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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 />

info@rheologysolutions.com<br />

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 />

elasticity, processability and temperature-related<br />

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 />

25<br />

20<br />

15<br />

10<br />

5<br />

0<br />

A<br />

B C<br />

0 0,8 1,6 2,4<br />

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F F<br />

3,2<br />

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4,0<br />

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 />

....................................................................................................................................................................................................................................<br />

....................................................................................................................................................................................................................................<br />

....................................................................................................................................................................................................................................<br />

....................................................................................................................................................................................................................................<br />

....................................................................................................................................................................................................................................<br />

....................................................................................................................................................................................................................................<br />

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

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