorded “Rheogram”<br />
(torque and melt temperature vs. time at constant<br />
speed) is characteristic for different material types<br />
and blends. It can be used as a fingerprint in<br />
quality control for outgoing and incoming product<br />
inspections. As changes in torque are related to<br />
HAAKE PolyLab with extruder shown as a bench<br />
model unit<br />
info@rheologysolutions.com<br />
structural changes in the material, a Rheogram<br />
can be used to investigate and verify reactions<br />
of different additive types or concentration on<br />
the samples melting behaviour.<br />
The HAAKE PolyLab QC Rheomix 600 is used to<br />
investigate:<br />
• The melting and degradation behaviour of<br />
polymers<br />
• Viscosity when adding nano particles or other<br />
additives<br />
• Gelation and plastification behaviour of PVC<br />
dry-blends<br />
• Flow and curing behaviour of thermosetting<br />
plastics<br />
• The influence of different additives such as<br />
carbon black, fillers, lubricants, accelerators<br />
and sulphur for rubber mixers<br />
• Masticating and vulcanising behaviour of<br />
elastomers<br />
• Oil adsorption of carbon black<br />
• Adsorption of DOP for PVC dry blends<br />
• Torque in regard to individual and combined<br />
influences of fillers and additives<br />
• Processability of plastics<br />
• Electric conductivity measurements for rubber<br />
mixers <br />
HAAKE PolyLab QC with Rheomix 600 Floor<br />
Model<br />
• product focus<br />
Modular Torque Rheometer<br />
with Twin-Screw Extruders<br />
polymer industries<br />
The Thermo Scientific HAAKE<br />
PolyLab QC with the HAAKE<br />
CTW 100 QC twin-screw<br />
extruder is used for continuous<br />
compounding and plasticising is<br />
the ideal extruder in the HAAKE<br />
PolyLab QC system.<br />
This is a counter rotating conical twin-screw<br />
compounder, with intermeshing screws, that will<br />
give well-defined residence time for faultless<br />
production of process-critical polymers.<br />
The gentle but intensive dispersing capabilities are<br />
ideal to mix additives and pigments. Dies and<br />
downstream ancillaries are compatible with the<br />
19/25 QC-D single-screw extruder.<br />
Applications<br />
• Testing of the plasticising behaviour<br />
• Testing the performance of additives and fillers<br />
• Measuring of the melt temperature and<br />
pressure along the barrel to optimise process<br />
parameters<br />
• Provide a homogeneous and constant flow melt<br />
• Production of strands, sheets, cast and blown<br />
films<br />
• Extrusion of ceramics and feed stock<br />
• Melt rheology<br />
Features<br />
• Rod dies & water bath for strand extrusion<br />
• Sheet & ribbon dies<br />
• Blown film dies & take off tower<br />
• Filter test<br />
The HAAKE PolyLab QC is available as a bench<br />
or floor model . <br />
biennial 07-08<br />
103
• product focus<br />
Modular Torque Rheometer<br />
with Single-Screw Extruder<br />
polymer industries<br />
The most common method in processing polymers<br />
are screw plastification and injection moulding,<br />
and The Thermo Scientific HAAKE PolyLab QC with<br />
• product focus<br />
Modular<br />
Twin-Screw<br />
Extruder<br />
polymer industries<br />
The PRISM EuroLab 16 mm<br />
operates with sample batches<br />
of 50 g up to outputs of<br />
10 kg/h., the bench mounted<br />
16 mm twin-screw extruder<br />
is the heart of a complete<br />
compounding and sample<br />
preparation system.<br />
The segmented screw configuration with modular<br />
barrel design give flexibility for the full range of<br />
polymer processes.<br />
A horizontally split barrel, up to 40:1 L/D, has a<br />
lift-off top half for easy access to the screws, and<br />
the screws themselves have a simple removal<br />
device for cleaning and configuration changes.<br />
Thermo “fuzzy logic” heater controls save energy.<br />
The segmented top barrel half is constructed in<br />
modules and is easy to reconfigure. Barrel<br />
segments are available for feeding solids and<br />
liquids or for venting. Secondary feeders and<br />
vacuum pumps can form part of the system.<br />
A rugged colour touch screen interface incorporates<br />
data acquisition as standard, with an option<br />
to download to a remote computer for archiving<br />
and analysis. The controls include recipe storage<br />
to programme set points for repeatable process<br />
conditions.<br />
During October in Melbourne at Ausplas, the<br />
PRISM EuroLab 16 mm system will be operational<br />
extruding and pelletising a range of plastic<br />
samples.<br />
biennial 07-08<br />
single-screw extruder is the ideal torque<br />
rheometer for this application.<br />
For testing quality and processability of those<br />
materials, the single-screw laboratory extruder<br />
19/25 QC-B is a proven tool.<br />
Specifications<br />
To shape a polymer for further processes and<br />
tests, different dies can be adapted to the<br />
extruder. Rod dies and water bath for strand<br />
extrusion, sheet and ribbon dies in various<br />
dimensions to produce bands or cast films, and<br />
blown film dies and take off tower complete the<br />
testing equipment.<br />
Thermo Fisher PRISM EuroLab 16mm<br />
Twin Screw Extruder<br />
Barrel Length L/D 25:1 25:1 40:1 40:1<br />
Barrel Bore Diameter mm 16 16 16 16<br />
Screw Diameter mm 15.6 15.6 15.6 16.6<br />
Channel Depth mm 3.3 3.3 3.3 3.3<br />
Centre-line Spacing mm 12.5 12.5 12.5 12.5<br />
Centre-line to Radius ratio 1.56 1.56 1.56 1.56<br />
Maxiumum Screw speed rpm 500 1000 500 1000<br />
Motor Power at Maximum Speed kW 1.25 2.5 1.25 2.5<br />
Torque per shaft Nm 12 12 12 12<br />
Torque/(C-line3 ) Nm/cm3 6.1 6.1 6.1 6.1<br />
Barrel zones 6 6 10 10<br />
Heater rating W 5x350 5x350 9x350 9x350<br />
Die heater rating W 250 250 250 250<br />
Extruder Dimensions<br />
Scale-up data<br />
L x W x Hm 1.5 x 7 x1.5m 1.5 x 7 x1.5m 1.5 x 7 x1.5m 1.5 x 7 x1.5m<br />
Internal Free Volume cm3 68 68 109 109<br />
Peripheral Surface Area cm2 316 316 505 505<br />
Surface Area per Unit Free Volume m2/1 0.47 0.47 0.47 0.47<br />
Typical output<br />
Services<br />
kg/h 0.5 to 5 0.5 to 10 0.5 to 5 0.5 to 10<br />
Electrical power Volt/ph/amp 220V/1ph/20A 400V/3ph/20A 220V/1ph/25A 400/3ph/25A<br />
Cooling Water 20ºC Litres/min 5 5 5 5<br />
104 www.rheologysolutions.com
Optical Control Systems PS25C<br />
Pellet Inspection system<br />
• product focus<br />
Web Inspection<br />
System<br />
polymer industries<br />
The OCS Web Inspection<br />
System FSP600 is a modular<br />
surface inspection system<br />
for use in production.<br />
The modular concept permits the use of several<br />
cameras working in parallel so that optimum<br />
adaptation can be achieved. The FSP600 is<br />
suitable for transparent, translucent and opaque<br />
films, sheets, coated web material, industrial<br />
textiles, paper and non wovens. The system will<br />
detect holes, thin spots, bubbles, contamination<br />
and gels, foreign particles, black specks,<br />
scratches, die lines, burst bubbles, repeated<br />
defects, insects, burns and folds.<br />
Fields of application<br />
• Films (transparent, translucent, opaque ...)<br />
• Sheets • Coated web material<br />
• Industrial textiles • Paper<br />
• Non wovens<br />
info@rheologysolutions.com<br />
• product focus<br />
Pellet Scanner<br />
polymer industries<br />
The OCS Pellet Inspection<br />
PS25C will be operational<br />
during the Ausplas 2008 in<br />
October in Melbourne<br />
inspecting a variety of<br />
transparent and opaque pellets<br />
for impurities, foreign bodies,<br />
and/or colour deviations.<br />
Applications<br />
• Opaque pellets<br />
• Coloured pellets<br />
• Non-transparent pellets<br />
• Transparent pellets<br />
Technical Data<br />
Resolution from 20 μ<br />
• Camera - 3 CCD chip colour matrix camera<br />
• Lighting - High Frequency synchronised<br />
fluorescent lamp. Power consumption:<br />
22 W. White light spectrum<br />
• Computer - Industrial CPU Pentium, up-to-date<br />
technology<br />
• Interfaces 0 Ethernet 10/100 M Base-T, Digital<br />
and analogue I/O, USB, MODBUS, PROFIBUS,<br />
RS232, OPC, DDE, SAP interface or SQL<br />
• Remote control - Extender max. 100 m.<br />
Service Remote control<br />
• Software - Operating system Windows XP<br />
• Size - Dimension (l, w, h) 50 x 50 x 80 cm ,<br />
Weight approx. 30 kg<br />
• Connection values - Power 230 V AC / 50 Hz<br />
• Temperature - +10°C – +40°C <br />
Optical Control Systems<br />
FSP600 Web Film Inspection System<br />
Types of defects<br />
• Holes • Thin spots • Bubbles • Contamination & gels<br />
• Foreign particles • Black specks • Scratches • Die lines<br />
• Burst bubbles • Repeated defects • Insects • Burns<br />
• Folds <br />
biennial 07-08<br />
105
heotalk biennial 07-08<br />
Information Request Form<br />
Name: .................................................................................................................................... Title: ...........................................................................<br />
Company: ............................................................................................................................... Department: ...............................................................<br />
Street: ..............................................................................................................................................................................................................................<br />
Suburb: ................................................................................................................................... State: ................................... Postcode: ...................<br />
Telephone: ....................................Fax: .................................... Email: ........................................................... please send me future issues by email<br />
From the Biennial 07-08 issue of RheoTalk, I am interested in the following:<br />
• Application Notes<br />
Tim’s Top Tips – How to Measure... Series<br />
Mineral Industries (please select) Thixotropy Yield Stress Flow & Viscosity<br />
Food Industries (please select) Thixotropy Yield Stress Flow & Viscosity<br />
Polymer Industries (please select) Thixotropy Yield Stress Flow & Viscosity<br />
Surface Coating Industries (please select) Thixotropy Yield Stress Flow & Viscosity<br />
Pharmaceutical, Cosmetic & Allied Industries (please select) Thixotropy Yield Stress Flow & Viscosity<br />
Building & Construction Industries (please select) Thixotropy Yield Stress Flow & Viscosity<br />
Chemical & General Manufacturing Industries (please select) Thixotropy Yield Stress Flow & Viscosity<br />
Tim’s Top Tips – Explanation & Evaluation... Series<br />
Tim’s Top Tips for Food Industries (please select) Mouthfeel Shelf Life Processability Cohesiveness<br />
Tim’s Top Tips for Surface Coatings (please select) Shelf Life Flow & Levelling Misting Mixing & Blending<br />
Tim’s Top Tips for Polymer Industries (please select) Compounding Shark Skin Processability Die Swell<br />
<strong>Rheology</strong> <strong>Solutions</strong> Information Kits (please select) Mineral Industries Food Industries Surface Coatings Polymer Industries<br />
Chemical & General Manufacturing Construction & Building<br />
Pharmaceutical, Cosmetics & Allied Industries<br />
• Application Notes<br />
biennial 07-08<br />
A New Approach to Rheological Modelling of an Electrostatic Ash & Water Mixture - Quadratic Law - RF-300902-SI-01<br />
A New Definition on Reactor Temperature Control with the Highly Dynamic HAAKE DynaMax System - TC06-01<br />
A Numerical Study of Temperature & Shear Flow in a Transiently Loaded Lubricant Film - RS-180902-SE-01<br />
Application of Liquid and Solid Rheological Techniques to the Textural Characterisation of Semi-Solid Food - Rheo049<br />
Breaking Strength of Chocolate - V222<br />
Cellulosic Derivatives in Capillary Break-up. Influence of the MWD & Gel Particles - V219<br />
Comparison of Rheological Techniques for the Characterisation of Semi-Solid Foods - Rheo027TP<br />
Characterisation of the Thixotropic Behaviour of Semi-Solid Foodstuffs - RF-110902-JO-01<br />
Correlation Between Mixer Tests & The Extrusion Behaviour of PVC Dry Blends - LR60<br />
Correlation of Misting During Printing with Extensional Rheological Investigation on Offset Printing Inks - V208<br />
Dynamic Master Curves of Polymer Modified Asphalt From Three Different Geometries - RF-110902-JO-01<br />
Evaluating the Plasticisation Process of Different Soft-PVC Samples - LR59<br />
Experimental Influences on the Casson-Viscosity. The Casson Yield Point for Chocolate Testing - V129<br />
Food & Beverage Material Characterisation - Introduction to the Influences of Rheological and Process Parameters - Rheo025TP<br />
High Quality Pharmaceutical Films - OCS007<br />
Please post or fax this form to:<br />
<strong>Rheology</strong> <strong>Solutions</strong> Pty Ltd - PO Box 754, Bacchus Marsh, Victoria, 3340<br />
Phone: 03 5367 7477 • Fax: 03 5367 6477 • Email: info@rheologysolutions.com • Website: www.rheologysolutions.com<br />
RHEO405
heotalk biennial 07-08<br />
Information Request Form<br />
Name: .................................................................................................................................... Title: ...........................................................................<br />
Company: ............................................................................................................................... Department: ...............................................................<br />
Street: ..............................................................................................................................................................................................................................<br />
Suburb: ................................................................................................................................... State: ................................... Postcode: ...................<br />
Telephone: ....................................Fax: .................................... Email: ........................................................... please send me future issues by email<br />
From the Biennial 07-08 issue of RheoTalk, I am interested in the following:<br />
• Application Notes<br />
biennial 07-08<br />
How to Select the Most Suitable Sensor for Your Application - V166<br />
Improved Torque Sensitivity & Normal Force Resolutions for Routine Measurements - V231<br />
NanoComposites - Examples on Compounding of Nanoclay Blends in Twin Screw Extruders - LR62<br />
New Measuring Cell for UV Assisted Thermal Curing at Elevated Temperatures - HA047<br />
Online Close-Loop Monitors Four Cast Film Extruders During Production - OCS008<br />
Online Quality Control of Polymers & Extruded Films - OCS004<br />
Overview of <strong>Rheology</strong>-Based Process Challenges for the Mineral Processing Industries - Rheo014<br />
Pharma MiniLab - Small Scale Compounder for Pharmaceutical Research - LR53<br />
QC Measurements for Liquid Food Products and Packaging - Rheo051<br />
Rheological & Microstructural Analysis of a Model Rennet Casein Gel as Influenced by Cooling Rate - RF-200902-US-01<br />
Rheological Analysis of Powder Coatings - Paint & Resin Issue 3-2007<br />
Rheological Analysis of Powder Coatings - V157<br />
Rheological Behaviour of Automotive Paint Systems - Rheo008TP<br />
Rheological Characterisation of Asphalt Binders - V-225<br />
Rheological Characterisation of Tooth Paste - V142<br />
Rheological Characterisation of Tooth Paste - COSSMA Article 9/2007<br />
Rheological Investigation of Three Rubbers with Different Shore Factors with Respect to Their Shape Stability Before Curing - V169<br />
Rheological Methods for Determining Molecular Weight & Molecular Weight Distribution - V230<br />
Rheological Properties of Fresh Building Materials - V217<br />
<strong>Rheology</strong> as a Tool for Immiscible Polymer Blends Characterisation: Interfacial Tension & Compatibilisation - RS-110902-BR-01<br />
Slurry <strong>Rheology</strong> & Pipeline Transport Properties, an Overview - Rheo013<br />
Small Scale Catheter Production - LR58<br />
Solvent Trap & Double Cone System for Reproducible Results in Rheological Measurements of Low Viscous Volatile Fluids - V229<br />
Test Methods for Characterisation and Optimisation of Recycling Polymers - LR45<br />
The Influence of Thickeners on the Application Method of Automotive Coatings and Paper Coatings - Rheological Investigation - V206<br />
The Rheological Properties of a Copper Concentrate Slurry: From Surface Chemistry to Pipeline Transport - RF-300702-AU-01<br />
Thickening of Electrostatically Stabilised Latices by Ethyl Acrylate-Methacrylic Acid Copolymers with Various Molecular Weight - V026<br />
Uncompromising Eyes - OCS005<br />
Wet-Shotcrete of Refractory Castables - RS-290802-BR-02<br />
What Happens When Rheological Properties Change? Looking into Theological Properties with Simultaneous Collection of Microscopic Images - V228<br />
New Die Design for the Characterisation of the Extensional and Shear Properties of Polymers for Laboratory and On-Line Use - LR39<br />
A Collaborative Study of the Structure and Rheological Properties of EVOH/SMA Blends Produced by Reactive Extrusion - LR42<br />
Continuous On-Line Rheometry for Industrial Slurries - RF-200902-AU-01<br />
Rheological Properties of Bitumen Modified with Polyethylene and Polyethylene Based Blends - RF-190902-ES-01<br />
Please post or fax this form to:<br />
<strong>Rheology</strong> <strong>Solutions</strong> Pty Ltd - PO Box 754, Bacchus Marsh, Victoria, 3340<br />
Phone: 03 5367 7477 • Fax: 03 5367 6477 • Email: info@rheologysolutions.com • Website: www.rheologysolutions.com<br />
RHEO405
heotalk biennial 07-08<br />
Information Request Form<br />
Name: .................................................................................................................................... Title: ...........................................................................<br />
Company: ............................................................................................................................... Department: ...............................................................<br />
Street: ..............................................................................................................................................................................................................................<br />
Suburb: ................................................................................................................................... State: ................................... Postcode: ...................<br />
Telephone: ....................................Fax: .................................... Email: ........................................................... please send me future issues by email<br />
From the Biennial 07-08 issue of RheoTalk, I am interested in the following:<br />
• Application Notes<br />
Small Scale Compounders for Pharmaceutical Research - PRISM004<br />
Measuring Coatings - HA030<br />
Rheological Measurements in the Coatings Industries - The Last 60 Years - Rheo050<br />
Recent Developments in Bench-Top Twin-Screw Compounders - LR51<br />
Quality Control in the Polymer Industry. Introduction to Cutting Edge Technologies and Their Application in the Polymer Industry - Rheo023<br />
<strong>Rheology</strong> for the Rubber and Elastomer Industries. Introduction to the Influences of Rheological and Process Parameters and Methods for their<br />
Measurement - Rheo 024<br />
• Products<br />
biennial 07-08<br />
NESLAB CC Series of Immersion Coolers NESLAB EX Series of Bath Circulators<br />
NESLAB HX Series of Process Chillers NESLAB RTE Series of Bath Circulators<br />
NESLAB ULT Series of Ultra Low Refrigerated Bath Circulators NESLAB ThermoFlex Series of Recirculating Chillers<br />
Temperature Control Range from NESLAB (please specify temperature range, application) ........................................................................................<br />
Marimex ViscoScope In-Line Viscometer Marimex VA-330M In Line Slurry Sensor<br />
Marimex ViscoView Software for Process Viscometer Optical Control Systems CR7/CR8 Chill Roll and Winding System<br />
Optical Control Systems FSA100 Film Surface Analyser Optical Control Systems FSP600 Wide Web Inspection System<br />
Optical Control Systems GM1 Gloss Meter Optical Control Systems HM1 Haze Meter<br />
Optical Control Systems OP5 Online Rheometer Optical Control Systems PA-66 Pellet Analyser<br />
Optical Control Systems PS-200C Online Pellet Scan System Optical Control Systems PS-25C Pellet Scan System (Colour Camera)<br />
Optical Control Systems PSSD Pellet Size and Shape Distribution System Optical Control Systems PT-2C Powder Testing System<br />
Optical Control Systems ST4 Sample Testing Unit Optical Control Systems APLAIRS Online FT-IR Spectrometry<br />
Schleibinger BT2 Compact Rheometer Schleibinger Building and Construction Materials Testing Systems<br />
Schleibinger Shrinkage/Expansion Unit Schleibinger Viscomat NT Rotational Viscometer<br />
PRISM EuroLab 16mm Twin Screw Extruder PRISM Pharma TSG<br />
PRISM PharmaLab 16 Extruder Continuous Granulation for Pharmaceutical Industry<br />
PRISM Extruder Accessories PRISM Twin Screw Extruder Range (please specify application)<br />
Thermo CoolTech 320 Cooling Circulator .......................................................................................................<br />
Thermo HeatTech 26L Heating Circulator HAAKE CaBER 1 Extensional Rheometer<br />
HAAKE Disposable Plate/Plate Geometry<br />
HAAKE MARS Modular R & D Rheometer<br />
HAAKE MARS Accessories<br />
HAAKE Falling Ball Viscometer Type C<br />
CD-Mode Curing Measurement (PS001-e) Cone/Plate Exchangeable Geometries (P005-e)<br />
Measuring Cell For <strong>Rheology</strong> of Building Materials (P006-e) New Solids Clamp (P004-e)<br />
Rheological Measurement with Optical Analysis (P016-e) RheoScope Module<br />
Please post or fax this form to:<br />
<strong>Rheology</strong> <strong>Solutions</strong> Pty Ltd - PO Box 754, Bacchus Marsh, Victoria, 3340<br />
Phone: 03 5367 7477 • Fax: 03 5367 6477 • Email: info@rheologysolutions.com • Website: www.rheologysolutions.com<br />
RHEO405
heotalk biennial 07-08<br />
Information Request Form<br />
Name: .................................................................................................................................... Title: ...........................................................................<br />
Company: ............................................................................................................................... Department: ...............................................................<br />
Street: ..............................................................................................................................................................................................................................<br />
Suburb: ................................................................................................................................... State: ................................... Postcode: ...................<br />
Telephone: ....................................Fax: .................................... Email: ........................................................... please send me future issues by email<br />
From the Biennial 07-08 issue of RheoTalk, I am interested in the following:<br />
• Products<br />
biennial 07-08<br />
Sample Fixture for Bending & Breaking Tests (P014-e) Sample Loading Tool (P002-e)<br />
SPIP Image Analysis Software for RheoScope Module (P009-e) Standard Liquids (P015-e)<br />
Support Fixture for the Analysis of Textile Samples (P012-e) Trimming Tool (P003-e)<br />
UV Curing Tool for CTC Oven (P017-e) Tribology Cell (P023-e)<br />
Vane Rotors for Pressure Cells (P021-e) SER Extensional <strong>Rheology</strong> System (P019-e)<br />
Universal Holder (P018-e) CR-Mode - Low Shear Rates (PS002-e)<br />
UV Curing Cell (P022-e) HAAKE RheoStress RS6000 Universal Rheometer<br />
HAAKE RheoStress RS6000 Sensor Systems HAAKE RheoStress RS6000 Accessories<br />
UV Curing Cell (P022-e) Double Cone Geometry<br />
Universal Holder (P018-e) Vane Rotors for Pressure Cells (P021-e)<br />
Measuring Cell for Construction Materials(P006-e) Disposable Measuring Geometries (P010-e)<br />
Tribology Cell (P023-e) HAAKE RheoStress 1 Controlled Stress Rheometer<br />
HAAKE RheoWin Software HAAKE RotoVisco 1 Controlled Rate Viscometer<br />
HAAKE Viscotester 550 Rotational Viscometer HAAKE Viscotester 550 Sensor System<br />
HAAKE Viscotester VT1/VT2 Plus Hand Held Battery Operated Viscometer HAAKE Viscotester 6 Plus Rotational Viscometer<br />
HAAKE Viscotester 7 Plus Rotational Viscometer HAAKE Viscotester 7 Plus Accessories<br />
Thermal Printer (P011-e) Adapters (P020-e)<br />
Sensor System for Viscometer/Rheometer (please specify model) ............................................................................................................................<br />
Temperature Control for Viscometers & Rheometers HAAKE DC10-K10 Refrigerated Circulator<br />
HAAKE C/DC Range of Circulators HAAKE DynaMax Viscometer Range Temperature Control Platform<br />
HAAKE EZ Cool 80 Heating/Cooling Circulator HAAKE Fogging Test Equipment<br />
HAAKE Phoenix Heating Circulator HAAKE Phoenix Refrigerated Bath<br />
HAAKE TC-Line Water Recirculators HAAKE Temperature Control Catalogue<br />
HAAKE MiniJet Injection Moulding Machine HAAKE Pharma MiniLab Micro <strong>Rheology</strong> Compounder<br />
HAAKE MiniJet II Piston Injection Moulding System / Sample specimen preparation instrument<br />
HAAKE MiniLab Micro <strong>Rheology</strong> Compounder & Reactor (20070712 - reference)<br />
HAAKE MiniLab II Micro/NanoLab Compounder for small sample amounts<br />
HAAKE PolyDrive Single Screw Extruder HAAKE PolyLab OS Torque Rheometer<br />
HAAKE PolyLab OS Docking Station HAAKE PolyLab OS Upgrade Package<br />
HAAKE PolyLab OS with Extruder HAAKE PolyLab OS with Mixer<br />
HAAKE PolyLab QC Torque Rheometer HAAKE PolyLab QC with Measuring Mixer Rheomix 600<br />
HAAKE PolyLab QC with Single Screw Extruder HAAKE PolyLab QC with Twin Screw Extruder CTW 100<br />
Food Industry Feature & Product Focus Comprehensive Materials Characterisation for Polymers<br />
Extrusion & Material Characterisation for Drug Development & Production Polymer Industry Feature & Product Focus<br />
Please post or fax this form to:<br />
<strong>Rheology</strong> <strong>Solutions</strong> Pty Ltd - PO Box 754, Bacchus Marsh, Victoria, 3340<br />
Phone: 03 5367 7477 • Fax: 03 5367 6477 • Email: info@rheologysolutions.com • Website: www.rheologysolutions.com<br />
RHEO405
heotalk biennial 07-08<br />
Information Request Form<br />
Name: .................................................................................................................................... Title: ...........................................................................<br />
Company: ............................................................................................................................... Department: ...............................................................<br />
Street: ..............................................................................................................................................................................................................................<br />
Suburb: ................................................................................................................................... State: ................................... Postcode: ...................<br />
Telephone: ....................................Fax: .................................... Email: ........................................................... please send me future issues by email<br />
From the Biennial 07-08 issue of RheoTalk, I am interested in the following:<br />
• Services<br />
Calibration & Service. Please provide details on model of product and serial number: ................................................................................................<br />
• Comments:<br />
biennial 07-08<br />
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Please remove me from future RheoTalk mailings Please add me to future RheoTalk mailings<br />
Please post or fax this form to:<br />
<strong>Rheology</strong> <strong>Solutions</strong> Pty Ltd - PO Box 754, Bacchus Marsh, Victoria, 3340<br />
Phone: 03 5367 7477 • Fax: 03 5367 6477 • Email: info@rheologysolutions.com • Website: www.rheologysolutions.com<br />
RHEO405