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Overview

Welcome to the second edition

of our cumulative Biennial

RheoTalk. This has been

complied to provide our

Australian customers and

readers of RheoTalk with an

easy reference and source

of the product information,

application articles and news

from 2007 - 2008.

The newsletter has been cross indexed and

referenced by industry, so that each key area

can identify the specific information that

relates to their industry. There classifications

that we have used are listed and are also

colour coded:

• Mining Industries

• Polymer Industries

• Food Industries

• Surface Coatings Industries

• Chemical & General Manufacturing

Industries

• Construction & Building Industries

• Pharmaceutical, Cosmetics & Allied

Industries

• All Industries

Additionally, the indexes have been divided

into three sections covering Application

Notes, News & Views, and Product News

& Industry Applications. There is an index

at the beginning of each of these sections,

listing the contents within that section with

a cross reference to the industry that it

applies to.

biennial 07-08


In This Issue...

Application Notes & Laboratory Reports Product News & Industry ApplicationsApplication Notes ............................ 2-31 Product Focus ........................... 56-105Laboratory Reports............................ 2-31 Product Reviews ........................ 56-105News & Views Product News ........................... 56-105Industry Solutions ............................ 32-55 Information Request Form... 106-110Company News ................................ 32-55

Application Notes& Laboratory Reports

Application Notes• Experimental Influences on the Casson-Viscosity. The Casson Yield Point for Chocolate Tests ........................................................................ 6 •• How to Select the Most Suitable Sensor for Your Application ........................ 7 •• Rheological Analysis of Powder Coatings........................................................ 4 •• Rheological Characterisation of Tooth Paste ................................................ 5 •• Rheological Investigation of Three Rubbers with Different Shore Factors With Respect to their Shape Stability before Curing ........................................ 5 •• Rheological Properties of Fresh Building Materials ........................................ 6 •• Breaking Strength of Chocolate ................................................................ 8 •• A New Approach to Rheological Modelling of an Electrostatic Ash & Water Mixture – Quadratic Law ........................................................ 11 •• A New Definition in Reactor Temperature Control with the Highly Dynamic HAAKE DynaMax System ........................................................................ 10 •• A Numerical Study of Temperature & shear Flow in a Transiently Loaded Lubricant Film ................................................................................ 10 •• Characterisation of the Thixotropic Behaviour of Semi-Solid Foodstuffs ........ 13 •• Dynamic Master Curves of Polymer Modified Asphalt From Three Different Geometries ................................................................ 13 •• Online Quality Control of Polymers & Extruded Films ................................ 11 •• Rheological & Microstructural Analysis of a Model Rennet Casein Gel as Influenced by Cooling Rate ................................................ 12 •• Rheology as a Tool for Immiscible Polymer Blends Characterisation: Interfacial Tension & Compatibilisation ................................ 12 •• Thickening of Electrostatically Stabilised Latices by Ethyl Acrylate-Methacrylic Acid Copolymers with Various Molecular Weights ........ 13 •• Rheological Analysis of Powder Coatings- Paint & Resin Article ................ 30 •• Rheological Characterisation of Asphalt Binders ........................................ 16 •• Rheological Characterisation of Tooth Paste – COSSMA Article 9/2007 ........ 14 •• What Happens When Rheological Properties Change? Looking into Rheological Properties with Simultaneous Collection of Microscopic Images 16 • • • • •• New Measuring Cell for UV Assisted Thermal Curing at Elevated Temperatures ........................................................................ 19 • • • • •• QC Measurements for Liquid Food Products and Packaging ........................ 17 • • • Rheological Behaviour of Automotive Paint Systems........................................ 18 •• Rheological Methods for Determining Molecular Weight & Molecular Weight Distribution ........................................................................ 20 • • • • •• Solvent Trap & Double Cone System for Reproducible Results in Rheological Measurements of Low Viscous Volatile Fluids ........................ 9 •• The Rheological Properties of a Copper Concentrate Slurry: From Surface Chemistry to Pipeline Transport ........................................................ 17 •• Wet-Shotcrete of Refractory Castables ........................................................ 18 • •• Cellulosic Derivatives in Capillary Break-up. Influence of the MWD & Gel Particles ................................................................................ 24 •

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biennial 07-08

2 www.rheologysolutions.com

Application Notes& Laboratory Reports

� Application Notes• Correlation of Misting During Printing with Extensional

Rheological Investigation on Offset Printing Inks ........................................ 24 •• Improved Torque Sensitivity & Normal Force

Resolutions for Routine Measurements ........................................................ 23 •• Overview of Rheology-Based Process Challenges

for the Mineral Processing Industries ........................................................ 23 •• Slurry Rheology & Pipeline Transport Properties, an Overview ........................ 22 • •• The Influence of Thickeners on the Application Method of Automotive

Coatings and Paper Coatings – Rheological Investigation ................................ 22 •• Continuous On-Line Rheometry for Industrial Slurries ................................ 29 •• Measuring Coatings ................................................................................ 29 •• Rheological Measurements in the Coatings Industries – The Last 60 Years 27 •• Rheological Properties of Bitumen Modified with

Polyethylene and Polyethylene Based Blends ................................................ 28 •• Small Scale Compounders for Pharmaceutical Research ................................ 30 •• Measurement of the Irganox Content in Polypropylene Polymers

During Extrusion ........................................................................................ 28 •

� Laboratory Reports

• Test Methods for Characterisation and Optimisation of Recycling Polymers 4 •• Correlation Between Mixer Tests & The Extrusion Behaviour of PVC Dry Blends 14 •• Evaluating the Plasticisation Process of Different Soft-PVC Samples ................ 15 •• NanoComposites – Examples on Compounding of Nanoclay

Blends in Twin Screw Extruders. ................................................................ 21 •• Pharma MiniLab – Small Scale Compounder for Pharmaceutical Research 21 •• Small Scale Catheter Production ................................................................ 21 •• A Collaborative Study of the Structure and Rheological Properties

of EVOH/SMA Blends Produced by Reactive Extrusion ................................ 27 •• New Die Design for the Characterisation of the Extensional

and Shear Properties of Polymers for Laboratory and On-Line Use ................ 28 •• Recent Developments in Bench-Top Twin-Screw Compounders ................ 25 •

ALL

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[email protected] 07-08

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biennial 07-08


Polymers are used daily in thousands of tons.

Recycling of the used polymers is essential to

reduce the amount of waste. One of the key

problems in polymer recycling is the separation of

the polymers to defined sorts of polymers such as

PE, PP, PVC and Polyesters etc.

Even sorted materials show a wide variation of

flow behaviour, which eventually precents a

smooth processing of the recycled polymers.

The report describes various test methods to

analyse the flow and processing behaviour of

polymers.

The test were mainly operated with a recycling

granulate, made of HDPE – cosmetic bottles. The

bottles were sorted, grinded and washed to clean

the material and to remove the paper sticking on

the polymer. After drying, the material was

packed in drums for further processing.

The laboratory report includes an overview of the

following test methods: Testing of Melt Flow Rate

(MFR); Capillary Rheology; Laboratory Extruder

Tests; and Laboratory Mixer Tests.

A full copy of “Test Methods for

Characterisation and Optimisation of

Recycling Polymers” is available by quoting

reference no: LR-45�

application notes & technical articles

Test Methods for Characterisation

and Optimisation of Recycling

Polymers

Powder coatings are a cost effective and

environmentally friendly alternative to liquid

coatings. Traditional coatings systems network

via a thermally activated process. This usually

involves placing a powder coated surface into an

oven between 160°C to 200°C in temperature.

The powder melts at around 80°C to 120°C and

becomes an even film. At temperatures of

between 110°C to 140°C the network reaction

begins. The curing time typically lasts between

15 and 30 minutes, depending on the

temperature and reactivity of the system. New to

the market place are U.V. curing powder coating

systems, where the curing process takes place in

a shorter amount of time, even at temperatures of

below 100°C. A further advantage of the U.V.

induced networking is that it works virtually

independently of temperature. This opens up new

application possibilities for coating heat sensitive

surfaces like wood or synthetics.

When powder coating different substrates it is not

only smooth, tough surfaces that are desired but

also adhesive strength, corrosion protection and

durability.

The melting and curing relationship of powder

coatings can be rheologically analysed using

oscillation tests with an air bearing rheometer.

The advantage of this method is that the

structural change of the coating as a function of

time or temperature can be demonstrated without

disturbing the process ie. at very small oscillation

amplitudes.

The rheological measurements that are usually of

interest are complex viscosity h*, complex

modulus G*, the loss factor tan d as well as the

phase displacement angle d. As many powder

coatings become very hard after the complete

curing process, parallel measurements using

plate plate geometry PP20 with 20 mm plate

diameter are recommended for the rheological

tests.

Rheological analysis of powder coatings takes

place at temperatures of somewhere between

80°C and 250°C. This range can easily be

covered using the electric temperature unit

TC501 with cone heating. The following outlines

some recommendations of practical examples

and typical measurement definitions. All

measurements have been carried out using the

air bearing rheometer Haake RheoStress, with the

high temperature measuring unit TC501 with

cone heating and the parallel plate geometry

PP20 (20mm plate diameter). As a standard

measurement the gap was set at 0.5 mm.

A full copy of “Rheological Analysis of

Powder Coatings” is available by quoting

reference no: V-157�


Rheological Analysis of Powder

Coatings

polymer industries

surface coatingsindustries


5

A great variety of rubber parts is produced for the

automotive industry. To minimise problems during

the assembly of the cars and to ensure best

performance, the parts have to be manufactured

with the smallest possible variation in size and

shape. The size can be controlled by the extrusion

and injection parameters – the shrinking of the

material can often be well estimated. But what

about the shape? The problem is not only the

relaxation of the rubber after leaving the mold –

this can be controlled by an appropriate design of

the injection process. There can also be variation

of the shape before entering the oven for

vulcanisation, which takes typically half an hour.

Due to gravitational force there can be significant

changes in shape of an injected part depending

on the rubber formulation used. To avoid such

effects and to improve production performance, it

would be highly advantageous to predict the

respective properties of the sample. The

presentation will show, that prediction of shape

stability is possible with appropriate rheological

investigations.

A full copy of "Rheological Investigation of Three Rubbers with Different Shore Factors with Respect to their Shape Stability before Curing" is available be quoting reference no: V-169


Rheological Investigation ofThree Rubbers with Different Shore Factors with Respect to their Shape Stability before Curing

What is actually in the tooth paste?

Tooth pastes are viscoelastic products well known

in every day life. Its main components are

abrasives, moisture agents, binding agents,

surfactants, sweeteners, preservatives, artificial

coloring, flavors and special active ingredients.

As abrasives often hydroxides, carbonates,

phosphates or silicates are used which are to

support the mechanical cleaning effect of the

tooth brush. Moisture agents like glycerin, sorbit,

lignite or polyethylenglycols prevent a drying out

of the tooth paste; at the same time they increase

the low temperature stability and have a texture

building effect.

Binding and thickening agents give the tooth

paste its desired texture and prevent a phase

separation between fluid and solid. Hydrocolloids

like Alginate, Carrageenan, Methylcellulose or

Xanthan are mainly used as binding agents. A

frequently used thickening agent is high-disperse

silicium dioxide or Bentonite.

Surfactants decrease the surface tension thus

improving the even distribution of the tooth paste

in the mouth. In dental care only tasteless, non-

toxic anion surfactants are suitable like e.g.

sodium lauryl sulfate, or coconut aliphatic

monoglyceride sulfonate.

Sweeteners as well as the flavors serve as taste

correctives. Preservatives are necessary as

protection from microbial decomposition.

Colors and pigments are finally used for the

coloring of striped tooth pastes. Besides this,

there may be active ingredients as protection

from caries or for the care of the gums or

painsensitive teeth.

How is tooth paste produced?

The production of tooth paste is either done

batch-wise in a vacuum mixer or in continuous

production processes. In the continuous

production 5 different process steps can be

differentiated: gel production, metering of liquid

components, metering of solids, mixing process

as well as homogenization and ventilation.

A full copy of “Rheological Characterisation

of Tooth Paste” is available by quoting

reference no: V-142


Rheological Characterisation of Tooth Paste

polymer industries

pharmaceutical, cosmetic& allied industries

biennial 07-08


After the introduction of the OICCC standard

recently, rheological tests are a must in the

industry for quality assurance of the chocolate.

They include measurements at different shear

rates up to 60s-1 to be performed after a defined

pre-treatment of the chocolate. With the

computerised rheometers available today the

measuring conditions and procedures can be

preset so that most of them can be carried out

automatically by the push of a button. This will

reduce the time effort for routine tests drastically

and the saved work capacity can be used

otherwise. However, even when working

accurately and, on the first glance, with identical

pre-treatment of the samples the results can

differ considerably especially in comparison with

tests performed by someone else and with

different instruments. Some of these

measurement-related aspects should be

introduced and explained. However, the

dependence of the flow properties of chocolate

on their composition will not be discussed here.

History

From the rheological point of view chocolate is

not an easy fluid: it is a suspension of cocoa,

sugar and solid milk particles in a continuous fat

phase. The mix of the substances and their

interactions are strongly dependent on production

and pre-treatment. The yield point of chocolate

e.g. increases with longer tempering time since

the cocoa butter is already partly crystallising (i.e.

physical networks are forming which have to be

broken off before a possible shearing). In order to

obtain comparable results special attention has to

be paid to the correct reproducibility of the pre-

treatment of the sample (there are tolerances

even within the OICCC standard which can have

their effects on the results, e.g. the cool-

down/tempering times when filling the chocolate

into the rheometer). The differences occurring for

thixotropic chocolate are especially dramatic:

Here, the viscosity depends on the stirring time

(shearing time).

However, allowing sufficient time for preshearing

can eliminate errors (the necessary time can be

determined by test with a constant shear rate).

Two successively recorded flow curves of a

sample of a nougat cream available on the

market (measuring time 3 min each) which also

had a different history is shown. A slight decrease

of the viscosity can be detected which can be the

result of the small thixotropy but also of

sedimentation or homogenizing effects by

shearing.

A full copy of “Experimental Influences on

the Casson-Viscosity...” is available by

quoting reference no: V-129�


Experimental Influences on the

Casson-Viscosity. The Casson

Yield Point for Chocolate Testing

The rheological behavior of building material

suspensions plays a central role in the

processability of cement bonded building

materials and thus also in the rheological

behavior of their properties in hardened state. On

account of the widely spread application of very

different admixtures and materials, the empirical

test methods at disposal are, up to date,

inadequate in their validity for assessing the

rheological properties of these materials in fresh

state. Investigations with the rotational rheometer

– HAAKE RheoStress 600 – however, enable a

comprehensive description of the rheological

behavior of these materials.

Different problems with the description of the

rheological behavior of fresh building material

suspensions will be briefly explained in this

article. Finally, individual measuring methods for

determining these properties, as well as the

results that were won in the scope of an

investigation program for the development of

pumping-capable self-compacting light-weight

concrete will be introduced.

A full copy of “Rheological Properties of

Fresh Building Materials” is available by

quoting reference no: V-217�


Rheological Properties of Fresh

Building Materials

food industries

construction &building industries


7

The objective of this tech-note is to provide the

information that will be very helpful in selecting

which sensor is most useful for a particular

material, deformation, or temperature range.

Comparisons between different sensor systems

give confidence to operators that they are really

seeing material behavior and not some

instrument artifact.

Basically, three different sensor systems are

compared, those sensors are: concentric cylinders

(Couette system), cone and plate, and parallel

plates.

The utilities for a concentric cylinder sensor are:

• Best for lower viscosities, η0<100 Pa.s

• Good for high shear rates

• Gravity settling of suspensions has less effect

than in cone and plate

• Normal stresses hard to measure because of

curvature and need to transmit signal through

a rotating shaft.

In the case of using a cone and plate, we find

the following utilities:

• Most common instrument for normal stress

measurements

• Simple working equations: homogeneous

deformation

• Nonlinear viscoelasticity G(t, γ)

• Useful for low and high viscosity materials

• High viscosity limited by elastic edge failure

• Low viscosity limited by inertia corrections,

secondary flow, and loss of sample at edges

For parallel plates, these are the next utilities:

• Sample preparation and loading is simpler for

very viscous materials and soft solids

• Can vary shear rate (and shear strain)

independently by rotation rate or by changing

the gap; permits increased range with a given

experimental set up

• Determinate wall slip by taking measurements

at two gaps

• Delay edge failure to higher shear rate by

decreasing gap during an experiment (requires

change of cone angle in cone and plate)

• Measure N2 when used with cone and plate

thrust data

• Preferred geometry for viscous melts for small

strain material functions

For polymer melts it is recommended to use the

cone and plate, but for viscosities exceeding 103

Pa.s and high elasticity, edge failure is a severe

limitation. Squeezing a viscous sample into the

conical shape is also very time-consuming.

Another possibility would be to use parallel plates

with sinusoidal oscillations. Dynamic

measurements with parallel plates are the first

choice for time-dependent studies like curing.

For polymer solutions, the best first option is to

choose cone and plate. Normal stress data can

be collected simultaneously and the entire range

of strain from linear to nonlinear is possible.

Temperature control is typically available over a

wide range, but solvent evaporation at the edge

can cause problems.

In case that we are trying to characterise a

suspension, a narrow gap concentric cylinder is

advised. The outer cylinder should rotate to avoid

inertia problems. Another good solution could be

to use cone and plate if the suspension does not

contain large particles. For both cases, stress-

controlled instruments are recommended

providing the lowest shear rate data and best

measure of yield stress.

A copy of “How to Select the Most Suitable

Sensor for your Application” is available by

quoting reference no: V166 (NP)�


How to Select the Most Suitable

Sensor for your Application

This table shows the comparison between the three sensors described:

Sensor System Advantages Disadvantages

Concentric cylinders Low η, high γ Homogeneous End correction High η fluids are difficult to

(Couette geometry) if Ri/R0 > 0.95 Good for clean N1 impractical

suspension settling

Cone and plate Best N1 High η: edge failure, loading difficult

Best for G(τ, γ) Homogeneous Low η: inertia Evaporation

β < 0.1 rad Need good alignment

Parallel plates Easy to load viscous samples Nonhomogeneous: not good for

Best for G’ and G” of melts, G(τ, γ) OK for G(τ) and η(γ) Edge

curing Vary γ by η and Ω failure Evaporation

(N1-N2)(γ)

all industries

biennial 07-08



Breaking Strength of Chocolate

food industries

Chocolate appeals to all of our senses. We see thecolour and the glossysurface of the bar, we smellthe elusive flavours, weweigh it in our hands andfeel how it melts, we hear itbreak and sense itsresistance, and savour thetaste. With so much“sensuality“, it is easy toforget how quickly thepleasure can be destroyed,if even just one of theseproperties is not as weexpect it or are accustomed to.

Even unconsciously, the breaking behaviour of

chocolate plays an important role in influencing

the consumer's impression. Chocolate experts

can even evaluate the quality of a sample by

breaking off a piece.

Rheology plays an important role in several steps

of chocolate production. The liquid chocolate

formulation and the fats used can be

characterised by their viscosities, yield stresses

and solidification behaviours. These parameters

are important for quality control and processing,

and can be determined using rotational or

oscillation measurements.

Sensory properties as experienced during the

melting process, or “mouth feeling“, can be

described with the viscosity curves and the yield

stress. However, these rheological parameters

contain no information about the breaking

strength of the final chocolate bar - and therefore

a new method and new equipment are necessary

to assess the resistance to break.

The HAAKE MARS rheometer, manufactured by

Thermo Scientific, features a highly sensitive

normal force sensor and a very precise lift motor

which allows the customer to apply controlled

axial forces to the sample, pushing or pulling it,

and to analyse its axial deformation.

For example, with a new measuring geometry

(figure 1), chocolate bars can be positioned on

the rheometer and submitted to an increasing

axial force until they break. The new measuring

geometry consists of two parallel support bars

which can be mounted onto a base plate in a

variable distance from 1 to 7 cm. The sample lies

on these bars and a user-defined piston can be

lowered onto the sample, making possible

bending, breaking and penetration tests.

The new bending geometry was used to

investigate the breaking behaviour of small bars

of milk and dark chocolate. The distance of the

support bars was fixed at 5 cm. The piston was

cylindrical with a diameter of 6 mm. The piston

was lowered at a rate of 1.3 mm/min.

The comparison of the results in figure 2 shows a

much greater deformation prior to breakage for

the dark chocolate - it is more elastic than the

milk chocolate. The normal force increases

quickly and then falls to zero almost immediately

(blue curve). This behaviour is typical for hard and

brittle samples.

Figure 1. Breaking test on a chocolate bar on the

HAAKE MARS using the new bending geometry

The milk chocolate is much “softer“, which can

be seen in the moderate increase in the normal

force (red curve). Only a third of the normal force

required for the dark chocolate is needed to

break the milk chocolate bar. The bar breaks in

two steps: first it cracks to about the middle of its

thickness before breaking completely.

Using the new bending geometry for the HAAKE

MARS rheometer, it was possible to characterise

two types of chocolate with respect to their

breaking behaviour. The axial deformation, the

necessary normal force for breakage and the

shape of the force/deformation curves can be

used as evaluation parameters. With the same

method, different formulations of a certain

chocolate type may be analysed for an efficient

product development, or the quality of different

production lots can be controlled.

Unlike subjective sensory tests which depend on

the test person, the new method provides

objective and reproducible results, independent of

the analyst.

� Continued on page 9


9

� Continued from page 8

This new accessory significantly broadens the

application range of the HAAKE MARS rheometer.

The determination of additional relevant product

properties can be performed on the same

instrument used for the analysis of flow and

visco-elastic behaviour of the samples - which is

much more cost efficient than the purchase of a

second specific instrument. The new geometry for

bending and breaking tests is just one example of

the wide range of application specific accessories

available for the HAAKE MARS.

A copy of this application note is available

by quoting V-222.�Figure 2. Breakage curves of half bitter (blue) and a mild (red) chocolate bars

• application notes

Solvent Trap & Double Cone System for Reproducible Results in Rheological Measurements of Low Viscous Volatile Fluids

all industries

AbstractRheological measurements of low viscous volatile

fluids require the control of the surrounding

atmosphere of the measuring gap. The solvent

trap creates a defined atmosphere around the

measuring gap and the unique HAAKE double

cone system provides a sealed system for low

viscous samples.

IntroductionLow viscous water-based glues are a good

example for volatile low viscous fluids. In order

to get good measuring results in the low shear

regime a controlled stress (CS) rheometer (HAAKE

RheoStress 600) was used. To show the

advantage of the solvent trap (Fig. 1) and the

unique HAAKE double cone system (Fig. 2),

measurements were performed with and without

solvent trap and double cone system.

A complete copy of this application note is

available by requesting V-229�

biennial 07-08


The new DynaMax platformis designed to control thetemperature in jacketedreactors more efficientlythan other types oftemperature controlsystems.

DynaMax systems' “time to temperature” is the

fastest in the industry. Temperature deviation

control is accomplished with the help of Dynamic

Heat Load Suppression (DHLS) technology. Most

importantly, DynaMax systems are designed not

only to increase yields, but also to safeguard

equipment and the operator.

Jacketed reactor vessels and temperature control

units have been used for years to respond to and

to maintain the temperatures of exothermic and

endothermic reactions. These partially or fully

automated systems can be found in such markets

as Chemistry, Pharmaceutical, Biotechnology, and

Food and Beverage. The typical uses for the

jacketed reactors are:

• product development

• process development

• process optimisation

• safety investigations

• scale up applications

Maintaining precise temperature control is

desirable to ensure the process is kept in control

for repeatability and reproducibility. Both low and

high pressure options are available to control

double-jacketed reactor vessels. Correct selection

of a temperature control unit can be difficult,

however, because there are many parameters

that determine the heating/cooling requirements

inside the reaction vessel. Here are some

examples:

• heat transfer efficiency of the jacketed vessel

(glass, stainless steel etc)

• flow rate of the heat transfer fluid through

the jacketed vessel

• flow state of the medium inside the reactor

boiler (stirrer speed, flow resistance, etc)

• temperature difference between medium

inside the reaction boiler and heat transfer

liquid

• viscosity and thermal capacity of the heat

transfer fluid

Written by: Toni Kölbli, Thermo Fisher Scientific,

Temperature Control, Karlsruhe, Germany

A full copy of this application note is

available by quoting TC06-01�


A New Definition in Reactor

Temperature Control with the Highly

Dynamic HAAKE DynaMax System


Abstract

A numerical study was undertaken to provide an

understanding of the influence of thermal

conditions on friction build-up for a paraffinic

mineral oil (PAM). Matlab 6.5 was used to

perform computations for two lubricated infinite

and rigid plates in relative motion, subjected to a

transient load pulse. Two different rheological

models, one nonlinear viscous and one nonlinear

viscoelastic (Ree-Eyring), were used.

From the friction coefficients calculated it is

concluded that viscosity effects do not account

for the phenomenon of decreasing friction

coefficient with increasing maximum pressure of

the loading pulse. It appears that an explanation

for this phenomenon must be sought in the

friction properties of the interface of the ruptured

solidified lubricant. It is also concluded that the

thermal properties of the lubricated medium

present in the contact affect friction and the

formation of shear bands.

Keywords: EHD, TEHL, transient, viscoelastic,

nonlinear, rheology, lubricant, friction,

thermodynamic, heat, equation.

A full copy of the paper is available by

quoting reference no. RF: 180902-se-01�


A Numerical Study of Temperature

and Shear Flow in a Transiently

Loaded Lubricant Film

chemical & allied industries


11

Abstract

In the paper a new rheological model for an

electrostatic ash and water mixture flow is

proposed. Fundamental equation of the

rheological model was used to determine the

relationship between the shear stress and the

shear rate as well as the equation of a velocity

profile for a flow through a straight pipe.

Experimental results obtained from a capillary

viscometer were used as the basis to determine

the parameters for the proposed model by the

nonlinear regression analysis.

With the Quadratic law a numerical analysis of a

mixture flow through a capillary pipe with the

finite volume method was performed. Derived

equations for the velocity profile, shear stress and

shear rate were validated through comparison of

numerically obtained and theoretical results.

Finally the comparison between the Quadratic law

and Power law is presented.

A full copy of the paper is available by

quoting reference no. RF- 030902-SI-01�


A New Approach to Rheological

Modeling of an Electrostatic Ash

and Water Mixture - Quadratic Law

mining industries

Abstract

Today in modern polymer plants online quality

control is done automatically and alarming the

operators immediately so that the operators can

react and avoid more damage to the final

product. This “close loop”-concept also allows a

grading of the pellet lot.

The Film producers, the customers of the polymer

plants, also use web inspection systems to

control their final product quality, the quality of

the raw materials and also their process

parameters.

Between both control concepts exist some

interrelationships and also problems, because the

environment parameters are different. This

relative correlation and the impact for the polymer

and film producers will be discussed with

practical examples.

This paper was written and presented at the

TAPPI European PLACE Conference 2007 in

Athens on May 14 - 16 by:

Oliver Hissmann - Dipl.-Oec., MBA (USA) ,

Sales Manager

OCS Optical Control Systems GmbH

Email: [email protected]

A full copy of the paper is available on

request by quoting OCS004�

High Speed Pellet Scanning System PS200C from

OCS. The online pellet scan systems inspect the

transparent or opaque granules on a vibrating

channel or moving belt and detect discolouration

and foreign particles. After inspection these

defects can be sorted out into a separate

container. The good material can be fed back into

the process. These systems reach throughputs up

to 250 kg/hr

polymer industries


Online Quality Control of Polymers

and Extruded Films

biennial 07-08


Polymer blends have gained an increasingpopularity in the field of polymer science andindustry during the last thirty years. The growth inthe use of polymer blends is mainly due to theirability to combine the properties of their phasesin a unique product, making polymer blendsbroadly employed in automobile, aerospace,packing, and general goods industries. Currently,about 40% of the world polymer market isinvolved with the production of polymer blends,representing trades of billions of US$ a year. Thefinal properties of polymer blends are directlyrelated to the quality of their morphology, which inturn depends on the rheological properties of thephases of the blend, on the composition of theblend, on the processing conditions of the blend,and on the interfacial tension between thepolymers forming the blend. However, mostpolymer blends are incompatible, resulting inmaterials with coarse morphology, weak adhesionamong phases and poor mechanical properties. Infact, the future of polymer blends is based on

methods to achieve stable morphologies, so thatthe enhanced and optimized properties ofpolymer blends do not change during the productprocessing due to phenomena such ascoalescence and breakup. This matter stillremains an industrial challenge and is the objectof intense research.

Interfacial tension between molten polymers hasreceived considerable experimental andtheoretical attention due to its implication inseveral industrial applications such as coating,composites and especially in polymer blends.Interfacial tension is the single most accessibleparameter that describes the thermodynamicstate and structure of an interface in polymerblends, therefore directly related to compatibilityand hence morphology of polymer blends. Also,interfacial tension can be considered as a keyparameter that measures the state of miscibilitybetween incompatible polymers. The compatibilitybetween the phases of a blend can be improvedby the addition of compatibilisers which result ina finer and more stable morphology, betteradhesion between the phases of the blends andconsequently better properties of the final

product. The exact definition of the optimumconcentration of compatibiliser to be added isassociated with the costs minimisation, sincemost compatibilisers are much more expensivethan ordinary polymers.

In this work, rheological measurements areshown to be a useful technique to study polymerblends. In particular, they can be used todetermine the interfacial tension betweenimmiscible polymers and define the optimumconcentration of compatibiliser to be added to theblend. This study is based on the execution ofsmall amplitude oscillatory shear (SAOS) tests inthe linear viscoelasticity region of the materials.The determination of interfacial tension is relatedto the study of relaxation spectrum of a polymerblend, which is a result of the contribution of thephases and the interface. The definition of theconcentration of compatibiliser is determinedstudying the applicability of time-temperaturesuperposition (TTS) for the blend as a function ofcompatibiliser concentration.

A full copy of the paper is available byquoting reference no. RF- 110902-br-01�


Rheology as a Tool for Immiscible

Polymer Blends Characterisation:

Interfacial Tension and

Compatibilisation

polymer industries

Cooling is a final process during process cheeseproduction and is therefore critical whendetermining the texture and functional propertiesof the product. It is well established that a slowercooling yields a firmer cheese. However, there is alack of quantitative description of this operation,and the mechanism behind the observation isneeded to better control the cooling process. Therheological data for process cheese cooled atdifferent rates was quantified and was consistentwith the industrial observation. To illustratephysical changes during cooling, rennet casein

gels were studied as our first step inunderstanding the cooling effects on processcheese texture and microstructure. A similar trendin storage modulus to process cheese wasobserved when the casein gels were cooled atdifferent rates. To explain this behavior, aschematic illustration was used as the physicalbases for microstructure of colloidal gels that canresult in different rheological properties. Fractaldimension, floc size, and floc order in the proteinnetwork were treated as three possible variables.The theory developed by Shih et al. (1990) wasused to determine the floc fractal dimension, anda confocal laser scanning microscope observedthe floc size and order. The results showed that

the floc fractal dimension and size were notsignificantly different when casein gels werecooled at different rates. However, the cooling didimpact floc arrangement in the protein network. Ahigher order at a slower cooling rate resulted in ahigher storage modulus, a smaller limit of linearviscoelastic range, and an increase in gelationtemperature. The rheological data were consistentwith the microscopic images, and thehypothesised variables sufficiently explained thephysical changes in casein gels during cooling atdifferent rates.

A full copy of the paper is available byquoting reference no. RF- 200902-US-01�


Rheological and Microstructural

Analysis of a Model Rennet Casein

Gel as Influenced by Cooling Rate

food industries


13

Abstract

Polymer modified asphalt is highly temperaturesensitive material. To obtain the master curves ofdynamic material functions, for this material, onehas to perform the testing over the temperatureinterval from -30ºC to at least 90ºC. Since the

polymer modified asphalt undergoes the transition

from a glass-like to the Newtonian-like material,

in this temperature range, the benefit of using the

three testing geometries is studied, here. The

geometries used were: plate-plate (for the mid

range temperatures); torsion bar (for the low

temperatures) and bob and cup (for the high

temperatures). The advantage of the combination

of these three geometries is discussed. Stress

and strain controlled rheometers were used to

conduct all dynamic experiments. Master curves

obtained by these geometries cover up to 20

decades of the reduced frequency.

Keywords: Polymer modified asphalt, dynamic

material functions, time temperature

superposition, different geometries.

A full copy of the paper is available byquoting reference no. RF- 110902-JO-01�


Dynamic Master Curves of Polymer

Modified Asphalt from Three

Different Geometriesconstruction &

building industries

Electrostatically stabilised lattices having varioussizes were used to study the thickening of alkalis-solutable ethyl acrylate-methacrylic acidecopolymer (50 wt. % of the acid; MW = 0.78 x105, 4.36 x 105 and 11.6 x105). It was foundthat the effect increases with the molecular

weight of the copolymers and with the decreasing

size of the latex particles. The pronounced

tendency towards non-dredging flocculation and

phase separation suggest that the thickening

effect of the materials results from depletion

(volume restriction) flocculation rather that

depletion stabilisation. The role of the effective

volume fraction of the dissolved copolymer as a

variable which controls the rheological properties

of the thickened lattices was testedexperimentally.

Keywords: Electrostatically stabilized lattices, Ethylacrylate-methacrylic acid copolymers,Flocculation, Rheological properties, Thickening

A full copy of the paper is available byquoting reference no. V-26�


Thickening of Electrostatically

Stabilised Latices by Ethyl Acrylate-

Methacrylic Acid Copolymers with

Various Molecular Weights

surface coatings industries

Abstract

Many food products exhibited the thixotropicbehavior, in which, the apparent viscosity ofmaterial decreases with time of shearing atconstant shear rate.

The structural kinetic model (SKM) was used to

characterise the thixotropic behavior of threedifferent kinds of food products. Foods selectedfor analysis represent the fluid and semisolid foodmaterials. They include milled sesame,concentrated yogurt and mayonnaise. Thestructural kinetic model postulates that thechange in the rheological behavior is associatedwith shear-induced breakdown of the internalstructure of the food product. This model for thestructure decay with time at constant shear rateassumes nth order kinetics for the decay of thematerial structure with a rate constant, k. The

dependence of the degree and the extent of

thixotropy of the materials on the temperature,

composition and shear history of the food product

was determined.

Key words: structural kinetic model, milled

sesame, concentrated yogurt, mayonnaise,

thixotropy.

A full copy of the paper is available byquoting reference no. RF -110902-JO-01�


Characterisation of the Thixotropic

Behavior of Semi-Solid Foodstuffs

food industries

biennial 07-08


Abstract

This report describes the correlation between

measurements done on a laboratory mixer with

PVC Dry Blends and their processing behaviour

on a counter-rotating twin screw extruder.

Introduction

On July 1st, 2006, the EU Directive 2002/95/EG

(RoHS-Directive, Restriction of Hazardous

Substances“) was put into force. It restricts

producing and trading of products containing i.e.

lead, mercury and cadmium.

Because a lot of PVC compounds still contain

lead as stabilising media, there is urgency for the

PVC industry to replace these stabilisers by less

dangerous materials like CaZn stabilisers.

Changing the formulation of a PVC compound by

using a new stabiliser, always takes the risk that

also the production behaviour will change. The

reason behind this is the fact that stabilisers also

work as a lubricant. So the change of stabilisers

will influence the fusion behaviour of the PVC

compound. To make sure that the PVC compound

keeps its processing properties it is necessary to

adapt the whole compound formulation.

The most common tool to check the fusion

behaviour of PVC compounds is the laboratory

mixer test. It is an easy and reliable method to

characterise the fusion and degradation behaviour

of PVC compounds.

The samples used for this investigation were

three PVC Dry Blends with new lead free

formulations.

Materials and Methods Polymer:

Three samples of a PVC Dry Blend with different

CaZn-Stabilisers

Test arrangements Mixer Test:

• Torque-rheometer: RheoDrive 4

• Double range torque CAN sensor

• Analysis software PolySoft OS

• Mixer Rheomix600 OS

• Roller Rotors

• Pneumatic feeding ram

Extruder Test:

• Laboratory twin screw extruder:Rheomex

CTW100 OS

• Extruder screws: Standard screws

• Sheet die 50 x 1.0 mm

• Hopper with vibrator

• Melt-pressure sensors


available by requesting LR-60�


Correlation Between Mixer Tests and the Extrusion Behaviour ofPVC Dry Blends

HAAKE Laboratory Mixer

polymer industries

HAAKE Laboratory Extruder

Certain product properties of toothpastes can besuccessfully quantifiedusing rheology tests.

In many cases it is possible to make appropriate

adjustments to the rheology during the

development of new products. This eliminates the

need for expensive storage tests and saves costs.

COSSMA is published by Health & Beauty

Business Media GmbH, and in their September

2009 issue the article “Rheological

Characteristics of Toothpaste” written by Dr. Han-

Michale Petri et al. Thermo Fisher Scientific,

Process Instruments, Karlsruhe, Germany will be

published.

Details on COSSMA can be viewed on their

website www.cossma.com

A copy of the full paper as a PDF can be

obtained from Rheology Solutions as

a PDF by quoting HA042.�

application articles

Rheological Characteristicsof Toothpastepharmaceutical, cosmetic

& allied industries


15

Abstract

A HAAKE PolyLab OS torque rheometer, equipped

with a Mixer was used to test four different soft

PVC samples. The type and amount of plasticizer

was varied. The corresponding torque curves

helped to differentiate the formulas. The PolySoft

Mixer data evaluation is explained in detail in this

application note, and valuable hints are given for

substituting PVC blend ingredients, e.g.

plasticisers, stabilisers.

Introduction

PVC blends are complex mixtures of PVC

particles, fillers, lubricants,stabilisers and

plasticizers. They are used to provide unique

properties to a wide range of end products.

However, manufacturers are often forced to

modify these complex recipes due to

technological advances, cost pressures or

regulatory requirements. For example, two EU

directives came into force, 2002/95/EG (RoHS)

restricting hazardous lead stabilizers in the waste.

CaZn systems now are well investigated, also in

Mixers tests. Another example is the

precautionary EU regulation on phthalate

plasticizers in children’s toys which was widely

discussed in the press.

Plasticisers are used in the PVC industry to soften

the product.

Approximately 100 different plasticizers are in

use, which represents an estimated 7 billion EUR

market. The type and amount of plasticizer have a

major influence on the melt and processing

behaviour when investigating alternate blends. In

addition to tests on the final product, small-scale

tests in a mixer are advisable before starting

production. The mixer test is used for quality

control during production.

The HAAKE Rheomix system offers a quick

method to characterize the influence of

plasticizers on the plasticization and flow process

of PVC dry blends. Using HAAKE Polysoft OS

Software for mixer tests, the evaluation

and comparison of different samples is quite

quick and easy. Different routines are available,

and it is also possible to create customised

evaluation methods. Maxima, minima, points of

inflection, thresholds and slopes can easily be

calculated from all measurement data curves.


Evaluating the Plasticisation Process of Different Soft-PVC Samples

HAAKE PolyLab OS Torque Rheometer

A complete copy of this application note is available by requesting LR-59�

polymer industries

biennial 07-08


To gain information about thereasons for certain changes inrheological properties, a newspecial module for the HAAKEMARS has been developed.

It combines a temperature control unit for

cone/plate- and plate/plategeometries

with a state-of the- art microscope. The

RheoScope module is presented and example

data from different applications is shown.

Rheology is a”macroscopic“method, which tells

us how a material behaves under given conditions

but never tells us why. For an understanding

about the reasons why a certain behaviour

occurs, we need to combine rheology with a

“microscopic method“ able to look into the

structure of the material.

Examples for such techniques complementing

rheological measurements are GPC, thermal

analysis, (FT)IR or microscopy. Running two

independent measurements on different

instruments, however, doubles instrument time

and measuring time and often leaves a bit of a

doubt whether the sample and its treatment

before measuring have been exactly the same.

The double effort of time and resources can be

avoided by running two different methods on the

same sample simultaneously, testing its

macroscopic and its microscopic properties. The

two resulting data sets can easily be correlated

since they have been collected at the same time

on the same sample.


available by requesting V-228�


What Happens When Rheological Properties Change? Looking into rheological properties with simultaneous collection of microscopic images

polymer industries


food industries



The bitumen binders used inasphalt are playing a crucialrole for the performance of theasphalt.

Today, 25% of the binders are polymer modified

bitumen (PmB), providing a more sophisticated

performance and a wider temperature range than

pure bitumen does. The future share of PmB is

likely to grow due to environmental regulations,

due to a higher quote of recycling asphalt and

due to requests for lower temperature processing

e.g. for air port run ways.

A first world-wide applied standard for asphalt

binders was determined in the US Strategic

Highway Research Program (SHRP) which was

started in 1987. The results were published in

1993, standardizing for rheological testing a

Dynamic Shear Rheometer (DSR) to investigate

and predict the fatigue behaviour (4°C and 40°C)

and the behaviour at elevated temperatures

(46°C and 82°C) with a steady state stepped

temperature profile with steps of 6 degrees –

corresponding to the performance grades.

Moreover, the processability of the binders is

tested at 135°C with a rotational viscometer or

rheometer.

In order to achieve the standard compliant

temperature accuracy of ± 0.1 deg

or better, particular SHRP temperature control

units were designed in the 1990s (Fig.2). Today,

more and more measurements are made with

Peltier temperature control units, e.g. for the

screening of differently modified PmBs. The

Peltier temperature control units provide a wider

temperature range – also facilitating the relevant

sub ambient temperatures.

When bitumen or PmB is subjected to cooling, it

shows exceptionally strong shrinkage leading to

higher forces than the already high forces that

are brought about by shrinking thermoplastics.

The shrinkage of asphalt binders may lead to

quality issues and it is therefore of interest to

determine the occurring normal force and the

shrinkage in micrometers.

A complete copy of this application note isavailable by requesting V-225�


Rheological Characterisation of Asphalt Binders


• application notes & technical articles

QC Measurements for Liquid Food Products and Packaging

polymer industries

food industries

Abstract Production quality and uniformity in food

processing and its subsequent packaging is

closely related to good quality control (QC) during

the manufacturing process. In order to achieve

high quality merchandise with minimal production

losses, good process control and monitoring is

critical. This is true for production of both the food

product itself, the packaging, and of course for

putting the former inside the latter efficiently.

Laboratory and on-line systems are capable of

delivering solutions for QC monitoring, and in

cases where extra information (related sometimes

to product development, and not to QC) about the

flow properties are unnecessary, an online option

can be the most useful.

On-line systems often provide streamlined data,

showing changes in more limited criteria for the

product during the process. In this way corrective

action can be quickly taken, minimising potential

for waste and reprocessing. Laboratory

instruments, designed for quick data collection

(only a few seconds or minutes) and intuitive

understanding of the data can also be useful in

this respect where no proven online alternative

exists. On-line monitoring of shear viscosity is

widely accepted for many kinds of materials

including for liquid foods, and molten polymer

packaging. In pipe or in-tank probes can closely

monitor the shear viscosity of the material in-situ,

allowing operators and engineers to take

appropriate action to maintain the specifications of

the food product. These probes can also be

mounted at the die end of an extruder, to monitor

the viscosity of molten polymer before the

moulding of packaging. Post-extrusion, the quality

of the packaging material can be monitored

optically to detect, catalogue and notify when user

defined flaws exist in the packaging material (eg

fish eyes, pinholes, dark/light spots etc). For filling

a liquid food into a package (by pouring, squirting,

spraying etc), extensional viscosity often

dominates the process. Unfortunately, there is no

proven on-line method for monitoring the

extensional viscosity of foods as they are

dispensed from above into their packaging.

Fortunately a novel, simple and quick laboratory

technique has been developed for exactly this

purpose – measuring the relative impact of the

extensional properties of a liquid. In this way the

product and the packaging can be monitored

on-line right through the process, until the product

has safely been deposited in its packaging

Introduction Several products exist today for testing in the

laboratory, both for QA and for product develop-

ment. Laboratory testing for product quality in the

food industry can include rheometers and

viscometers, to measure liquid flow properties

such as yield stress, viscosity and elasticity under

different shear flow conditions. These instruments

can also measure the flow properties of packaging

materials, eg molten plastics etc, to ensure that

they can be properly moulded etc. Testing of solid

like properties in the laboratory is possible for both

foods and their packaging with uniaxial testing.

Miniature uniaxial testers – texture analysers –

can be used to objectively quantify textural

properties of a food, while units with larger

capacities can also be used to investigate the

tearing, stretching, crushing etc of the finished

packaging product. Often, during filling, a liquid is

poured, squirted, sprayed or otherwise dispensed

into the package.

For some materials ‘stringy’ strands hang from the

nozzle and soil the packaging, necessitating an

extra process step to clean the packaging. This

stranding is related to the extensional viscosity of

the material (completely different to the shear

viscosity measured by rotational viscometers).

Recently developed techniques now enable these

extensional properties to be properly measured in

the laboratory using extensional rheometers.

Laboratory analyses are good solutions for

material characterisation and in many cases can

not be otherwise replicated online. However,

during production it is sometimes preferable to

have an on-line system for QC, so that any

deficiencies in the product or its packaging can be

detected as quickly as possible. This technical

note seeks to explore and to explain on-line

viscosity monitoring, online quality control for

packaging film and ingredients and a novel

laboratory technique for monitoring the extensional

properties of liquids to diagnose excessive

stranding.

A complete copy of this article is available on

request by quoting Rheo051.�


The Rheological Properties of a Copper Concentrate Slurry: From Surface Chemistry to Pipeline Transport

mining industries

The rheological properties of a copper concentrate

slurry produced from a real mining operation have

been investigated. In particular, the yield stress

and viscosity of the slurry was measured after

various chemical treatments were used to alter the

surface chemistry and thus, interactions between

the particles within the slurry. These chemical

treatments are: (1) the addition of acid and (2) the

addition of polyphosphate or naphthalene

suffocate formaldehyde condensate (dispersants).

The changes in surface chemistry of the slurry

under the various chemical treatments were

investigated by X-ray photoelectron spectroscopy

(XPS) and used to describe the changes in the

observed rheological properties. The rheological

data collected was then utilised to calculate the

energy required to pump the slurry down a

pipeline under the various different chemical

regimes. Finally, a simple analysis of the reagent

cost against energy price was used to compare

the financial viability of each scheme.


request by quoting RF-3000702-AU-01.�


17


Rheological Behaviour of Automotive Paint Systems



Wet-Shotcrete of Refractory Castables

mining industries

construction & building industries

In recent years, the refractory

industry has focused much

effort on discovering novel

techniques for castable

installation that combine

high placing rate and low cost

while maintaining final material

properties.

The use of versatile and automated placing

methods such as pumping of self-flowing

castables and shotcrete has been encouraged to

replace the traditional vibration moulding

technique.

Based on these aspects, wet shotcrete is highly

interesting from a technological standpoint,

particularly for the lining of large areas and/or for

the repair of damaged surfaces.

The technique consists of pumping the castable

from the miser to the pipeline nozzle, where

high-pressure compressed air is injected so as to

project the pumped castable onto the surface to

be covered. This promotes a spray flow that

ensures a high installation rate and the formation

of a thick layer.

The difficulties involved in the shotcrete technique

relate mainly to the bonding of the material on the

area to be lined. The primary condition for a

successful operation is that the projected material

does not flow over the back lining refractory

surface, and this requires a sudden loss of the

castable’s fluidity. Traditionally, this effect is

achieved by the controlled use of cement settling

accelerators, which are also injected into the

nozzle.

Although they ensure the material’s cohesion,

conventional accelerators such as sodium silicate

and aluminium sulfate usually deteriorate the

mechanical properties of castables at high

temperatures. Therefore, proposals have been

made for novel additives based on distinct

concepts to promote the rapid reduction of

castable fluidity.

In most bases, material waste is generated during

shotcrete application due to the so-called rebound

effect. This wastage occurs when a portion of the

sprayed castables, which may amount to as much

as 30%, fails to adhere to the applied surface. The

rebound effect, which is also enhanced by the use

of accelerators, can be minimised by selecting

additives that simultaneously impart adhesive and

plastic characteristics to the castable, resulting in

homogeneous and cohesive linings, even when

successive layers are applied

In addition to the intrinsically complex pumping

operation, wet-shotcrete applications must also

take into account: (a) an abrupt increase in the

castable shearing rate and the injection of

additives, controlled by the air rate supplied in the

nozzle, and (b) the material’s adhesion and

consolidation on the surface.

The conventional testing techniques, however do

not properly evaluate shotcrete castables, given

the rheological behaviour of these castables under

similar shearing conditions during their installation

is not analysed. The traditional approaches focus

mainly on the influence of additives on the

castable’s consistency (fluidity measurements) and

on post-setting properties.

The main objective of the present study was to

develop a novel shotcrete characterisation

technique based on castable rheometry that

simulates the material’s application. Commercial

wet-shotcrete additives and other compounds with

a high potential for this application were also

evaluated using the new testing procedure.


request by quoting Rf-290802-BR-02.�

Modern Characterisation

Methods Show Good

Correlations to Observable

Effects

In this paper the most important measuring

methods for studying the rheological behaviour of

modern paint systems (oscillation tests,

determination of low yield points) are described.

These methods were at first used to describe the

rheological/physical properties of model

polyurethane micro gels. The measured values for

storage modulus, phase shift and yield point in

waterborne Pearle scent/coloured pigment

systems were compared with flop-index values.

The results show good correlations between the

observable effect and the rheological parameters

of the liquid paint.

Also measurements of powder and electrode

position coatings and clear coats with the

oscillation technique to determine the viscosity-

temperature behaviour correlate well with

technical properties of the final films.


request by quoting Rheo008TP.�

biennial 07-08


[email protected]


New Measuring Cell for UV Assisted Thermal Curing at Elevated Temperatures

InstrumentationRheometer

Rheological properties (G’, G” etc.) were measured

using the HAAKE MARS rheometer in combination

with CTC environmental test chamber for the

temperature control.

UV curing tool

The new UV curing tool is a modular extension for

the existing CTC test chamber (temperature range

-150°C up 600°C.)

The UV curing tool consists of a hollow lower shaft

with a removable light guide. The light guide can

be connected to any suitable commercially

available light source. Mounted on top of the light

guide a removable and disposable quartz glass

plate forms the lower part of the measuring

geometry. The upper plate consists of a disposable

aluminium plate mounted on a special shaft.

Figure 3a: UV Curing cell integrated

polymer industries

food industries


pharmaceutical, cosmetic & allied industries


19biennial 07-08

Disposable lowerquartz glass plate

Disposable upperaluminium

Hollow lower shaft

UV light guide

Sample

Rheometerdrive shaft

CTC shell

UV l ight

Introduction

In industry thermal curing is used in a wide range

of applications like powder coating, adhesives,

sealants, soldering materials, inks, etc. Recently

there is an increased interest in replacing thermal

curing by UV assisted thermal curing in an effort to

improve product properties, increase productivity

and reduce production costs, for example by

reducing the amount of energy needed for

initiating the curing reaction, at the same time.

For the development of, and measurements on,

such kind of samples a new high temperature UV

curing tool was developed for the HAAKE MARS

rheometer.

The new UV curing tool for the CTC oven as well

as selected results of measurements on different

adhesives are presented.

UV curing tool

Figure 2: Schematic drawing of UV curing cell

The UV light source can switched on/off by means

of a trigger signal from the rheometer which is

controlled by the rheometer software. By

programming an automatic measuring routine the

sample can first be pre-cured by the UV light and

then thermally cured using the CTC oven.

continued on page 20 �

[email protected]


Rheological Methods for Determining Molecular Weight & Molecular Weight Distribution

polymer industries

food industries


pharmaceutical, cosmetic & allied industries


Abstract The molecular weight and molecular weight

distribution (MWD) of linear polymers can be

derived by using rheological methods. The

mechanical excitation of polymers leads to a

characteristic response of the material depending

on its macromolecular structure. Using the HAAKE

RheoWin software with optional tools like TTS

(Time Temperature Superposition), Spectra and

MWD (Molecular Weight Distribution) master

curves, relaxation time spectra and molecular

weight distributions can be easily generated out of

dynamic tests (Oscillation frequency sweeps).

Practical results are presented and discussed in

this application report.

Introduction A well-established method to measure the

molecular weight distribution is the gel permeation

chromatography. This conventional method

however has some disadvantages, which are e.g.

solubility of the polymer, expensive instruments,

time-consuming procedure and less sensitivity for

high molecular components. Accordingly

rheological methods are an interesting alternative.

The theoretical relationships between the

molecular weight distribution and material

functions that can be determined through rheology

are well investigated. Powerful numerical methods

have been developed, which together with PC

technology provide a means to determine MWD

from rheological measurements.

A complete copy of this application note is available by requesting V-230�

Figure 5: UV curing behaviour of an epoxy resin

adhesive with post thermal curing

The measured normal force signal (up to 50 N

with a 10 mm diameter plate!) shows that this

sample under goes a rather large volume

expansion with increasing temperature. This is

something that should be accounted for during

the production process.

Conclusions The measurement result shows that modern

rheometry is a versatile tool for analysing the

properties of materials during UV curing and

subsequent thermal curing. The curing behaviour

of the sample and the mechanical properties of

the final cured product could be determined in

one continuous measuring job.


available by requesting HA-047�

Figure 4: UV curing behaviour of an acrylic resin

adhesive without thermal curing

After a waiting time of 15 min (in which the

temperature was increased to 35°C) the glass

transition temperature Tg of the cured sample

was determined by gradually increasing the

temperature from 35°C to 95°C. The Tg was

found to be 74.5°C.

Curing behaviour of an epoxy resin adhesive Figure 5 shows the UV and thermal curing

behaviour of an epoxy resin adhesive which is also

used in the production of flat panel displays. In this

case UV light with a wave length of 360 nm and a

light intensity of 500 mJ/cm2 was applied to the

sample for a duration of 7 min. A post heat

treatment was used to improve the product

properties in respect of adhesion and stiffness.

Figure 4a: Detailed view of the in CTC new UV

curing cell

New Measuring Cellfor UV Assisted Curing� continued from page 19

Results

Curing behaviour of an acrylic resin adhesiveFigure 4 shows the UV curing process of an acrylic

resin adhesive, which is used in the production flat

panel displays, at a temperature of 20°C. UV light

with a wave length of 360 nm and a light intensity

of 500 mJ/cm2 was applied to the sample for a

duration of 4 min. The measurements were

performed using a 10 mm diameter parallel plate

measuring geometry. For this application no post

heat treatment was necessary.

biennial 07-08



Small Scale Catheter Production

Pharma MiniLab – Small Scale Compounder for Pharmaceutical Research

polymer industries


Nanocomposities – Examples on Compounding of Nanoclay Blends in Twin Screw Extruders

polymer industries

Abstract Catheters were produced of Polystyrene (PS) and

Polycaprolactone (PCL). A PolyDrive extruder

system, as stand alone extruder was used with the

catheter die. For stable extrusion it was necessary

to use a water bath and the take off system. By

varying take off speed and output different sizes of

the catheter were obtained..

Introduction Catheters are widely used for medical applica-

tions, new developments focus on biodegradable

materials and compounding of contrast media for

x-ray depiction. Though the commercial products

are highly sophisticated and produced on

“pharma“ extrusion lines, proof of concept studies

and first developments can be run on a standard

PolyDrive single screw extruder. Obviously, in the

same way a Poly-Lab OS with single screw

extruder 19/25 OS can run the same application.



AbstractHot melt extrusion and continuous process leads

to cost efficient production.

In development of new drug/ excipients small

scale extrusion systems reduce time to market

and use comparable processes to production.

Applications and products for development with

the HAAKE Pharma MiniLab are described.

IntroductionThe pharmaceutical industry involves numerous

batch processes. Recently a trend to continuous

processes is visible as continuous processing has

a couple of advantages. Especially the hot melt

extrusion can produce more efficiently and with

higher output. Furthermore allows the extrusion

process the monitoring of processing parameter.

As compounding takes place directly in the molten

stage, aqueous solutions are avoided. Reduced or

removed drying steps help to save energy.

Extrusion is a predominant technique in polymer

processing. Profiles, sheets and bags are

produced as end products, compounds as

intermediate products. Even in the huge

installation of a petrochemical plant we see

extruders producing LDPE, PP resins with an

output of 40 t per hour. In pharmaceutical

technology the extrusion is known for more than

35 years. Developed in industries for products far

less expensive on a kilogram basis the extrusion

gives a key to survival under growing cost

constraints.



AbstractThis report describes practical examples of

nanoclay – polymer compounds processed

successful in the Karlsruhe PI Demo centre

during 2006. Nanoclay was compounded with

commercially available resins such as PP, PA

and ABS. Test setup and instrument parameters

are given as a guide line.

IntroductionNanomaterials enter the consumer market. The

focus shifts from science to standard applications.

For polymer based Nanocomposites the research

is often driven by the automotive industry

searching alternatives to bulk materials. Especially

nanoclaypolymer blends are known to improve

nanoclaypolymer blends are known to improve

material characteristics such as flame resistance,

barrier properties or toughness. Decreasing prices,

high availability, readymade Masterbatch, vast

research work, make nanoclay compounds perfect

systems to start development or assess a

machines performance.




21


The influence of thickeners on the application method of automotive coatings and paper coatings – rheological investigations


Spraying automotive coatings

and the application of paper

coatings are industrial

processes, in which

elongational flows play an

important role.

As a result, the application behaviour of these

fluids often cannot be sufficiently characterised

with traditional shear experiments. Products with

similar shear viscosities can have very different

elongation properties.

With the Thermo Scientific HAAKE CaBER 1

extensional rheometer, a liquid filament is created

that is stretched under the influence of surface

tension. Using the decrease in the filament

diameter as a function of time and the life of the

filament, it is possible to characterise the

elongational behaviour of low viscosity to pasty

liquids in a simple way. The rheological properties

of typical water-based automotive coatings and

paper coatings are determined by the thickeners

used and their interactions with the other recipe

components. In the CaBER 1 experiment, different

types of thickener display a characteristic

decrease in the filament diameter as a function

of time. Different break-up times are desirable,

depending on the application.

When automotive coatings are sprayed, short

break-up times are advantageous in order to

obtain the finest possible drop distribution.

When paper coatings are applied with rollers,

spraying and „misting“ should be prevented as

much as possible, which means that formulations

with long break-up times are advantageous.

A full copy of the application note is available on

request by quoting V-206.�


Slurry rheology and pipeline transport properties, an overview


Slurry transport in the mining

industry is a commonly used

technique for moving partially

and fully processed materials,

and waste.

Often this type of treatment is more economical

and rapid than other transportation methods, such

as those involving conveyor systems or haulage.

Additionally, the materials on a mine-site are often

slurried for processing, and pipeline transport is

necessary.

However frequently utilised, efficient slurry

transport still poses serious engineering problems

through the properties of the slurry. These

include, but are not limited to, particle settling,

attrition, pipe/fitting/impeller wear, degradation of

flocculated or friable solids, and the pumpability of

the slurry. In addition, the effects of these

challenges can be exacerbated, or reduced by

process or environmental variables, such as

temperature, pH or solids loading.

In-transit particle settling leads to stratified flow,

which in turn can cause uneven and excessive

wear in the transport system, and in extreme

cases, pipeline blockage due to solids build-up

around fittings or inclined sections. Particle

attrition has several drawbacks. Firstly, the

product before the pump and pipe is not identical

to that afterwards if the particles are friable, this

may be a QC matter both for disposal and

in-process. Secondly, changes in particle size

distribution may affect the ability of the particles to

remain suspended in the carrier fluid. Problems

with the pumpability of slurries potentially include

the fact that they often behave as a solid, e.g.

when at rest, making it expensive to initiate

pumping. Many fluids, including slurries have flow

properties which depend on the ‘rate of deforma-

tion’ (analogous to their flow-rate).

Rheological techniques can help the engineer or

technician to design for and manipulate

processes. A range of instruments is available

which measure the effects of solids loading,

carrier fluid, particle size distribution and viscosity

or pH modifiers on the propensity of particulate

matter to flocculate, be suspended, settle etc.

through a knowledge of the characteristic flow

properties of the slurry. These rheometers and

viscometers allow the engineer to directly measure

and assess the causes and effects listed above.

Physical quantities such as yield stress (the

minimum force required for a slurry to flow),

plastic viscosity (how ‘runny’ a slurry will be at a

given laminar flow-rate), hysteresis (the changes

in plastic viscosity and/or yield stress which are

due, usually, to particle attrition or settling) can be

better predicted with the appropriate equipment.

Sensitive, high precision versatile equipment is

available for repeatable and reliable measurement

of all flow properties in the laboratory, and durable,

precise, robust units for in the field use are also

commercially available. These units have been

shown to be of value for both QC and product

development.


request by quoting Rheo013�

biennial 07-08



Overview of rheology-based process challenges for the mineral processing industries


Mineral processing involves the

transportation and processing

of large quantities of materials.

Mineral processing involves the transportation and

processing of large quantities of materials.

Combining solid materials with a carrier fluid

(usually water) to create a slurry has long been

popular in the industry, principally due to the

increased efficiency and alacrity of mineral

processing steps through use of a slurry, since the

finely ground particles afford greater surface area

exposure to the extracting medium. Also, the ease

with which the particulate matter can be

processed in this form is important for unit

processes including grinding, classification,

separation processes (settling, thickening,

screening, filtration) and transport processes like

pump/gravity flow through pipes and launders,

mixing, etc.

Slurry characteristics pose many engineering

challenges. These characteristics include particle

settling, pH, bulk/carrier fluid viscosity, particulate

flocculation or dispersion, attrition,

pipe/fitting/impeller wear, degradation of

flocculated or friable solids and the pumpability of

the slurry. The effects of these challenges can be

further altered by process or environmental

variables such as temperature or solids loading.

Wet communition and classification can be

effected by viscosity, particle size distribution, fines

concentration etc. For example, hydrocyclone

classification is effected by the presence of a yield

stress (the minimum force required for a slurry to

flow). Often, cut point increases and efficiency

decreases with increasing yield stress. Separation

processes are influenced by inter-particle

attraction and viscosity (how easily the fluid flows

once it is in motion). These variables may be

manipulated through the addition of modifying

agents to the slurry. The key effects of these

additions should be monitored through changes in

the rheological parameters of the slurry, which are

directly related to process performance. In-transit

particle settling causes uneven and excessive

wear or complete blockage in the transport

system. Particle attrition may be a QC matter both

for disposal and in-process and, changes in

particle size distribution may affect the ability of

the particles to remain suspended. Problems with

the pumpability of slurries include the high cost of

initiating and continuing pumping of fluids with

high yield stresses or viscosities.

Rheological techniques can help assess process

design and manipulation processes. A range of

instruments is available to measure the rheological

effects, through knowledge of the characteristic

flow properties of the slurry. These rheometers

allow the engineer to directly measure and assess

the causes and effects listed above. Physical

quantities such as yield stress, plastic viscosity

and hysteresis (the changes in plastic viscosity

and/or yield stress which are due, usually, to

particle attrition or settling) can be quantified and

predicted with the appropriate equipment.

Sensitive, precise equipment is available for

repeatable and reliable measurement of flow

properties in the laboratory, and durable, robust

units for in-the-field use are also available. These

units are of value for both QC and product

development.


request by quoting Rheo014�


Improved torque sensitivity and normal force resolutions for routine measurements

The new HAAKE RheoStress

6000 benefits from the latest

MARS technology

developments.

The improved specifications are regarding two

components, improved air bearing specifications

and the change of the normal force sensor

technology.

The normal force sensor of the HAAKE RheoStress

6000 is based on temperature-compensated

strain gauge technology and enables normal force

measurements in the range of 0.01 to 50 N in

both positive and negative direction.

This technology offers the possibility to perform

sensitive normal force measurements even on

samples with low viscoelasticity.

In addition the new sensor enables to control the

normal force in the sample to compensate for

sample shrinkage and expansion when measuring

semisolids.

The patented 4th generation air bearing in the

HAAKE RheoStress 6000 is the result of more then

25 years of experience with the design and

manufacturing of porous carbon air bearings.

The air bearing consists of three individual air

bearings:

• One axial air bearing that supports the motor

shaft in the vertical (axial) direction and is

responsible for excellent axial stiffness.

• Two widely spaced radial air bearings that

support the motor shaft in the radial direction

and prevent the shaft from tilting.



all industries


23


Correlation of misting during printing with extensional rheological investigations on offset printing inks


The tendency for misting

on offset printing inks was

examined on two samples

using the rotational rheometer

Thermo Scientific HAAKE

RheoStress 600 and the

extensional rheometer Thermo

Scientific HAAKE CaBER 1.

The results for the amplitude and frequency curve,

the creep and recovery test and the flow curve

measurement with the rotational rheometer do not

correlate with misting during printing.

With the rotational rheometer, it was possible with

the aid of the filament break-up time to easily and

quickly draw distinctions between different

tendencies for misting with offset printing inks.




Cellulosic derivatives in capillary break-up. Influence of the MWD and gel particles


CaBER 1 extensional rheometer

is able to detect slight differ-

ences in the MWD (molecular

weight distribution) of blended

polystyrene standards.

However, the question remains if these results

obtained on a standard system can be transferred

to more complex polymers in solution like

cellulosic derivatives?

In order to control the adaptability of this method,

commercially available, blended methylhydroxy

ethyl celluloses (MHEC, e.g. used as thickener

agent in construction materials) were

characterised by uniaxial elongation in capillary

break-up experiments with the CaBER 1

extensional rheometer. The determined break-up

and relaxation times t resp. τ were then

correlated with the blending composition of the

methylhydroxyethyl celluloses and hence with the

high molar mass fraction of the sample.



polymer industries

biennial 07-08


• feature article

Recent developments in bench-top twin-screw compounders

polymer industries

Abstract

Twin-screw compounders are widely used for

dispersion of pigments and additives in the

manufacture of masterbatch. This paper describes

the availability small-scale twin-screw extruders

together with a range of ancillary equipment, to

assist the masterbatch producer in sample

preparation, and testing of the product. It also

describes the key element of heat transfer in

scale-up from laboratory extruders to production

plant.

Introduction

There are many new materials available for the

formulator of Masterbatches, but how can these

be investigated and new products developed in

readiness for the eventual up-turn in the market?

Before putting a new material into full-scale

production, different formulations need to be

tested and sample quantities made for customer

evaluation.

The presentation will describe some of these test

methods, and in particular a new technique using

an Optical System to evaluate dispersion in

polymer films. It will also outline other test and

sample preparation equipment that can be used

directly on the end of the extruder.

These include a simple blown film system;

extrusion dies for sheet and ribbon, a screen life

pressure filter test, and alternative pelletising

methods.

A simple PLC based data logging will be described

that can be used to monitor results, and with links

to a PC can be used for analysis and archiving of

sample data.

Finally, operation of small laboratory extruders,

and what are the critical factors for a reliable

scale-up to production plant will be discussed.

Twin-Screw Mixing

The melting and mixing process in a twin-screw

compounder is a rapid process. The polymer is

melted by the mechanical shear energy of the

intermeshing screws. The narrow distribution of

residence time in a twin screw means that all the

material is subjected to a similar thermal history,

giving very uniform product.

Filter Test

The Thermo Scientific PRISM twin-screw Filter test

system was described at Masterbatch 2002. The

filter test technique will soon become a recognised

standard in quality control. To apply this to the

twin-screw compounder, a simple screen changer

is bolted onto the extruder, and through the plc

control and data logging, pressure increase over

time is monitored, and using a computer can be

matched to standards for evaluation.

Film Equipment

For the film producer, a blown film die with cooling

tower and wind-up can be fitted to the extruder

allowing direct preparation of blown film samples.

A recent application of this equipment has been

particularly useful in evaluating the film blowing

properties of a biodegradable polymer, manufac-

tured from renewable, natural raw materials.

If the laboratory needs a thicker sheet of rigid or

flexible film, different sheet dies can be fitted onto

the EUROLAB to extrude sheets up to 170mm

wide with thickness from 0.5 to 2.0mm.

Dedicated cooling rolls are used to calibrate and

cool the sheet with either a cutting table for rigid

sheets or a wind-up spool for flexible films.

Optical Quality Testing

The Optical Quality Testing System measures the

transparency of a film or sheet, and counts the

number of embedded inhomogeneous particles



25

� continued from page 25

and other impurities. By measuring the transmitted

light through a polymer film, the CCD camera

processes the image and identifies discontinuities

in the film.

The camera scans an area of 400 mm2 at a rate

of 4 pictures per second, with a resolution to 60 μ

m. There are options for higher resolution on a

smaller area or scanning a larger area at a lower

resolution.

The results can be displayed and analysed on

different formats. This first display logs the counts

of different particle sizes over time.

This analysis gives the distribution of particle sizes

over the test.

Finally this analysis shows the distribution of

particles by size and frequency.

Other applications of the twin-screw use the

dedicated ancillary equipment that designed to

make up the EUROLAB System.

Pelletising

When samples are required in pellet form, then a

strand die and traditional cooling bath and

pelletiser are used. This system includes a variable

length pelletiser, where the pellet length can be

selected from 1mm to 3mm in 0.5mm steps. If

mini-pellets are needed for micro-moulding, them

a combination of high draw-down with high cutter

rotation will give 1mm X 1mm pellets.

When working with highly filled compounds, or

water sensitive products, an air quench, face cut

system is available. Here the product is cut on the

face of the die, propelled into an air stream and

conveyed to a cyclone for collection. This method

is also very useful for new water sensitive,

biodegradable polymers being studied today.

Data Logging

When many different materials need sampling, it is

very useful to be able to record operating

conditions so that reproducible samples can be

prepared. This can be even more reliable if the key

operating conditions can be recorded and stored

as a recipe for future use. The touch screen

interface and PLC control allow this to be done

simply, with added security of password

protection.

Scale-up

In any laboratory system, the operator is always

concerned with scale-up to larger production scale

equipment. Form our experience the most critical

element in this scale-up, is heat transfer capability.

Most twin-screw extruders are variable speed, and

so shear rates can be matched between laboratory

and production extruders. Residence time in the

extruder depends on a combination of product

feed rate and screw speeds. Because generally

output is determined by the motor power installed,

and that is usually scaled to the volume of the

extruder, which again gives a good scale up.

However, heat transfer in dependent on the

surface area to volume ratio. This means that the

ratio of surface area to volume is inversely

proportional to the barrel diameter. i.e. if you

double the diameter of the screws, then volume

(and hence output) will increase by 8 times while

surface area, and (hence heat transfer capability)

will increase only 4 times.

Surface Area, Free Volume relationships

Conclusion

In a modern masterbatch plant, quality control and

product sampling are key factors in the efficient

operation. By using small-scale extruders, fitted

with suitable ancillaries, and with reliability in

scale-up, the operator can have confidence in

developing new materials and formulations. This

paper has shown availability of such equipment.

A copy of this article is available on request by

quoting LR-51�

biennial 07-08



Rheological measurements in the coatings industries – the last 60 years


Abstract.

Rheology is the science of studying and predicting

flow and deformation of matter. It has long been

an important technique for verification of design,

manufacture, storage, application and cure of

coatings. As coatings formulations have increased

in complexity, meeting diverse customer needs, so

discriminatory testing techniques allowing different

materials to be compared for all conditions has

become crucial.

For sixty years the industry has gradually moved

from reliance on qualitative ‘guesstimates’ based

on operator experience, to quantitative measure-

ments. These quantitative techniques have

included Ford and Zahn cups, still used in the field

today, but which have been shown to be little more

than rough estimates for the performance of

rheologically complex materials, though they may

still work well for Newtonian or near-Newtonian

coatings. Simple Hoeppler (falling ball) or

mechanically driven rotational devices such as the

Krebbs or Stormer viscometers, and later

Brookfield viscometers emerged, reducing much

of the inaccuracy associated with cup-type

measurements. They have proven themselves

useful but there remains the problem that, if the

material is non-Newtonian the measurements are

not absolute, and data from the different

instruments cannot be compared (the units of

measurement are Krebbs Units, Brookfield Units,

HAAKE Units etc).

The ICI or “Cone & Plate” viscometers were the

first to utilise a finite gap and viscometric

geometry to measure absolute viscosity, but had

the limitation of rotating at a fixed rpm, restricting

the output of the viscometer to high shear

applications only. Now that the science is maturing

and high speed computing, combined with

inexpensive electronics and manufacturing costs,

have made low-cost rheometers and viscometers

available. They are capable of providing reproduc-

ible data for all aspects of manufacture, use and

performance of coatings (including cure), in

absolute (SI) units, allowing direct comparison of

different materials and processing conditions. The

current state of the art includes measurement of

materials in extension, quantifying the likelihood of

spatter, stranding and misting.

A full copy of this paper is available on request by

quoting Rheo-050�

Published in Pure & Applied

Chemistry. Vol. 68, No. 8, pp.

1665-1682, 1996.

© 1996 IUPAC

Synopsis

Blends of ethylene-vinyl alcohol copolymer (EVOH)

and styrene-maleic anhydride copolymer (SMA)

have been produced by reactive extrusion and

characterised in terms of their rheology, phase

morphology and the degree of covalent bonding

interaction (ester linkages) between phases, as

determined by FTIR.


A collaborative study of the structure and rheological properties of EVOH/SMA* blends produced by reactive extrusion (Technical Report)

polymer industriesStrongly synergistic behaviour in terms of viscosity

and melt elasticity was seen in all blends, for low

frequency dynamic and low shear rate capillary

tests, the largest increases occurring in blends

containing 50-60% EVOH. Finely dispersed droplet

phase morphologies were seen in most of the

blends, the minor phase forming the dispersed

phase. However the blends containing 50-60%

EVOH were co-continuous or partly co-continuous;

it was also notable that the blends containing 60%

EVOH exhibited a surprisingly low value of Melt

Index. Evidence of covalent bonding was apparent

in all blends, the highest interaction levels again

being seen for the 50-60% EVOH blends, despite

a very low anhydride/alcohol molar ratio (only

0.05). Increased mixer speed and vacuum venting

during processing also improved reaction levels.

These findings suggest that the availability of

reactive groups is restricted by the phase

morphology of the blend during production.

As a result, more reaction occurs at or near

co-continuous phase compositions, where the

surface area is maximised. The synergistic

behaviour in viscosity and elasticity can be seen

as consistent with the observed increased

bonding levels, which causes more efficient

stress transfer into the dispersed phase.

*EVOH = ethylene-vinyl alcohol copolymer; SMA =

styrene-maleic anhydride copolymer

A full copy of this technical report is available by

requesting LR-42�


27

Introduction.

Nowadays a very large majority of the roads are

constructed using a mixture of bitumen (5 wt. %)

and mineral aggregates. Notwithstanding this low

bitumen content, the performance of the road

pavement is determined by the properties of the

bitumen, as bitumen is the continuous phase and

the only deformable component. On the other

hand, from a technological point of view, the


Rheological properties of bitumen modified with polyethylene and polyethylene based blends


continuously increasing traffic load on road

pavements has resulted in tightening of binder

specifications in order to obtain higher mechanical

stability of asphalt roads. However, the limit of

increasing pavement performance with conven-

tional pure bitumen seems to have been reached.

To achieve this improvement, it is necessary the

addition of natural or synthetic polymers to the

bitumen. The aim of this project is to obtain

modified bitumens, using several synthetic

polymers, like polyolefins or rubbers. The

optimisation of composition and processing

conditions will be carried out by taking into

account the stability and rheological properties of

bitumens for road paving under extreme

conditions, which should be processed with

conventional or slightly modified machinery.

Keywords.

EPDM/PE blends; Polyolefin modified bitumens;

Bitumen rheology; Polymer/bitumen blends


quoting RF-190902-ES-01�

The rheological properties of

polymers in shear as well as in

extensional flow are essential

for their processing.


New die design for the characterisation of the extensional and shear properties of polymers for laboratory and on-line use

polymer industriesUnfortunately their complete characterisation in

the laboratory requires the complementary use

of sophisticated techniques which are time

consuming and need great expertise.

Therefore quality control is mainly limited to

the measurement of a melt flow index, a shear

viscosity and eventually a melt strength test to

assess extensional properties. The on-line

monitoring of material parameters would be very

helpful but is today mostly restricted, whenever

performed, to MFI or a capillary shear viscosity

measurement.

The HAAKE X-die has been developed to cover

the need for a quick characterization in shear

and extension, with little or even no operator

intervention. It can be mounted on a traditional

capillary rheometer or directly on-line with a melt

pump feeding it. Data obtained by this die with a

standard LDPE already tested in round robin tests,

are presented and confirm the validity of this new

approach.

A full copy of the laboratory report is available on

request by quoting LR-39�


Measurement of the Irganox content in polypropylene polymers during extrusion

Abstract.

Near infrared spectroscopy was used as an in-line

control system for the measurement of polypropyl-

ene filled with different amounts of Irganox

additives. For this purpose transmission probes

were installed in an extruder. The probes can

withstand temperatures up to 300oC and

pressures up to 60 MPa. Transmission spectra of

polypropylene mixed with Irganox with a coefficient

of models were generated with partial least square

regression which resulted in a model which

estimated Irganox with a coefficient of determina-

tion of 0.984 and root square error of prediction of

0.098%. Furthermore the possibilities for

controlling process conditions by measuring

transmission at a specific wavelength were shown.

Keywords.

polymer, irganox, extrusion, in-/on-line

Reference: W. Becker and N. Eisenreich, J. Near

Infrared Spectroscopy. 13, 147 – 154 (2005).

© NIR Publications. www.impublications.com

polymer industries

biennial 07-08



Continuous online rheometry for industrial slurries

Abstract

Mineral solids are usually processed, produced

or handled in the form of two-phase slurries.

Accurate and reliable measurements of the

rheological properties of settling slurries using

conventional viscometric instruments can be

difficult, if not impossible, since the solid particles

settle rapidly under the influence of gravity. In this

paper we report on the development of an on-line

flow rheometer specially designed and constructed

for characterising the rheological behaviour of

settling slurries. The instrument design is based

on the principles of helical flow, which is the

combination of tangential Couette and axial

Poiseuille flows. The data reduction procedure

developed is firmly based on the theory of helical

flow and has been extensively tested and validated

with fluids of different rheological behaviour. Good

results have been obtained using the rheometer

for various Newtonian liquids, pseudoplastic

polymeric solutions and mineral slurries.

Keywords

Flow rheometer, on-line viscometer, mineral slurry,

rheological characterisation, helical flow

Introduction

The control of the rheology of settling suspension

is of great importance to the mineral industry as it

is a critical factor in optimising plant life cycle

costs. Many processes involve handling particles

of diverse sizes, usually in the form of rapid

settling (unstable) slurries and it is the slurry

viscosity not the solids concentration that effects

the energy consumption and many of the design

factors of mineral processing units. It is therefore

essential that the rheological properties of these

slurries be determined accurately under conditions

that resemble closely those found in the actual

processes.

A full copy of the paper is available on request by

quoting RF-200902-AU-01.�

mining industries


Measuring coatings


Published in Polymers Paint

Colour Journal, May 2006,

pp: 50 – 53.

www.coatingsgroup.com

A wide range of measurements with viscometers

and rheometers is used to characterise the

rheological properties of coatings such as inks,

varnishes, dip coatings, paints, dispersions,

paper coatings, printing ink, security printing

pastes and powder coatings.

This paper is intended to give a brief overview

of which properties can be measured with which

tests and which instrumentation is required.

Besides the well-established shear flow testing

in rotation, creep and oscillation, the benefits of

extensional testing are discussed for viscoelastic

fluids.

In order to keep the quality of coatings on a high

level, continuous quality control is required as well

as sound knowledge of raw materials, processing

steps, storage conditions and application

procedures.

Rheology plays a crucial role in each of the steps

which a coating undergoes: After development of

the formulation, production starts with quality

control of raw materials like binders, solvents,

pigments, fillers and additives. For processing,

the components require the ability of mixing,

dispersing, pumping, stirring, homogenising and

stabilising. A good coating shows stability during

shelf life and transportation without sedimentation,

flocculation, agglomeration and coagulation.

Rheological measurements help to select proper

dimensions of pipelines, pumps and stirring

vessels as well as filling machines.

A variety of application processes uses high shear

rates or high extensional rates – eg painting,

spraying, printing, dipping which is followed

usually by gravity-driven steps – for example by

levelling in order to obtain a homogeneous film

with good properties in texture, appearance and

protection of the coated substrate.

While stability during shelf like and properties like

levelling or sagging are best characterised by a

controlled stress (CS) measurement, the various

shear rates of stirring, pumping, filling, painting

are well represented in controlled rate (CR)

measurements. Creep testing is performed in

CS mode. Gelation, cross linking and curing are

best recorded with oscillatory measurements in

controlled deformation (CD) mode while amplitude

sweeps as well as frequency or time sweeps can

be performed in CS as well as CD oscillatory

mode.

In order to understand the extensional processes

in printing and roll coating as well as in dies for

filling, spraying or spray dying, the extensional

properties require experimental determination.

A full copy of this paper is available on request

by quoting HA-030�


29


Small scale compounders for pharmaceutical research

pharmaceutical, cosmetics& allied industries

Abstract

Hot melt extrusion and continuous granulation

provide for rapid product and process design,

flexible manufacturing, a well controlled process

and cost-efficient pharmaceutical production. In

the development of new drugs/excipients, small

scale continuous extrusion systems reduce time

to market, reduce consumption of expensive

ingredients, and use processes comparable to

production. Applications and products for

development with small scale twin-screw

compounders are discussed.

Introduction

Manufacturing of clinical and commercial scale

pharmaceuticals is traditionally accomplished

using batch processes. Recently, because of its

many advantages, a trend toward continuous

processing is becoming more prevalent. For

example, hot melt extrusion can deliver increased

efficiency and higher throughput, when compared

with a classical batch process. Continuous

processing also allows for the real-time monitoring

of processing parameters and in-process material

properties. Extrusion is an established technique in

polymer processing, and is particularly important

for PAT. With real-time monitoring and process

understanding, a continuous process can more

easily be controlled to yield the highest quality

product in the most efficient way. In addition, as

compounding takes place directly in the molten

stage, aqueous solutions are avoided, reducing or

removing drying steps which helps to save energy.

In pharmaceutical technology, extrusion has been

studied and deployed for more than 35 years[1].

gives a The following article is discussing the

smallest scale of extrusion with an output of

several grams to 150 grams per hour leading to

development and production scale extruders with

outputs in the 10 to 20 kilogram per hour range.


quoting PRISM 004�

biennial 07-08


Powder coatings are acost effective and anenvironmentally friendlyalternative to liquid coatings.

Traditional coating systems form networks via a

thermally activated process. This usually involves

placing a powder coated surface into an oven at

temperatures between 160°C and 200°C. The

powder melts at around 80°C to 120°C and

becomes an even film. At temperatures

between 110°C and 140°C the cross linking

reaction starts. The curing time typically lasts

between 15 and 30 minutes, depending on the

temperature and reactivity of the system.

UV curing powder coating systems have been

established, where the curing process takes place

in a shorter amount of time, even at temperatures

below 100°C. A further advantage of the UV

induced network formation is that it works virtually

independently of temperature. This opens up new

application possibilities for coating of heat

sensitive surfaces like wood or synthetics.

The melting and curing relationship of powder

coatings can be rheologically analysed via

oscillatory tests with an air-bearing rheometer.

The advantage of this method is that the

structural change of the coating as a function of

time or temperature can be monitored without

disturbing the process i.e. at very small oscillation

amplitudes. The rheological measurements that

are usually of interest are complex viscosity η)*,

complex modulus G*, the loss factor tan δas well as the phase displacement angle δ.

As many powder coatings become very rigid after

the complete curing process, parallel


news & views

Rheological Analysis ofPowder Coatings



31

�continued from page 30

measurements using a plate/plate geometry PP20

with 20 mm plate diameter are recommended for

these rheological tests. Rheological analysis of

powder coatings take place at temperatures of

somewhere between 80°C and 250°C. Below are

experimental results which can be measured with

an air-bearing rheometer such as the HAAKE

Mars (see photo). The temperature range can be

easily covered using an electric temperature

control unit consisting of a lower and an upper

heating system.

The following outlines some recommendations of

practical examples and typical measurement

methods. A disposable plate/plate measuring

geometry made of aluminium with a diameter of

20 mm and a measuring gap of 1 or 0.5mm is

recommended.

1. Analysis of the curing process of powder

coatings at a constant temperature

The change in complex viscosity η* was analysed

as a function of time at a constant oscillatory

frequency. As the sample cures while measuring,

the oscillatory amplitude τ had to be gradually

increased in order to maintain a constant sample

deformation γ.

A desired deformation γ is assigned to the sample

(typically γ=0.5% ), the rheometer then controls

the recommended amplitude τ.

It is important for the reproducibility of the

measurement results to maintain the same

conditions for powder filling and for setting the

start of the test. In Fig. 1 an oscillation time curve

of a powder coating is illustrated. The

measurement was carried out at 200°C with a

frequency of 1 Hz. A deformation of 0.5% was

chosen. 200 data points per segment were taken.

Each oscillation was only carried out once

(number of repeats 1, no waiting time) so that the

time dependent changes of the sample could be

monitored. The complex viscosity η* and the

phase shift angle b are shown as a function

of time in the diagram. Analysis of the same

powder coating at two different temperatures

under the same conditions, establishes that the

curing process is clearly slower at 150°C than at

200°C (Fig. 2). At lower temperatures the curing

process is slower and therefore the complex

viscosity of the sample has a lower value. While

the plateau value of the complex viscosity is

reached after around 10 minutes of measuring

time at 200°C, η* still increases at 150°C after

16 minutes measuring time. For the latter

measurement, no plateau value was reached after

a measuring time of 16 minutes. A prediction

as to whether the same end value would be

achieved as at 200°C and after what time, is not

possible from the available results.

2. Analysis of the melting and curing

process as a function of temperature

The examination of changes in complex viscosity

as a function of temperature is interesting given

that two influences, namely temperature and time

are tracked simultaneously.

Firstly the powder is melted and the complex

viscosity drops to a minimum and then increases

for the curing process. The position of the

minimum and also the value of viscosity at the

minimum are dependent on the substance

itself as well as on the chosen heating rate.

Fig. 3 shows η* in relation to temperature at a

heating rate of 6 K/min for two different powder

coatings. Powder A reaches a minimum viscosity

at around 180°C, while the minimum viscosity of

sample B is reached at 160°C.

Examination of the minimum viscosity values in

the curves however, yield a much lower value for

sample A than for sample B (120 Pas compared

to 400Pas).

For processing purposes coating A should result

in a more even coating as the lower viscosity

should give a better development (film formation)

on the surface. In Fig. 4 a powder coating sample

analysis at three different heating rates is shown.

At a lower heating rate (1 K/min) the complex

viscosity runs at a minimum at 110°C after

around 30 minutes. Afterwards it increases again

and reaches a plateau value after around 80

minutes. After this the networking formation is

virtually complete. At higher heating rates the

viscosity minimum shifts to a higher temperature.

The effects of the two influences can be seen: the

viscosity decreases with increasing temperature,

the system simultaneously cross-links and the

viscosity rises again. At higher heating rates the

decrease of the viscosity predominates

momentarily because the curing process develops

more slowly.

Therefore at the highest heating rate (10K/min)

the viscosity at the curve minimum is somewhere

around 10 times lower than at the lowest heating

rate (1 K/min). The minimum viscosity at the

highest heating rate is achieved after around 7

minutes, at the mid-rate (5 K/min), after around

11 minutes. In Fig. 4 the three curves are shown

only as a function of temperature, not as a

function of time. This explains why the complete

cross-linking process is only recognisable at one

point on the graph.

This report was published in Paint & Resin,

Issue 3 - 2007�

Fig. 1: Curing of a powder coating at 200°C(f=1 Hz, γ = 0.5 %)

Fig. 2: Oszillation time curves at two temperatures(f=1 Hz, γ = 0.5 %, 150 and 200°C)

Fig. 3: Comparison of two powder coatings(f=1 Hz, γ = 0.5 %, heating rate 6 K/min)

Fig. 4: Influence of the heating rate on theProcess η* (f=1 Hz, γ = 0.5 %)

News & Views

� Industry Solutions• Feature Story- Qenos Install A Pellet Size & Shape Distribution (PSSD) System 33 • • CoolTech Application Story – Rehau Pty Ltd ................................................ 42 • • Feature Story – Uncompromising Eyes ........................................................ 43 • • • • • Sensor System to Measure Viscosity of Tailings from Marimex ........................ 41 • • Customer Installation - Plantic Technologies Ltd in Altona Victoria recently

purchased a HAAKE PolyLab with Rheology Dies ........................................ 47 • • High Quality Pharmaceutical Film –

Customer Story Klockner Pentaplast, Germany ........................................ 48 • • • Industry Overview – Material Characterisation Solutions ................................ 49 • • • • • • Feature Article - OnLine Close-Loop Monitors Four Cast Film Extruders

During Production ........................................................................................ 51 • • Food Industry Feature & Product Focus ........................................................ 54 • • How to Measure Series for Mining Slurries ................................................ 43 •

� Company News• A Brand New Year – A Brand New Look! ........................................................ 35 • • Australian Food Engineering Association

– Technical Meeting – September 2006 ........................................................ 38 • • Conferences & Exhibitions in 2007 – 29th Australian

Polymer Society Conference & Exhibition........................................................ 36 • • Conferences & Exhibitions in 2007 – 8th Joint Conference of Australian

Society of Cosmetic Chemists........................................................................ 36 • • Conferences & Exhibitions in 2007- Paste & Thickened Tailings- A Guide 2007 36 • • How to Series of Workshops– Calls for Expressions of Interest ........................ 39 • • New Addition to our Rheology Team ........................................................ 35 •• New Website Additions – Biennial Rheotalk ................................................ 40 •• New Website Additions – Interactive Dictionary ........................................ 40 •• Polymers Extrusion & Compounding Workshops

– Calls for Expressions of Interest ................................................................ 33 •• New Website Now Online! – www.TemperatureControlBaths.com ................ 37 •• Staff Update ................................................................................................ 38 •• Update on Paste & Thickened Tailings Conference ........................................ 42 • • Workshop – High Temperature Micro-Rheology ........................................ 41 • • • • • Staff Update ................................................................................................ 46 •• Staffing Changes - Administration Manager ................................................ 35 •• The Mayonnaise Jar & Two Cups of Coffee ................................................ 48 •• Service Department Update ........................................................................ 50 •• Rheology Solutions – 10th Anniversary ........................................................ 39 •• Staff Update ................................................................................................ 50 •• Company News – Home of a New High Technology Facility ........................ 55 •• Exhibitions - 30 APS Australian Polymer Symposium ................................ 36 • • Exhibitions - Ausplas 2008 ........................................................................ 43 •• Exhibitions - FoodPro 2008 ........................................................................ 66 •

ALL

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FOO

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SU

RFA

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biennial 07-08



33

Qenos in Altona has takendelivery of an OpticalControl Systems (OCS),Pellet Size, Shape andDistribution (PSSD) Systemin December 2006.

The decision to purchase the PSSD system was

based on a rigorous process of evaluation,

testing, trials and discussions between the Qenos

Technical Centre personnel, Rheology Solutions

and Optical Control Systems. The process of

discussion and trials commenced prior to Ausplas

in 2005 and resulted in Qenos bringing samples

(natural and pigmented polyethylene pellets) to

the exhibition to run them on the OCS PSSD

system to obtain bench mark results on pellet

geometry. Further samples were then sent to OCS

in Witten in Germany for geometry testing. The

objective was to compare and correlate the

current manual testing conducted at Qenos with

optical inspection results from the PSSD.

In early July, Rheology Solutions in conjunction

with OCS conducted a workshop for the polymer

industry where customers could bring their pellet

and powder samples for testing. Qenos attended

a private workshop session and discussed their

final system requirements. These requirements

and specifications were then taken back to OCS

where their program development team

incorporated these additional requirements into

their software and tailored the software to report

and show the specific results in the format that

they needed to allow them to determine the

quality and consistency of their pellet geometry.

The software configuration was modified to meet

all the Qenos reporting requirements and further

samples were run at OCS to compare the results


feature story – customer installation

Qenos install a Pellet Size Shape

& Distribution (PSSD) System

polymer industries

all industries

During 2005, Rheology Solutions in conjunction

with Thermo Electron Stone ran a series of

workshops using the PRISM EuroLab 16 mm Twin

Screw Extruder. The inaugural workshop was well

attended by over 75 people during a 7 day

timeframe. Based on the success and interest in

the 2005 workshop, Rheology Solutions is

planning on running the series in 2007.

Equipment planned for the workshop includes:

• PRISM EuroLab 16 mm Twin Screw Extruder

• Water Bath & Palletiser

• Extrusion Dies, Chill roll system and filter test

equipment.

The workshop will be half day in duration and run

as either private or public sessions where

attendees can run their own samples.

The workshop is of interest to all those in the

polymer industry including:

• Previous attendees at the 2005 workshop

• R&D personnel • Universities

• Raw material & end product manufacturers

Interested? Contact Rheology Solutions

to register your interest in the series.

Each workshop will be limited to 6 – 9 attendees

to ensure that each attendee will have maximum

opportunity for hands on training and operation of

the PRISM EuroLab 16mm Twin Screw Extruder

and ancillary equipment and adequate discussion

with Dr Tim Kealy during the workshop.

Further information on the PRISM range of

Twin Screw Extruders can be obtained from

http://www.rheologysolutions.com/prodtwin.

html�

news & views - call for expressions of interest...

Polymer Extrusion & Compounding

Workshops

biennial 07-08



Qenos install a Pellet Size Shape

& Distribution (PSSD) System

of the sample from the PSSD to their manual

testing results. The results from the comparison

on the same sample were positive and an order

for the PSSD unit was placed with Rheology

Solutions in November 2006.

The PSSD will be used at Qenos as a quality

management tool for pellet geometry. The system

has been installed in the Physical Laboratory

within the Technical Centre. The unit will be used

for rapid and reliable characterisation of Qenos

polyethylene’s, replacing the intensive manual and

time consuming techniques that had been

previously employed within the Technical Centre.

The use of the PSSD will be complementary to but

not replace the in-plant quality control pellet

geometry tests.

Qenos use Australian oil and gas feedstocks from

Bass Strait and the Moomba Basin. Qenos employ

approximately 800 people and their plants

produce olefins and a full range of polyethylene

products, including high density polyethylene

(HDPE), low density polyethylene (LDPE), linear low

density polyethylene (LLDPE) and medium density

polyethylene (MDPE). This makes Qenos a vital

link in the Australian manufacturing chain,

supplying industries that employ hundreds of

people. Polyethylene is manufactured at Qenos

plants in Botany and Altona with the capacity in

the order of 200,000 tonnes HDPE, 90,000

tonnes LDPE and 125,000 tonnes of LLDPE.

The Australian market for virgin polyethylene is

approximately 450 kt and of this, nearly 65% is

used in the packaging industry. The rigids market

is made up predominantly of bottles and

containers for milk, juice, household and industrial

chemicals, plus caps and closures. The flexibles

market is made up primarily of films for food

packaging including frozen foods, bread and fresh

produce; shopping bags; sling and shrink wraps;

industrial films and extrusion coating applications

such as liquid paper board.

In addition to its use in the packaging market,

some of Qenos’ end products are used for water

management activities such as polyethylene

piping and rotational moulded water tanks.

Polyethylene is used for pipes and fitting; in wire

and cable applications; in the automotive

components sector for tanks and storage; in

household goods and in construction.

The breadth and depth of the applications and

uses for the polyethylene is immense. The

addition of the OCS PSSD system will further

ensure that Qenos continues to provide products

of consistent quality.

Full training and commissioning of the PSSD

system will be undertaken in January 2007 for

the Technical Centre staff at Qenos. The training

will be provided by OCS and will include an

intensive two days of hands on training for all

staff. The training will also be supported by Dr Tim

Kealy – Technical Manager and Mr Richard

Donaldson – Service Engineer from Rheology

Solutions.�

Tracey Boseley replacing the lid for sample feedto the PSD.

Tim Kealy setting up the OCS software beforerunning a sample on the PSSD.

Administration Manager Jackie Wrigglesworth


35

Rheology Solutions ispleased to provide you witha new look RheoTalk fortheir first issue in 2007.

RheoTalk will continue to be published three

times per year and be available as a printed full

colour newsletter or electronically as a PDF.

The newsletter has been expanded to reference

each article in the newsletter to specific industry

classifications. An industry quick reference guide

can also be found on page 1. This will guide you

to the contents that may be of most interest to

you. The cross referencing by industry

classification was also introduced in the electronic

version of the Biennial RheoTalk for 2005 – 2006

which is available on our website.

We welcome your comments, feedback and

suggestions on what you would like to see

included in future issues of RheoTalk. We trust

that 2007 is a successful year for each of you

and we look forward to working with you during

the coming year. Cheers and happy reading.�

note from the editor

A Brand New Year

- A Brand New Look!

Rheology Solutions ispleased to introduce Evie,the newest team member.

Evie joined Rheology Solutions on Thursday, 23

November 2006 at the young age of 5 weeks

and 4 days. Evie, is a Border Collie and was born

on 15 October, 2006 to Maggie and Sam.

Evie comes to work every day along with her

older canine friend, Mal who is an Alaskan

Malamute of 101/2 years old. Mal has been

coming to work for over 81/2 years and has

welcomed the newest team member to assist

him in his day to day activities.

Mal and Evie look forward to greeting you when

you next visit Rheology Solutions.�

rheology solutions news

New Addition to our

Rheology Team

Mal and Evie relaxing before they get back into their days work.

all industries

For the past four years, Jackie Wrigglesworth has

been employed as the Marketing Assistant. From

1 July, 2007 her position in the company has

expanded to incorporate office administration as

well as her marketing support role on a full time

basis in the position of Administration Manager.

This now places Jackie as the first point of contact

for all enquiries across; general information;

product information; updating contact information;

status of delivery for current orders; scheduling of

service, repairs and calibrations (either on site or

off site); accounts receivable and payable.

Please assist us in welcoming Jackie into her

expanded role with Rheology Solutions.�

news & views

Staffing Changes – Administration Manager

all industries

biennial 07-08


During 2007, RheologySolutions will be attendingthe following nationalconferences and exhibitions.

• 29th Australian Polymer Society

Conference & Exhibition

11-15 February, 2007, Hobart, Tasmania

www.29aps.org

Rheology Solutions will be exhibiting a range of

materials characterisation products from Thermo

Fisher Scientific specifically to meet the

requirements of the polymer industry in R&D,

QA/QC and production applications. The products

will include:

• HAAKE MARS – Modular High

Temperature/High Pressure R&D Rheometer

available with interchangeable temperature

control units, and application oriented

measuring systems.

• HAAKE MiniLab – Co- and counter-rotating

twin screw extruder with integrated viscosity

measurement for compounding sample

volumes up to 7 ml.

• HAAKE MiniJet – Injection moulding machine

for sample preparation system to produce test

specimens from 5 gm of material from

powders, pellets or melts.

• PRISM Twin Screw Extruder – Segmented

barrel with lift off top half for easy access to

screws. Available with ancillary equipment

including pre-mixers, screen changers, chill

rolls, strand pelletising lines, air-cooled face-

cut system and cast sheet or blown film lines.

The conference will be attended by Dr Tim Kealy

and Mr Patrick Griffin and both will be available

on the Rheology Solutions stand number 5 to

discuss your materials characterisation and

rheology requirements.

• Paste and Thickened Tailings

– A Guide 07

13-15 March 2007, Perth, WA

www.acg.uwa.edu.au

Rheology Solutions will be exhibiting during the

Paste 2007 Seminar. On display at the exhibition

will be the HAAKE ViscoTester 550 which is

widely accepted and used within the mining

industry.

The HAAKE ViscoTester 550 will be fully

operational and demonstrated during the

exhibition. In addition, Rheology Solutions will

have a range of information kits specifically

developed and produced for the mining industry.

These kits will be made available on request and

cover: Contract Testing Capabilities for Mining

Slurries; Solutions for Mining Slurries; Tim's Top

Tips - How to Measure Thixotropy, How to

Measure Yield Stress, How to Measure Flow &

Viscosity Curves. The series of Tim's Top Tips

have been specifically written for the HAAKE

ViscoTester 550 which has been established over

the last 10 years as the mining slurries industry

standard and choice for viscosity & flow curves,

yield stress and thixotropy testing.

For further information on the HAAKE ViscoTester

VT550 visit www.rheologysolutions.com/

viscotester550_techs.html

• 8th Joint Conference of Australian

Society of Cosmetic Chemists

22-25 March 2007, Wollongong, NSW

www.ascc.com.au/news/conferences

Dr Tim Kealy from Rheology Solutions will be

presenting a paper titled “Measurements of the

viscoelastic properties of cosmetic foam products

using a vane sensor“. The paper was co-authored

by Alby Abram and Richard Buchta from

Connectics Australia and Dr Tim Kealy from

Rheology Solutions. Tim will be available for

questions regarding application, contract testing

facilities, instrument evaluation for materials

characterisation and rheology applications.•

news & views

Conferences & Exhibitions in 2007

polymer industries

mining industries


QC with Rheomix 600 - from Thermo Scientific.

The HAAKE PolyLab QC with Rheomix 600 is a

modular torque rheometer with measuring mixer.

Matthias Jährling, Senior Application Specialist,

Manager MC Application Laboratories, Process

Instruments from Thermo Fisher Scientific in

Germany will be joining Rheology Solutions on

the stand.=

• exhibitions

Australian Polymer Symposium

The Australian Polymer Symposium, is being held

in Melbourne from 30 November – 4 December,

2008 and Rheology Solutions will be participating

in the exhibition on stand number 13.

The stand will be showcasing the HAAKE PolyLab

polymer industries


37

temperaturecontrolbaths.comoffers the best selection oftemperature controlproducts within Australia

Our range covers solutions for heating and

cooling applications for industries including:

• biological • environmental

• laboratories • manufacturing

• packaging • printing

• process • raw materials

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Some 100 products are itemised on this website

across 12 category types (Accessories/Options,

Baths, Cryostats, Fogging Tester, Heating Bath

Circulators, Immersion Circulators, Laboratory

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Baths, Temperature Control Systems) and each

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The range and diversity of the temperature

control baths available has been established to

meet the control requirements across the depth

and breadth of temperature control applications.

Currently, there are two products which can be

purchased on-line (CoolTech 320 and HeatTech

26L) and this will expand to meet the needs and

requirements of the customer enquiries over the

coming months.

Buy on-line with delivery ex-stock ready to

despatch within 48 hours (or two full working

days) from receipt of official company purchase

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TemperatureControlBaths.com is owned and

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privately owned company based in Victoria.

The diversity of applications, industries and extent

of the product range instigated the creation of

this dedicated website for

TemperatureControlBaths.com

Rheology Solutions was established in April 1998

to service the requirements of the materials

science market in Australia by providing the

world's leading products and supporting sales

and distribution with service, technical support

and education. The vision is to recognise the

importance of specialisation and dedication to a

specific science and provide full technical support

and service throughout Australia. The Company

goal is to integrate industry experience and

materials characterisation techniques to provide

practical solutions for customers.

Building on the underlying vision that dedication

and specialisation is key to providing customers

with the right solution through knowledge,

experience and support,

TemperatureControlBaths.com was created.

The goal of the TemperatureControlBaths.com

website is to provide service, support and meet

the needs and application requirements within the

area of temperature control and offer the best

selection of products from recognised world

leading manufacturers.

We look forward to working with you and to

providing you with the best products, service and

support for temperature control products.

We welcome your feedback and will actively work

to provide the highest level of efficiency, customer

support and service.�

for more information visit:temperaturecontrolbaths.com

all email enquiries welcome:[email protected]

all industries

news & views

NEW Website - Now Online!

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biennial 07-08


Rheology Solutions and The Australian FoodEngineering Association,(AFEA) present a seminar for the food industry inMelbourne.

The paper was presented by Dr Tim Kealy -

Technical Manager, Rheology Solutions Pty Ltd.

“Some theory and techniques for

rheological measurements for food

and beverages”

Rheological characterisation for product design

and process control is becoming increasingly

common in the food industry, as understanding of

the power of these measurement techniques and

instruments improves amongst professional food

engineers and scientists. In September 2006,

Rheology Solutions and the AFEA collaborated to

bring the AFEA members a brief introductory

seminar on rheology and rheological techniques

applied to the food industry as the first part of a

two-part series of seminars.

The seminar was held at the Institute of Engineers

Australia buildings in Parkville, Melbourne, with

about thirty or so Food Professionals – Engineers,

Chemists and Food Scientists – in attendance.

Obtaining a good understanding of the rheology of

a food product is critical for situations as diverse

as lifecycle assessment, QC and customer

satisfaction. It is the rheology of the product

which, in large part, dictates its processability, its

structural stability and its texture. Rheological

measurements can therefore provide a valuable

insight into how a material will behave during

processing, during storage, and when the

customer finally consumes it.

New applications for foods – usually improved

products with increased functionality – are being

developed and marketed almost weekly. These

new functionalities usually result from a small

change in the ingredients making up the food

recipe. These small changes in formulation can

often have a startling impact on the food as it is

processed, filled into containers, stored and

eaten. Rheological analyses can evaluate the

extent of these impacts and help predict their

effect.

So, intelligent food design must involve some

rheological measurements and understanding to

ensure success. Without understanding the

consequences of changes in the process,

ingredients, storage conditions and so on, we

cannot hope to reliably manufacture a food

product to meet with the full approval of the

consumer.

The seminar consisted of explanations and

examples of how some of the most common

rheological measurement techniques including

extensional properties, yield stress, flow curves

and viscosity curves can be conducted, and what

the data can tell us. Along the way, introductions

to and explanations of the technical jargon and

concepts encountered in rheology were made,

and the measurement principles of different

rheometers, viscometers and measurement

geometries were introduced, in particular

rotational and extensional instruments for liquids

and uniaxial testers (“texture analysers”) for solids

and semi-solids. The concepts were illustrated

using real examples and data from the food

industries. The seminar was interactive with an

excellent question and answer session at the

close when the attendees had an opportunity to

discuss their specific queries.�

news & views

Australian Food

Engineering Association

Technical Meeting -

September 2006

food industries

Another day at the office for Evie which comprises

sleeping, greeting delivery people, a run and game

in the car park outside the office or a game with

some of the toys at work.

Mal, however prefers to spend the day outside

resting and relaxing – just visiting from time to

time to have a drink of water or join us for lunch.

He knows when it is lunch time and always is on

hand to assist us with our food.

It is tough at work and often a break from sitting

under the desk and sleeping away the hours is

needed – a game of fetch and catch is a favourite

pastime – then, it’s back to sleep under the desk

for the next while.

Sometimes however, Evie likes to serenade us all

– by squeaking her purple and pink football in her

mouth and howling at the top of her voice – most

entertaining except when you are on the phone to

a customer – which has happened on a few

occasions.�

news & views

Staff

Update

all industries

Mal takes a break with a bit of shut eye outside

Evie with her favourite purple and pink football


39

Rheology Solutions is planning to run a series of

workshops based on the Tim’s Top Tips series

covering rheology across:

• How to Measure Thixotropy

• How to Measure Yield Stress

• How to Measure Flow Viscosity Curves

The workshops will be half day in duration and

provide all attendees with hands-on training using

the HAAKE ViscoTester VT550 running their own

samples. The concept of the workshop will be to

provide attendees with a clear understanding of

what tests should be conducted, what the results

mean based on real data and real results, how to

use the results to improve the process or the

product.

The session will include a round table discussion

to determine each attendee’s objective and what

is important for them to have at the end of the

workshop. A brief theoretical overview will be

provided to cover the theory of each of the

measurements being conducted and how to use

the data once the results have been obtained.

Each attendee will be provided with an induction

on the HAAKE ViscoTester VT550, hard copy of

the full method and procedures for each

measurement conducted, copies of their results,

and an information folder including the theory of

rheology, dictionary definitions, copies of the Tim’s

Top Tips – How To series for their specific

industry and relevant product information.

At the conclusion of the testing of customer

samples, a wrap up session will be conducted to

cover questions and review of the data and

results.

Each half day workshop will be industry specific

and conducted either as public or private

sessions.

This series of workshops is of particular interest

to all QA/QC, process engineers, production and

laboratory staff across the following industries:

• Food Industries

• Pharmaceutical, Cosmetics & Allied Industries

• Surface Coatings Industries

• Mineral Slurries

• Construction and Building Materials Industries

• Chemical & General Manufacturing

Interested? Contact Rheology Solutions

to register your interest in the series.

Each workshop will be limited to 6 – 9 attendees

to ensure that each attendee will have maximum

opportunity for hands on training and operation of

the HAAKE ViscoTester VT550 and adequate

discussion with Dr Tim Kealy during the

workshop.

Further information on the HAAKE

ViscoTester VT550 can be obtained from

www.rheologysolutions.com/viscotester550_

techs.html�

news & views - call for expressions of interest...

How to Series of Workshops

all industries

On Wednesday 30 April, 2008,

Rheology Solutions turned 10.

There have been a lot of changes over the 10

years since Rheology Solutions was formed, with

the business starting out of a home office in rural

Victoria. Four years ago, the office moved to

facilitate the growing business needs some 15

kms closer to Melbourne in Bacchus Marsh. The

move has meant that the local staff that we

employ also moved with us.

Rheology Solutions was established by Pat &

Kaye Griffin and both are still full time and active

in the business. I think that there is the hope that

long service leave may apply at some point in the

near future for both of them.

Jackie joined us just over six years ago as a

Marketing Assistant working part time, and now

has the diverse role of Administration Manager

and works full time.

Richard has always had an involvement with the

business, and has been with us since Pat & Kaye

relocated back to Victoria after a four year stay in

Sydney over 10 years ago. Richard’s role is

National Service Engineer across the entire

product range we offer – it certainly keeps him

on his toes and ensures that his frequent flyer

points continue to rack up.

Rheology Solutions will continue to offer the world

leading products in temperature control, polymer,

rubber, optical scanning systems, rheology and

viscometry instruments and equipment and are

committed to maintaining their specialisation

and dedication to the science of materials

characterisation.

Our vision is to recognise the importance of

specialisation and dedication to a specific science

and to provide full technical support and service

throughout Australia. Our company goal is to

integrate industry experience and materials

characterisation techniques to provide practical

solutions for customers.

All of us at Rheology Solutions thank you for your

business over the last ten years and we look

forward to being of continued service to you.�

news & views

Rheology Solutions 10th Anniversary

all industries

biennial 07-08


During 2007 a numberof new features andfunctions will be madeavailable on the RheologySolutions websitewww.rheologysolutions.com

Biennial RheoTalk – Now available as a PDF on line

This inaugural cumulative Biennial RheoTalk issuehas been compiled to provide our Australiancustomers and readers of RheoTalk with an easyreference and source of the product information,application articles and news from 2005 – 2006.

The newsletter has been cross indexed andreferenced by industry, so that each key industryarea can identify the specific information thatrelates to their industry. The industryclassifications that we have used are colourcoded and cover:• Mineral Slurries• Polymer Industries• Food Industries• Surface Coatings Industries• Chemical & General Manufacturing Industries• Construction & Building Industries• Pharmaceutical, Cosmetics & Allied Industries

Additionally, the indexes have been divided intothree sections covering Application Notes, News &Views, and Product News & Industry Applications.There is an index at the beginning of each ofthese sections, listing the contents within thatsection with a cross reference to the industry thatit applies to.

The PDF enables the reader to utilise the searchfacility with the software. This means thatsearching can be conducted by any word, phrase,industry type, brand name, application or productmodel.

At the end of the cumulative issue of RheoTalk aninformation request form has been provided forthose that require further information. The formcan be printed and filled out and then either faxedor posted. Alternatively, requests can be sent by

email direct to [email protected] with

details of the information requested.

We trust that the Biennial RheoTalk will be a

useful and easy source to access industry

specific rheology and materials characterisation

information that we have provided during 2005 –

2006.�

Interactive Dictionary… Coming soon

As a continuation of our commitment to providing

education, knowledge and resources to industry,

Rheology Solutions has developed an extensive

materials characterisation dictionary covering

seven key industry areas. The dictionary explains

both rheological and industry specific terminology

and relates it to measurement techniques and

instrumentation.

The interactive dictionary will be available on line

as a PDF which can be searched according toindustry type (Food, Chemical, Pharmaceutical,Cosmetics, Construction, Building, SurfaceCoatings, Polymer, and or Mineral), term, andproduct brand.

The dictionary will have links to a summary pagespecific to each industry classification which willdetail all the available information for thatindustry. This information can then be requestedand will be supplied as hard copy.

The interactive dictionary has been developed toprovide industry with a reference source thatrelates their terminology to the governingproperties and measurement information formaterial characterisation solutions. The benefit ofthis dictionary is that it has been created from theindustry perspective using their process termsand providing an overview of how to identify,measure, and apply testing protocols.�

news & views

New Web Site Additions

all industries


41

A new sensor style fromMarimex Industries Corp.now extends its applicationbase into the miningindustry.

This sensor is based on a standard Marimex

design but employs a special coating to inhibit

the abrasive conditions often found in the mining

industry. Previously such sensors have already

been used without coating in similar industries

like cement and concrete applications, where

abrasion is also very high. The use of this special

coating is expected to extend the lifetime of the

sensor.

As environmental impacts are being felt around

the world, it is also felt in the mining industry

especially as it applies to water usage. In many

areas water has become a precious resource and

steps need to be taken to limit use of water.

Viscosity measurement can assist in determining

and limiting such water usage as an example in

tailings streams. Already a relatively small

additional amount of water to a tailings stream

will lower the viscosity of the stream by an

amount measurable with a Marimex viscometer.

Marimex viscometer sensors provide a high

resolution measurement in process and yet are

rugged for the application. Different styles are

available to cover a wide range of measurement.

Every system is factory calibrated and capable to

measure over multiple decades of viscosity.

Systems can be easily field configured to

measure 1% of the calibrated range as a full

range yet again with the resolution still being 1%

of the configured range. No change or physical

modification to the sensor is required. A

configuration change on the transmitter is all that

is required.

Together with the introduction of this new sensor

Marimex is also introducing new electronics.

Based on the proven technology of the model VS-

4450 the new model VS-D250 reduces both the

size and the price of the transmitter. This has

been achieved by repacking the electronics and

leaving off a few capabilities, which are often not

required in some applications. The model VS-

D250 is housed in a DIN rail housing and can

easily be mounted in a back panel rather than

taking up front panel space. It is capable to carry

two output cards which are available as 4 to 20

mA analog outputs or RS485 and RS232 serial

outputs. An additional RS232 output is available

on the front plate as well and can be used for all

included Modbus capabilities including

configuration via a computer. Power supply for

this transmitter is 24 VDC, which makes it easy to

be connected to a non-interruptible 24 VDC

power supply. A model VS-C250 with the similar

capabilities as the model VS-D250 is also

available. This model is for insertion directly into a

sensor. however due to the mounting inside the

sensor, this electronics can only be configured via

a computer, whilst the model VS-D250 can also

be configured by hand via three push buttons.�

new & views

Sensor System to Measure

Viscosity of Tailings from Marimex

mining industries

High temperature rheology and simultaneousmicroscopy on polymer melts is now achievable.Thermo Scientific have developed the HAAKEMARS with RheoScope module to meet thecustomer requirements for high temperaturerheology and microscopy applications.

Rheology Solutions will conduct an applicationsworkshop with the equipment in Victoria wherecustomers can bring their own samples fortesting.

This product will be of interest to R&D, ResearchOrganisations, Universities, Food, Polymer,

Pharmaceutical, Cosmetic & Allied Industries and

Chemical Industries.

If you are interested in purchasing this equipment

to meet your application requirements, let us

know now. We will then coordinate the

workshop with the support of Thermo Scientific

and advise you of the planned date.

Send an email with details of your

application and any questions that you have

to [email protected] �

workshop

High Temperature Micro-Rheology

food industries

polymer industries



biennial 07-08


Recently Rheology Solutions sold a CoolTech 320refrigerated circulator toREHAU Pty Ltd for usein a display at a recentexhibition in Melbourne. The application where theCoolTech was used wasquite unusual and outsideof the 'square'.

At the DESIGNEX expo held at the Melbourne

convention centre 19 - 21st April, 2007, REHAU

used the Thermo Scientific CoolTech 320

refrigerated circulator unit and 16mm RAUPINK

under floor heating pipe to set up an ice bar

along side their 'Under floor heating display'. The

aim of which was to provide a visual indicator to

their customers and show them the conductive

nature of their RAUPINK pipe.

The pipe was set up in a snail formation within a

stainless tray. The CoolTech 320 was set up at

-8ºC for the duration of the three day expo.

Customers were able to physically see and touch

the ice, which was then used to serve shots of

schnapps to them at the afternoon tea break.

According to REHAU the project was a great

success and proved to be very popular with their

customers.

REHAU is an independent and privately owned

company with over 120 branches, 44 plants and

12 training academies across 53 countries,

REHAU is one of the world's leading polymer

solutions providers. Their products are found in a

wide range of applications from energy efficient

uPVC windows and automotive bumper systems

to life-preserving medical components for the

healthcare industry. www.rehau.com.au�

news & views

CoolTech Application Story

all industries

CoolTech 320 installed RAUPINK under floor heating pipe Afternoon tea

In March 2007 RheologySolutions attended theconference in WA andexhibited the HAAKEViscotester VT550 and tookover 150 copies of Tim's

Top Tips “How to Measure

Series” for the mining

industry.

The response from the attendees to the HAAKE

ViscoTester VT550 was positive with 10 HAAKE

ViscoTester VT550 Slurry Packages being sold

during the exhibition. The copies of the “How to

Measure Series” for the mining industry was also

of great interest - especially the booklet covering

'Yield Stress'. Almost all the copies were gone by

the middle of the second day of the conference,

and before the end of the conference there were

no copies left.

If you missed out on the 'How To Series'

for mining industries and would like copies,

complete the information request form

and we will send them to you.�

news & views

Update on Paste and Thickened

Tailings Conference

mining industries


43

feature story

Uncompromising Eyes

Film Inspection. Onlineinspection systems are anestablished part of high-qualityfilm production today. Amanufacturer of PE laminatingand surface protection films isused to illustrate theincorporation of an integratedquality concept with the aid ofpractical examples

By Gerd Finn - Orbita Film

Oliver Hissmann - Optical Control Systems

PE surface protection, interlayer, label and

laminating films have to meet very high quality

requirements. In particular, these films must

have the lowest possible number of fish-eyes,

which are unavoidable in PE films. Fish-eyes are

small film homogeneities characterised by their

area (size in transmitted light) and protrusion

above the film surface. The fish-eye count is to

some extent an inherent film property. Film

manufacturers and users therefore try to

minimise the fish-eye count and fish-eye size to

a level where the fish-eyes pose no problem for

the particular film converting process and

intended application. See Figure 1.


polymer industries


food industries


• news & views

How to measure series for mining slurries

Three “How to Measure” tips

have been written for mining

slurries and are available on

request. The series provides a

booklet which details tips on

measuring thixotropy, flow &

viscosity curves, and yield

stress.

Thixotropy is a relative measurement and as such

depends on the experimental conditions and

technique used to measure it. There are several

such techniques, the simplest being modified flow

curves, or constant shear rate or shear stress

measurements. A more complicated, but perhaps

more intuitively understood method is the shear

and recovery method.

In order to attain repeatability the most appropriate

technique should be selected and the sample

handling and experimental procedures defined

fully. These should be unchanged for all tests, so

that thixotropy for different materials can be

properly compared.

Thixotropy is a relative measure of the extent and

seed of recovery of the internal structure of a

material during and after shear. It is useful

because it allows and estimate of the effects of

agitation, pumping etc for prolonged periods, and

also the effects of ceasing the agitation etc (i.e.

how quickly the structure will rebuild, and how

difficult it will be to restart the process as a result).

Flow & Viscosity Curves. A flow curve is used to

define the interdependency of the shear rate and

shear stress for a material. To generate a flow

curve either a range of shear rates or of shear

stresses can be imposed on the material, and the

other of the pair – the response of the material –

is measured. A viscosity curve shows the viscosity

of a material at each shear rate from the flow

curve. Flow and viscosity curves can be presented

either on logarithmic or linear axes. They describe

the flow behaviours at a variety of shear rates, so

that pump, pipe, impeller, etc sizing can be

correctly achieved. They are also important

because they define the type of flow behaviour

one can expect from a material – Newtonian,

pseudoplastic (shear thinning), dilatant (shear

thickening) etc.

Yield Stress has an impact on the mining industry

in a variety of ways. In pumping and mixing at

start-up, it must be overcome so that the impellers

can turn. In pipeline transport yield stress

influences the velocity profile of the material, and

under some circumstances can cause the material

to flow as a solid plug carried by a lubricating

liquid layer at the wall where shear stresses are

high. The yield stress of a material dictates

whether or not a solid fraction will settle to the

bottom of a tank, pipe or other container, and also

whether gaseous materials can rise through it.

Disposal of mining waste is an important issue

and the yield stress influences the slope of

beaches in disposal areas, the ability of high solids

pastes to be compressed and to flow after

disposal and so on.

Note: Each Tip includes working definitions.

Copies of How to Measure … Yield Stress,

Thixotropy, Flow & Viscosity Curves are available

on request. �

mining industries

• exhibitions

Ausplas 2008

polymer industries

Rheology Solutions will be participating

in this exhibition (booth number 100) in

Melbourne from 7 – 10 October 2008

showcasing a range of equipment and

instruments specifically for the polymer

industry.�

biennial 07-08


Feature Story

Uncompromising Eyes


Figure 1. Film with foreign contaminant

Causes of Fish-eyes

In higher-molecular-weight constituents from the

polymeristaion process or foreign polymeric

materials do not completely melt, they form fish-

eyes. Contaminants such as dust from bulk

containers, abraded particles in material transfer

lines and foreign materials, e.g. from poorly

cleaned silos, can also cause fish-eyes. During

the transfer of PE pellets in pipelines, some of the

PE pellets melt and smear on the walls of the

pipelines due to abrasion and form ribbon-like

streamers (angle hair) that gradually flake off into

the pellet stream. While the streamers are still

adhering to the pipeline walls, their large surface

area comes into prolonged contact with

atmospheric oxygen. This gives rise to reactive

molecular groups, which form fish-eyes. Deposits

on the inside wall of the extruder or excessively

long thermal exposure during a stoppage can

lead to fish-eyes with characteristic brownish

occlusions. Poorly homogenised additives such as

pigments, antiblocking agents, etc. act as nuclei

around which polymer accumulates to form fish-

eyes. See figures 2 & 3.

Figure 2. Fish-eye in a coextruded centre layer

Figure 3a & Figure 3b. 3-D view of a fish eye

Problems withContaminants

Surface protection films are coated with adhesive

and bonded to high-gloss metal surfaces

(aluminium sheet, stainless steel sheet) or

scratch-sensitive plastic surfaces (PMMA, PC,

PVC) to protect these vulnerable surfaces during

further processing and transport. In

thermoforming - for example into headlamp

reflectors or kitchen sinks - excessively large fish-

eyes press slightly into the surface and leave

behind noticeable imperfections, which are not

accepted in final quality control inspection.

The same effect can occur with interlayer films

wound up in aluminium coils to protect the

aluminium layers from each other. As a result of

the winding pressure, marks can be left.

Fish-eye mark in an aluminium sheet

Labeling films and special laminating film are

printed with sophisticated motifs. The fish-eyes

give rise to blank unprinted dots, which show up

particularly in large plain-coloured areas. In

addition, in the laminating process, the fish-eyes

can be pressed into the film. This results in

indentations that are many times larger and

therefore much easier to see that the fish-eyes

that produced them. In the subsequent printing

operation, no link is deposited in these

indentations and once again, there is a “halo”

around the fish-eye. See figure 4.

Figure 4. Black fish-eye with halo in a filmlaminated to aluminium

PE Laminating films are bonded to other materials

(e.g. PET, PP, PA, aluminium) with adhesive. If

there are fish-eyes present in the film, a “halo” is

again formed around the fish-eye, rather like an

air-filled bubble, which is far larger than its origin

and therefore much easier to detect as a flaw.

The most critical flaws are brownish or black fish-

eyes from extruder deposits, which are

interpreted as contamination. Such defects are

absolutely impermissible in the pharmaceutical

and food packaging industries. In film composites

with aluminium foil, large fish-eyes can even

impair barrier properties in the worst case

scenario.

Film Inspection

Modern-day inspection systems have a data rate

of up to 160MHz per camera (see Figure 5)



45


because of the “embedded PC” concept. This

concept permits the storage and transfer of all

measurement data via the Ethernet to a server.

According to the application, CCF line cameras

with 2,048, 4,096, 6,144 or 8,192 pixels can be

used. These achieve image acquisitions rates

ranging from 72,000/s at 2,048 pixels to

18,000/s at 8,192 pixels. So even at very high

web speeds, high resolution in the web direction

is obtained. Through the use of special lenses

and the further development of CCF sensors, the

reproduction quality of long CCD lines (e.g. 8,192

pixels) is just as sensitive as for shorter CCD lines

(e.g. 2,048 pixels). This means equally good

inspection results for considerably lower

investment costs.

Figure 5. Inspection system for a blown film line

A simple example will serve to illustrate the

advantages of using long CCD sensors. A blown

film line with a width of 2,600mm and maximum

web speed of 120mm/min is to be inspected with

a resolution of 200μm in both the web travel and

transverse directions. To achieve this resolution,

either four cameras with 4,096 pixels each or two

cameras with 8,192 pixel cameras, a better

price/performance ratio is obtained with equally

good inspection results because of the lower

purchase, maintenance and operating costs.

The systems detect and distinguish defects such

as fish-eyes, gel particles, scorch marks, black

specs, streaks, lines and insects. Depending on

its configuration, the inspection system can warn

the operator of critical individual defects (e.g. a

fly), defect trends (e.g. more than 10 gel particles

in a diameter between 200 and 300 m/m2) or

film rolls that are off-spec. Online, production

trends can be mapped over extended periods of

time, e.g. the last twelve hours. Offline, whole

runs can be compared and analysed in order to

assess, for example, the fish-eye count obtained

with different raw material batches on specific

extruders. See Figure 6.

Figure 6. Fish-eye count plotted against time

Self-learning Systems

By using the so-called easy-teach-in-function, the

operator can identify defects with the aid of

defect pictures and sort them into classes. The

classifier then automatically specifies the

inspection parameters for the individual defects.

Since these systems work with fuzzy algorithms,

they are able, for example, to differentiate flies

from black specs. This differentiation is crucially

important, since the cause of the defect may lie

in either the clean room environment or the

production process. Similarly, fluff attracted by

static charges is classified as such and therefore

not identified as a defect. See Figure 7.

Figure 7. Topographical representation (rollingmap) of the fish-eyes with photos of defects

Lighting Technology

The use of the right lighting technology is vitally

important for film inspection. The standard

lighting normally comprises fast-pulse fluorescent

tubes. But fibre-optic or LED lighting is also

employed. The lighting may be used as reflected

or transmitted light. If possible, transmitted light is

preferred because it enables both sides of the

film to be inspected. On the other hand, physical

irregularities, such as scratches, in opaque

surfaces can be more reliably detected in

reflected light. Another bonus of film surface

inspection is that the absolute and relative opacity

of transparent and translucent materials can be

determined.

Integrated QualityConcept

For quality control of PE films, even today, film

samples are still sometimes taken from the end

of the roll and visually inspected by employees.

The results of such an inspection are very

subjective and relate to only a tiny product

quantity. In other words, they are not statistically

meaningful. Counting the fish-eyes is a more

objective method but very time-consuming. But

here again, only a small random sample is taken

and the assessment of fish-eyes is also

subjective. Counting the fish-eyes on the running

machine by manual assessment is even less

objective because of the film movement. In the

random sample inspection at the end of the roll,

defects are not identified until some hours after

production. If the film is faulty, considerable

amounts of material are wasted in this way and

production times are squandered.

To ensure continuous monitoring of the

production process, the subjective assessment of

quality must be replaced by an objective method.

For this purpose surface inspection systems like

the FSP600 film quality inspection system from

OCS GmbH, Witten, Germany, can be used. At

Orbita-Film GmbH, Weißandt-Gölzau, Germany,

several such inspection systems have been

installed since 1994. Some systems operate with

one camera and scan widths of 300mm or

700mm. One system is equipped with three

cameras and monitors a film width of 3,000mm.

The systems operate in transmitted light for

transparent, translucent and opaque films up to a

certain degree of opacity.

Most equipment does not inspect the whole film

width but only a section. With this philosophy,

only the homogeneously distributed defects are

statistically detected. Depending on the film

width, 30 to 70% of the entire film width is

scanned in contrast to the maximum of 0.005%

with manual inspection.

In transmitted light, only the optically effective

surface of the fish-eyes in the plane of the film is


biennial 07-08



detected. The fish-eyes that are actually

detrimental, i.e. those which protrude significantly

above the film surface, are far fewer in number

than the measured and displayed fish-eye count.

Because of the difficulty of picking out these

“projecting” fish-eyes from the rest, the total fish-

eye count is generally recognised as an index for

the level of fish-eyes. The principal advantages of

these systems are objective, reproducible

inspection of surface quality and the possibility of

reacting immediately to changes in the fish-eye

level.

The systems are integrated in the company's

internal network. With each roll change, the

inspection data for the particular roll are

automatically stored on an internal server by roll

number and production data.

Application Examples

An example of the successful use of fibre-optic

lighting by Orbita is the inspection of black and

white surface protection films for stainless steel

in transmitted light. Each fish-eye causes an

optical dint in the stainless steel. This

phenomenon is intensified by a thermoforming

process. Because of its high opacity, the film is

very difficult to inspect in transmitted light but

double-sided inspection in reflected light is very

costly and technically complex to achieve.

Inspection systems with a camera are used in the

blown film lines. Only a section of the films are

inspected with resolutions up to 100μm. This

statistically monitoring is sufficient to guarantee

fish-eye-free film quality.

The cast film lines for self-adhesive film with

widths of up to 2,600mm are 100% inspected. In

this case, a very high resolution is achieved to

detect even the smallest defect. The 100%

inspection also enables optimum setting of both

the extruder and the die.

In the adhesive coating zone, Orbita also monitors

the complete web. Here a wide variety of defects

in the film are detected as defects of adhesive

application. In this way, the coating process is

optimised and absolute quality control achieved.

Conclusion

The use of online inspection systems for surface

inspection of PE films has proved successful in

practice and permitted faster, more efficient

detection of surface defects in recent years. As a

result, it has been possible to reduce the number

of rejects and complaints. With these systems, it

is possible to meet continually increasing product

quality requirements, while ensuring efficient

production.

About the Authors

Dipl-Phys. Gerd Finn, born 1943, is Quality

Control Manager at Orbita-Film GmbH, Weißandt-

Gölzau

Dipl-Oec. Oliver Hissmann, born in 1970, is Sales

Manager at OCS Optical Control Systems, Witten

Poli-Film Group

As a subsidiary of the globally active Poli-Film

Group, Orbita-Film GmbH is a leading German

manufacture of polyethylene films. Films ranging

in thickness from 7 to 500μm are produced in

widths from 50 - 18mm at this manufacturing

facility, which has a built area covering 51,000m2

and total area of 210,000m2. The company's site

at Weißandt-Gölzau is home not only to Orbita-

Film but also to its sister companies Orbita-Cast

and Poli-Coat, which offer a similarly wide range

of products. The films are used in the packaging,

construction, agricultural and horticultural sectors

as well as in industry and the retails trade.

At Orbita-Film, some 50 blown film machines are

installed in total. At Orbita-Cast (stretch film

producer) and Poli-Coat (manufacturer of surface

protection films), the products are extruded using

the cast film method. www.orbita-film.de

A full copy of the paper is available on

request by quoting OCS005�

Evie has grownconsiderably since her firstphoto début in RheoTalk(January - April 07 issue).

She turned 6 months on April 15 and is nearly

full grown at just under 17 kg in weight, which is

still a long way from Mal's weight of 43 kgs. Mal

celebrated his 11th birthday on March 19 and is

finding that keeping up with a young Border

Collie is challenging. Mal has the strength to play

for a long time - but Evie certainly has the turn of

speed when needed.

Being at work for them is part of their daily

routine - as soon as the car keys are picked up

they are at the door and ready to leave - this is

regardless of whether it is time to come to work

or time to leave. A trip in the car anywhere is

always a happy outing for them both.�

news & views

Staff Update


47

news & views

Customer Installation

polymer industries

Plantic Technologies Ltd inAltona Victoria recentlypurchased a HAAKE PolyLabwith rheology dies.

The system that was purchased included the

HAAKE Rheocord torque rheometer drive unit with

mixer (with Banbury, sigma and roller rotors) and

single screw extruder (with an adjustable lip film

die, and slit and capillary rheology dies).

Plantic Technologies Limited is a world leading

innovator in bioplastics, with a track record of

science and industry awards, an international

network of corporate customers and distributors,

and a growing list of premium quality

multinational research and development partners.

Plantic Technologies is based in Australia, where

its head office, principal manufacturing and R&D

facility is located. The company also has sales

offices in German and the United Kingdom, and

employs approximately 40 people internationally.

A New Approach to Plastic

Plantic has achieved a unique place in the world

market for bioplastics through proprietary

technology that delivers a completely

biodegradable and organic alternative to

conventional plastics based on corn; which is not

genetically modified. The entire process integrates

the science of organic innovation with commercial

and industrial productivity in a new way. The

result is both a broad range of immediate

performance and cost advantages, and long-term

environmental and sustainability benefits.

Plantic's single-minded commitment is to provide

bioresponsible materials solutions for the world

market that deliver all the functionality of

conventional petrochemically derived plastics in

an economical and ecosensitive way.

The torque rheometer will be used to measure

the relative processing properties of various

thermoplastic starch (TPS) blends and resins in

R&D. The sheet die will be used to mimic larger

scale processes, to optimise screw

configuration & processing conditions for the

different TPS grades in R&D. The rheology (slit

and capillary) dies will help to characterise the

TPS grades for efficient processing.�

Rod capillary die at Plantic Technologies isused for rheological characterisation of polymericmaterials.

biennial 07-08


This article discusses defectsthat may possibly occur duringproduction of film oncalendaring equipment as wellas the sources of black spots,their detection, evaluation andpossible means of prevention.

The article was written by Andreas Schnabel

(works in the filed of metrology and process

technology at Klochner Pentaplast GmbH & Co

KG, Montabaur, Germany; and Oliver Hissmann

(employed by OCS GmbH, Witten, Germany).

Pharmaceutical products are packaged in plastic

blister packs around the world. Every customer

expects that the film used satisfies increasingly

stringent requirements. In addition to economy,

hygiene, protection in different climates and

atmospheres, this also means a guarantee of

maximum safety for the product packaged in

compliance with new and ever more demanding

requirements.

The monolayer film that is produced primarily on

calendaring equipment is converted into blister

packs or serves as the substrate for high-quality

coatings and laminates. These calendered

monolayer films are plasticizer-free rigid PVC

films that are manufactured in various

thicknesses and colours. They can be classified

into three product groups: With their good

thermoforming characteristics and their good

chemical resistance, homopolymer films are well-

suited for production of standard blister packs.

For demanding blister geometries or maximum

processing speeds, copolymer and high

copolymer films offer greatly improved flow

characteristics.

A reprint of the paper from Kunstoffe

international 7/2007, is available on

request from Rheology Solutions by quoting

OCS-007�

news & views

High-Quality Pharmaceutical Film – Customer story Klockner Pentaplast, Germany.

polymer industries


When things in your life seemalmost too much to handle,when 24 hours in a day arenot enough, remember themayonnaise jar and the 2 cups of coffee.

A professor stood before his philosophy class and

had some items in front of him. When the class

began, he wordlessly picked up a very large and

empty mayonnaise jar and proceeded to fill it with

golf balls. He then asked the students if the jar

was full. They agreed that it was.

The professor then picked up a box of small

pebbles and poured them into the jar. He shook

the jar lightly. The pebbles rolled into the open

areas between the golf balls. He then asked the

students again if the jar was full. They agreed that

it was.

The professor next picked up a box of sand and

poured it into the jar. Of course, the sand filled up

everything else. He asked once more if the jar

was full. The students all responded with a

unanimous "YES".

The professor then produced two cups of coffee

from under the table and poured the entire

contents into the jar effectively filling the empty

space between the sand. The students laughed.

"Now", said the professor as the laughter

subsided, "I want you to recognise that this jar

represents your life. The golf balls are the

important things--your family, your children, your

health, your friends and your favourite passions -

and if everything else was lost and only they

remained, your life would still be full".

"The pebbles are the other things that matter, like

your job, your house and your car".

"The sand is everything else - the small stuff".

"If you put the sand into the jar first" he

continued, "there is no room for the pebbles or

the golf balls. The same goes for life. If you spend

all your time and energy on the small stuff you

will never have room for the things that are

important to you".

"Pay attention to the things that are critical to

your happiness. Play with your children, look after

your health, take your spouse out to dinner. Play

another 18 holes. There will always be time to

clean the house and fix the car. Take care of the

golf balls first--the things that really matter. Set

your priorities. The rest is just sand".

One of the students raised her hand and inquired

what the coffee represented. The professor

smiled, "I'm glad you asked". "It just goes to

show you that no matter how full your life may

seem, there's always room for a couple of cups

of coffee with a friend".�

news & views

The Mayonnaise Jar& Two Cups of Coffee

all industries


49

Thermo Fisher Scientificoffers a comprehensive rangeof material characterisationproducts that analyse andprocess material forrheological and thermalproperties.

These instruments analyse and measure viscosity,

elasticity, processability and temperature-related

mechanical changes of plastics, foods, adhesives,

coatings, and a wide variety of liquids or solids.

A brief overview of innovative solutions across a

number of industries for R&D, Process, and QC

applications follows:

Ceramics

Rheological measurement data relating to

dispersability and flow characteristics of ceramic

injection moulding compounds and pastes provide

the ceramics industry with valuable information to

optimise products. To do this, a flexible, modular

rheometer platform is needed to evaluate product

processes used for manufacturing ceramics and

suspensions for porcelain and/or ceramics.

Food

Innovative recipe development, comprehensive

reproduction simulation, and reliable quality

assurance require a powerful rheometer platform

in conjunction with pioneering measurement

extruders and mixers.

Paints, Dyes & Powder Coatings

Innovative paints and dyes demand extensive and

precise rheological measurements. This begins

with reliable quality control of raw materials and

products and continues in the research and

development of new formulations. Stability, time

dependence, process characteristics when

spraying or coating, and structural properties of

these products must be derived in the early

stages of development.

Petrochemistry

In the petrochemical industry simulation of pump

characteristics and measurements for oils and

drilling fluids under pressure is vital.

Pharmaceutical & Cosmetics

Understanding the processability, consistency,

time- and temperaturedependent properties of

raw materials and end products in order to

develop innovative and successful products is

critical.

Polymers

Processing-related data such as melt

characteristics, the effect of additives,

temperature, shear stability and dynamic viscosity

during shear are of great significance to the

development of innovative polymers. Process

simulation in compounding and extrusion of rods,

profiles or films, combined with rheological or

visual measurements, help the plastics industry to

optimise procedural parameters, to create

inspection bodies for tests or to perform quality

checks at incoming and outgoing goods for

viscosity, dispersion or plastifying characteristics.

Rubber

The impact of carbon black on the cross-linking

characteristics of a rubber compound and the

dispersion or vulcanisation and flow properties of

rubber are key to product quality. Furthermore,

optimised end product mixing times are important

not only to ensure efficient use of production

plants, but also to successfully launch competitive

products onto the market.

Further information on your application

requirements is available by requesting

detailed information specific to your

industry.�

industry overview

Material Characterisation Solutions

polymer industries


food industries



• news & views

Service Department Update

Recently, our service engineer

Richard Donaldson has been

travelled around Australia

conducting installations

and calibrations on a variety

of the HAAKE Viscometers

and Rheometers.

Additionally, there were installations during this

period for Optical Control Systems products.

During an eight week period he has carried out

calibrations on the HAAKE Viscotester VT550,

HAAKE RheoStress, HAAKE RheoStress 600,

HAAKE RheoStress 100 and HAAKE RotoVisco

RV1. A total of 28 viscometers and rheometers

have now been calibrated across, Queensland,

Victoria, South Australia, Western Australia and

New South Wales. His frequent flyer miles by now

will be adding up to a sizable amount and well

deserved.

Just to ensure that he was kept fully occupied, he

has also been involved in the installation of three

HAAKE PolyLab's –one in Victoria and two in

Queensland, and one PRISM EuroLab 16 mm twin

screw extruder in Victoria.

But the installations didn’t stop with the

rheological instruments; there were also a

number of Optical Control Systems (OCS) units

installed during this same eight week period both

into Victoria into separate companies. The

systems installed were the OCS Surface

Inspection system for the laboratory - FSA100,

and the modular surface inspection system for

in use in production - FSP600.

Calibration overview The ability of a measurement device to accurately

measure a physical quantity changes with a

number of factors. Time in service, temperature,

humidity, environmental exposure, and abuse can

all affect your measurement accuracy of your

instrument.

Calibration quantifies this change in measurement

accuracy and, when required, adjusts the device's

measurement capability to decrease error.

Whether your calibration needs are driven by

ISO-9000 requirements, by company mandates, or

by Good Laboratory Practice, Rheology Solutions

Pty Ltd can tailor our service to suit your needs.

all industries Why Re-Calibrate? The accuracy of the electronic components used

in all instruments drifts over time. The effects of

time in service as well as environmental conditions

add to this drift. As time progresses, changes in

component values cause greater uncertainty in

your measurements. At some point in time, the

drift causes the instrument's uncertainty to

become undefined, meaning the manufacturer can

no longer predict the uncertainty and guarantee

measurement results. To resolve this issue

instruments must be calibrated at regular intervals

as defined by the manufacturer.

Richard Donaldson, Service Engineer

Calibration is the comparison of an instrument's

performance to a standard of known accuracy.

The result of a calibration may be documentation

showing the deviation of a measurement from the

known standard or it may also include adjusting

the instrument's measurement capability to

improve measurement accuracy.

The goal of calibration is to quantify and improve

the measurement accuracy of your instrument.

The benefits of maintaining properly calibrated

equipment include:

• Reduced measurement errors

• Consistency between measurements

• Increases in production yields

• Assurance you are making accurate

measurements

We recommend that you periodically calibrate your

hardware to ensure measurement accuracy and to

keep your devices operating in peak precision.�

If you have any queries regarding the timing

or arranging for your HAAKE viscometer or

rheometer to be calibrated, contact Jackie by

email [email protected].

• news & views

Staff Update

At last there has been some well needed rain in

Bacchus Marsh, not enough to do more than just

wet the ground, but every drop counts.

With the colder weather now approaching, both

Mal & Evie spend more time in the office keeping

warm.

A game of chase in the office is often on the cards

– it certainly breaks the routine of the day for

them, and also for all of us. When the game is

over, they are happy to lie back and catch up on a

bit of shut eye. It doesn’t seem to matter to them

where they lay down, they are happy for us to walk

around them or over them – once they are settled

they are down for the count – happy to rest and

recuperate.�

all industries

Mal & Evie just getting ready to start a game in the

office - it starts with a gentle torment and then

fires up to tumbling and chasing

biennial 07-08


• feature article

Online Close-Loop Monitors Four Cast Film Extruders During Production

polymer industries

Applying the close-loop

concept, a raw material

producer’s off-line laboratory

can perform continuous online

metering, making optimisation

of the process achievable.

Following the principle of the close-loop concept,

the conventional off-line laboratory is connected

to the production process right on line, so the

producer can control process and quality.

Small quantities of raw material are taken during

processing, to obtain representative information

to oversee the entire production. Before the

introduction of the close-loop concept, data on

the quality of production could take an entire

shift before it was available.

Online quality controlOnline quality control comprises two areas:

measurement of the granules and measurement

of the extruded cast or blown flim.

Measuring the granules produces information on

LAB colour value, Melt Index (MI), pellet size

distribution (pellet size and shape distribution

Online close-loop monitoring four

production lines (cast film extruders).

systems) as well as dust/abrasion and

contamination (pellet scan systems).

Yet, measuring the extruded film online makes

statements on bittiness (gel count), additive

content and physical properties (IR spectroscopy),

brilliance (glossmeter) and/or the value of turbidity

(hazemeter).

Online pellet analysisConducting pellet analysis online, a sampler

withdraws the granules from the flow of

continued on page 52�


51

biennial 07-08


giving the operator parameters crucial for reactor

control (Fig. 1). This is done by continuously taking

specimens out of the granule flow, heating them

up and submitting them to high pressure to

compress them carefully. This process causes only

relatively slight changes in molecule structure,

reaching reproducible accuracies of 0.5% which is

better than off-line laboratory equipment. At the

same time, metering without screw shear does not

change the polymer structure and maintains better

correlation with the ASTM/ISO methods.

Measuring extruded sheets online The analysis methods mentioned above, however,

fails to provide any information on the granules’

speck content and their actual quality. To enable

this measurement, a narrow film is extruded, in

parallel, while regular extrusion takes place, and

its speck content determined continuously. It is of

major significance here, to seize the utmost

number of small specimens, in order to safeguard

continuous process control. A gel shower, for

instance, may last five to 10 minutes, then

disappear. Therefore, it is recommended that

cycles should comprise at least 50 specimens

per hour.

Following cast or blown film extrusion, the sheet

passes below a line scan camera and is wound

without a tube on a pneumatic mandrel (Fig. 2).

The winding unit is suspended at one side (godet

structure) and comprises several servo drives.

These provide for the film guidance to be

absolutely stable and they avoid fluttering.

Sheet guidance is just as essential as a clean

environment (up to a clean room), since granules

OnLine Close-Loop Monitors� continued from page 51

production. The system then automatically takes

them to the measuring system, examines and

sorts them. Those granules that meet the specified

demands, are returned to the process.

For the purpose of measuring the colour, the

pellets are transported into a cuvette, where LAB

values, yellowness index and several other colour

values are determined.

The Online Pellet Scan System, on a vibrating

table or swivel plate, passes the transparent or

opaque granules below a colour matrix camera.

The pellets are examined as to colour soiling or

foreign particles, and rejected if necessary.

The Pellet Shape and Shape Distribution analysis

examines the granules during free fall. It uses a

line scan camera to check granule size

distribution, sphericity, angel hair, dust/wear,

doubles and triples.

All of these systems mentioned can be connected

right in series and be controlled by an integrated

software solution, using an interface such as

Modbus; they are linked to the Production Data

Acquisition (PDA) system. In case of deviation, the

operator is alerted automatically.

At-line rheologyThe rheometer of the newly patented OCS

technology is a hybrid between measurement of

granules and extruded films. Highly precise off-line

laboratory measurement following ASTM 1283

and ISO 1133 is carried out continuously as well

as right “at-line” next to the production facility,

Fig. 2. Online Close-Loop concept

(blow moulding plant)

for applications such as high-voltage cables have

resolutions of down to 5 μm, which must be

inspected. For downmarket raw materials such

as polyethylene, standard resolutions are 50μm

to 25μm.

The process has been optimised for raw material

control and it works almost autonomously. Other

measurements, e.g. of haze according to ASTM

1003, of additive density and composition (IR

spectroscopy), of brilliance or thickness can easily

be integrated into the winding unit and software.

The Web Browser supports remote control and

maintenance of the plant. The systems are

inter-linked internally with an OPC server, and

connected externally to the customer’s PDA

system.

Quality concept fora polymer plantA world-scale raw material supplier has integrated

into their polymer plant a standardised online

close-loop concept. In order to minimise problems

resulting from granule transport, such as

generation of dust or abrasion, a container was

placed right next to the extruders, suited to

perform clean room measurements. (Fig. 3).

Analytical software is integrated into the PDA

system with a Modbus, Profibus, Ethernet OPC

interface etc. enabling the operator to control the

plant from the control room. From here, the raw

material specimens can be automatically allocated

to the individual measuring systems.

Pellet analysis systems sort out contaminated

granules, camera systems evaluate speck content,

IR spectroscopy determines additive content and

composition. In case of a problem, the plant


Fig. 1. At-Line rheometer

OnLine Close-Loop Monitors� continued from page 52

operator is alerted immediately and the

contaminated material is diverted into a different

silo. Simultaneously, the system significantly

reduces changeover times, anticipates

maintenance and optimises maintenance intervals.

Inspection of extrudedfilms during productionProducers of high-quality sheets today use sheet

inspection systems, which monitor 100% of

outputs. These systems detect flaws such as

specks, brands, fish eyes, streaks, flow lines or

insects, mark them and alert the operator

immediately. This monitors the process itself,

the raw material and the final product.

The system raises an alarm in case it detects e.g.

a critical individual flaw (a fly for instance), flaw

trends (more than 10 gels of 200 to 300 mm

diameter per square meter), or if there is a roll or

use error, that is not specified. The data is stored

in the system and can be accessed at any time.

Production tendencies can be presented online

for relatively long periods of time (12 hours). In an

off-line mode, entire campaigns can be compared

to each other and evaluated, enabling the

engineer, e.g. to evaluate the bittiness of a raw

material charge applied on a certain extruder.

The system provides protocols of roll pressures,

tailored to the individual manufacturer’s

requirements.

Inspection technologyToday’s inspection systems reach pixel frequen-

cies up to 160 MHz per camera, being processed

by an Embedded PC right beside the camera.

A single camera can buffer up to 1,800 photos of

flaws a second. All measured data is transmitted,

via Ethernet, to a server, visualised and stored.

Analysis is conducted in real time, alerting the

operators, in case of irregularities.

Subject to the individual application, CCD line

cameras can be used with either 2,048; 4,096;

6,144 or 8,192 pixels. The scan rates achieved

range from 72,000 per second with 2,048 pixels,

up to 18,000 per second with 8,192 pixels.

This way, solutions are high in web direction, even

with very high web speeds. While using special

objectives and technological development in CCD

sensors, the image quality of long CCD lines (e.g.

8,192 pixels) today is reproduced just as

sensitively as with short CCD lines (e.g. 2,048

pixels). For the sheet manufacturer, this means

that findings from inspections remain good while

investment costs are significantly lower, since the

price of a CCD camera for long lines is only

slightly higher.

With standard sheet processing, control is

performed on speeds achieving up to 600 or even

800 m/min (roll slitting machine, coating) and

widths reaching up to 10 m (biaxial stretching unit)

(Fig. 4). Solution is 50 μm, in optical films, while

ranging between 200 and 300 μm in thermo

formed high-barrier films. In laminated sheets, the

value is between 100 and 200 μm, while ranging

from 300 to 400 μm in diaper films. Generally, the

solution is determined by the end customers’

specifications as well as the production process.

Examples of practical application While producing surface-protecting films, the

causes of specks were examined. Having

evaluated the situations of alert, engineers found

Fig. 3.Container designed for online

Close-Loop measuring

out the following: 40% of all specks are caused by

dust and abrasions during raw material transport.

This comprises silos and silo tankers, as well as

pellet conveying systems in the factory to transport

the material from the silo to the extruder. Specks

caused by the raw material itself, e.g. by

inter-linkage or insufficient shearing, make up

25%. The extrusion plant causes 20% of the

specks, due to dissatisfactory screw geometry or

dead zones, while 15% are attributed to the

production process, for instance screen changes

or wrong temperature parameters.

An enterprise producing sanitary film also

compounds the blends it requires. In the

compounding sector, each charge is submitted to

continuous examination on a laboratory extruder

that includes units designed for winding, as well

as gel count. Using an interface, the data is

transmitted to the PDA system. The information

serves as a basis for producing the film according

to the customer’s quality specifications. On the

cast film extruder, 100% film inspection is carried

out, while the film is 2,000 mm wide and speed is

100 m/min. The data obtained from the two

inspection systems is evaluated by the same

off-line analysis software, which also relates them

to each other.

Fig. 4. System to inspect films in a stretching

unit online

Conclusion Close-Loop today is a standard concept applied in

raw material production. Not only does it monitor

qualities; it controls and optimises the production

process.

Author. Oliver Hissmann, DIPL.-PEC., MBA. Sales

Manger, Optical Control Systems, Witten,

Germany.

A copy of this article is available on request by

quoting OCS-008.


53

• rheotalk special issue

Food Industry feature

Rheology Solutions offer

material characterisation

solutions to measure, monitor

and provide reproducible data

for quality control, development

and production applications

that will improve performance

within the food industries.

Services An extensive range of technical articles have been

produced specific to the challenges found within

the food industry, these include:

• Food and Beverage Material Characterisation

- Introduction to the influences of rheological

and process parameters. Rheo 025TP

• Comparison of Rheological Techniques for

the Characterisation of Semi-Solid Foods.

(Rheo 027TP)

• Application of Liquid and Solid Rheological

Technologies to the Textural Characterisation

of Semi-Solid Foods. (Rheo049)

• QC Measurements for Liquid Food Products

and Packaging. (Rheo051)

• Tim's Top Tips - Explanation & Evaluation

of Mouthfeel. (Rheo253)


of Shelf Life. (Rheo254)


of Processability. (Rheo255)


of Cohesiveness, Cohesion Strength and

Cohesive Quality. (Rheo256)

• Tim’s Top Tips – How to Measure Flow

& Viscosity. (Rheo358)

• Tim’s Top Tips – How to Measure Thixotropy.

(Rheo360)

• Tim’s Top Tips – How to Measure Yield Stress.

(Rheo362)

Additionally, an information kit – Rheology

Solutions for the Food Industry is available. Copies

of the technical papers and the solutions kit are

available on request from Rheology Solutions.

special issue

Products Rheological parameters are reliable pointers for

food performance and are critical factors for

processability and product quality.

Measuring these parameters will improve process

and product performance within the food

industries.

There are a range of instruments and measure-

ments that can be used to quantify rheology

related challenges (processes or consumption)

some of which may be described by the following

terms:

• adhesion • build

• cohesion • cover

• crispiness • elasticity

• mouthfeel • spread

• stringiness • viscosity

• and many more

Rheology Solutions will be exhibiting at Foopro

(stand no. 6084) in Sydney in July 2008, and

following is an overview of the products and

services that will be available at the stand and

fully operational during the exhibition.

food industries

biennial 07-08


• company news

Bacchus Marsh – Home of a new high technology facility

all industriesMr Dennis Silvers of CSIRO stated that: “The

initiative brought to the table a viable offer that

otherwise would not have occurred, which will

result in about $2 million in royalties and a small

manufacturing and distribution facility to be built in

Bacchus Marsh, a town west of Melbourne, that

will employ between 15 and 20 people and bring

in more than $16 million to the local community”.

“The Moorabool Shire Council and the Victorian

State Government have given much support to the

project in terms of assisting to finalise the

agreement with CSIRO”, said Mr Griffin. “We will

be seeking on-going financial assistance from the

Local and Federal Government as we progress the

development of the instrument. This project will

inject significant revenues into the region and will

also increase employment.”

What is the On-Line

Rheometer?

Developed by CSIRO Industrial Physics, this novel

instrument delivers fast, accurate results with a

single measurement over a range of frequencies.

The OLR reduces wastage, saving time and money

with potential environmental benefits. Its simple

design and stainless steel construction makes it

easy to use and clean.

To date, when more detailed knowledge of the

viscoelastic properties of the fluid is required test

volumes must be removed from the process

stream and measured using an off-line laboratory

rheometer. This is a time consuming procedure

that may require the process line to be shut down

until the results are available to confirm, or

otherwise, the quality of the product. Alternatively,

the process flow may continue with the potential

loss of product. In some cases, the volume of lost

product could be large and this could be

particularly problematic when processing high

value materials (such as pharmaceuticals),

products that cannot be reprocessed or products

that incur a disposal cost (such as, an environ-

mental levy). Thus a genuine process control

rheometer which can be operated in an in-line or

on-line configuration and measure the viscoelastic

properties of a process fluid in real time, has the

potential to improve product quality and reduce

processing costs.

The CSIRO designed On-Line Rheometer (OLR)

is such an instrument, and uses a patented

multi-frequency squeezing flow technique that

allows the viscoelastic flow properties of a

material to be measured in a very short time.

The measured rheological parameters can be

used as process controls in a feedback system

to control the process, and hence the quality,

of the final product.�

Above: (from left) Bruce Fox (CSIRO), Pat Griffin

(Rheology Solutions), Dennis Silvers (CSIRO),

and Jennifer Labourne (Rheology Solutions)

at the signing of the License Agreement.

Left: Mr Pat Griffin (right), Managing Director of

Rheology Solutions Pty Ltd and Mr Bruce Fox (left)

of CSIRO with the phototype of the New On-Line

Rheometer.

Rheology Solutions based in

Bacchus Marsh Victoria has

signed a license agreement

with CSIRO to develop and

manufacture a novel process

control instrument known as

the On-Line Rheometer (OLR).

Mr Pat Griffin, Managing Director of Rheology

Solutions announced that after a long period of

discussion and negotiation, agreement with CSIRO

had been reached for taking on the license for the

OLR. CSIRO initially released an Expression of

Interest (EOI) in early 2007 to seven international

companies that were known to have expertise in

the appropriate markets, and we are pleased to be

the successful partner.

The OLR will be developed by Rheology Solutions

and will be taken to the world market. A world

class manufacturing facility will be established in

Bacchus Marsh employing 20 highly skilled

technical and engineering staff adding to the

region’s skill base. This is a significant develop-

ment for the region with the establishment of a

purpose built manufacturing facility.


55

Product News& Industry Applications

� Product Focus

• HAAKE MARS RheoScope Module ................................................................ 61 • • NESLAB ThermoFlex Recirculating Chillers ................................................ 64 • • New Heating Circulator ................................................................................ 60 • • New Cooling Circulator ................................................................................ 59 • • Disposable Plate/Plate – Measuring Geometry for the

Controlled Temperature Chamber (CTC) ........................................................ 72 • • Marimex ViscoScope In Line Torsional Viscometer ........................................ 73 • • • • • Optical Analysis and Rheology ................................................................ 71 • • • • • Schleibinger presents a New probe for SCC Mortar for the Viskomat NT ........ 67 •• Cooling Recirculators ................................................................................ 76 •• HAAKE MiniLab Compounder & Reactor ........................................................ 81 • • Heating Recirculators ................................................................................ 74 • • High Speed Pellet Scan System throughput up to 250kg / hr ........................ 77 • • Higher Instrument Precision & Reliable Quality Control

– Hand Held Viscometer – HAAKE Viscotester 1 Plus & 2 Plus ........................ 80 • • Nano-Composites ........................................................................................ 74 • • NanoLab Compounder Package ................................................................ 80 • • • • • New NESLAB ThermoFlex 2500 Recirculating Chiller ................................ 75 • • Twin-Screw Extrusion at a Lab Scale ........................................................ 76 • • HAAKE MARS with CTC ................................................................................ 67 • • HAAKE PolyLab QC ................................................................................ 83 • • HAAKE RheoStress 6000 – The Universal Rheometer ................................ 87 • • Heating & Cooling Recirculators ................................................................ 63 • • The OP5 Online Rheometer ........................................................................ 86 • • New Device for Rheological Measurements.

A Measuring Device for Special Mortars ........................................................ 91 •• New Product – Circulator to Heat &

Cool External Applications from -10ºC to 80ºC................................................ 68 • • Rheological Measurement with Optical Analysis

– High Temperature Version Extends Testing up to 300ºC ........................ 69 • • • • • • The Industry Choice for Viscosity Measurements of

Mineral Slurries and Suspensions HAAKE Viscotester 550 ........................ 92 •• Extended Product Range - Recirculating Chillers ........................................ 101 • • Using a Refrigerated Circulator with a Rotary Evaporator

– Environmentally Friendly Solution................................................................ 98 •

� Industry Applications

• Continuous Granulation for the Pharmaceutical Industry ................................ 65 • • CR-Mode – Low Shear Rates ........................................................................ 70 • • Tim’s Top Tips – How to Measure Series ................................................ 59 •

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� Industry Applications

• Food Industry Feature & Product Focus- Extensional Rheometer

HAAKE CaBER1 ........................................................................................ 95 • • Food Industry Feature & Product Focus

- Heating Bath Circulator Thermo HeatTech 26L ........................................ 96 • • Food Industry Feature & Product Focus

- Process Viscometer Marimex ViscoScope ................................................ 94 • • Food Industry Feature & Product Focus

- Rotational Viscometer HAAKE Viscotester 6L plus. ........................................ 94 • • Food Industry Feature & Product Focus

- Refrigerated Bath Circulator Thermo CoolTech 320 ................................ 96 • • Food Industry Feature & Product Focus

- Recirculating Chiller NESLAB ThermoFlex 900 ........................................ 95 • • Polymer Industry Feature & Product Focus

- Modular Torque Rheometer with Measuring Mixer ........................................ 103 • • Polymer Industry Feature & Product Focus

- Modular Torque Rheometer with Twin-Screw Extruders ................................ 103 •• Polymer Industry Feature & Product Focus

- Modular Torque Rheometer with Single-Screw Extruder................................ 104 •• Polymer Industry Feature & Product Focus

- Modular Twin-Screw Extruder PRISM EuroLab ........................................ 104 •• Polymer Industry Feature & Product Focus – Pellet Scanner PS-25C................ 105 •• Polymer Industry Feature & Product Focus – Web Inspection System FSP600 105 •

� Product News

• Accessories for HAAKE MARS –

- Cone/Plate-Exchangeable Measuring Geometries ........................................ 62 • - Measuring Cell for Rheology of Building Materials ........................................ 62 • - Sample Loading Tool ................................................................................ 61 • - Trimming Tool ........................................................................................ 62 • - Solids Clamp ........................................................................................ 62 • - CD Mode Curing Measurement. ................................................................ 78 • • - Standard Liquids. ................................................................................ 79 • - Sample Fixture for Bending & Breaking Tests ........................................ 78 • • • • - Support Fixture for the Analysis of Textile Samples. ................................ 78 • • - Tool For Checking the Optical Quality of the RheoScope Module ................ 79 • • • • • - (SER)Extensional Rheology System ........................................................ 100 • - Universal Container Holder for HAAKE MARS and RheoStress 6000. ........ 99 • • Process Viscometer – Software Options. ........................................................ 82 • • • • •


57

ALL

IND

US

TRIE

S

PO

LYM

ER

FOO

D

SU

RFA

CE

CO

ATI

NG

S

MIN

ERA

L

CH

EMIC

AL

PH

AR

MA

CEU

TIC

AL

BU

ILD

ING


� Product News

• New Product Brochure –

- HAAKE PolyLab OS Docking Station ........................................................ 71 • • - PolyLab OS Torque Rheometer RD4 Application Packages ........................ 71 • • - HAAKE PolyLab OS Open System. Measuring Mixer Extruder System

from Thermo Fisher. ................................................................................ 90 • - Micro Compounder for Small Sample Amounts ........................................ 66 • • - Sample Specimen preparation Instrument. ................................................ 66 • • - Food Industry Feature & Product Focus........................................................ 97 • - Comprehensive Material Characterisation for Polymers ................................ 97 • - Extrusion & Material Characterisation for Drug Development & Production 97 •• HAAKE Viscometers ................................................................................ 89 •• Polymer Industry Feature & Product Focus ................................................ 102 •• Accessories for HAAKE Viscotester 7Plus –

- Thermal Printer ........................................................................................ 70 • - Adapters for HAAKE Viscotester models 6 and 7 plus for measuring

range extension and sample temperature measurement (optional) ................ 99 • • Product Accessories - UV Curing Cell for an individual

arrangement of optical components ........................................................ 99 •• Bath Recirculators - NESLAB RTE & EX Series ................................................ 97 •• Product Accessories - Vane Rotors for HAAKE MARS & HAAKE

RheoStress 6000 ........................................................................................ 100 •• Product Accessories - Tribology Cell for HAAKE RheoStress 6000 ................ 100 •

biennial 07-08



59

CoolTech 3320 Specifications

Temperature Range -28°C to +100°C

Temperature Accuracy +/- .02K

Heater Capacity (230V) 2.0 kW

Cooling Capacity at 20°C 320 W

at 0°C 205 W

at -20°C 75 W

Pump Pressure (Maximum) 300 mbar

Pump Flow Rate (Maximum) 12.5 lpm

Bath Opening (W x L x D) 13cm x 10cm x 15cm

Bath Volume 4.5 L

Overall Dimensions 23cm x 46cm x 58cm

Unit Weight 29.8 kg

Order number 230V/50Hz 426-2601

CoolTech 320 Features & Benefits:

• Rapid cool down and heat up times

• Powerful pump accommodates the bath plus

connections to external applications

• Front access drain for easy cleaning

• Safety for temperature & fluid level

• CFC-free refrigeration system

CoolTech 320 Applications:

• Condensers • Rotary Evaporators

• Catalyst Reactions • Electrophoresis

• Bioreactors • Instrument Calibration

• Refractometers • Spectrophotometers

• Sample Preparation

news & views

NEW Cooling Circulator

Cool Down – Time to Temperature

Pumping Capacity

all industries

$3999

EXCLU

DING G

ST

Place your order now for despatch within 24 hours of order receipt.

Fax your purchase order to Rheology Solutions Pty Ltd on 03 5367 6477or email your purchase order to [email protected]

ORDER TODAYDELIVERY EX STOCK!

The series has now been expanded to cover

seven key industries, and each industry has a

series of three How to measure … notes for

three key characterisation techniques, which are:

• How to Measure Thixotropy

• How to Measure Yield Stress

• How to Measure Flow & Viscosity Curves

The new industry application areas now covered

are: Food; Pharmaceutical, Cosmetic & Allied

Industries; Surface Coatings; Chemical & General

Manufacturing; Building & Construction

Industries; and Polymer Industries. The series was

introduced last year with the first industry covered

by the How to measure … series was for

Mineral Slurries

Rheology Solutions is planning a series of

workshops based on the “How To Measure”

Series” - please see page 10 for more

information.�

industry applications

Tim’s Top Tips - How to Measure...

all industries

biennial 07-08


news & views

NEW Heating Circulator

Heat-Up – Time to Temperature Curve

Pumping Capacity

all industries

ORDER TODAYDELIVERY EX STOCK!

HeatTech 26L Specifications

Temperature Range Ambient +8°C to +100°C

Temperature Accuracy +/- 0.02K


Pump Pressure (Max) 300 mbar

Pump Flow Rate (Max) 12.5 lpm

Bath Opening (W x L x D) 30 x 35 x 20cm

Bath Volume 26 L

Overall Dimensions 34 x 56 x 40cm

Unit Weight 10.9 kg


HeatTech 26L Features & Benefits:

• Large bath area accommodates more samples

• Quiet system ensures pleasant environment



• Safety for temperature & fluid level


HeatTech 26L Applications:

• Fecal Coliform Testing • Enzyme Assays

• Quality Control Testing • Tissue Baths

• Instrument Calibration • Viscosity Testing

• Sample Preparation • DNA Melting Curves

$2399

EXCLU

DING G

ST


61

The HAAKE MARS is a modular hightemperature/high pressureR&D rheometer that wasdesigned for flexibility withan architecture that permitscustomer modules to beintegrated into the system.

A RheoScope Module was developed for the

HAAKE MARS system that combines high

resolution microscopy and advanced rheometery

technology. With this module the connection

between a sample’s microscopic structures and

rheological properties can be monitored

simultaneously, and the rheological and optical

data can be saved in the same file. Visible

textures and structures in solutions, suspensions,

thixotropy, emulsification, coalescence,

aggregation, gelification, dissolution and

flocculation. Together with the user-friendly

HAAKE RheoWin 3 measuring and evaluation

software, all functions of the microscope and

camera can be controlled in addition to the

rheometer. The rheological and optical data can

be monitored online during the measurement as

well as saved and exported in different formats

for further analysis.�

product news & industry applications

HAAKE MARS Rheoscope Module

Specifications

Microscope Servo motor-driven, focus and

position adjustment controlled

with software

Lenses Magnification: 5x, 10x, 20x

and 50x

Light source 150 W, 12 V, wave length

range: 380 - 750

Resolution 1 um (20x lenses)

Field depth 5 um (20x lenses)

Contrast improvement Polariser servo motor-driven

Data acquisition Maximum 15 images / second

and storage with standard image format

(eg: TIFF) or video acquisitions

with user-definable data

compression

Image analysis Option for the determination of

software the particle size and its

distribution

Measuring geometries Polished plates and cones with

different diameters

all industries

Sample loading tool for measurements

on pellets and powders using a

plate/plate- or cone/plate- measuring

geometry

In most cases rheological investigations on

polymers were performed using a rheometer with

plate/plate- or cone/plate- measuring geometry.

Too much or too little sample volume can result in

an experimental error of up to 20% for the

viscosity or the modulus.

In order to get reliable experimental data with a

high reproducibility a suitable sample preparation

is necessary, e.g. production of specimen using an

injection moulding machine. The feed material can

be modified due to the fact that the sample

preparation is carried out at the processing

temperature of the polymer.

A sample loading tool was designed for

measurements using the feed material in form of

pellets or powder. This tool consists of a forming

tool for measuring geometries with different

diameters (20, 25 and 35 mm), a tool to check the

forming as well as a set of disposable strips made

of stainless steel.

The strips have a thickness of 0.2 mm. Using a

moulding tool these strips can be shaped into

loops with diameters corresponding with the lower

plates of our cone/plate or plate/plate geometries.

Having this border around the lower plate, the

geometry can easily be filled with pellets or

powders. Afterwards, the automatic lift, controlled

by HAAKE RheoWin, will move the upper geometry

into the measuring position and the metal strip

can be opened and taken away.

This procedure leads to an optimum filling of the

geometry with a correct sample volume and no air

bubbles. � Continued on page


NEW Accessories for HAAKE MARS

all industries

HAAKE MARS Rheoscope Module

biennial 07-08


Sample loading tool for cone/plate – measuringgeometries consisting of forming tool (left), tool to check the geometry (middle) and strips out of stainless steel (in the front); measuring platecover with sample loading tool (right)

The filling procedure should be carried out at the

measuring temperature in order to eliminate a

thermal modification of the sample.

Trimming tool to remove overfilling

in a plate/plate-and cone/plate

measuring geometry

In order to get reliable measuring data with a

high reproducibility an optimised gap filling is

necessary: using an underfilling the measured

value for the viscosity is too low, whereas an

overfilling results in a too high viscosity value.

The fringe effect depends on the diameter of the

measuring geometry: the effect increases with

decreasing diameter.

For samples with a medium and higher viscosity

a special trimming tool is available as an optional

accessory to remove the overfilling.

Plate/Plate – measuring geometry with measuringplate cover (MPC) for optimized gap filling

This tool is made out of stainless steel, robust

and ergonomically designed to remove surplus

material easily and without residue.

For all plate/plate – and cone/plate – measuring

geometries measuring plate covers are available

with standard diameters of 8, 20, 35 and 60 mm.

These measuring plate covers are designed with

a plateau, in which surplus material can be

collected automatically.

Trimming tool to remove surplus material formedium and high viscous samples

New solids clamps for measurements

on (semi)-solids

For the controlled test chamber (CTC) a new

solids clamping tool according to DIN/ISO 7621-1

has been designed. It consists of an upper and a

lower holder. Each is equipped with two moving

jaws, which guarantee an automatic centering of

the sample relative to the rheometers axis.

The automatic clamping force adaptation for the

sample as well as a very simple semi-automatic

gap adjustment for a wide range of sample

thicknesses with just one fixture allow the user to

measure over a wide range of temperatures in

one go without ever loosing the grip on the

sample.

The jaws are easily removable for cleaning. Also

jaws with various profiles for different sample

types (soft, medium, hard) are available.

The sample can be 5.0 – 12.7 mm wide, 0.15 –

4.0 mm thick and have a maximum length of 68

mm.

Solids clamps set (left) and a sample held by theclamps (right)

The bottom clamp can be adjusted in height.

Samples of different lengths can all be fixed with

their middle part being close to the centre of the

CTC. Thus all samples of different lengths are

exposed to the same extremely low temperature

gradient. Using a flexible temperature sensor the

temperature is measured very close to the

sample.

Cone/plate-exchangeable measuring

geometries for maximum flexibility

For the temperature control chamber (CTC) a new

design for cone/plate- measuring geometries

have been developed, in order to fulfill individual

customer requirements without restrictions.

The exchangeable measuring geometry consists

of an upper and a lower holder with integrated

temperature sensor. Both holders are equipped

with an adapter for a plate or a cone.

Selection of different exchangeable geometries(right)

Plates and cones made of stainless steel with

different diameters (8, 20, 25 and 35 mm) and

cone angles are available. The lower plate is

designed to collect surplus material.

Geometries made of aluminum with diameters 20

and 25 mm are available as reusable plates. For

this kind of geometry a collection device is

recommended, in order to protect the

temperature chamber against fouling.

Thanks to the modular design individual

requirements for material (e.g. Titanium,

Hastelloy), special surfaces (e.g. profiles) and

diameters can easily be realized. They are

available on request.

New measuring cell for rheology

of building materials

In order to carry out measurements on samples

with medium and large particles, a special

measuring geometry is often the only way to get

meaningful data with a high reproducibility.

For measurements on building materials a new

measuring cell has been developed, which can be



63

NEW Accessories for HAAKE MARS


used for HAAKE MARS as well as rheometers of

the HAAKE RheoStress series.

This measuring cell is characterized by its variable

profile. For all existing coaxial cylinders the profile

is fixed and can not be changed. The profile of the

new measuring cell is exchangeable: for each

lamella the profile depth can be individually

chosen.

Lamellas with a profile depth of 2mm are included

in the standard delivery. Lamellas with 1 mm is

available as an option, whereas other profile

depths are available on request.

Specially shaped vane rotors are included in the

price list with 26 and 29,5 mm diameters.

The measuring cell is made of stainless steel in a

very robust design. The surface with an optimized

structure guarantees an easy cleaning.

Using the cell for construction materials in

combination with a HAAKE MARS rheometer the

temperature can be controlled; a suitable

circulator is required. The temperature control unit

is mounted on an adapter plate, in an overhung

position and centered by the measuring cell. Using

a temperature sensor the temperature can be

measured within the sample. With a swing-

mechanism the temperature sensor can be

positioned automatically and on a reproducible

position.

A measuring cell cover is available as an optional

accessory.�

Cross-section of the measuring cell for buidling

materials with adapter plate,

temperature control unit incl. vane rotor

• product information

Heating & Cooling Recirculators

all industries

In Stock – Despatched within

48 hours from receipt of order.

CoolTech 320 HeatTech 26L Refrigerated circulator Heating circulator

Temperature range Temperature range

-28ºC to +100ºC ambient to = 100ºC

$3,999 $2,399 All prices quoted exclude GST and local delivery

Full product information is available on line

for these products plus an extensive range

of temperature control baths to meet the

application requirements of diverse industries.

For full product information and technical

specifications please visit our dedicated website

for temperature control products:

www.temperaturecontrolbaths.com

www.temperaturecontrolbaths.com

The website covers the entire range of temperature control baths currently available across

the diverse product range and depth.

biennial 07-08



Neslab ThermoFlex Recirculating

Chillers

all industries

Reliable, easy-to-use chillersoptimised for the mostdemanding applications

NESLAB ThermoFlex Recirculating Chillers deliver

a continuous cooling capacity up to 1400 watts.

These units are reliable, easy-to-use chillers

optimised for the most demanding applications.

These units are ideal for diverse applications

within the following markets:

• Laser • Packaging

• University • Research

• Analytical instrumentation

• Medical equipment

High Reliability

You can expect years of operation from the

NESLAB ThermoFlex 900 and 1400 recirculating

chiller. The unit features a robust refrigeration

system designed for continuous use in a variety

of environments. The recirculation system

incorporates highly reliable plumbing connections

to eliminate leaks. Integrated air and fluid filters

minimise wear to mechanical parts, which lowers

lifetime maintenance costs and improves system

reliability.�

NESLAB ThermoFlex 900

Recirculating Chiller

Setpoint Temp. Range 5°C - 40°C

Ambient Temp. Range 10°C - 40°C

Temperature Stability +/- 0.1°C

Setpoint Cooling 60 Hz 900W (3072 BTU)

Capacity at 20°C 50 Hz 750W (2560 BTU)

(see graph below for cooling curves)

Reservoir Volume 7.6 Liters

Dimensions (HxWxD) 69.6 x 36.1 x 62.7cm

Unit Weight 57.2kg

Pumps (see graph below for performance curves)

PD 1 - Positive 60 Hz 2.1 gpm @ 60 psi

Displacement 50 Hz 1.7 gpm @ 60 psi



Compliance NRTL Certified to CSA and

UL Standards; CE-Marked

NESLAB ThermoFlex 1400


Setpoint Temp. Range 5°C - 40°C

Ambient Temp. Range 10°C - 40°C


Setpoint Cooling 60 Hz 1400W (4778 BTU)

Capacity at 20°C 50 Hz 1170W (3995 BTU)

(see graph below for cooling curves)

Reservoir Volume 7.6 Liters

Dimensions (HxWxD) 69.6 x 36.1 x 62.7cm

Unit Weight 57.2kg

Pumps (see graph below for performance curves)





Compliance NRTL Certified to CSA and

UL Standards; CE-Marked

Specifications obtained at sea level using water as the recirculating fluid, at a 20°C process setpoint, 25°C ambient condition,at nominal operating voltage. Other fluids, fluid temperatures, ambient temperatures, altitude or operating voltages will affectperformance. Thermo Electron reserves the right to change specifications without notice. Pump performance results obtained with no restrictions on return to the system.

Cooling Capacity

Pumping Capacity

Cooling Capacity

Pumping Capacity


65

The pharmaceutical industry needs consistent,continuous, small scaleproduction capabilities and easy cleaning. Thesystem needs to provideflexibility for new productdevelopment, with reliableand repeatable operatingconditions, plus accurateprocess data for productaudit.

The PRISM Pharmalab 16 Extruder system meets

the needs of the pharmaceutical industry with:

• Small-scale twin screw continuous granulation

• Crevice-fee design with opening barrel and

ancillaries

• Flexible screw and barrel configurations

• Programmable recipe storage

• Integrated data logging and analysis

The benefits of the PRISM Twin screw systems for

the pharmaceutical industry is:

• Continuous granulation delivering consistent

quality on small scale production

• Opening barrel and easily dismantled product

contact parts ensure reliable clean down

• Modular design of screws and barrel gives

flexibility for new product development

• Recipe storage delivers reliable and repeatable

operating conditions

• Integrated data logging provides accurate

process data for product audit�


Continuous Granulation for the

Pharmaceutical Industry

pharmaceutical, cosmetic& allied industries PRISM PHARMALAB 16

Granulator with feederand dosing pump.

PRISM PHARMALAB 16 Granulator showingproduct discharge

PRISM PHARMALAB 16 Extruder showing allcontact sections removed for cleaning

PRISM PHARMALAB 16 Granulator showingdischarge area

PRISM PHARMALAB 16 Granulator showinghopper stirrer

• new product brochure

A micro compounder for small sample amounts

The Thermo Scientific HAAKE

MiniLab II needs a sample

amount of only 5 g.

Compounding expensive or small scale materials

such as nano-composities, bio-polymers or

pharmaceutical is no longer a problem.

Simultaneously, the rheological properties can

be recorded to document structural changes.

By using the optional force feeder, continuos

extrusion with very small flows is possible.

Main features:• Co –rotating twin screws (option: counter-

rotating twin screws)

• Integrated viscosity measurement

• Automatic bypass operation for

circulation/extrusion

• Pneumatic feeding

• LCD screen for graphical data display

• Manual or computer control

• Easy to clean due to exit in split barrel

• Fits into laboratory fume hood=


Sample specimen preparation instrument

The Thermo ScientificHAAKE MiniJet II optimisedthe development process,enabling the testing of the mechanical properties ofspecimens as small as 5 g.

The need to produce various sample geometries

coupled with common reality of limited material

quantities can often create a challenge during

product development.

Main features:• Small sample volume

• Quick & easy to use

• Interchangeable moulds

• Test samples can be produced from

powders, pellets or melts

• A control and design concept that provides

simplistic handling with consistent,

reproducible results

Applications:• Sample preparation for

- Rheometry

- Optical testing

- Mechanical testing

• Preparation of special specimen

for pharmaceutical testing=

polymer industries


polymer industries


Visit Rheology Solutions on stand no: 6084Sydney Convention & Exhibition Centre • www.foodproexh.com • 21-24 July 2008

FoodPro - the trade event for the food and beverage industry

biennial 07-08


• product information

HAAKE MARS with CTC Developed specifically for the HAAKE MARS

platform, the Controlled Temperature Chamber

(CTC) moves smoothly on guide rails. The CTC

consists of two halves that allow convenient

handling and optimal access to the sample. They

can be moved independently backwards and

sidewards, and can be opened and closed easily

by hand. No special tools are needed. The two

halves automatically center themselves around the

sample automatically when closed. Each chamber

half is equipped with a window to observe the

sample during measurement.

A unique feature is the "parking" position, which

allows another temperature control unit to be

attached without removing the CTC.

Above: HAAKE MARS with CTC


67

At the 16 Conference on“Rheology of BuildingMaterials” at the Universityfor Applied ScienceRegensburg Germany,March 2007, Schleibingerpresented a new probe formeasuring SCC mortars.The conference has beenrunning for 16 years and isorganised by Schleibingerand was attended by some80 participants from Europe.

The new design developed by Professor R. Vogel,

Weimar Germany, in cooperation with Schleibinger

is called a “Basket-Probe” for measuring SCC

(Self-Consolidating Concrete) mortars.

It has a flat double gap standard geometry, so you

can get real rheological parameters but in

opposite to other standard systems it minimises

Professor Vogel (left) in discussion with some

conference participants

the wall slippage effects. The cylinder is like a

gasket or a basket so strong cohesion effects

between the materials dominates above the weak

adhesive forces.

The probe works best with very fluid but stable

pastes and mortars used for groups, SCC or Self-

Leveling compounds. Patent pending.

The Viskomat NT is a versatile rotational

viscometer for determining the workabilty of fine-

grained building materials such as cement paste,

mortar, fine concrete, plaster etc. with a maximum

particle size of 2 mm. With the Viskomat NT, you

can obtain information on:

1. flow curves and rheological parameters

2. temperature dependent workability properties

3. stiffening behaviour as a function of time an

stirring speed

4. effects of concrete admixtures and mineral

blending agents on workability�

Schematic drawing of the Basket-Probe for use

with the Viskomat NT viscometer

news & views

Schleibinger Presents

a New Probe for

SCC-mortar for the

Viskomat NT



EZ Cool 80 circulator is a versa-

tile and economical option for

laboratory cooling and heating

needs from -10ºC to +80ºC.

Its bathless design minimises the evaporation of

temperature fluid during daily use. The stainless-

steel circulator is both quiet and robust, making it

well suited for laboratory use.

The HAAKE EZ Cool 80 supports diverse

applications that include cooling and temperature

control of analytical instruments. It can also be

used as an economical chiller with heating options

to replace tap water cooling in small laboratory

applications.

Applications:• Analytical instrumentation control

• Bioreactors • Catalyst reactions

• Chemical reactors • Closed-loop systems

• Condensers • Electrophoresis

• Instrument calibration • Refractometers

• Rotary evaporators • Spectrophotometers

Features & Benefits• Rapid cool down and heat up times

• 4 pre-set temperatures

• Real temperature adjustment for display

of external temperature

• Limits for customised high & low

temperatures

• Powerful pump accommodates connections

to external applications


• Variable over temperature protection

• Fault identification system

• CFC-free refrigeration system �

Product Specifications

Temperature Range -10°C to +80°C

Temperature Accuracy +/- 0.1K


Cooling Capacity 20°C 220 W 0°C 60 W

Pump Pressure (Maximum) 250 mbar

Pump Flow Rate (Maximum) 12 lpm

Internal tank volume 3.5 L

Overall Dimensions (WxLxH) 26x50x40cm

Unit Weight 30 kg


• new product

Circulator to heat & cool external applications from -10ºC to +80ºC

all industries

Left: The HAAKE EZ Cool 80 is ideal to control temperatures within a variety of laboratory applications

including: Pharmaceutical, Biotechnology, Academic Research, Food and Beverage, Chemical, Petrochemical

Right: Front panel showing display panel and control for temperature settings

Heat-Up – Time to Temperature Curve Pumping Capacity

Time (Minutes)

10

20

30

40

50

60

70

80

90

2 4 6 8 10 12

Tem

pera

ture

(ºC

)

Flow (LPM)

100

200

300

400

10 20 30

Pres

sure

(mba

r)

Time (Minutes)

Cool-Down – Time to Temperature Curve

100

15

5

-5

20

10

0

-10

-15 10 0 20 30 40 50 60

Tem

pera

ture

(ºC

)

Bath Liquid: Ethanol

biennial 07-08


Rheology and Microscopy The Thermo Scientific RheoScope module for

HAAKE MARS Rheometer simultaneously records

rheological properties and changes in the

microscopic structure of the tested sample at a

macroscopic level. Understanding micro structures

enables researchers to characterise a product’s

mechanical properties. The module is comprised

of an optical microscope, digital video camera and

temperature control unit that is used in conjunc-

tion with the HAAKE MARS rheometer platform.

The HAAKE RheoWin software used to control the

rheometer also positions and focuses the scope

and polarisation filter. Rheological data and images

(video sequences) can be viewed on line next to

• product news

Rheological measurement with optical analysis - high temperature version extends testing up to 300ºC

food industries

polymer industries


pharmaceutical, cosmetics & allied industries


each other. In addition, the data and images can

be stored in various formats for further evaluation

and export. The RheoScope’s architecture allows

the module to be adapted quickly for customised

user configurations. The RheoScope module is

available in two versions. The temperature range

of the standard version is -5 to 120°C. In the

high-temperature version the temperature is

extended to 300°C.

Simultaneously measures rheological properties

and changes in the microscopic structure of the

tested sample. The results allow researchers to

speed formulation development, process

optimisation and product processability.

Applications / Examples • Food: fat, starch

• Polymer: solution, melt

• Pharma/Cosmetic: cream, lotion

• Paint/Inks: printing paste, thickening agents

• Petrochemical: crude oil, drilling fluid

• Others: medical

Formulations • Gels • Suspensions

• Emulsions/Dispersions • Solutions

• Foam • Melts

Rheological phenomena and structural changes

that can be observed:

• Shear thinning • Dilatancy

• Thixotropy • Aging

• Emulsification • Gelification

• Disaggregation • Flocculation

• Homogeneity • Orientation

• Melting behaviour • Mixing

Benefits: • Compact and full integration in the HAAKE

MARS rheometer platform

• All measuring modes including normal force

measurement available with simultaneous

recording of microscopic properties

• Camera and microscope control with software

• Simultaneous rheological and optical

measurements

• Visualisation of data and images in one

software package

• Analysis of structural changes under shear

• Image analysis software for determination of

particle sizes, particle size distribution and

structure analysis �

Temperature ramp measured on potato wild type starch in water Thermo Scientific RheoScope module for the HAAKE Mars Rheometer


69

biennial 07-08


Thermal printer for HAAKEViscotester 7 plus forrecording and loggingmeasured data.

The rotational viscometer HAAKE Viscotester 7

plus in combination with the thermal printer, is a

set-up for routine measurements conforming to

the ISO 2555 standard and fulfils the requirement

for recording and logging measured data.

The HAAKE Viscotester 7 plus is designed for

measurements compliant with the standard ISO

2555. Each rotational viscometer which fulfils the

requirements of this standard is conforming to

the Brookfield method and the measurement data

of such viscometers are fully comparable with

one another as long as the same viscometer type

(L or R), same spindle and same rotational speed

is used.

Operating of the HAAKE Viscotester 7 plus can be

either manual or computer controlled via the

user-friendly HAAKE RheoWin 3 software

(additional options: DFA 21 CFR Part 11 Tool).

In the manual operation mode, the parameters;

viscosity, percentage of maximum torque,

rotational speed, spindle number, maximum

viscosity and temperature are displayed. For

recording and logging measure results, the

thermal printer can be connected via the RS232

port on the viscometer. At the end of a

measurement the displayed data, as well as date

and time, can be printed out at the push of a

button. Moreover, the print-out has a filed for the

signature for the operator. Thus the measured

data is ready for archival storage.

Ordering number: 999-0118. Thermalprinter for HAAKE Viscotester 7 plus(including connecting cable for HAAKEViscotester 7 plus).�


Accessories for HAAKE

Viscotester 7 plus - Thermal Printer

all industries

Figure 1. Rotational viscometer HAAKE Viscotester 7 plus (left), thermal printer (centre), Loading of anew paper roll (right).

Applying (very) low shear rates

Most (very) low shear rate measurements are

performed in CS Mode, because most real live

applications in which (very) low shear rates are

important are driven by a constant stress.

Examples are sagging, sedimentation, shelf live,

phase separation, all phenomena that are driven

by a constant force i.e. gravitation. These

processes are simulated in a rheometer by

applying a constant stress. However, under

certain circumstances applying a (very) low

shear-rate might be required, for example when

the flow of material which is slowly stirred in a

large container needs to be simulated

(measured). The measurement data below shows

that the HAAKE MARS is very capable of applying

very low rotational speed, i.e. very low shear

rates.

Reliable data down to n = 10-5 rpm

The graphs below show the result of an

experiment in which the rotational speed was

stepwise increased from 10-5 rpm to 10-2 rpm.

Even at a very low rotational speed (and a very

low torque) the measured viscosity is within 5%

from the specified value.

A full copy is available by quoting PS002-e�


CR-Mode - Low Shear Rates

all industries

Instrument: HAAKE MARS, UTC Peltier, PP35, gap= 0.5 mm. Sample: Newtonian Oil, η = 175 Pas


71

Simultaneously measurerheological properties andmicroscopic structure ofyour tested sample.

Gain insight in to rheological phenomena like:

• Shear thinning • Dilatancy

• Thixotropy • Gelification

• Aging • Emulsification

The Thermo Scientific HAAKE MARS Rheometer

with RheoScope module combines rheology with

microscopy allowing you to speed formulation

development and process optimisation.

Benefits include:

• Camera and optical control with HAAKE

RheoWin Software

• Observation of data and images in one

software package

• All measuring modes including normal force

measurement available with simultaneous

recording of microscopic properties

• mage analysis software SPIP for the

determination of particle size, particle

distribution and for structural analysis.

Formulations: Gels, suspensions, solutions, foam,

dispersion/emulsion

An application note on the Image

analysis software SPIP is available by

quoting P009-e�


Optical Analysis and Rheology

food industries

polymer industries



HAAKE PolyLab OS TorqueRheometer RD4 ApplicationPackages

RD4 application packages for the Thermo

Scientific torque rheometer HAAKE PolyLab OS

are dedicated to serving the polymer processing

and polymer formulation laboratory. These

application packages incorporate batch mixers

and single-screw extruders to form test samples

required for polymer melts and ceramic slurries.

The typical combination for the characterisation of

these types of materials is:

• PolyLab OS Mixer Package

• PolyLab OS Extruder Package

• PolyLab OS Upgrade Packages

HAAKE PolyLab OSDocking Station

Mobile bench for measuring mixers and

measuring extruders. When existing measuring

mixers and extruders need to be upgraded with

newer torque rheometer drives and software, the

modular Thermo Scientific HAAKE Docking Station

OS is the right accessory to use.

Applications:

• Mobile bench for Rheocord mixer 600 and

Rheocord miser 3000

• Docking station for existing single-screw

extruders

• Adapter bench for CTW 100 conical twin

screw extruder

• Modular bench to integrate mixers and

extruders of different brands

Product brochures are available on

request by completing the information

request form�


New Product Brochures

polymer industries


biennial 07-08


For the controlledtemperature chamber (CTC)a new plate/plate measuringgeometry has beendeveloped.

The set consists of an upper shaft and a lower

shaft with an integrated temperature sensor.

By using the supplied press tool an exact

perpendicular alignment and reproducible

mounting of the disposable plates on the shafts is

guaranteed (Fig.1).

The standard aluminium plates have a diameter

of 20 mm. Plates with other diameters are


It is recommended to use the optionally available

sample collection ring (below the lower plate); in

order to protect the temperature chamber against

spilled sample material.

After a measurement the disposable plates are

easily removed from the holders by using the

supplied removal tool (Fig. 2).

A copy of this is available by quoting

P010-e�


Disposable plate/plate-measuring

geometry for the controlled

temperature chamber (CTC).

all industries Handling information:

Figure 1 Mounting of a disposable plate on a shaft: press tool, upper shaft and disposable plate (left).Mounting of a disposable plate on a shaft (middle). Disposable measuring geometry consisting of upperan lower shaft with sample collection ring build into a HAAKE MARS (right)

Figure. 2 Removing of a disposable plate from a shaft: removal tool positioned on the lower shaft (left).Handling of the removal tool (middle). Disassembled disposable geometry (left)

Order information:222-1808 Disposable plate/plate-measuring geometry consisting of a lower and an upper shaft, incl.

press tool for mounting the disposable plates on the shafts and removal tool to remove

the disposable plates from the shaft

Necessary accessories:222-1769 Temperature sensor for lower shaft

222-1295 Disposable aluminium plates PP20E, diameter = 20 mm (100 pieces)

Plates with other dimensions are available on request, e.g.:

603-0021 Disposable aluminium plates PP35E, diameter = 35 mm (100 pieces)

Recommended accessories:222-1778 Sample collection ring (5 pieces), stainless steel for plates PP20E

If you have an application and interest in high temperature rheology& simultaneous microscopy and would like to be a part of a workshop

where you can run your own samples, refer to the information on page 4.


73

ViscoScope viscosityanalysers from Marimexhave been applied in manydifferent industries. Whetherit is ambient temperatureapplications in thepharmaceutical industry likeherbal ointments or a hightemperature application inthe polymer industry likephosphorous pentasulfide.

If you have an application as yet unsolved, send

us details of the application and we will work with

Marimex to provide you with a constructive

solution.

Following are some examples of ViscoScope

applications and their related specifications:

The ViscoScope process viscometer measures the

viscosity of liquids continually and precisely in-

line.

The measurement system consists of a sensor,

transmitter and the transmission cable. Safety

barriers are added, if the sensor is being used in

a hazardous area.

The sensor does not employ any moving parts

and it is maintenance free. To measure the

viscosity, the viscometer utilises the torsional

oscillation principle. The power required, to

maintain the small amplitude at the resonance

frequency of the sensor, is a measure for the

viscosity (mPa.s x gr/cm3 / η x ρ)�


Marimex - In Line Torsional

Viscometers

Application Instrument Used & Conditions

Herbal Ointment VA-300M with VS-4550 or VS-B450

Ambient temperature, pressure <5 bar

Polymer Slurry VA300L with VS-4450 or VS-B450

Temperature up to 80ºC, pressures <400 psi

Phosphorous Pentasulfide VA-300L with VS-4450 or VS-B450

Temperature up to 450ºC, pressures <25 bar

Polyester Resin Batch VA-300L, VA-300M or VA-300H with VS-4450 or VS-B450

Temperature up to 300ºC, pressures <10 bar

Black Liquor VA-300M or VA-300L with VS-4450 or VS-B450

Temperatures up to 160ºC, pressures <40 psi

Crude Oil in Pipeline VA-300L with VS-4450 or VS-B450

Ambient temperature, pressures <600 psi

Clay Slurry VA-300M or VA-300H with VS-4450 or VS-B450

Ambient temperature, pressure <5 bar

Key:

- VA-300L for low viscosity between 0.1 & 2,500 cP

- VA-300M for medium viscosity between 1 & 25,000 cP.

- VA-300H for high viscosity between 10 & 250,000 cP.

- VA-300X for extra high viscosity between 100 & 2,500,000 cP.

- VA-4450 / VS-B450 ViscoScope Transmitter

Marimex ViscoScope Sensor with model caption.



polymer industries

mining industries

biennial 07-08


polymer industries

Nano compounds are often prepared in solid form

using the traditional and available mixing and

extrusion devices. Now you can optimise these

sensitive processes.

Nanotechnology – typical applications:

• Improving mechanical properties

• Increasing the electrical conductivity

• Increasing thermal conductivity

• Biocide / antibacterial

• UV absorption

Dispersive and distributive mixing:

• For nearly all mixing applications a well

dispersed and well distributed mixture is

required

• Distributive mixing can be achieved by

splitting and reorienting the flow repeatedly

• Dispersive mixing can be achieved by

passing the mixture through small regions of

intense deformation

• Mixing and composites, M. Kontopoulous

Chee18.2. p390 presentation Queens

University.

A copy of the PowerPoint presentation is

available on request by quoting

Nano Composites 2007.�


Nano Composites

Poorly distributed - Well dispersed Well distributed - Well dispersed

...Screw design...

...Split Barrel

...Feed ports...

...Length...

Maximum flexibility is available with twin screw extruders for HAAKE PolyLab OS

Poorly distributed - Poorly dispersed Well distributed - Poorly dispersed

In Stock – Despatchedwithin 48 hours from receiptof purchase order.

HeatTech 26L heating circulator – temperature

range ambient to +100ºC. $2,399 excluding GST

and local delivery

Full product information is available on line plus

an extensive range of temperature control baths

to meet the application requirements of diverse

industries.

Visit www.temperaturecontrolbaths.com

for full product information and technical

specifications�

product information

Heating Recirculators

all industries

HeatTech 26L


75

product news

New NESLAB ThermoFlex 2500 – Recirculating Chiller

all industries

This is the third configurationof the ThermoFlex platformreleased by ThermoFisher Scientific.

Suitable for a diverse range of applications

and industries:

• Semiconductor

• Packaging

• Analytical instrumentation

• Laser

• Research

• Medical equipment

Key Options Include:

Auto refill Allows for self-filling of the chiller to

ensure that the proper level in reservoir is

maintained, saving valuable time.

Anti-drainback Ensures reservoir does not

overflow when chiller is shut down. This allows

the chiller to be installed more than 24 ft. below

the application.

DI resistivity internal DI filtration internal to the

chiller is used to maintain the resistivity level

below 3 Mohm, with an alarm at 1 Mohm. This

minimises footprint and eliminates downtime

needed to change the filter, while ensuring

constant quality of DI water to your application.

Pressure relief Easily adjustable pressure relief

valve allows for control of the outlet pressure

from the chiller to be regulated, ensuring your

process performance requirements are met.

Flow Control Utilizes a 3-way valve that allows

you to control the amount of flow to the

application. The process flow is measured on the

return to the unit, ensuring the appropriate

amount of flow is provided to the application.

Pressure/Flow Control Allows you to control the

pressure as well as the flow in your application.

Utilises a pressure relief valve and monitors the

flow through the process return and displays the

reading on the controller.

The NESLAB ThermoFlex 2500 is a reliable, easy-

to-use chiller optimised for the most demanding

applications. Delivers continuous cooling capacity

up to 2500 watts.

Water-Cooled Uses facility water to cool the

system, minimizing heat dissipation into the

environment.

Key Accessories Include:

Installation Kit Supply and return plumbing

available in 25 and 50 ft lengths, suitable for

temperatures up to +80°C.

Fluid Quality Kit Complete fluid quality system

includes algaecide and corrosion inhibitor to

ensure your process has optimal fluid quality.

Ethylene Glycol Laboratory-grade ethylene glycol

allows circulation to temperatures down to -20°C

in a 50/50 mixture with water. Available in a 5

gallon container.

Propylene Glycol Laboratory-grade propylene

glycol allows circulation to temperatures down to

-20°C in a 50/50 mixture with water. Available in

a 5 gallon container.

Maintenance Kit Includes condenser air filters and

in-line fluid filters for ease of maintenance.�

A dedicated website for temperature control has been establishedby Rheology Solutions …www.temperaturecontrolbaths.com

The website covers the entire range of temperature control baths

currently available to meet the diverse needs of industry applications

across QA/QC, R&D and Production areas

biennial 07-08


PRISM small scale extruders and ancillaries allow

research and development at a laboratory scale.

The twin screw extruders from 16mm to 36mm

diameters are supplemented by purpose built

ancillaries including bench-top blenders,

pelletisers and sheet and film take-off units.

For complete details and product

information, complete the information

request form or send an email detailing

your application requirements.�

product information

Twin-Screw Extrusion at a Lab Scale

all industries

Product Specifications

Setpoint Temperature Range 5°C - 40°C

Ambient Temperature Range 10°C - 40°C


Setpoint Cooling Capacity at 20°C

(see graph above for cooling curves)

60 Hz 2500W (8538 BTU)

50 Hz 2200W (7513 BTU)

Reservoir Volume Litres 7.2

Footprint or dimensions

(HxWxD) cm 73.8 x 43.5 x 65.2

Unit Weight kg 80.3

Pumps

(see graph above for performance curves)

PD 1 - Positive Displacement

50 Hz 1.7 gpm @ 60 psi

PD 2 - Positive Displacement

50 Hz 3.3 gpm @ 60 psi

Power options 230V/50Hz/1 Phase

16A Circuit

Compliance NRTL Certified

to CSA and UL

Standards;

CE-Marked

Specifications obtained at sea level using water as the

recirculating fluid, at a 20°C process setpoint, 25°C ambient

condition, at nominal operating voltage. Other fluids, fluid

temperatures, ambient temperatures, altitude or operating

voltages will affect performance. Thermo Fisher Scientific

reserves the right to change specifications without notice.

PRISM 16 mm EuroLab twin screw extruder

In Stock – Despatchedwithin 48 hours from receiptof purchase order.

CoolTech 320 refrigerated circulator -

temperature range -28ºC to +100ºC. $3,999

excluding GST and local delivery

Full product information is available on line plus

an extensive range of temperature control baths

to meet the application requirements of diverse

industries.

Visit www.temperaturecontrolbaths.com

for full product information and technical

specifications�

product information

Cooling Recirculators

all industries

CoolTech 320


77

The PS200C inspectionsystem from Optical ControlSystems is used to analysetransparent and opaquepellets.

The pellets are inspected with a high-resolution

3-Chip CCD colour camera for impurities, foreign

bodies, or colour deviations as well. The testing

material is fed into the appliance through a

hopper. The pellets are conveyed separately over

the inspection zone. After the optical evaluation

the contaminated pellets can be separated into a

different container (sorting unit option).

Measuring errors are eliminated by use of

numerous additional optical components.

There is no colour dependency as with many

other optoelectronic appliances.

A high level of efficiency is achieved by powerful

image processing software. The synchronisation

of the transport system with the image

processing offers a major contribution to the

reproducibility of the measurement results.

Installation in the bypass guarantees production

monitoring and rapid reaction to any occurrences.

The system provides a variety of individual

configurations, which guarantee an improved

adaptation to specific requirements.

The measurement data are stored in a test report

to enable future analysis. The recorded images

and measured data can be observed on a screen

during the measuring process. The results can be

shown and printed in tables or graphs.

Along with a pure inspection of pellets the system

can also be used to record, file and document.

Each defined deviation is recorded in the

measurement protocol via a multidimensional

characteristics vector with an error map.

The system can be adapted exactly to the

respective requirements with the

help of the extensive software packages.�

product focus

High Speed Pellet Scan System – Throughput up to 250 kg/hr

High Speed Pellet Scan System PS200C

polymer industries

VisConfig software for easy configuration of allparameters

Applications

• Opaque pellets

• Coloured pellets

• Transparent pellets

• Material throughput up to 250 kg/hr

Technical Data

Camera 3 Chip CCD colour matrix camera

Lighting High frequency synchronised

fluorescent lamp. White light

spectrum

Computer Industrial CPU: Intel Pentium 4,

up-to-date technology

Interfaces Ethernet 10/100 M Base-T,

Digital and analogue I/O, USB,

MODBUS, PROFIBUS, RS232,

BDE, SAP interface or SQL

Remote Extender max. 100 m Service

Control Remote control

Software Operating System Windows XP

Size Dimensions (l x w x h)

650 x 770 x 770 mm

Weight approx. 100 kg

Connection Power supply 230 V

values AC / 115 V AC

Temperature 10ºC to 45ºC

Benefits

• Optimising the production process through

detailed characteristics specifications

• 24 hour online production surveillance trend

analysis parallel to productionPellet conveyor line

biennial 07-08


The HAAKE MARS is equipped with a self-learning

deformation control loop based on neural network

technology for controlled deformation (CD)

oscillation measurements.

In CD-Mode the deformation sine wave is

continuously controlled, this enables the control

loop to react almost instantaneously to changes in

the material. A quick reaction to material changes

is required when the mechanical properties of a

material are measured, during a curing reaction,

using constant strain oscillation.

The brochure provides an example of curing

of a dental material. A copy is available by

requesting PS001-e�


New Product Brochures& Information Sheets



The HAAKE MARS rheometer is now available

with a support fixture for the comparative analysis

of elasticity and sensoric (haptic) properties of

textile samples.

The brochure provides full details on the

fixture, tests recommended and ordering

information. A copy is available by requesting

P012-e�



The HAAKE MARS rheometer is equipped with a

highly sensitive normal force sensor and a very

precise lift motor which allows applying controlled

axial forces to the sample, pushing or pulling the

material.

A new sample fixture has been developed to

investigate the bending and breaking behaviour of

a wide range of materials.

The brochure provides details on the tool,

and adapting it to the HAAKE MARS, plus full

ordering information. A copy is available by

requesting P014-e�

polymer industries

food industries

polymer industries


Support fixture for the analysis oftextile samples - Accessories forHAAKE MARS

Sample fixture for bending andbreaking tests – Accessories forHAAKE MARS

CD-Mode Curing Measurement – HAAKE MARS


79

The functionality and/or calibration of any

measuring instrument should be checked

regularly. Checking a rheometer or viscometer is

usually and most easily done by measuring a

standard liquid with a certified viscosity value.

A standard liquid is a Newtonian fluid for which

the viscosity value is certified for one or several

temperature values.

A wide range of standard liquids with different

viscosity values and uncertainties as well as

different reference temperatures and chemical

structures (mineral oils, synthetic oils) are

available.

Standard liquids from Thermo Fisher Scientific are

delivered with a certified viscosity at 20°C and an

uncertainty of ±2% (±4% for E7). Standard

liquids with viscosity values between 5 mPas and

40000 mPas are available in 100ml or 500 ml

containers.

Standard liquids with other viscosity values or

other reference temperatures as well as the

delivery in other containers (e.g. 1.0 l) are


Standard liquids with a lower uncertainty of the

viscosity (±0.4%) and/or certified viscosity values

at other temperatures between 20°C and 100°C

are available from the German Calibration Service

(DKD – Deutscher Kalibrierdienst) amongst

others.

Because of their lower viscosity - temperature

dependence silicon oils are often used for

checking simple viscometers which do not

provide any means of temperature control. For

this application the slight shear thinning

behaviour of silicone oils (decreasing of the

viscosity with increasing shear rate) should be

neglected.

For checking a specific viscometer or rheometer

configuration it is important to use a standard

liquid that matches the parameters (temperature,

viscosity, etc.) of the routine measurements

normally run on that instrument.

When comparing the measured viscosity value

with the standard liquid's certified value it is

important to take the instruments uncertainty into

account also.

An information sheet is available covering

the above text and also includes full

ordering information. A copy is available on

request by quoting P-015-e�

polymer industries


food industries



all industries

A new tool for checking the quality of images

acquired with the RheoScope module for the

HAAKE MARS has been developed.

This tool consists of a closed cell with a reflective

upper plate and a lower glass plate, containing a

watery solution with standard particles with

diameters of 1.5, 4, 8 and 20 μm.

Full information is available in the brochure

and a copy is available by

requesting P016-d�

Tool for checking the optical quality of the RheoScope module – HAAKE MARS

Standard Liquids


New Product Brochures& Information Sheets

biennial 07-08


Higher instrument precision is now requested for basicrheology measurement withhandheld instruments.

The VT 2 plus allows the 1% calibration accuracy

needed to fulfil this requirement.

The entire VT 1 plus and VT 2 plus series is

the standard in quality control and combines ease

of use with exact and reliable measurements.

The HAAKE Viscotester 1 plus & 2 plus are quick,

exact and reliable rotational viscometers with a

one button operation which can be operated

hand-held or on a stand. A digital display delivers

clear results. Battery powered, these units do not

require external power. These Viscotester models

are delivered in a sturdy carrying case as a

complete ready-to-use package with 3 measuring

systems.

During the past decades HAAKE Viscotesters have

successfully proven their value wherever quick

and reliable tests and comparative measurements

are part of daily routine work. They have also

been established as standard instruments for

quality control. The new generation – HAAKE

Viscotester 1 plus & 2 plus – continues this

tradition and fulfils the highest demands

regarding design and convenience.

Main features:

• Quick, exact and reliable

• One button operation

• LCD display

• No mains supply needed (battery-operated)

Typical application fields:

• Quick viscosity tests, e.g. for process

optimization or machine adjustment

• Batch control in production

• production in control

Typical samples:

• Printing inks, paints, inks

• Shampoos, creams, lotions

• Oils, greases, pastes, lubricants

• Sauces, thickeners�

product news

Higher Instrument Precision and Reliable Quality ControlHAAKE Viscotester 1 plus and 2 plus

all industries

HAAKE Viscotester 1 / 2 plus

The Thermo ScientificNanoLab compounderpackage contains the toolsto mix or compound Nanoparticles (Nano tubes) in abase polymer.

Based on recommendations from users in the

industry and Universities it is recommended to:

• use the standard Thermo Scientific HAAKE

MiniLab micro compounder for temperatures

up to 350°C

• use the control panel for quick test runs,

trials and the cleaning

• employ the application software to run

defined and reproducible tests

• compound Nano particles and do rheometry

with counter-rotating screws

• use the co-rotating screws for applications

with additives requiring less shear force

A copy of this product information brochure

is available by request.�

product news

NanoLab Compounder Package

polymer industries




HAAKE MiniLab II compounder with co- andcounter-rotating screws


81

The use of a conical twinscrew extruder with backflowchannel combines aspects ofmixing and extrusion in abatch process.

Tests and results of the new MiniLab micro

compounder are discussed in the following paper.

With a total filling volume of 7 ml and a built in

slit capillary die the applications focus on

compounding and reactions of small amounts of

polymers in molten stage.

Selecting the screw types: Co- or counter

rotating?

In order to open up an even wider spectrum of

applications for the customer, the MiniLab works

as co-rotating or as counter-rotating double-

screw extruder. This results in different types of

screws.

Simply exchanging two gear wheels in the

gearbox changes the rotating direction of the

screws. Figure 2 shows the co-rotating pair of

screws. It also shows a faster compounding of

the master batch in comparison to Figure 4.

In the following table further characteristics of

the used screws are summarised.

Table 2 Characteristics of the screw types

Co- Counter

rotating rotating

Resident time distribution wide narrow

Forced extrusion - +

Cleaning + -

Extruder amount + 0

Blending of sensitive products ++ 0

High shear rates, dispersing - ++

Rheological measurements 0 ++

Required duration of blending ++ +

A number of topics and applications have been

presented on the HAAKE MiniLab in a combined

product information flyer. The topics included are:

• Toughness enhancements in poly (methyl

methacrylate) by addition of oriented

multiwall carbon nanotubes

• The effect of processing variables on the

structure and rheological properties of

polymer/clay nanocomposites: Nylon 6/clay

• Improving polymer blend dispersions in mini-

mixers

product information

HAAKE MiniLab –Compounder & Reactor

HAAKE MiniLab II Complete System

polymer industries

Fig. 2: Co-rotating screws: a) PE melt, b) Asaclean (PS cleaning compound) + Remafin orange durationof the test t = 90 s, test conditions like in Figure 4.

HAAKE MiniLab II Barrel Section

A copy of this product information is

available by request and includes the

above mentioned topics.�

biennial 07-08


Marimex ViscoScope processviscometers measure theviscosity of liquids continuallyand precisely in-line.

ViscoScope sensors do not have any moving

parts and are maintenance free. A constant

amplitude torsional oscillation principle is utilised

to measure the viscosity. Various ViscoScope

sensors and transmitters are available. All sensors

work with all transmitters.

All transmitters are delivered with VisConfig

configuration software to simplify the start-up

process. Optionally ViscoView software for PC

compatible computers and a touch panel display

are available as a graphical interface.

ViscoView Software – Optional Software

Collected data is stored in a tab delimited ASCII

format. The file is being closed after each data

collection, this enables the file to be copied into a

different directory at any time. The data collection

rate can be adjusted between 10 and 600

seconds. The file can be imported into a

spreadsheet like Excel, where additional

calculations and graphical manipulations can be

accomplished. The following parameters can be

collected:

• Viscosity (all available)

• Process Temperature

• Coil Temperature (transducer dependent)

• Resonance Frequency (transmitter dependent)

• External Input (transmitter dependent)

• Date and Time

VisConfig Software

The VisConfig Software provides an easy interface

for the configuration of all customer accessible

parameters via a PC compatible computer.

VisConfig has been configured to work with the

ViscoScope firmware version MMX1.011. Special

issues are available to interface to others

firmware versions. VisConfig also provides a tool

to check all ViscoScope Modbus addresses

and instrument types connected to the PC. A

single Modbus address can be reconfigured in

the first screen. A functionality check is available

to check the function of the sensor in air after the

zero procedure. The result will show if the sensor

works within known parameters. VisConfig also

does a one time check of all measurement

parameters and can be used to continuously

sample selected measurement parameters –

the last 20 samples can be observed.�

product information

Process Viscometers – Software Options

ViscoView® data collection software for ViscoScope viscometer systems


food industries


mining industries


VisConfig software for easy configuration of all parameters

• new product

HAAKE PolyLab QC

polymer industries

The HAAKE PolyLab QC

is a new measuring mixer

& extruder system that meets

todays and future quality

control (QC) needs.

The modular torque rheometer

can be connected to an

interchangeable mixer,

single-screw extruder, or

conical twin-screw extruder.

Concept• Modular torque rheometer with

interchangeable mixer, single-screw extruder,

conical twin-screw extruder

• Bench or floor model

• Control via HAAKE PolySoft software

Backwards Compatibility• Hardware compatible with old mixers,

extruders

• Existing accessories can still be used

• Data compatibility (importing of old data)

Specifications• Torque range: 0 - 300Nm

• Speed range: 0 - 200 rpm

• Temperature control zones: 5

• Temperature reading channels: 4

Interfaces/Communication• CAN open control communication with

temperature, motor controller

• CAN open data communication for pressure

and remote signals

• USB interface to host computer (LAN as

option)

HAAKE PolyLab QCMeasuring Mixers

A typical mixer test is run at a defined rotor speed

(shear rate). The material’s response to the shear

is recorded as torque and displayed versus time.

As a material’s properties are very sensitive to

temperature, the mixer chamber is separated into



83

• Measuring oil absorption of carbon black

• Quantifying the absorption of DOP for PVC

dry-blends

• Measuring the stable torque in regard to

individual and combined influences of fillers

and additives such as stabilizers, lubricants

and colour pigments

• Testing high performance plastics to check

processability

• Performing electric conductivity

measurements for rubber mixtures.

Due to the backwards compatibility of the

mechanical and electrical interfaces of the HAAKE

PolyLab QC, existing mixing equipment can be

used with a state-of-the-art torque rheometer that

is equipped with reliable digital controls and

operated using the modern, user-friendly Thermo

Scientific HAAKE PolySoft software package.

Mixer Software Small laboratory mixers are traditionally used to

mix and/or measure the viscosity of a 40-70 g

mixture as a function of time and temperature with

different shaped rotors. Typical examples are PVC

dry blend mixing, PVC degradation test,

rubber/carbon black mastification, cross linking of

polymers, curing of resins and thermosetting

properties.

HAAKE PolyLab QC Single & Twin Screw Extruders Single-screw extruder The most common methods in processing

polymers are screw plastification and injection

moulding. For testing quality and processability of

those materials, the single-screw laboratory

extruder 19/25 QC-B is a proven tool. With over

35 years of expertise, we’ve developed a wide

variety of different screw designs that are

guaranteed to provide the best performance.

Special solutions such as chemical or wear

resistance are also available to extrude harsh

materials. To shape a polymer for further

processes and tests, different dies can be adapted

55

0

5

20

30

45

50

0 0,8 1,6 2,4 3,2 4,0

25

t [min]

] m

N

[

M

40

35

10

15

F F F

A

B C

PVC_Sample A M = f(t)

PVC_Sample B M = f(t)

PVC_Sample C M = f(t)

to the extruder. Rod dies and water bath for strand

extrusion, sheet and ribbon dies in various

dimensions to produce bands or cast films, and

blown film dies and take off tower complete the

testing equipment. Besides the standardised filter

test (EN 13900-5), comprehensive rheological

studies can be conducted.

Applications• Testing of the plasticizing behaviour

• Testing the performance of additives

and fillers

• Measuring of the melt temperature and

pressure along the barrel to optimize process

parameters

• Provide a homogeneous and constant flow

melt

• Production of strands, sheets, cast and blown

films

• Extrusion of ceramics and feed stock

• Melt rheology

Conical twin-screw extruderFor continuous compounding and plasticising, the

Thermo Scientific HAAKE CTW 100 QC is the ideal

extruder in the HAAKE PolyLab QC system. This is

a counter rotating conical twin-screw compounder,

with intermeshing screws, that will give

well-defined residence time for faultless

production of process-critical polymers are ideal to

mix additives and pigments. Dies and downstream

ancillaries are compatible with the 19/25 QC-D

single-screw extruder.

Applications• Extrusion of thermally critical materials such

as PVC

• Compounding of fillers and reinforcing

materials

• Blending of polymers

• Pilot plant production of master batches

• Continuous mixing of recycling materials

• Mixing of nano clays and carbons

• Discharge for further process states


Haake PolyLab QC� continued from page 83

As a material’s properties are very sensitive to

temperature, the mixer chamber is separated into

different sections. These are individually

temperature-controlled by the HAAKE PolyLab QC.

Optimum temperature control quality can be

achieved by an automated recognition of the

connected mixer.

Although the temperature of the mixing chamber

is constantly controlled, the material’s melt

temperature during a test may rise due to the

shear introduced. The melt temperature is also

recorded during the test by a separate

thermocouple. The recorded “Rheogram” (torque

and melt temperature vs. time at constant speed)

is characteristic for different material types and

HAAKE PolyLab QC mixer - Intelligent measuring

mixers simplify your quality control

blends. It can be used as a fingerprint in quality

control for outgoing and incoming product

inspections. As changes in torque are related to

structural changes in the material, a Rheogram

can be used to investigate and verify reactions of

different additive types or concentrations on the

sample’s melting behaviour.

Typical Investigations• Testing the melting and degradation behaviour

of polymer melts

• Quantifying viscosity when adding nano

particles or other additives

• Testing gelation and plastification behaviour

of PVC dry-blends

• Measuring the flow and curing behaviour

of thermosetting plastics

• Characterizing the influence of different

additives such as carbon black, fillers

lubricants, accelerators and sulphur for

rubber mixtures

• Recording the masticating and vulcanizing

behaviour of elastomers

biennial 07-08


Typical Investigations • Testing the melting and degradation behaviour

of polymer melts

• Quantifying viscosity when adding nano-

particles and other additives

• Testing the gelation and plasticizing behaviour,

and the thermal stability of PVC dry-blends

• Measuring the flow and curing behaviour of

thermosetting compounds


behaviour of elastomers


measurements during the mixing process

Melting, Conveying, Compressing, Compounding Extruders are melting, conveying and

compounding polymers under temperature,

pressure and shear. The extruded polymer is

pressed through a die to form a solid material

such as a profile, sheet, film, strand or fibre. The

extrusion process is characterized by monitoring

processing power (torque), temperature, pressure

and throughput. Special rheological dies (slit, rod)

allow the determination of shear viscosity at

defined shear rates.

HAAKE PolyLab QC Measurements - Measuring

options provided by the HAAKE PolyLab QC

Typical Measurements • Simulation of production processes like blown

film, wire coating, profile extrusion

• Testing individual and combined influences of

additives (stabilizer, lubricant) and functional

additives (antioxidation, UV-stabilizers,

pigments and fillers)

• Investigating the extrudability of newly

developed materials

• Manufacturing films, sheets, strands and

profiles for optical, mechanical and

weathering tests

• Small scale production

• Measuring rheological behaviour (dynamic

viscosity)

• Compounding and blending of polymers, fillers

and additives

• Dispersion and exfoliation of nano-fillers in

a polymer matrix

Flow curve LLPDE Online capillary rheology with HAAKE PolyLab QC

is performed using a well defined die geometry

(slit or capillary) on an extruder. The shear stress is

derived from the pressure drop in the die (CAN

pressure transducer signals) and the shear rate

from the weight of the extrudate in a defined

period of time.�

M = f(t)

n = f(t)

p1 = f(t)

TM9 = f(t)

Data File

400

0

50

140 190

t [min]

] m

N

(

M

150

150 160 170 180

] r a

b

[

p

100

200

250

300

350

2,5% Nanoclay

5% Nanoclay

t_res: 30sec.

no filler

10000

10

100

0,01 100000

y t i s o

c s i V

1000

0,1 1 10 100 1000 10000

Slit-Capillary (Rheocord)

Rod Capillary (Rheocord)

Oscaillation (RS Rheometer)

Shear rate

Haake PolyLab QC� continued from page 84

Compatibility of existing extrudersSingle-screw extruders and conical twin-screw

extruders that are operated with the driving unit

HAAKE Rheocord 90 or 9000, HAAKE RheoDrive

5000 or System 40 are compatible to the HAAKE

PolyLab QC. Laboratory extruders from other

manufacturers can be adapted, too.

HAAKE PolyLab QC Extruder - Powerful extruders

continuously control your quality

Measuring options provided by the HAAKE PolyLab QC

Mixing, Kneading,Compounding & PlasticisingIn conjunction with measuring mixers, the HAAKE

PolyLab QC offers a wide range of different

applications. A typical mixer test is run at a

defined speed (shear rate) versus time, and the

material’s response is recorded as torque. This

"Mixer-Rheogram" (torque, melt temperature vs.

time at constant speed) is characteristic for

different materials or blends and is often used as

a "fingerprint" in quality control for incoming or

outgoing product inspection.


85

• new product

The OP5 Online Rheometer

polymer industries

Performance Features

• Controls - Menu-driven Windows interface

and easy customisation

• Access - Password protected to 5 levels

• Optimum location - Use of laboratory

environment to ensure high run time and

accessibility for calibration and any

maintenance

• Low delay time - Fast sampling, sample

preparation and measurement results in delay

time more than adequate for control

• Accuracy - Calibration is established by

Porpoise Transfer Standard ™ Optional

full-time statistical process control packages

• Full-time calibration - A statistical calibration

system that conforms OP5 to the ISO 1133 or

ASTM D1283 standards full time

• Tables - Tabular display according to

individual cycle measurements of

temperatures, Pressure, flow rate, consumed

weight of material, test results

• Set points - Tabular display of all set points

• Real time display - Continuous trend display

of MI with tramlines and product name

overlays. Additional trend displays,

temperatures, pressures, mass flow, total

mass flow

• Recipe control of cycle and conditions -

Operator control via menu of parameters,

sequences and user Product Names

• Sample size control - Adaptive sample sizing

to minimise delay of measurement

• Statistical analysis packages - User friendly

calculations of averages, standard deviation,

Cpk and other process variables. Export

facilities

• Alarms - External alarm interface

• Open database - All records can be converted

into any standard file format

Scope Of Application

• Powder or pellets from polymer processes

• Powder ex-reaction

• Pellets post extrusion

• Samples transported to Laboratory via

OCS-Porpoise systems

Benefits

• Integrated process control through Porpoise

measurement technology

• Improvement of process efficiency

• Improvement of quality at source – All product

made to recipe

• Improvement of quality selection facility

• Measurements certified to ISO 1133 or ASTM

D1283 standards

• High availability, high reliability

• Low maintenance budget, low time to repair

• Third party certification of product via SGS

• Elimination of customer complaints

• Fast return of investment

• Perfect for all polymer processes

A system for plant optimisation

and improved product quality.

The function of the OP5 from Optical Control

Systems (OCS) is to make certified measurements

of the Melt Index and/or Polydispersity of small

solid polymer samples. The primary duty of these

measurements is overall control of many types of

polymerisation processes. This ensures that the

product can be made to specific formulations. The

secondary duty is Quality Control in final product

selling specification and in batch control. The OP5

is logically situated in the plant analysis laboratory,

which ensures best reliability and maintainability

for these calibrated, precision measurements.

Representative samples are therefore transported

from various locations of the polymer

manufacturing plant at the call of each analyser.

Process Control and QC are full time activities,

which require, as a minimum, one sampling point

for each analyser.

Representative samples are extracted from each

reactor stage and from the finished product. In

simple plant configurations, such as LDPE, PS,

PET and Nylon this usually means one OP5 but in

complex plants such as PP, HDPE and LLDPE two

or more OP5 analysers would be required. The

complex plants have powder samplers, which have

degassing and catalyst deactivation stages close

the analyser. At the plant end, these samplers can

extract at the main discharge valve(s) of the

reactor or at the primary de-gassing vessel, etc.

according to the plant configuration. In the case of

the pellet samples, these would normally be

supplied from central (OCS) source, and in such

cases the supply to the rheometers carries a

priority to minimise the sampling delay time.

Melt flow measurements are performed after the

solid sample is melted and conditioned to the

appropriate test temperature. In the OP5 the

melting process minimises any changes to the

structure of the polymer but making a very rapid

transition from solid to liquid, which substantially

obviates shear damage, cross-linking, thermal

degradation and other degradation processes. This

sample preparation removes the last traces of any

trapped air or gas and overall makes an important

contribution to making the sample at the point of

measurement fully representative of the process.

In this unique way the OP5 makes control through

rheology as reality.

The melt flow is regulated by a sealed gear pump,

which transports a metered quantity through a

shaped die which has the normal MI die L/D. The

shaping of the die is to minimise the delay in the

slow moving polymer near the walls, without

deviating the actual rheology relationships too far

from the standard MI die.

Measurements of pressure and flow rate are used

to derive the standard Melt Index. Many features

of the apparatus for measurements are covered in

the patents. The patent, Melt Flow determination in

Polymer process, has the following grants, EU 989

45440, GB 233 4958 and US 09/622558. These

patents also have integrated process control

application. Systematic correlations are applied to

compensate for the relationship between the OP5

die and the lab test die (both ASTM D1283 and

ISO 1133 tests use the same die form). The

corrections derived from these correlations are

specific to the actual polymer process and the

local test methodology used to make the test. This

is because each plant produces subtly different

polymer structures and the manual test method

result varies with operator and procedures. Once

established the corrections continued on page 87 �

biennial 07-08


The OP5 OnlineRheometer� continued from page 86

do require regular verification, which is supplied

through the OP5 operating software. The IPR of

the operations are described in the EU CTM,

Registration Certificate No 002729309. The

methodology of calibration and measurement

gives the OP5 class leading accuracy, which can

be used to certify the finished product and thus

completely replace routine testing using the Lab

Melt Indexers. It is normal to certify these

calibrations through a third party specialist. SGS,

who are respected globally for such duties, have

contract approval with major polymer producers

for such onerous tasks.

The OP5 measurement of Melt Index is performed

in a batch process, termed a cycle. The MI result

is based on a tiny part of the sample, which gives

the OP5 a pin point accuracy. The result shows

every small variation in the polymer product and

which can be used to steer polymer reactions in a

way not possible by long term averaging or less

than adequate sample preparation. The MI result

can of course be used for Quality Control but the

finely resolved and accurate measurements will

bring a better precision and thus maximise the

added value of the production.

Typically the OP5 samples every 5 minutes to fit in

with the cleaning – measurement-sequence. The

delay of measurement is slightly greater than cycle

time of the sequence. Although the cycle has been

optimised for accuracy but by using the necessary

cleaning part of the cycle, the delay is made nearly

independent of sample MI value. The real time

delay (7-15mins) between the reaction and the

measurement, which includes any sampling and

sample preparation delay, is comfortably below

process requirements whether it is used for

reaction control and QC. In fact provided the delay

is adequate, process control and QC places a very

strong requirement on full-time calibration and

best accuracy.

The unique features of the OP5 equipment open

up the huge opportunity of process control through

rheology.�

• new product

HAAKE RheoStress 6000 – The Universal Rheometer

all industries

The HAAKE RheoStress 6000

is the new generation of the


RheoStress series that is

focused on standard

application in R&D and QC.

The HAAKE RheoStress 6000 is fully compatible

with existing accessories of previous RheoStress

models including temperature control units,

measuring geometries and application oriented

measuring cells.

A variety of temperature control units is available

to reliability and accurately handle temperatures

ranging from -80ºC up to 500ºC

A variety of temperature control units is available

to reliability and accurately handle temperatures

ranging from -80ºC up to 500ºC

Peltier, electrical or liquid temperature control unit

for coaxial cylinders, plate/plate and cone/plate as

well as special measuring geometries.

A number of application oriented accessories are

available:

• Pressure cell for use in crude all, drilling

fluids, food

• UV cell for use in coatings, dental material,

contact lenses

• Measuring cell for construction materials for

use with cementitious pastes and mortars and

samples with large particles

• Double cone geometry for use with low

viscous material where a small quantity is only

available or where there is a tendency of

evaporation

• Disposal measuring geometries for samples

which are difficult to remove such as

cross-linking and curing material

• Universal holder for individual containers for

paints, inks and food

• 3 point bending tool for food

The HAAKE RheoStress 6000 offers:

• CR (controlled rate) mode: Optimised speed

control loop and a low motor inertia (I=10

_Nms2) for fast speed steps within few

milliseconds without significant overshoot

• CS (controlled stress) mode: Advanced

patented air-bearing technology plus accurate

torque correction (MSC = Micro Stress

Control) for measurements at low torque limit

• CD (controlled deformation) mode: Self-

learning deformation control loop based on

neural network technology for fast parameter

adaptations

• Combinations of measuring modes: Flexible

software and firmware for creative job

definitions

• Normal force measurements: Robust and very

sensitive normal force sensor based on

extremely sensitive and robust strain gauges

for measurements between – 50 N and

+ 50 N�


87

Fixed measuring head

consisting of:

• Drag cup motor with the

lowest available inertia

(10μNms2)

• High resolution optical

encoder (12 nrad)

• Patented 4th generation air

bearing system*

• Temperature compensated

normal force sensor based

on strain-gauge technology

for positive and negative

normal force measurements

Adapter for upper

measuring geometries

Recepient of temperature

control units and application

oriented measuring cells

Compact design by one

column aluminum frame

with integrated control

and power electronics

HAAKE

RheoStress

6000

Optional display/control unit. Monitoring data online even without a PC.

The display/control unit of the

HAAKE RheoStress 6000

facilitates manual operation of lift

movement and gap setting as

well as starting measuring and

evaluation jobs with or without

PC. The colour display monitors

rheological and instrument-

specifi c data online.

Glass plate with high

resistance against chemicals

for easy cleaning

* DE 10 2004 050 753 A1; US 7,181,956 B2

Thermo Scientific HAAKE RheoStress 6000 Specifications

Min. torque rotation CS 200 nNm

Min. torque rotation CR 200 nNm

Min. torque oscillation CS 200 nNm

Min. torque oscillation CD 200 nNm

Max. torque 200 mNm

Torque resolution 0.5(a) nNm

Motor inertia 10 μNms2

Angular resolution 12(b) nrad

Min. angular velocity CS 10-7 min-1

Min. angular velocity CR 10-5 min-1

Max. angular velocity 1500, 4500(c) min-1

Min. oscillation frequence 10-5 Hz

Max. oscillation frequence 100 Hz

Min. Normal force 0.01 N

Max. Normal force 50(d)N

(a) at the lowest torque (b) internal resolution (c) high shear option (d) in both positive and negative direction (e) depending on temperature control unit

Normal force resolution 0.001 N

Min. lift speed 0.2 μm/s

Max. lift speed 7 mm/s

Lift positioning accuracy 0.5 μm

Temperature range -80 to +500(e) °C

Dimensions (W x D x H) 400 x 400 x 780 mm

Weight 42 kg

biennial 07-08


Overview of HAAKE

Viscometers

Model HAAKE Viscotester

1 plus & 2 plus

Measurement Relative

Standards -

Viscosity Viscometer 1 plus: low

Viscotester 2 plus: medium

Model HAAKE Viscotester

6 plus & 7 plus

Measurement Relative

Standards ISO 2555

Viscosity L – Version: Low to medium

R – Version: medium to high

Model HAAKE Falling Ball

Viscometer type C

Measurement Absolute*

Standards Din 53015, ISO 12058

Viscosity Low to high

Model HAAKE Viscotester VT550

Measurement Absolute**

Standards DIN 53018 / 53019,

ISO 3219

Viscosity Low to high

*For Newtonian substances

**Using absolute measuring geometries

• new product brochures

HAAKE Viscometers

all industries

Basic principles in rheology,

selecting a viscometer

Viscometry Measuring instruments for the determination of

the flow behaviour of fluids are called viscometers.

Viscosity is a material property which is dependent

on different parameters such as mechanical stress

and strain, time as well as temperature and other

ambient conditions.

Flow behaviour In rheology we differentiate between so-called

Newtonian and non- Newtonian materials.

Newtonian materials are characterized by a

viscosity which may depend on temperature but is

independent of the shear rate (and shear stress).

In contrast, the viscosity of non- Newtonian

materials depends on the shear rate. For most

non- Newtonian materials the viscosity decreases

with increasing shear rate. This behaviour is called

shear thinning, or pseudoplastic. A material which

viscosity increases at increasing shear rates is

called shear-thickening or dilatant.

Materials that do not flow until the applied shear

stress surpasses a certain value are said to have

a yield-stress.

Rotational viscometers Using a rotational viscometer, the viscosity is

calculated from the measured torque and

rotational speed as well as the dimensions of the

measuring geometry. If the measuring geometry

fulfils certain requirements (e.g. small gap), which

is the case for coaxial cylinder, plate/plate and

cone/plate measuring geometries (DIN 53018, DIN

53019...), the absolute value of the viscosity can

be calculated.

If the dimensions of the measuring geometry are

not well defined, only a relative value for the

viscosity can be determined. In this case, the

measured viscosity value not only depends on the

ambient conditions, but also on the test method,

i.e. the measuring geometry.

Falling ball viscometers The falling ball viscometer is a conventional and

highly accurate instrument for the determination of

the absolute value of the viscosity of a Newtonian

material. The viscosity can be calculated from the

falling time of the ball, the density of the ball as

well as the diameter of the tube and the ball.�

Shear Rate

The brochure provides full product specifications, accessories and measuring sensor systems available.

A full copy of the Viscometer brochure is available on request.


89

polymer industries

• new product brochures

HAAKE PolyLab OS - Open System

Measuring Mixer and Extruder

System from Thermo Scientific

The HAAKE PolyLab OS provides process relevant

material data including:

• Melting behaviour

• Influence of additives

• Shear stability

• Temperature stability

• Melt viscosity

The torque rheometer supports process modelling

activities such as:

• Compounding polymers with additives to

reduce flammability, viscosity, etc.

• Scale-up extrusion processes by using

different L/D ratios to extrapolate to your

master process line.

• Simulating master processes using only as

little as 50 g of material to optimise extrusion

or mixing in respect to temperature and shear

profile

• Extrusion of strands, profiles or films in

combination with rheological or optical

measurements

HAAKE POLYLAB OS-SYSTEM

Twin-Screw Extruder

Single-Screw Extruder

Mixer

Additional Analyzing Sensors

Feeding Systems Rotors Screws Dies Postex

Controller PC / Software

HAAKE PolyLab OS – Measuring Mixer Typical Investigations

• Testing the melting and degradation

behavior of polymer melts

• Quantifying viscosity when adding

nano-particles or other additives

• Testing the gelation- and plasticizing behavior

of PVC dry-blends

• Measuring the fl ow- and curing behavior of

thermosetting plastics

• Characterizing the infl uences of different

additives such as carbon black, fi llers,

lubricants, accelerators or sulphur for rubber

mixtures


behavior of elastomers

• Measuring the oil absorption of carbon black

• Quantifying the absorption of DOP for PVC

dry-blends

• Measuring the stable torque in regard to

individual and combined infl uences of fi llers

and additives such as stabilizers, lubricants

and color pigments

• Testing high performance plastics to check

processability


measurements for rubber mixtures

This allows you to optimise your process

parameters, create test specimens or perform

quality control on incoming and outgoing goods for

viscosity, dispersion or plasticising behaviour.

The brochure provides full product specifications,

accessories and measuring sensor systems

available. A full copy of the HAAKE PolyLab OS

brochure is available on request.�

biennial 07-08


• product news & industry applications

New device for rheological measurements - A measuring cell for special mortars Reproduced with the permission of BFT International – Concrete Plant & Forecast Technology (P 552, 01/08). www.bft-online.info

Both quality and quantity of

rheological tests are mainly

determined by the available

range of measuring cells.

In this field, unmet needs exist

especially with respect to

building materials testing.

This article describes one of

these cells that are suitable

for highly flowable mortars.

This so-called basket cell

enables fluid-in-fluid shear,

and thus suppresses wall

shear effects. The basket cell

has been designed as a double

annular gap cell ensuring high

performance at low yield

stresses.

Working principle Under the assumption that solids of revolution can

be used to create an appropriate shear area (see

DIN 53018 or 53019), it must be observed, as a

restrictive condition, that aqueous fluid may

segregate at the interfaces when subjected to

compression and/or shear. From a processing

point of view, this is often a useful characteristic of

mortars. However, this behavior results in the

well-documented wall shear in the measuring cells

referred to above, and thus leads to a distortion of

measurement results. This effect may be limited

by providing the measuring cells with a special

surface texture, such as a ribbed pattern. Another

possible solution could be to replace the adhesive

fluid-wall bond with a cohesive bond. When

pursuing this idea further, at least the critical cell

walls would have to be replaced with fluid walls.

Following a large number of various experiments

to create such cell walls, i.e. a “fluid-in-fluid

shear” using external fields of force and the

correspondingly high effort, the experience gained

has been used to identify an easy-to-implement

compromise solution. The setup comes very close

to fluid-in-fluid shear if the intended fluid wall is

established by means of a filigree framework. If a

cylindrical framework is chosen – which would

inevitably create an inner and outer fluid wall leaf,

it would appear logical to also look for a solution

similar to a double annular gap cell.

Measuring cell design

The double annular gap geometry is a favorable

design not only on the basis of the considerations

outlined above. It is also a suitable option because

of the anticipated low limit yield stresses that

result from the stability criterion [1] for

self-compacting mortars (SCM).

Co-axial double gap measuring cells are not a new

invention. For example, DIN 54453 recommends

the use of such a cell to determine the dynamic

viscosity of anaerobic adhesives. While the cell's

basic design is retained, its inner cylinder forming

the double gap is replaced with the framework

referred to above. As a result, the new measuring

cell consists of an annular gap vessel – as shown

in Fig. 1 – and the basket-like framework forming

the sensor (Fig. 2). The framework is enclosed by

a disc-shaped keyseat at the top and stiffened by

an annular insert at the bottom. Following the infill

of mortar into the annular gap vessel, the sensor

will be moved coaxially, at low speed, to its

measurement position. The fluid displaced during

immersion can run off through the leveling

openings of the sensor to fill the overflow

receptacle of the annular gap vessel. The effective

shear height L is determined by the immersion

depth of the basket into the “fluid bath” in the

annular gap space.

This cell setup has been subjected to numerous

tests, in particular with respect to determining

relative gap widths and framework designs. In

order to ensure a sufficiently stable bottom flow in

the gap against the impact of inertial forces, an

instrument drive similar to the Hatschek device

was used.

On this basis, diamond-shaped framework mesh

structures were found to be particularly

well-suited. These also allow for particle

incorporation while ensuring a strong bond

between the inner and outer fluid interface of the

mortar attached on both sides.

For mortars with a maximum particle size (mesh

aperture) of 2 mm and a permissible oversize of

up to 2.5 mm, tests involving various wall

distances in the range 32≤ (4Δ ≈ D4 - D1) ≤8dK,max

demonstrated extreme measuring fluctuations, up

to a total standstill of the cell, only at the lowest

distances. This effect was caused by a more or

continued on page 92�

construction & building industries

Above Left: (Fig.1) Section of the fluid-filled annular gap vessel of the measuring cell.

Above Right: (Fig. 2) Photo of the measuring cell sensor (1) Coupling adapter (2) Mesh lining

(3) Openings for fluid leveling

L D1

D4

Mitn

ehm

er-N

ut

‹berlauf-Tasse

1

2

3

L

D3


91

New servicefor rheologicalmeasurements� continued from page 91

less significant wedging of the natural particles

used. The wall distance ultimately chosen to

determine the main dimensions equals

Δ ≈ 3dK,max, and is usable only in conjunction with

the framework design shown in Fig. 2.

Further design features were determined on the

basis of a rather pragmatic approach. These

include the position and design of the overflow

receptacle and the minimization of the total weight

of the annular gap vessel. These features also

include the sensor immersion depth, which was

determined at T [mNm] =τ [Pa] on a preliminary

basis to enable a quick overview in the course

of individual measurements.

Prior to its use, the measuring cell must be

calibrated. It is always advisable to calibrate the

cell together with the other instruments available.

Findings and outlook

According to the experimental results obtained to

date, the basket cell is suitable for all highly

flowable fluids that are characterised by several

phases, such as self-compacting mortars, grouting

mortars, float finishes and fillers, as well as

cementitious binder glues, ceramic slips, slurries

of all types, and paints. Solutions can also be

subjected to testing. As a prerequisite to any

rheological materials testing, the object to be

tested must be stable. This is also required for the

setup described in this article.

The experience gained in the course of

development, testing and application enables

continuous improvement of the basket cell

depending on the specific requirements.

This includes both the main dimensions of the

measuring cell determined by varying maximum

particle sizes and the adjustment of the framework

structure to special modes of application.

Prof. Dr.-Ing. habil. Ruprecht Vogel

Malerstieg 6

99425 Weimar / Germany

[email protected]

References andfurther information

[1] Vogel, R. Ein Stabilitätskriterium für Selbstverdichtenden Beton, BFT Betonwerk+Fertigteil-Technik 12 (2005), S.42 bis 49 .

[2] Vogel, R.; Riedel, M. Untersuchungen mit dem Rotationsviskosimeter RHEOTEST 2 zur Abgrenzung des Einsatzbereiches ,Silikattechnik 41 (1990), Heft 2, S.59...64

[3] Vogel, R. Stabilität und Fließverhalten von Selbstverdichten-dem Beton, Vortrag Ibausil Weimar Sept. 2006, Druck Bd.2, S.1047...1058

[4] Vogel, R. Fließen von Selbstverdichtenden Beton – Das Fließgesetz; www.vogel-labor.de (Mitteilung 04/6)

• product highlight – industry application

The industry choice for viscosity measurements of mineral slurries & suspensions

mining industries


Viscotester model VT550

viscometer is suitable for

viscosity measurements of

particular suspensions using

standard sensors to provide

relative or absolute results

which are highly reproducible.

The HAAKE VT550 viscometer:

• Provides the data to allow accurate

calculations for pumping slurries and

suspensions

• Can be operated manually by the key pad

or PC controlled

• Measures yield points using Controlled

Deformation (CD) mode

• Measures inhomogeneous materials with

particles in mm size

• Records flow curves automatically to monitor

the flow behaviour of a liquid or paste

• Has interchangeable rotors to extend the

measuring range and application

• Can be upgraded to a coaxial- or cone and

plate viscometer.

The HAAKE VT550 provides results on viscosity

and yield point which allows you to:

• Correctly size pumps

• Minimise wear in pipes & fittings

• Identify start-up energy requirements for

pumping

• Predict the longevity of hydraulic transport

equipment

• Design better disposal systems�

HAAKE ViscoTester VT550

biennial 07-08



Food Industry feature








within the food industries.

ServicesAn extensive range of technical articles have been


the food industry, these include:

• Food and Beverage Material Characterisation

- Introduction to the influences of rheological

and process parameters. Rheo 025TP

• Comparison of Rheological Techniques for

the Characterisation of Semi-Solid Foods.

(Rheo 027TP)

• Application of Liquid and Solid Rheological

Technologies to the Textural Characterisation

of Semi-Solid Foods. (Rheo049)

• QC Measurements for Liquid Food Products

and Packaging. (Rheo051)


of Mouthfeel. (Rheo253)


of Shelf Life. (Rheo254)


of Processability. (Rheo255)


of Cohesiveness, Cohesion Strength and

Cohesive Quality. (Rheo256)


& Viscosity. (Rheo358)


(Rheo360)

• Tim’s Top Tips – How to Measure Yield Stress.

(Rheo362)


Solutions for the Food Industry is available. Copies

of the technical papers and the solutions kit are

available on request from Rheology Solutions.

special issue

ProductsRheological parameters are reliable pointers for

food performance and are critical factors for

processability and product quality.


and product performance within the food

industries.

There are a range of instruments and measure-

ments that can be used to quantify rheology

related challenges (processes or consumption)

some of which may be described by the following

terms:

• adhesion • build

• cohesion • cover

• crispiness • elasticity

• mouthfeel • spread

• stringiness • viscosity

• and many more

Rheology Solutions will be exhibiting at Foopro

(stand no. 6084) in Sydney in July 2008, and

following is an overview of the products and

services that will be available at the stand and

fully operational during the exhibition.

food industries


93

The Marimex range of

ViscoScope process

viscometers measures the

viscosity of liquids continually

and precisely in-line.

The ViscoScope provides continuous measure-

ments during food processing to ensure

manufacturing is always monitored and

adjustments are able to be made to keep the

product within its viscosity specification range,

eliminating waste and out of specification

products.

The Marimex range of ViscoScope systems

provide maintenance free viscosity

measurement for in-line applications within

the food industry. Installations in the food

industry currently include: Chocolate, Dairy,

Gelatin, Pectin, Pipeline monitoring, Slurries,

Spray dryers and the Sugar industry.

Features include:• Smooth rugged sensor

• Virtually no moving parts

• High precision, no operator required

• product focus

Process Viscometer• Factory calibrated with NIST traceable oils –

in house calibration not required

• Flexible mounting – works in any direction

• High temperature capability to 450°C

• High pressure capability to 5,000 Psig/350 bar

• Flow rate fluctuations do not have any

influence on accuracy of data

• LAN diagnostic systems control

ViscoScope viscometers manufactured by

Marimex Industries (Germany) are available for

process applications up to 450ºC and 350 bar.

The sensor has torsional oscillation rotation

and is constructed without any moving parts

avoiding any cross contamination with the

material being measured.

The sensor can be mounted in any orientation in

reactors, vessels and pipes for measuring in batch

and continuous processes.

All measurements are precise, reliable and

reproducible making the ViscoScope ideal for all

applications within the food industry.

food industries


Viscotester series provide

accurate viscosity results for

QA/QC in the laboratory ensur-

ing quality control throughout

the manufacturing process.

The HAAKE Viscotester 6L plus is a classic

rotational viscometer for QA/QC applications and

provides fast determination of viscosity as defined

in ISO 2555 and many ASTM standards.

The Viscotester VT6L plus is one in the range of

HAAKE viscometers suitable for viscosity testing

applications within the food industry.

• product focus

Rotational Viscometer

Model Viscotester 6L plus

Viscosity range 3 – 6,000,000 mPas

Accuracy +/- 1% full scale

Reproducibility +/- 0.2%

Standards ISO 2555 (+ others)

ASTM 115, 789, 1076

Features• RS232 interface for data transfer to a PC

for evaluation

• Digital display with viscosity, torque, speed

and spindle readout

• Supplied complete with spindles, stand

& carry case

Options• Model VT6R plus which differs in the torque

by a factor of 6, i.e.: 20 - 40 000 000 mPas

food industries

The VT6L plus offers great value for money, high accuracy,

ease of use, good design and software options

Marimex ViscoScope in-line measurement system

provides continuous viscosity results and has been designed

for maintenance free operation in process applications

biennial 07-08



CaBER 1 is a Capillary Breakup

Extensional Rheometer which

measures the extensional

properties of samples to

optimise filling and spatter

behaviour during filling

processes.

Knowledge of the elongational behaviour of fluids

is important for both industrial and basic research

purposes. Complex flows that contain strong

extensional components occur in many industrial

processes and applications. Some examples are

extrusion flows, coating flows, contraction flows

and fibre spinning flows. Most materials exhibit

very different responses in an extensional flow

compared to a shearing flow. The thinning and

breakup of a fluid filament that is analysed with

the HAAKE CaBER 1 instrument provides valuable

information about the materials physical properties

that rotational rheometers simply can not provide.

• product focus

Extensional Rheometer

Model CaBER 1

Hencky Strains: up to 0 = 10

Strain Rate Range: Imposed strain rate

0.01 < 0 < 300 s-1

Fluid strain rate

10-5< 0 < 10 S-1

Shear Viscosity Range: 10 - 106 mPas

Plate Diameter: 4 < Dplate < 8 mm,

standard = 6mm

Temperature Range: 0 - 80ºC

Diameter Resolution: 8 μm

System Response Time: 10 ms

Features• Computer controlled

• Class 1 laser micrometer

• Easy to operate and easy to load samples

and clean

• Linear motor drive with variable speed

• Closed temperature-controlled sample

chamber

• Automatic repeated testing

• Exchangeable geometries

• User defined strains

• Sample volume <0.2ml

food industries

The HAAKE CaBER 1 is the only commercially available rheometer for measuring extensional properties

• product focus


Model ThermoFlex 900

Setpoint Temp Range +5ºC to +40ºC

Ambient Temp Range +10ºC to +40ºC

Temperature Stability +/- 0.1ºC

Set Point Cooling

Capacity @ 20ºC 750 W (2560 BTU) at 50 Hz

Reservoir Volume 7.6 L

Pumps PD1 8 lpm @ 60 psi

PD2 13.2 lpm @ 60 psi

Features• Auto refill

• Anti-drainback

• DI resistivity internal

• Pressure relief

• Flow control

• Pressure/Flow control

Other Models - 1400W and 2500W units

available.

food industries

The Thermo Scientific NESLAB

ThermoFlex range are reliable,

easy to use chillers and is

suitable for diverse and

demanding applications.

NESLAB ThermoFlex 900 recirculating chiller

delivers a continuous cooling capacity up to 900

watts.

The NESLAB ThermoFlex range features a robust

refrigeration system designed for continuous use

in a variety of environments. The recirculation

system incorporates highly reliable plumbing

connections to eliminate leaks. Integrated air and

fluid filters minimise wear to mechanical parts and

improves system reliability.

A reliable, easy to use chiller

for diverse and demanding

applications


95

Thermo Fisher HeatTech 26L

heating bath circulator operates

from ambient to +100ºC.

It is a reliable and economical unit that provides

flexibility to laboratories as either a fluid bath or

circulator.

Features• Large bath area accommodates more

samples

• Quiet system



• Safety level for fluid and temperature


• product focus

Heating Bath Circulator

Model HeatTech 26L

Temperature Range Ambient to +100ºC

Temperature Accuracy +/- 0.02ºC


Pump Pressure (max) 300 mbar

Pump Flow Rate (max) 12.5 lpm

Bath Volume 26 L

Order Today - delivery ex stock

$2,399excluding GST and local delivery

• product focus

Refrigerated Bath Circulator

Model CoolTech 320

Temperature Range -28ºC to +100ºC

Temperature Accuracy +/- 0.02ºC

Heater Capacity 2.0 kW

Cooling Capacity @ 20ºC 320W

Pump Pressure (max) 300 mbar

Pump Flow Rate (max) 12.5 lpm

Bath Volume 4.5 L

Order Today - delivery ex stock


food industries

food industries

A reliable and economical unit that provides flexibility to laboratories as either a fluid bath or circulator

Thermo Fisher CoolTech 320

refrigerator bath and circulator

operates at -28ºC to +100ºC.

A versatile and economical

option for laboratory cooling.

Features• Rapid cool down and heat up times



• CFC-free refrigerant system

• Safety level for fluid and temperature


A versatile and economical option for laboratory cooling

biennial 07-08



Food industry feature & product focus

Rheology Solutions offer material characterisation

solutions to measure, monitor and provide

reproducible data for quality control, development

and product applications that will improve

performance with the food industries.

A four page overview of products and services

specifically available for food industry applications

has been produced.�


Material characterisation for polymers

No matter what stage of the polymer’s life cycle,

eliminating waste and keeping production levels at

peak capacity are crucial to ensuring profitability

in today’s highly competitive environment.

This brochure from Thermo Scientific provides a

comprehensive overview of products to cover:

• R&D of new polymers

• Lab scale process, pilot plant and small

scale production

• Quality control�

food industries


Extrusion & material characterisation for drug development & production

In material characterisation rheological properties

are of the utmost importance for the determination

of the best drug format. The ability to analyse and

describe the material’s mechanical or formulation

properties can have a direct impact on precise


Bath recirculators

polymer industries

dosing and optimisation of the manufacturing

process.

This brochure from Thermo Scientific provides a

comprehensive overview of products to cover:

• Extrusion technology

• Material characterisation�

pharmaceutical, cosmetics& allied industries

all industries

The Thermo Scientific NESLAB RTE and EX Series

of bath circulators brochure have been updated to

incorporate more product and technical informa-

tion.

The NESLAB RTE Series of bath circulators cool

and heat from -25ºC to +200ºC and the NESLAB

EX Series of bath circulators heat from ambient to

+200ºC.�


97

Rotary Evaporators are widely

used in various R&D and QC

laboratories and also in

academia.

The main use of rotary evaporators is solvent

recovery from various mixtures by single step

distillation and they are sometimes used for

organic chemistry syntheses under controlled

temperature and vacuum.

The basis of this procedure is the evaporation and

condensation of solvents using a rotary evaporat-

ing flask under vacuum. Distilling products under

vacuum increases the performance and helps to

protect the products. Condensers are cooled using

tap water circulation or alternatively by cooling

recirculators.

To achieve optimal distillation conditions, the

distillation energy supply by the heating bath must

be removed by the condenser. To ensure this,

operate the instrument according to the following

rule of thumb:

Cooling water: max. 20ºC

Vapour: 40ºC

Bath: 60ºC

This rule can also be applied to lower bath

temperatures, for example:

Cooling water: max. 0ºC

Vapour: 20ºC

Bath: 40ºC

This is achieved by:

• Setting the bath temperature

• Setting the cooling water temperature. When

the cooling water is tap water, the tempera-

ture is sometimes (especially in summer)

above 20ºC. With the Thermo Scientific EZ

Cool 80 refrigerated recirculating bath

connected to the system it is easy to set the

cooling medium temperature to the desired

value between -10ºC to +20ºC.

• Allowing cooling tap water to flow through the

condenser at approximately 40 – 50 l/h. With

the EZ Cool 80, the recirculator flow is 720

l/hr (without loosing the cooling medium),

providing a better, stable and efficient heat

transfer.



Using Refrigerated Circulators with Rotary Evaporators – Environmentally Friendly Solution

receiving flask is also thermostated in a

cooling bath

• The spiral of the condenser is always clean

Ono 426-1624


Thermo Scientific EZ Cool 80, recommended for

Rotary Evaporators –the environmentally friendly

solutions

Prepared by: Onur Cebeci, Chemist, Anamed &

Analitik Group, Chemistry Technologies Depart-

ment, Turkey. References were taken from the

Rotavapor Operation manual, Buchi Labortechnik

AG, Swtzerland.�

• Defining the operating vacuum in such a way

that at the vacuum, the boiling point of the

solvent equals the vapour temperature. Refer

to the solvent tables provided in the rotary

evaporator manual.

Advantages associated with bath temperatures of

60ºC and below:

• The evaporating flask can be replaced without

risk of burns

• The evaporation rate of the water from the

heating bath is low (low energy loss)

• The heating bath energy is used at a good

degree of efficiency

Other Advantages using the EZ Cool 80:

• Environmentally friendly working conditions

since no waste of tap water at 40 – 50 l/h

• Four pre-set temperatures enables the

practical switch of solvents which evaporate

at significantly different temperatures

• Ability to distil solvents with boiling points

under room temperature, provided that the

biennial 07-08


A universal holder for sample containers which

can be used for the HAAKE MARS and the

RheoStress 6000 (as well as all of its predeces-

sors) has been developed. Thanks to the three

individually adjustable clamps, sample containers

like glass jars, cans, beakers, cups, etc., can be

mounted solidly onto the rheometer. This allows for

the insertion of a (vane) measuring geometry into

the sample without comprising its structure.

A copy of this brochure is available by requesting

P018e�

• product news & industry applications - product accessories

Universal container holder for HAAKE MARS and RheoStress 6000

all industries

Fig. 1 (above): Universal container holder with

three adjustable clamps (left),

Fig. 2 (right): Universal clamp holder with a peanut

butter glass jar mounted on the HAAKE MARS

with a vane rotor FL22 (right)

The rotational viscometers HAAKE Viscotester 6 &

7 plus are described in the standard ISO 2555. In

comparison to the HAAKE Viscotester 6, the

HAAKE Viscotester 7 is equipped with a tempera-

ture sensor and a serial interface. Both models are

available in two versions: whereas the ‘’L’’-version

is suitable for measurements on low and medium


Adapters for HAAKE Viscotester models 6 and 7 plus for measuring range extension and sample temperature measurement (optional)

all industriesviscose samples (3 up to 6.000.000 mPas) the

‘’R’’-version can be used for medium and higher

viscose materials (20 up to 40.000.000 mPas).

Using a low viscosity adapter (UL) the lower

viscosity limit can be extended. Reproducible

viscosity measurements can be performed down

to 1.0 mPas using the L-version respectively 6.4m

Pas for the R-version. It has to be taken into

account that high rotational speeds are needed for

measurements of very low viscosities and Taylor

vortices cause hereby can have a negative

influence on the experimental results.

For samples, which are available in small amounts

only, a small sample adapter can be used.

Depending on the Viscotester version used

different sets of cylindrical spindles are available

which have to be ordered separately.


P020-e�


UV curing cell for an individual arrangement of optical components

all industries

In order to measure a given sample’s rheological

properties before, during and after controlled

exposure to UV radiation, a cylindrical UV curing

cell has been developed for the HAAKE MARS,

HAAKE RheoStress 6000 rheometers and the

respective predecessor models.

The cylindrical UV curing cell has an outer

diameter of 48 mm and fits into fluid or electrically

controlled cylindrical temperature control units.

Any UV light source can be connected via light

guide (outer diameter 24.5 mm). The

UV light source should be capable of providing

different intensities in order to measure the

dependence of the curing behaviour as a function

of the light intensity applied. Moreover, the light

source should be equipped with a timer, a manual

control switch or a foot-operated switch as well as

a trigger input facilitating control of the light

source via the rheometer’s measuring software.


P-022e�


99

• SER – Extensional rheology system for HAAKE MARS

The SER system is a new accessory for the HAAKE

MARS with CTC oven which transforms a

(rotational) shear rheometer in an extensional

rheometer for melts and semi-solids.

The measuring principle of the SER system, which

was developed by Dr. Martin Sentmanat (Xpansion

Instruments), is based on clamping the sample on

two counter rotating windup drums. With the SER

system a truly uniform extensional deformation in

the sample is achieved. In additional to the uniaxial

extension, the SER tool can be used for solid

tensile testing, pear and peel testing, as well as

friction testing.

The operating temperature range of the SER tool

covers 0ºC to +250ºC.

The combination of convection and radiant heating

in the CTC guarantees fast temperature changes

and an even temperature distribution within the

sample.

The SER system is fully integrated in the HAAKE

RheoWin measuring and evaluation software.

Measurements can be made in both controlled

extensional rate and controlled tensile stress

mode. The extensional properties of the sample

are calculated automatically and presented directly

in the software.


P-019e�

Fig. 1 (left): SER tool integrated in Controlled

est Chamber

Fig. 2 (right): Schematic setup of the SER tool

all industries


Vane rotors for pressure cells for HAAKE MARS and HAAKE RheoStress 6000

all industries

Different vane rotors have been developed for

pressure dependent measurements on samples

containing particles. Each rotor consists of 4

blades mounted around a shaft, which is equipped

with two sapphire bearings.

With these bearings the rotors can be precisely

centred on two steel pins inside the pressure cell.

The vane rotors differ in the size of the blades. The

biggest vane rotor FL 25/90 has a diameter of 25

mm and a blade height of 90 mm. This rotor is

particularly suitable for measurements on low

viscous samples.

For measurements on samples with higher

viscosities vane rotors with a blade height of 8.8

mm are recommended. For choosing the suitable

rotor the diameters of the suspended particles

have to be taken into account. As a rule of thumb

the minimum width of the gap between the rotor

blades and the inner wall of the pressure cell

should be 3 times larger than the biggest

suspended particles.

The inner diameter of the pressure cell D100/200

is 40 mm. For example, using a FL36/8.8 vane

rotor the measuring gap between the rotor and the

inner side of the pressure cell is 2 mm. Therefore

a suspension with particles with a maximum size

of 0.6 mm can be measured. For bigger particles

a rotor with a smaller diameter has to be selected.


P-021e�

For the rheometers HAAKE MARS, RheoStress

6000 and predecessor models identical in

construction and equipped with a normal force

sensor, a measuring cell has been developed for

testing the tribological behaviour of bearing

materials.

The tribology cell described here consists of a

lower and an upper part. Both are made of

stainless steel. The lower measuring geometry is

• Tribology cell for HAAKE Rheometers

all industriesdesigned as a reservoir.

Measurement of the friction of bearing materials

with and without lubricant can be performed. To

measure the influence of a lubricant the reservoir

can be filled with the lubricant to be tested.

The upper measuring geometry is equipped with

a flexible shaft, which ensures the concentric

position of a ball with a diameter of ½” in the

measuring cell. Usually steel bearing balls are

used but other materials like e.g. ceramic are

also possible.

Replacing the ball is easily and quickly done,

to perform every test with a fresh ball as

recommended. For temperature dependent tests

between - 40°C and +200°C the lower measuring

geometry can be adapted on a modified

measuring plate cover for a Peltier temperature

control unit. Also the measuring cell can be

integrated into the Control Test Chamber by

adapting the lower measuring geometry onto

a suitable holder.


P-023e�

biennial 07-08


Thermo Scientific NESLAB ThermoFlex range

Two models have been added to

the Thermo Scientific NESLAB

ThermoFlex range. The range now

extends to 3500 W and 5000 W

cooling capacity at 20ºC.

The NESLAB ThermoFlex range is reliable, easy to

use chiller and is suitable for diverse applications

across all industry areas within QA/QC, R&D and

production applications.

The range offers 1400W, 2500W, 3500W and

5000W of cooling capacity and is the ideal chiller

for demanding cooling applications within the

polymer industry.

Options - Fluid Recirculation

• Pressure Relief – Allows for regulation of the

chiller’s outlet pressure and is available as an

internal or external option.


Extended product range - recirculating chillers

all industries

• Flow Control with Flow Readout – Controls flow

to the application and displays on the controller.

• Pressure Relief with Flow Readout – Pressure

relief valve allows for regulation of the chiller’s

outlet pressure and displays on the controller.

• Auto Refill – Allows for automatic refilling to

ThermoFlex 900 ThermoFlex 1400 ThermoFlex 2500 ThermoFlex 3500 ThermoFlex 5000

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

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

Temperature Stability ±0.1°C ±0.1°C ±0.1°C ±0.1°C ±0.1°C

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

Reservoir Volume 7.2 liters 7.2 liters 7.2 liters 7.2 liters 7.2 liters

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

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 -

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

P3 - Centrifugal Pump 50 Hz 10 gpm @ 20 psid 10 gpm @ 20 psid

P4 - Centrifugal Pump 50 Hz - - - 15 gpm @ 34 psid 15 gpm @ 34 psid

temperature setpoint

co

oli

ng

ca

pa

cit

y

BTU/Hr

°C

°F

Watts

7000

6000

5000

4000

2000

3000

10004000

8000

12000

16000

20000

24000

10 20 30 40

50 6040 70 80 90 100

3500 @ 50 Hz

3500 @ 60 Hz

5000 @ 50 Hz

5000 @ 60 Hz

temperature setpoint

co

oli

ng

ca

pa

cit

y

BTU/Hr

°C

°F

Watts

3500

3000

2500

2000

1000

1500

5002000

4000

6000

8000

10000

12000

10 20 30 40

50 6040 70 80 90 100

900 @ 50 Hz900 @ 60 Hz1400 @ 50 Hz1400 @ 60 Hz2500 @ 50 Hz2500 @ 60 Hz

Cooling Capacity for NESLAB ThermoFlex 900/1400/2500 Cooling Capacity for NESLAB ThermoFlex 3500/5000

ensure the proper fluid level is maintained.

• Anti Drainback – Prevents the reservoir from

overflowing when a chiller is installed below

the application.

• DI Water – Maintains fluid resistivity and is

available as an internal or external option.


101


Polymer Industry feature








within the polymer industries.

ServicesAn extensive range of technical articles have been


the polymer industry, these include:

• Quality Control in the Polymer Industry.

Introduction to cutting edge technologies and

their application in the polymer industry.

Rheo 023

• Rheology for the Rubber and Elastomer

Industries. Introduction to the influences of

rheological and process parameters and

methods for their measurement. Rheo 024

• Tim’s Top Tips – Explanation and Evaluation

of Compounding. Rheo 289


of Processability. Rheo 290


of Shark Skin. Rheo 291


of Die Swell. Rheo 292


and Viscosity Curves. Rheo 364


Rheo 366

• Tim’s Top Tips - How to Measure Yield Stress.

Rheo 368


Solutions for the Polymer Industries is available.

Copies of the technical papers and the solutions

kits are available on request from Rheology

Solutions.

ProductsPolymer processing includes unit operations such

as compression, injection and blow moulding and

extrusion through a variety of dies. Specifically for

the polymer industries, materials characterisation

is of critical importance (including fluid related

issues like sedimentation, time related structural

decay or build-up and post-cure issues like

strength of compression or extension) for

prediction and management of sharkskin, melt

special issue

fracture, calendering, die swell, melt homogeneity

and short- and long-term dimensional stability of

extrudates or moulded parts. These processes

depend on fluid rheological parameters such as

viscosity, viscoelasticity, creep and recovery, and

solid material properties such as behaviour under

various compressive and extensional loafing

conditions. Extensional flow properties dominate

processes where stranding occurs and influences

time, quality and energy requirements.

Material characterisation parameters are reliable

pointers for polymer performance and are critical

factors for processability and product quality.


and product performance within the polymer

industries.

Rheology Solutions exclusively offers a range of

instruments and equipment that can be used to

quantify rheology related challenges specific for

polymer applications.

Rheology Solutions will be exhibiting at Ausplas

2008 (stand no: 100) in Melbourne during October

2008, and also at 30 APS (stand no: 13) in

Melbourne during November 2008, and following

is an overview of the products that will be

available at the stand and operational.�

polymer industries

biennial 07-08


• product focus

Modular Torque Rheometer with Measuring Mixer

structural changes in the material, a Rheogram

can be used to investigate and verify reactions

of different additive types or concentration on

the samples melting behaviour.

The HAAKE PolyLab QC Rheomix 600 is used to

investigate:

• The melting and degradation behaviour of

polymers

• Viscosity when adding nano particles or other

additives

• Gelation and plastification behaviour of PVC

dry-blends

• Flow and curing behaviour of thermosetting

plastics

• The influence of different additives such as

carbon black, fillers, lubricants, accelerators

and sulphur for rubber mixers

• Masticating and vulcanising behaviour of

elastomers

• Oil adsorption of carbon black

• Adsorption of DOP for PVC dry blends

• Torque in regard to individual and combined

influences of fillers and additives

• Processability of plastics

• Electric conductivity measurements for rubber

mixers �

HAAKE PolyLab QC with Rheomix 600 Floor

Model

polymer industries


PolyLab QC with Rheomix 600

will be shown for the first time

in Australia in October.

The HAAKE PolyLab QC is a new modular torque

rheometer which can be connected to an

interchangeable measuring mixer, single screw

extruder or conical twin-screw extruder.

A typical mixer test is run at a defined rotor speed

(shear rate). The material’s response to the shear

is recorded as torque and displayed versus time.

Although the temperature of the mixing

chamber is constantly controlled, the material’s

melt temperature during a test may rise due to

the shear introduced. The recorded “Rheogram”

(torque and melt temperature vs. time at constant

speed) is characteristic for different material types

and blends. It can be used as a fingerprint in

quality control for outgoing and incoming product

inspections. As changes in torque are related to

• product focus

Modular Torque Rheometer with Twin-Screw Extruders

HAAKE PolyLab with extruder shown as a bench

model unit


PolyLab QC with the HAAKE

CTW 100 QC twin-screw

extruder is used for continuous

compounding and plasticising is

the ideal extruder in the HAAKE

PolyLab QC system.

This is a counter rotating conical twin-screw

compounder, with intermeshing screws, that will

give well-defined residence time for faultless

production of process-critical polymers.

The gentle but intensive dispersing capabilities are

ideal to mix additives and pigments. Dies and

downstream ancillaries are compatible with the

19/25 QC-D single-screw extruder.

polymer industries Applications • Testing of the plasticising behaviour

• Testing the performance of additives and fillers

• Measuring of the melt temperature and

pressure along the barrel to optimise process

parameters

• Provide a homogeneous and constant flow melt

• Production of strands, sheets, cast and blown

films

• Extrusion of ceramics and feed stock

• Melt rheology

Features • Rod dies & water bath for strand extrusion

• Sheet & ribbon dies

• Blown film dies & take off tower

• Filter test

The HAAKE PolyLab QC is available as a bench

or floor model . �


103

The PRISM EuroLab 16 mm

operates with sample batches

of 50 g up to outputs of

10 kg/h., the bench mounted

16 mm twin-screw extruder

is the heart of a complete

compounding and sample

preparation system.

The segmented screw configuration with modular

barrel design give flexibility for the full range of

polymer processes.

A horizontally split barrel, up to 40:1 L/D, has a

lift-off top half for easy access to the screws, and

the screws themselves have a simple removal

device for cleaning and configuration changes.

Thermo “fuzzy logic” heater controls save energy.

The segmented top barrel half is constructed in

modules and is easy to reconfigure. Barrel

segments are available for feeding solids and

liquids or for venting. Secondary feeders and

vacuum pumps can form part of the system.

A rugged colour touch screen interface incorpo-

rates data acquisition as standard, with an option

to download to a remote computer for archiving

and analysis. The controls include recipe storage

to programme set points for repeatable process

conditions.

During October in Melbourne at Ausplas, the

PRISM EuroLab 16 mm system will be operational

extruding and pelletising a range of plastic

samples.�

• product focus

Modular Twin-Screw Extruder

polymer industries

The most common method in processing polymers

are screw plastification and injection moulding,

and The Thermo Scientific HAAKE PolyLab QC with

• product focus

Modular Torque Rheometer with Single-Screw Extruder

single-screw extruder is the ideal torque

rheometer for this application.

For testing quality and processability of those

materials, the single-screw laboratory extruder

19/25 QC-B is a proven tool.

polymer industriesTo shape a polymer for further processes and tests, different dies can be adapted to the extruder. Rod dies and water bath for strand extrusion, sheet and ribbon dies in various dimensions to produce bands or cast films, and blown film dies and take off tower complete the testing equipment.�

SpecificationsBarrel Length L/D 25:1 25:1 40:1 40:1

Barrel Bore Diameter mm 16 16 16 16

Screw Diameter mm 15.6 15.6 15.6 16.6

Channel Depth mm 3.3 3.3 3.3 3.3

Centre-line Spacing mm 12.5 12.5 12.5 12.5

Centre-line to Radius ratio 1.56 1.56 1.56 1.56

Maxiumum Screw speed rpm 500 1000 500 1000

Motor Power at Maximum Speed kW 1.25 2.5 1.25 2.5

Torque per shaft Nm 12 12 12 12

Torque/(C-line3) Nm/cm3 6.1 6.1 6.1 6.1

Barrel zones 6 6 10 10

Heater rating W 5x350 5x350 9x350 9x350

Die heater rating W 250 250 250 250

Extruder Dimensions 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

Scale-up data

Internal Free Volume cm3 68 68 109 109

Peripheral Surface Area cm2 316 316 505 505

Surface Area per Unit Free Volume m2/1 0.47 0.47 0.47 0.47

Typical output kg/h 0.5 to 5 0.5 to 10 0.5 to 5 0.5 to 10

Services

Electrical power Volt/ph/amp 220V/1ph/20A 400V/3ph/20A 220V/1ph/25A 400/3ph/25A

Cooling Water 20ºC Litres/min 5 5 5 5

Thermo Fisher PRISM EuroLab 16mm

Twin Screw Extruder

biennial 07-08


• product focus

Web Inspection System

The OCS Web Inspection

System FSP600 is a modular

surface inspection system

for use in production.

The modular concept permits the use of several

cameras working in parallel so that optimum

adaptation can be achieved. The FSP600 is

suitable for transparent, translucent and opaque

films, sheets, coated web material, industrial

textiles, paper and non wovens. The system will

detect holes, thin spots, bubbles, contamination

and gels, foreign particles, black specks,

scratches, die lines, burst bubbles, repeated

defects, insects, burns and folds.

Fields of application• Films (transparent, translucent, opaque ...)

• Sheets • Coated web material

• Industrial textiles • Paper

• Non wovens

polymer industries

The OCS Pellet Inspection

PS25C will be operational

during the Ausplas 2008 in

October in Melbourne

inspecting a variety of

transparent and opaque pellets

for impurities, foreign bodies,

and/or colour deviations.

Applications• Opaque pellets

• Coloured pellets

• Non-transparent pellets

• Transparent pellets

• product focus

Pellet Scanner

polymer industriesTechnical DataResolution from 20 μ

• Camera - 3 CCD chip colour matrix camera

• Lighting - High Frequency synchronised

fluorescent lamp. Power consumption:

22 W. White light spectrum

• Computer - Industrial CPU Pentium, up-to-date

technology

• Interfaces 0 Ethernet 10/100 M Base-T, Digital

and analogue I/O, USB, MODBUS, PROFIBUS,

RS232, OPC, DDE, SAP interface or SQL

• Remote control - Extender max. 100 m.

Service Remote control

• Software - Operating system Windows XP

• Size - Dimension (l, w, h) 50 x 50 x 80 cm ,

Weight approx. 30 kg

• Connection values - Power 230 V AC / 50 Hz

• Temperature - +10°C – +40°C �

Optical Control Systems PS25C

Pellet Inspection system

Types of defects• Holes • Thin spots • Bubbles • Contamination & gels

• Foreign particles • Black specks • Scratches • Die lines

• Burst bubbles • Repeated defects • Insects • Burns

• Folds �

Optical Control Systems

FSP600 Web Film Inspection System


105

Name: .................................................................................................................................... Title: ...........................................................................

Company: ............................................................................................................................... Department: ...............................................................

Street: ..............................................................................................................................................................................................................................

Suburb: ................................................................................................................................... State: ................................... Postcode: ...................

Telephone: ....................................Fax: .................................... Email: ........................................................... please send me future issues by email

From the Biennial 07-08 issue of RheoTalk, I am interested in the following:

• Application Notes

Tim’s Top Tips – How to Measure... Series

Mineral Industries (please select) Thixotropy Yield Stress Flow & Viscosity

Food Industries (please select) Thixotropy Yield Stress Flow & Viscosity

Polymer Industries (please select) Thixotropy Yield Stress Flow & Viscosity

Surface Coating Industries (please select) Thixotropy Yield Stress Flow & Viscosity

Pharmaceutical, Cosmetic & Allied Industries (please select) Thixotropy Yield Stress Flow & Viscosity

Building & Construction Industries (please select) Thixotropy Yield Stress Flow & Viscosity

Chemical & General Manufacturing Industries (please select) Thixotropy Yield Stress Flow & Viscosity

Tim’s Top Tips – Explanation & Evaluation... Series

Tim’s Top Tips for Food Industries (please select) Mouthfeel Shelf Life Processability Cohesiveness

Tim’s Top Tips for Surface Coatings (please select) Shelf Life Flow & Levelling Misting Mixing & Blending

Tim’s Top Tips for Polymer Industries (please select) Compounding Shark Skin Processability Die Swell

Rheology Solutions Information Kits (please select) Mineral Industries Food Industries Surface Coatings Polymer Industries

Chemical & General Manufacturing Construction & Building

Pharmaceutical, Cosmetics & Allied Industries


A New Approach to Rheological Modelling of an Electrostatic Ash & Water Mixture - Quadratic Law - RF-300902-SI-01

A New Definition on Reactor Temperature Control with the Highly Dynamic HAAKE DynaMax System - TC06-01

A Numerical Study of Temperature & Shear Flow in a Transiently Loaded Lubricant Film - RS-180902-SE-01

Application of Liquid and Solid Rheological Techniques to the Textural Characterisation of Semi-Solid Food - Rheo049

Breaking Strength of Chocolate - V222

Cellulosic Derivatives in Capillary Break-up. Influence of the MWD & Gel Particles - V219

Comparison of Rheological Techniques for the Characterisation of Semi-Solid Foods - Rheo027TP

Characterisation of the Thixotropic Behaviour of Semi-Solid Foodstuffs - RF-110902-JO-01

Correlation Between Mixer Tests & The Extrusion Behaviour of PVC Dry Blends - LR60

Correlation of Misting During Printing with Extensional Rheological Investigation on Offset Printing Inks - V208

Dynamic Master Curves of Polymer Modified Asphalt From Three Different Geometries - RF-110902-JO-01

Evaluating the Plasticisation Process of Different Soft-PVC Samples - LR59

Experimental Influences on the Casson-Viscosity. The Casson Yield Point for Chocolate Testing - V129

Food & Beverage Material Characterisation - Introduction to the Influences of Rheological and Process Parameters - Rheo025TP

High Quality Pharmaceutical Films - OCS007

Please post or fax this form to:Rheology Solutions Pty Ltd - PO Box 754, Bacchus Marsh, Victoria, 3340

Phone: 03 5367 7477 • Fax: 03 5367 6477 • Email: [email protected] • Website: www.rheologysolutions.com

rheotalk biennial 07-08


RHEO405

biennial 07-08

Name: .................................................................................................................................... Title: ...........................................................................


Street: ..............................................................................................................................................................................................................................





How to Select the Most Suitable Sensor for Your Application - V166

Improved Torque Sensitivity & Normal Force Resolutions for Routine Measurements - V231

NanoComposites - Examples on Compounding of Nanoclay Blends in Twin Screw Extruders - LR62

New Measuring Cell for UV Assisted Thermal Curing at Elevated Temperatures - HA047

Online Close-Loop Monitors Four Cast Film Extruders During Production - OCS008

Online Quality Control of Polymers & Extruded Films - OCS004

Overview of Rheology-Based Process Challenges for the Mineral Processing Industries - Rheo014

Pharma MiniLab - Small Scale Compounder for Pharmaceutical Research - LR53

QC Measurements for Liquid Food Products and Packaging - Rheo051

Rheological & Microstructural Analysis of a Model Rennet Casein Gel as Influenced by Cooling Rate - RF-200902-US-01

Rheological Analysis of Powder Coatings - Paint & Resin Issue 3-2007

Rheological Analysis of Powder Coatings - V157

Rheological Behaviour of Automotive Paint Systems - Rheo008TP

Rheological Characterisation of Asphalt Binders - V-225

Rheological Characterisation of Tooth Paste - V142

Rheological Characterisation of Tooth Paste - COSSMA Article 9/2007

Rheological Investigation of Three Rubbers with Different Shore Factors with Respect to Their Shape Stability Before Curing - V169

Rheological Methods for Determining Molecular Weight & Molecular Weight Distribution - V230

Rheological Properties of Fresh Building Materials - V217

Rheology as a Tool for Immiscible Polymer Blends Characterisation: Interfacial Tension & Compatibilisation - RS-110902-BR-01

Slurry Rheology & Pipeline Transport Properties, an Overview - Rheo013

Small Scale Catheter Production - LR58

Solvent Trap & Double Cone System for Reproducible Results in Rheological Measurements of Low Viscous Volatile Fluids - V229

Test Methods for Characterisation and Optimisation of Recycling Polymers - LR45

The Influence of Thickeners on the Application Method of Automotive Coatings and Paper Coatings - Rheological Investigation - V206

The Rheological Properties of a Copper Concentrate Slurry: From Surface Chemistry to Pipeline Transport - RF-300702-AU-01

Thickening of Electrostatically Stabilised Latices by Ethyl Acrylate-Methacrylic Acid Copolymers with Various Molecular Weight - V026

Uncompromising Eyes - OCS005

Wet-Shotcrete of Refractory Castables - RS-290802-BR-02

What Happens When Rheological Properties Change? Looking into Theological Properties with Simultaneous Collection of Microscopic Images - V228

New Die Design for the Characterisation of the Extensional and Shear Properties of Polymers for Laboratory and On-Line Use - LR39

A Collaborative Study of the Structure and Rheological Properties of EVOH/SMA Blends Produced by Reactive Extrusion - LR42

Continuous On-Line Rheometry for Industrial Slurries - RF-200902-AU-01

Rheological Properties of Bitumen Modified with Polyethylene and Polyethylene Based Blends - RF-190902-ES-01





RHEO405

biennial 07-08

Name: .................................................................................................................................... Title: ...........................................................................


Street: ..............................................................................................................................................................................................................................





Small Scale Compounders for Pharmaceutical Research - PRISM004

Measuring Coatings - HA030

Rheological Measurements in the Coatings Industries - The Last 60 Years - Rheo050

Recent Developments in Bench-Top Twin-Screw Compounders - LR51

Quality Control in the Polymer Industry. Introduction to Cutting Edge Technologies and Their Application in the Polymer Industry - Rheo023

Rheology for the Rubber and Elastomer Industries. Introduction to the Influences of Rheological and Process Parameters and Methods for their

Measurement - Rheo 024

• Products

NESLAB CC Series of Immersion Coolers NESLAB EX Series of Bath Circulators

NESLAB HX Series of Process Chillers NESLAB RTE Series of Bath Circulators

NESLAB ULT Series of Ultra Low Refrigerated Bath Circulators NESLAB ThermoFlex Series of Recirculating Chillers

Temperature Control Range from NESLAB (please specify temperature range, application) ........................................................................................

Marimex ViscoScope In-Line Viscometer Marimex VA-330M In Line Slurry Sensor

Marimex ViscoView Software for Process Viscometer Optical Control Systems CR7/CR8 Chill Roll and Winding System

Optical Control Systems FSA100 Film Surface Analyser Optical Control Systems FSP600 Wide Web Inspection System

Optical Control Systems GM1 Gloss Meter Optical Control Systems HM1 Haze Meter

Optical Control Systems OP5 Online Rheometer Optical Control Systems PA-66 Pellet Analyser

Optical Control Systems PS-200C Online Pellet Scan System Optical Control Systems PS-25C Pellet Scan System (Colour Camera)

Optical Control Systems PSSD Pellet Size and Shape Distribution System Optical Control Systems PT-2C Powder Testing System

Optical Control Systems ST4 Sample Testing Unit Optical Control Systems APLAIRS Online FT-IR Spectrometry

Schleibinger BT2 Compact Rheometer Schleibinger Building and Construction Materials Testing Systems

Schleibinger Shrinkage/Expansion Unit Schleibinger Viscomat NT Rotational Viscometer

PRISM EuroLab 16mm Twin Screw Extruder PRISM Pharma TSG

PRISM PharmaLab 16 Extruder Continuous Granulation for Pharmaceutical Industry

PRISM Extruder Accessories PRISM Twin Screw Extruder Range (please specify application)

Thermo CoolTech 320 Cooling Circulator .......................................................................................................

Thermo HeatTech 26L Heating Circulator HAAKE CaBER 1 Extensional Rheometer

HAAKE Disposable Plate/Plate Geometry HAAKE Falling Ball Viscometer Type C

HAAKE MARS Modular R & D Rheometer

HAAKE MARS Accessories

CD-Mode Curing Measurement (PS001-e) Cone/Plate Exchangeable Geometries (P005-e)

Measuring Cell For Rheology of Building Materials (P006-e) New Solids Clamp (P004-e)

Rheological Measurement with Optical Analysis (P016-e) RheoScope Module





RHEO405

biennial 07-08

Name: .................................................................................................................................... Title: ...........................................................................


Street: ..............................................................................................................................................................................................................................




• Products

Sample Fixture for Bending & Breaking Tests (P014-e) Sample Loading Tool (P002-e)

SPIP Image Analysis Software for RheoScope Module (P009-e) Standard Liquids (P015-e)

Support Fixture for the Analysis of Textile Samples (P012-e) Trimming Tool (P003-e)

UV Curing Tool for CTC Oven (P017-e) Tribology Cell (P023-e)

Vane Rotors for Pressure Cells (P021-e) SER Extensional Rheology System (P019-e)

Universal Holder (P018-e) CR-Mode - Low Shear Rates (PS002-e)

UV Curing Cell (P022-e) HAAKE RheoStress RS6000 Universal Rheometer

HAAKE RheoStress RS6000 Sensor Systems HAAKE RheoStress RS6000 Accessories

UV Curing Cell (P022-e) Double Cone Geometry

Universal Holder (P018-e) Vane Rotors for Pressure Cells (P021-e)

Measuring Cell for Construction Materials(P006-e) Disposable Measuring Geometries (P010-e)

Tribology Cell (P023-e) HAAKE RheoStress 1 Controlled Stress Rheometer

HAAKE RheoWin Software HAAKE RotoVisco 1 Controlled Rate Viscometer

HAAKE Viscotester 550 Rotational Viscometer HAAKE Viscotester 550 Sensor System

HAAKE Viscotester VT1/VT2 Plus Hand Held Battery Operated Viscometer HAAKE Viscotester 6 Plus Rotational Viscometer

HAAKE Viscotester 7 Plus Rotational Viscometer HAAKE Viscotester 7 Plus Accessories

Thermal Printer (P011-e) Adapters (P020-e)

Sensor System for Viscometer/Rheometer (please specify model) ............................................................................................................................

Temperature Control for Viscometers & Rheometers HAAKE DC10-K10 Refrigerated Circulator

HAAKE C/DC Range of Circulators HAAKE DynaMax Viscometer Range Temperature Control Platform

HAAKE EZ Cool 80 Heating/Cooling Circulator HAAKE Fogging Test Equipment

HAAKE Phoenix Heating Circulator HAAKE Phoenix Refrigerated Bath

HAAKE TC-Line Water Recirculators HAAKE Temperature Control Catalogue

HAAKE MiniJet Injection Moulding Machine HAAKE Pharma MiniLab Micro Rheology Compounder

HAAKE MiniJet II Piston Injection Moulding System / Sample specimen preparation instrument

HAAKE MiniLab Micro Rheology Compounder & Reactor (20070712 - reference)

HAAKE MiniLab II Micro/NanoLab Compounder for small sample amounts

HAAKE PolyDrive Single Screw Extruder HAAKE PolyLab OS Torque Rheometer

HAAKE PolyLab OS Docking Station HAAKE PolyLab OS Upgrade Package

HAAKE PolyLab OS with Extruder HAAKE PolyLab OS with Mixer

HAAKE PolyLab QC Torque Rheometer HAAKE PolyLab QC with Measuring Mixer Rheomix 600

HAAKE PolyLab QC with Single Screw Extruder HAAKE PolyLab QC with Twin Screw Extruder CTW 100

Food Industry Feature & Product Focus Comprehensive Materials Characterisation for Polymers

Extrusion & Material Characterisation for Drug Development & Production Polymer Industry Feature & Product Focus





RHEO405

biennial 07-08

Name: .................................................................................................................................... Title: ...........................................................................


Street: ..............................................................................................................................................................................................................................




• Services

Calibration & Service. Please provide details on model of product and serial number: ................................................................................................

• Comments:

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biennial 07-08

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