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PolyLab® SystemTorque Rheometer, Extruders, Mixers

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● Flow and compoundingbehavior

● Critical processing pa-rameters of temperature,pressure, torque and vis-cosity

The PolyLab SystemIn The Application

The complexity of polymersand their blends is subjectto continuous development– this is also true of meas-urement technology.

PolyLab® System – The Complete System

sors (Slaves) such as meas-uring extruders and mixersdetermine the application.They are equipped withmeasuring and control tech-nology according to thespecific application and de-liver the necessary data tothe Master via a measuringbus system. This shared re-sponsability relieves the sys-tem, so more data can be

test results. Furthermorethe flexibility and applica-tion oriented system solu-tions are becoming moreimportant.

PolyLab System is the inno-vative, market-oriented con-tinued development of theThermo Haake Rheocordproduct range which fullymeets these requirements.

safely transported on thisdata highway and new appli-cations can be introducedeasily.This flexibility means thatthe test setup can be adapt-ed to exactly match therequired application whileensuring that your system isready for new applicationsin the future.

In Quality Control...

One has to carry out teststhroughout all stages ofprocessing like:

● Viscosity● Homogeneity● Additive dispersion

After all, your customerexpects a constant level ofproduct quality.Torque rheometers are usedto carry out these tests underprocessing conditions in thelaboratory – requiering onlysmall sample volume. Theyare designed to meet thehighest standards with re-gards to accuracy, handlingand reproducibility, for de-termining fast and reliable

In Research...

One has to determine theinteraction of his additivesin new formulations

● New UV stabilizers forthe automobile or con-struction industry

● Polymer additives tostarch for biodegradablepackaging materials

● Polymer-based ceramicsfor high-performanceinjection molded parts

The Process Technology ...

... has to carry out tests un-der in-the-field conditionsfor a more accurate determi-nation of processing charac-teristics such as:

Master And Slave ShareThe Intelligence

The PolyLab System con-sists of the Rheocord torquerheometer which includesall functionality for drivingand controlling the measur-ing sensors. It is the controlcenter for the external PC aswell as the other systemcomponents: “The Master!”Intelligent measuring sen-

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+ ++

Page 4 Page 6 Page 8 Page 9

Rheocord®Base Unit

MeasuringSensors

MeasuringDies

Postex

The PolyLab System Welcoming Thermo Haakeas your partner in rheometrymeans:

● Working out solutionstogether with our spe-cialists

● Support for installationsand software updates

● Advice and counselingand a reliable mobileservice support

For further information askfor our detailed data sheetsor speak directly to our spe-cialists.

The functionally orienteddesign particularly empha-sizes the integration of thebase unit and the measuringsensors to form a completesystem which has been real-ized within an ergonomicworking environment.

PolyLab System –Born From Experience

Thermo Haake can look backon decades of experience inthe field of rheologicalmeasurements. The PolyLabSystem has been designedon this basis together withexperienced Thermo Haakecustomers. It is a productwhich reflects ThermoHaake’s reputation for ap-plication-related solutions.

values are set accordingly.The measuring ranges ofthe sensors are also auto-matically adopted for meas-urement and calibration aswell as the test setup visuali-zation and the user inter-face. Manual pre-testing aswell as process optimizationare remote controlled bythe user from the positionwhere he or she has the bestoverview of the process.

Safety And Comfort

PLUG and PLAY is theconcept.Mobile mixer and extrudersensors mean easy and safeunit handling in the labora-tory. Once a measuring sensorhas been docked on to thebase unit, the Rheocord au-tomatically detects the con-figuration and all unit spe-cific limits and characteristic

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Rheocord® – The Base Unit

The Technology

A new modern control con-cept drives the measuringsensors enabling operationat the optimum drive work-ing point at any time.This results incharacteristic lineswhich meet thehighest require-ments of extremeapplicationssuch as hightorqueand/or highspeed. Torque

measurement is carried outvia a direct coupled torquemeasuring cell with an inte-grated amplifier developedspecially for the Rheocord.

Rheocord – one base unitfor all applications

The Rheocord base unitcontains all the parts of atorque rheometer which arerequired for driving themeasuring sensors andmeasuring the resultingtorque.

Interfaces enable communi-cation with:● the control and evalua-

tion module● the remote control● the measuring sensors

● external devices● networks

The flexibility of the meas-uring bus technology meansthat only this one unit isrequired for all current andfuture applications.Invest in the future!

This guarantees you:● special solutions for to-

day’s problems● the option of remaining

open for tomorrow’snew application

This ensures the highestlevel of measuring accuracyand fault safety for your ap-plication.All standard applications arecovered with the selectedmeasuring accuracy class.However, if you need an es-pecially high resolution inthe extreme application limitarea, we can supply you withinterchangeable, codedtorque sensors necessary forthis purpose. The drive con-trol and the transfer of themeasuring data is carriedout via an MS-WindowsTM

user interface with a realtime operating system anda field bus data transfer line.This is the main prerequi-site for safe data communi-cation and guarantees therequired data security.

Apart from the interfacesfor the field bus and the PC,three RS232C and two ana-log I/O interfaces are avail-able as standard for the pur-pose of connecting up to ex-ternal devices or networks.

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Comprehensive SystemSafety

System safety means safetyfor the user and the instru-ment as well as data integ-rity. This system safety isbuilt into the Rheocord withits control and monitoringmodules due to:

● complete safeguarding ofall rotating parts

● safety cut-off function ifrotating parts are exposed

● internal motor tempera-ture monitoring withcut-off warning andcut-off

● torque limit cut-off forthe drive unit and meas-uring sensors

● real time operatingsystem for data security

● real time fault handling- causes the system toreact promptly and in adefined way to alarmsignals

● on-line data storagewhich enables the inter-mediate storage of yourmeasuring data at anytime

● user defined start condi-tions which guarantee:- System safety due to e.g.the maintenance of tem-perature start conditions- a high degree of repro-ducibility- an automatic test pro-cedure

● easy-fit coupling and me-chanical safety lockingmechanism which ensure:- simple handling- quick preparation times

Comfort And Operation…

…begins with setting up theunit and ends with cleaning.In this respect, the Rheo-cord and its operating ele-ments are designed to offeroptimum working efficiencyin the laboratory.Once you have docked onthe measuring sensor, the

control module automat-ically recognizes therespective configura-

tion. This is displayedon screen and the oper-

ator is then promptedthrough the further con-

figuration of the measure-ment. The processing con-ditions are reached quicklydue to the self-optimizingtemperature control feature.The optimum operatingpoint for subsequent switch-ing to programmed opera-tion can be set “on location”via the remote control. Pre-defined start conditions en-sure that no limit values areexceeded. Once these con-ditions are fulfilled, themeasurement is started au-tomatically. After the meas-uring program has termi-nated, the unit switchesitself back to the user-

What do you do while thetest is running?

You can evaluate and docu-ment the previous measure-ment parallel to running thecurrent measurement(Fig.1) – our system featuresgenuine multitasking withregard to the soft- and hard-ware!You can also prepare a sec-ond measuring sensor forthe next docking maneuverparallel to the current meas

defined status. Cleaning canbe carried out after the au-tomatic data storage proce-dure.Cleaning tools can be locatedclose at hand and the clean-ing process can be startedvia the remote control.

- displaying faultmessages on screen at

all times even if themeasurement is being

carried out in the back-ground

Fig. 1

Torq

ue [

Nm

]

Time [min]

Tem

pera

ture

[°C

]

Safety Specifications

Technical Specifications

Motor power

Speed range

Torque range

Torque loadcells

Speed remotecontrol

Temperaturecontrollers

Interfaces

Mains supply

Dimensions(W/H/D)

Weight

7.5 kW (10 hp)

2 - 200 min-1

0 - 300 Nm

interchangeable

standard

integrated insensors

2 x analog I/O3 x serial

3 x 400/230 V50/60 Hz, N, PE, 63 A

42/125/95 cm

240 kg net

According to the laboratory instrumentstandard EN61010 T1 and T2.1.

● Safety warnings and cut-offs for:

– Motor

– Torque

– Control temperature

– Melt temperature

– Melt pressure

– Speed

● Electromagnetic compatibilityaccording to:

– EN50081

– EN50082 T2

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The Rheomix Family

R600 electric temperature controlup to 450 °C for: thermo-plastics, rubbers, thermosetsVolumes: 70 -100 ccm

R610 Liquid temperature controlup to 150 °C for: foodstuffs,ceramics

R3000 As for the R600 except for:Volumes: 300 - 540 ccm

R3010 As for the R610 exceptfor: Volumes: 300 - 540 ccm

R540 electric temperature controlup to 450 °C for: thermosetsChamber: conical Volumes:approx. 70 ccm

R200 Measurements carried out atambient temperature for: DBPabsorption of carbon black

Rheomix®/Rheomex® – The Intelligent Measuring Sensors

Rheomex & Rheomix – TheApplication Specialists

Thermo Haake offers acomprehensive program ofmeasuring extruders andmixers which can be attachedto the Rheocord base unit.These measuring sensorsdetermine the usage of thePolyLab system for yourapplication. Typical applica-tions in the polymerprocessing, foodstuffs andceramics industries include:

● Determination of theprocessing behavior

● evaluating processability● Formulation development● compounding● producing small profiles

and films for furthertesting

● rheological testing

Every measuring sensorcontains the necessarymeasuring, control andmonitoring technology forthe respective application.Rheomex and Rheomix con-trol the data administrationas well as the communicationwith the master unit via thedata highway. All measuringsensors are coded so thatthe master unit automati-cally senses which unit isconnected. The measuringsensor automatically informsthe base unit and thus theoperator of the configurationi.e. the number and positionof the temperature controlzones and measuring ports,unit-specific limit values aswell as the possible sensoroptions. The connectedpressure sensors are onceagain independently coded.

A new concept simplifieshandling in the laboratoryand enables secure opera-tion. This is characterizedby:● mobile measuring sen-

sors – avoid the necessityof handling of heavy andhot parts

● integrated heating andcooling circuits – reducethe number of plug con-nections and thus thedanger of making incor-rect connections

● several peripheral unitssuch as feeding and post-extrusion units are com-puter controllable –meaning better repro-ducibility and documen-tation

Rheomix – ExchangeableMixer Sensors

Mixer sensors are used totest processes such as themixing, compounding andplastifying of polymers,chemicals, ceramics andpigments under production-style conditions. ThePolyLab System used to-gether with the Rheomixmixer sensor producesrheograms from which pro-duction-related informationcan be derived such as:

● dynamic viscosity depend-ing on the shear load

● melt behavior in theextruder

● the influence of additives● temperature and shear

load behavior

Mixers used for standardapplications enable the test-ing of highly viscous sub-stances such as thermoplas-tics, thermosets and rub-bers. The electric heatingalso enables the measuringof high temperature plasticsup to 450 °C. They are ad-ditionally equipped with:

● exchangeable rotors● 3-piece measuring

chambers● compressed air cooling

The model equipped with alarger chamber volume isalso suited for producingsmall batches for furthertesting.If special demands are madeon the units when measuringyour products, Thermo Haakecan supply you with mixersensors and accessories

which can be individuallyadapted to suit the respectiveconditions such as:

● liquid temperaturecontrol

● special surface finishingsuch as wear protectionagainst abrasion orchemically aggressivematerials

● conical measuring cham-ber for hardening mate-rials

● pneumatic feedingdevices

● gas volume sensors forthe quantification ofpropellants during theplastification phase

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Rheomex – SpecializedExtruder Sensors

The extruder sensors of theRheomex range enable thedetermination of rheolo-gical variables as well as theexamination of processingcharacteristics and the pro-duction of polymer samplesfor further analysis. The ex-truders are supplied withmeasuring ports for melttemperature and pressurefor evaluating the process-ing parameters along the ex-truder barrel and the subse-quent measuring or profiledies. The Thermo Haake

Postex system ensures thedefined continued transportof the extruded material afterit has left the die. Both singleand twin-screw extrudersare available. Typical appli-cations include:

adaptation of extruderprocess to the application.For example:

● standard screws withcompression ratios of1:1, 2:1, 3:1, 4:1 and 5:1

● venting and mixingscrews

● wear-protected screws● corrosion-resistant

screws

A selection of feeding devic-es ensures the problem-freehandling of pourable, pow-dery, sticky and pasty mate-rials.

The Rheomex Family

R102 For temperatures up to 450 °C1 heating/cooling zonePressure up to 700 barD = 19.05 mm, L/D = 10 for:hardening substances

R104 For temperatures up to 250 °C1 heating/cooling zonePressure up to 700 barD = 19.05 mm, L/D = 10 withroll feeder for rubber strips

R202 For temperatures up to 450 °C2 heating/cooling zonesPressure up to 700 barD = 19.05 mm, L/D = 20 for:thermoplastics, thermoplasticceramics

R203 For temperatures up to 250 °C2 heating/cooling zonesPressure up to 700 barD = 19.05 mm, L/D = 20 withroll feeder for rubber strips

R252/254 For temperatures up to 450 °C3 heating/cooling zonesPressure up to 700 barD = 19.05 mm, L/D = 25 for:thermoplastics, ventingoptional

R302 For temperatures up to 450 °C4 heating/cooling zonespressure up to 700 barD = 19.05 mm, L/D = 30 for:expanded foam applications

CTW100 Conical twin screw extruderfor temperatures up to 450 °C3 heating/cooling zonesPressure up to 700 barD = 31.80/20 mm, L = 300 mmfor: continuous compounding

PTW25 Parallel twin screw extruderfor temperatures up to 450 °CPressure up to 300 (150) barD = 25, L/D = 18-36 for:continuous compounding

● extruding PVC com-pounds for a variety ofprofiles

● film-blowing LDPE andHDPE films

● compounding masterbatches

● feeding in additives andventing volatile compo-

nents

A variety of differentscrew geometries areavailable to guaran-

tee the optimum

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Dies & Postex For Extrusion-Related Applications

Testing At ConditionsClose To ActualProduction

Dies and post-extrusionunits are used in addition toextruders for testing therheological characteristicsand processability of poly-mers and for producing testsamples in the laboratories.

Dies enable the defined ge-ometries for profiles, filmsor rheological measure-ments. The post-extrusionunits (Thermo Haake Postexunits for short) can transportthe extruded material forwardin a defined manner andprepare it for further tests.

Both dies and Postex unitsdiffer scarcely in designfrom their larger-scale “bigbrothers”. Testing at condi-tions which approximate ac-tual production is guaran-teed. Integrated measuringtechnology increases the ap-plication possibilities in thelaboratory.

Measuring Dies Usage InLaboratory Applications

Measuring dies create pro-files of a defined geometry.Temperature and pressuremeasurements along the ex-truder barrel and die enablethe accurate definition of

melt conditions. The pre-cise monitoring and controlof the desired processingconditions is thus possible.The flow geometries takethe behavior of differentpolymer types during extru-sion into consideration.

A variety of dies are availablefor the Rheomex range ofThermo Haake extruders for:

● blown films● flat films● pellets● pipes● fibers● coated wires● screen life tests

The PolyLab System can betransformed into a powerfulextrusion capillary rheome-ter when used together withcapillary dies. Rheologicaldata such as shear stress andviscosity functions can beevaluated.These are of para-mount importance for thedesign of injection molds.

The shear rate ranges whichcorrespond to those experi-enced during processing inthe polymer industry can befully covered using both rodand slit capillary dies.

Thermo Haakeutilize 3D-CADin all areas ofProductdevelopment.

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Postex = Post-ExtrusionUnits

The handling of the oftenhot and still formable ex-truded material is an impor-tant part of extrusion testingwhich cannot be neglected.It influences the materialcharacteristics and surfacefinish to a great extent.These tasks are carried outby the Postex systems devel-oped by Thermo Haake toensure that your require-ments with respect to theextruded material are ful-filled.

Apart from the defined tak-ing off and preparation ofextrudate for further analysis,they also enable the labora-tory and processing techni-cian to carry out tests in

The PolyLab System: TestsWith Extruder Sensors,Dies And Postex Units

The PolyLab System is ideal-ly suited for tests carried outunder conditions similar toactual production with labo-ratory-scale extrusion sys-tems. A few examples arelisted below:

● the testing of the pigmentdispersal of PVC dryblends with the twinscrew extruder RheomexCTW100, a sheet dieand the sheet, tape andribbon take-off

● the testing of the extru-sion behavior of SBRmixtures with the singlescrew extruder Rheomex104, the Garvey die andthe conveyor belt accord-ing to ASTM D2230

● testing for transparencyand fish-eyes with thesingle screw extruder252, the blown film dieand blown film take offand the OQT512

● the water bath/pelletizer:for the cooling and pel-letizing of one or severalstrands of extruded ma-terial

● conveyor belt: for thedefined taking off of ex-truded profiles

The optical testing systemsand the melt pump are thespecialties of the Postexfamily.

● the fish-eye testerOQT512: integratedwithin the blown filmtake-off or sheet, tapeand ribbon take-off fortesting films for fish-eyesand black spots

● the die swell tester: fordetermining the die swellgiving relative informationon the elastic character-istics of the extrudedmaterial

● the melt pump: for im-proving the melt pres-sure constancy before theextruded material entersthe die

conditions similar to thoseexperienced during produc-tion. The production ofsmall batches of “finishedproducts” is a frequent ap-plication for the ThermoHaake Postex systems,especially when alterationsto the formulation andproduct processing are to beevaluated.The Postex family consistsof:

● the blown film take-off:for the defined coolingand taking off of blownfilms

● the sheet, tape and rib-bon take-off: for thesmoothing, cooling andtaking off of flat films

● the wire coating take-off:for the joining up ofwires and the melt forthe cooling, taking offand coiling up of coatedcables

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Rheometry – Practical Application Examples

Examples from theThermo Haake Rheocordlaboratory

Example 1: Determining

a PE reference curve

The reference curve illus-trates the viscosity values ofa polymer measured overseveral decades of shearrate. In the example in ques-tion the comparability oftwo completely differentmeasuring methods, capil-lary measurement with anextruder and oscillationmeasurement using a con-trolled stress rheometer,should be illustrated viameasurements on anLLDPE. The dynamic vis-cosity of the capillary meas-urement and the complexviscosity of the oscillationmeasurement are shown in adiagram dependent on theshear rate (Fig. 1). The re-sults of the capillary and os-cillation measurementsoverlap in the transitionalarea of structural viscosity.A good correlation of theindividual measuring sec-

Rheometry is becomingmore and more importantin the plastics industry, bothin the areas of developmentand processing. Injectionmolding technology, wherevery high shear rates occurat the injection channals andlow shear rates are prevalentduring the final filling outof the form, is just oneexample of the wide range.The quality control depart-ment must assure that thepolymers supplied do notdeviate from the standardduring processing in the ex-truder.

Thermo Haake can supply arange of measuring systemsfor the rheological testingof your polymers:

● the PolyLab System usedtogether with a Rheomexextruder sensor and cap-illary dies as an extrusioncapillary rheometer

● the PolyLab System usedtogether with a Rheomixmixer sensor for relativerheological measure-ments

● the RheoStress andRotovisco rotationalrheometers equippedwith plate/plate or cone/plate sensor systems

tions can be arrivedfrom this and theCOX-MERZ rule canthus be confirmed.

Example 2:

The differentiation of

compounds and

masterbatches

Mixer sensors are of-ten used for the dif-ferentiation of com-pounds and master-batches. In the exam-ple in question, amanufacturer wassupplied two differenttitanium dioxides.When using one ofthese pigments, theproduction machinecut out due to an ex-cessive power con-sumption. After examinationin the mixer sensor, it wasshown that the torqueabsorption of the one TiO2

was much higher than thatof the other supplier (Fig. 2).These type of measurementsare often carried out in or-der to find quick solutionsand e.g. to select the right

Time [min]

Torque [Nm] TTQ [Nm *min]

Fig. 2

Fig. 1

supplier and as such theycan save time and moneyconsuming productiontests.

Viscosity curve of PE-LLD at 220 °C measuring temperature

OSZ SLIT ROD Angular velocity/shear rate [1/s]

OscillationThermo Haake RheoStress

Slit capillaryThermo Haake Rheocord

Rod capillaryThermo Haake Rheocord

10000

1000

100

10

0,001 0,01 0,1 1 10 100 1000 10000 100000

Dyn

amic

Vis

cosi

ty η

'/Vi

scos

ity

η [P

as]

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Thermo Haake places itsexperience at your disposalin the form of laboratoryand technical reports

We have listed a few exam-ples below:● Differentiating PVC Dry

Blend Batches with anExtruder Sensor

● Pigment Differentiationin Masterbatches

● Testing the FlowCharacteristics ofGlass Fiber ReinforcedTPU

● Examining the Plastiy-ing and Degradation Be-havior of PVC

● ......

● Flow and Cross-LinkingBehavior of Cross-Link-ing Polyethylenes(XLPE)

● The Curing Behavior ofReaction Resin Com-pounds

● Characterizing Master-batches Using the ScreenLife Test Method

Example 3:

Die swell and viscosity

The viscosity behavior ofmelts influences the process-ing behavior to a great ex-tent. For instance the vis-cosity determines whetherthe form is completely filledin the injection moldingprocess and the elasticitydetermines the geometry ofyour finished product. Fig. 3shows the results of two

Fig. 3 Shear rate

rubbers which exhibitedsimilar flow characteristicsi.e. viscosities duringprocessing. They howeverresulted in completely dif-ferent finished productcross sections. It can berecognized that the viscosityof both materials is reducedto virtually the same levelwith increasing load but theinfluence of the elasticityclearly increases.

100000

10000

1000

50

40

30

20

10

010010

Die swell (D9) [%] Viscosity (Eta) [Pa*s]

Die swell + Viscosity

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Gebr. HAAKE GmbHDieselstr. 4 . D-76227 KarlsruheGermanyTel. +49(0)721 40 94-0Fax +49(0)721 40 94 300Hotline +49(0)18 05 04 22 53info@thermohaake.comwww.thermohaake.com

A Thermo Electron business

Thermo Haake Inc.53 W. Century RoadParamus, NJ 07652, USATel. 201 265 7865Fax 201 265 1977infousa@thermohaake.comwww.thermohaake.com

RHEO S.A.99 route de VersaillesF-91160 Champlan, FranceTel. +33(0)1 64 54 01 01Fax +33(0)1 64 54 01 87info@thermorheo.comwww.thermorheo.com

Rheology PolymerTechnologyTemperatureControl ThermalAnalysis

PolyLab, Rheocord, Rheomex and PolyView are registered trademarks of Gebrüder Haake GmbH. The product information in this document was correct at the timeof printing, however specifications are subject to alteration without notice due to the ThermoHaake philosophy of continual product innovation and development andany information contained herein should not be construed as a contractual commitment by Thermo Haake. All orders are accepted subject to our current Conditionsof Sale, copies of which are available on request. © Thermo Haake / 07.2001 623-3001