News & Views Expanded contract testing · PDF fileInstruments & equipment in ... ambient - +400°C (electrical temperature ... measurements for polymeric materials has mostly....

dec 10-mar 11

[email protected] 1 www.rheologysolutions.com

Rheology Solutions has purchasedthe newest HAAKE MARS IIIRheometer to be housed in ourapplications laboratory in BacchusMarsh, Victoria.

The new HAAKE MARS III Rheometer will extendour capabilities in product testing and systemdemonstration, and for progressing thecommercialisation of our Online Rheometer (OLR).

The HAAKE MARS III is a high-end, modular,controlled stress rheometer. Rheology Solutionshave also invested in the High Temperature(60ºC-400ºC) and RheoScope modules extendingthe HAAKE MARS III's capabilities even further.Our laboratory includes a broad range ofconcentric cylinder, cone/plate and plate/platesensor systems which allow us to test very high-and very low-viscosity liquids, suspensions,emulsions and solutions, also a vapour trap tominimise losses at elevated temperatures orwhere solvents etc. are involved.

The High Temperaturemodule will allow controlled

temperature (constant orramped) testing of materialsfrom food, pharmaceuticaland cosmetics through to

polymer melts, and anything in-between.

The RheoScope module combines the advantagesof a microscope and a rheometer, allowing us tocapture short movies or individual images of thetest material in the measurement gap, as well asindividual images. Each image is coupled with adata-point, to allow the user to relate rheologicalinformation to an image of the material under thespecific flow conditions in the measurement gapat that instant. This allows rheologicalphenomena to be more readily explained, in

particular unusual or transitional/transientbehaviour. The RheoScope module has hightemperature capability, allowing testing up to300ºC.

Expanded capabilities -polymer IndustriesOur contract testing customers in the polymerindustry, can now expect polymer melt testingand visualisation up to 300ºC (with theRheoScope module), and standard melt testing upto 400ºC (with the High Temperature module).

Expanded capabilities - food,pharma, coatings & miningFor food, pharma, coatings and miningcustomers, we now have the capability of testingand diagnosing flow stratification, rheodestructionetc. at high shear rates, especially in cases wherea micron-scale structure is present, which can beobserved using the RheoScope module. In asimilar way, structural build-up (e.g. flocculation,aggregation, cross-linking) at low and moderateshear can be monitored and investigatedrheologically and microscopically (in the micronsize range).

Contract testing servicesContract testing services specifically for industrialapplications is available. A range ofcomprehensive data can be provided for:• Liquid properties.• Creep & recovery tests.• Viscoelastic moduli.• Flow curves.• Yield stress.• Viscosity curves.• Extensional properties including:

- Apparent extensional viscosity.- Time to break-up of strands.- Extensional constants.

• Concentration and temperature profiles.• Effects of particle size distribution.• Effects of additives and viscosity modifiers.• QA/QC for optimal processing.

These tests will provide valuable information for process design, modification and control.Test results can be provided simply as data files or supplied with complete interpretation and recommendations.

Rheology Solutions can facilitatetesting at our overseas suppliers

laboratories when required.

Instruments & equipment inthe applications laboratoryThe Rheology Solutions applications laboratory is equipped with a comprehensive range ofequipment and instruments to meet therequirements of material characterisation.

This combination of instruments and equipmentallows the testing and definition of the materialproperties of most solids and liquids. In this wayRheology Solutions can provide unparalleledexpertise and customer advice for sensibleinstrument and sensor selection as well asconsultation and test procedure development.•

Thermo Scientific HAAKE MARS III with RheoScope Module

• News & Views

Expanded contract testing capabilities

all industries

Contract testing at high temperature will be available from February 2011. Enquiries? Send an email to [email protected] with full details.

• in this issue:

Technical Papers

09 Article: Standard Search forSpecks

09 Oscillatory Squeeze Flow forProcess Rheometry

08 Accurate Temperature Control forthe Separation of Solvents fromLiquid Samples

10 Filter Pressure Value Test10 Understanding Temperature

Control in Bioreactor Systems10 What Happens When Rheological

Properties Change?

News & Views

05 K Show Overview08 Commercialisation Australia

Funding Announcement04 2011 Exhibitions07 Service & Calibration Program01 Expanded Contract Testing

Capabilities

Product News &Industry Applications

03 Rotational Viscometers06 Laboratory Chiller02 New - Rheology & FT-IR Module14 Temperature Control Baths16 Film Surface Analyser15 New Product - Rheometer for

Mortar and Fresh Concrete13 New - Peltier Temperature Control

UnitNew Literature

12 Best Quality Control for thePetrochemical Industry

11 Comprehensive MaterialCharacterisation for Polymers - updated

13 Modular Rheometer Platform - updated

11 Process Control Rheometers - updated

12 Thermo Scientific Viscometer

dec 10-mar 11

2 www.rheologysolutions.com

all industries

polymerindustries

food industries

mining industries

construction & building industries

surface coatingsindustries

pharma, cosmetic& allied industries

chemical & allied industries

Pg. 1, 2, 3, 6, 7,8, 9, 12, 13, 14

Pg. 4, 5, 8, 9, 10,11, 12, 13, 16

Pg. 9, 10, 16

Pg. 4

Pg.15

Pg. 8, 10

Pg. 8, 9,10, 16

Pg. 8, 10, 16

• In This IssueSpecific Industry Key

• Product News

Simultaneous rheological and FT-IR spectra measurements

all industries

The Thermo Scientific HAAKEMARS III has a number ofapplication solutions within its suiteof models and now this has beenexpanded to include simultaneousrheological and FT-IR spectrameasurements.

Discover simultaneous rheometry and FT-IRspectroscopy with the unique HAAKE MARS III -Rheonaut technology. The module offers:• Simultaneous rheology and FT-IR

spectroscopy• Rheonaut as compact module for HAAKE

MARS III rheometer• ATR (attenuated total reflection) principle• Analysis of structural changes under shear /

deformation• Extensive investigation of thermal / UV curing

reactions

Specifications of the Rheonautmodule

Spectrometer• compatible with several standard IR

spectrometers (side port required)Measuring principle• ATR using single reflection crystal (diamond)• DTGS (deuterated triglycine sulfate) detector

Data acquisition and storageHAAKE RheoWin software with integrated controlof the FT-IR spectrometer (for selectedspectrometer models), automatic synchronisationof rheological data and FT-IR spectrum data.

Temperature rangeStandard version0°C - +120°C (Peltier temperature control unit)High temperature optionambient - +400°C (electrical temperature control unit)

Measuring geometriesPlates and cones with diameters up to 60 mm

The HAAKE MARS III offers:• Reliable and accurate rheological

measurements• Modular rheometer solutions to suit individual

application requirements in differentindustries 00W through to 10,000W coolingcapacities.•

[email protected] 10-mar 11

3

• Product News

Rotational viscometers - to suit those seeking convenience up to the expert model measurements

all industries

ApplicationThe Thermo Scientific HAAKE Viscotester E, D andC units can be used for tests and comparativemeasurements for quality control according torecognized standards.

Measuring principleThe HAAKE Viscotester E, D and C are classicalrotational viscometers that measure theresistance of a test substance against a presetspeed. The resulting torque or resistancemeasures the viscosity of the fluid. The higher thetorque, the higher the viscosity. Due to the type ofstandardised geometries, the shear ratesgenerated can only be determined precisely forNewtonian substances.

CompatibilityThe basic ISO 2555 standard describes thedesign and the characteristic measuringtechnique of a viscosity measuring instrument(torque, speed, rotor geometry). If rotationalviscometers meet these requirements, resultscomply.

Common features of theHAAKE Viscotester E, D and C• Ready to go package - unpack, switch on

and start measuring viscosity• Digital display of viscosity, % torque, speed,

spindle, upper viscosity limit, temperature(optional), in selectable units

• Integrated automatic diagnostic functionality• Visual and acoustic signals at critical

measuring conditions• Easy viscosity and temperature (optional)

calibrations• 10 user interface languages

StandardsThe HAAKE Viscotester E, D and C meet thefollowing standards:BS: 6075, 5350; ISO: 2555, 1652ASTM: 115, 789, 1076, 1084, 1286, 1417,1439, 1638, 1824, 2196, 2336, 2364, 2393,2556, 2669, 2849, 2983, 2994, 3232, 3236,3716

Technical data• Viscosity range: depending on version (L or R)• Accuracy: +/- 1% FSD• Reproducibility: 0.2%• Supplied at 100 - 240V/50 - 60 Hz •

HAAKE Viscotester C The convenient model

For easy, fast and accurate manual viscosity measurements.

Additional features:• Simple and intuitive operation• 4 line LCD display with 6 keys• Rotational speeds: 21 between 0.1 rpm and 200 rpm• Viscosity range:

R-Version: 100 mPas – 13.000.000 mPasL-Version: 15 mPas – 2.000.000 mPas

HAAKE Viscotester D The distinct model

For routine viscosity measurements with data transfer.

Additional features:• 6 line LCD display with 6 keys• Internal memory for 9 basic measuring routines• USB interface for data transfer to PC• Rotational speeds: 21 between 0.1 rpm and 200 rpm• Viscosity range:


Optional:• Temperature sensor Pt 100• Display of sample temperature• One hand quick fit coupling for spindles• HAAKE RheoWin data evaluation software

HAAKE Viscotester EThe expert model

For automatic flow curve measurements with full PC control.

Additional features:• 6 line LCD display with 12 keys• Display of sample temperature, shear rate and shear

stress for coaxial spindles, routine parameters, etc.• Internal memory for 9 advanced measuring routines• Routine programming functions• USB for software control• Rotational speeds: 54 between 0.01 rpm and 200 rpm• Viscosity range:


Optional:• One hand quick fit coupling for spindles• HAAKE RheoWin measuring and evaluation software

www.rheologysolutions.comdec 10-mar 11

4

• News & Views

2011 Exhibition programDuring 2011, Rheology Solutions are participating in the following major industry exhibitions and conferences:

mining industries

13 - 17 February 201132 Australasian PolymerSymposiumCoffs Harbour, NSW

Visit Rheology Solutions on Stand no: 1Products on display: HAAKE MARS III - Fullyoperational with RheoScope Module

www.32saps.org.au

The Australasian Polymer Symposium is a feast ofpolymer science covering all topics ranging frompolymer synthesis, characterisation, physics ofpolymers, engineering to materials. Topics willspan from fundamental polymer science such asmodelling to applied materials. A considerableportion of the APS is always dedicated to theinterface of polymer science with other disciplinessuch as biomaterials, nanomaterials and surfacescience.

The Online Rheometer (OLR) Group will present apaper at 32APS, in Coffs Harbour, NSW. Thispaper will introduce to the dilute polymer andbiopolymer communities the OLR concept, bycomparing the OLR with traditional measurementtechnologies for process control and qualityassurance. The contrasting of the measurementsmade by traditional on-line and laboratoryrheological measurement techniques with those ofthe OLR will be presented. The data will becollected using our newly commissioned pipe-loopfacility and a high-end laboratory rheometer, theHAAKE MARS III.

Paper from the OnlineRheometer (OLR) Group,Rheology Solutions

On-line rheometry for industrial process andquality controlT.J. Kealy, P.K. Bhattacharjee

Traditional industrial process control and QualityAssurance/Quality Control (QA/QC) by rheologicalmeasurements for polymeric materials has mostlybeen limited to capillary-type measurements forpolymer melts. Forced flow of the melt at variousvelocities through single- or twin-bore capillariesof known geometry is used to generate a flowcurve for the polymer as it is processed throughan extrusion system. These measurementsprovide the interested engineer with a measure ofthe polymer flow properties over a relatively widerange of shear rates. The flow properties usuallytake the form of either a steady shear flow curve,relating the shear viscosity of the material toshear rate, or the Melt Flow Index (MFI).

In contrast with these measurements the commontechniques for dilute polymer systems, such ashigh molecular weight polysaccharides typicallyused for the texturisation of surface coatings, foodor cosmaceuticals (hand soap, shampoo, bodycrème etc.) usually have only a single pointpseudo-viscosity measurement in-the-pipe. Themeasurements are most often based on atorsional principle, whereby the vibration of aprobe is damped by the viscous fluid around it.The damping effect of the fluid is related to theviscosity. These techniques are widely used, butthe results from these techniques are oftendifficult to directly compare with those obtained inlaboratory instruments. In fact, they most oftenoffer a single-point pseudo-viscosity, which isoften insufficient for good process control, QA/QC,

or reliable diagnosis of process problems. There isa clear need for more comprehensive on-linemeasurements for process control.

Oscillatory Squeeze Flow (OSF) has beendiscussed and proposed as a viable QA/QCalternative for dynamic oscillatory shear flowmeasurements in the laboratory. In recent times,some commercially available OSF laboratoryrheometers have arrived on the market (notablythe prototype C-20 previously available from TAinstruments until around 2003/2004, and theMFR 2100, currently available from GBCScientific). So far an on-line variant of theseinstruments has not been available. CombiningOSF techniques with Fast Fourier Transforms(FFTs) can facilitate rapid turn-around ofmeasurements, faster than is possible for thetraditional laboratory measurements in shear flow.This combination has facilitated the developmentof an Online Rheometer (OLR) based on OSFtechniques for near-continuous measurement ofcharacteristic dynamic flow curves in-the-pipe.

This paper presents the contrasting data availablefrom traditional on-line rheological techniques(pressure-drop measurements, and two differenttorsional damping technologies) with the new OLRtechnique. The measurements were made fortypical process conditions, at a pipe-loop facilityusing well characterised aqueous long-chainpolysaccharide solutions as the test material, andthe data from all of the techniques are contrastedwith steady shear and dynamic data from alaboratory rheometer. We show that the OLRtechnique compares well with dynamic data fromthe laboratory rheometer, and that it hassignificant process-related advantages overtraditional torsional techniques for process controland QA/QC.

polymer industries

4 - 8 April 2011Paste 2011Fremantle, Western Australia

Visit Rheology Solutions on Stand no: 8Products on display: HAAKE Viscotester VT550

Keep a watch out for the HAAKE VT550 purchaseoffer that is only available to those that attend theconference and visit us on Stand no: 8.

www.paste2011.com

Paste 2011 will explore the latest advances in thepreparation, transportation and deposition of pasteand thickened tailings (P&TT) that will bereinforced by current case studies. This seminar

will also address the important part that P&TTplays in incremental rehabilitation and its impacton mine closure goals.

The organisers expect state-of-the-art andinnovative papers from leading experts and toppractitioners throughout the world. These will bepresented during one of the most dynamic eventson paste and thickened tailings to be held inAustralia.


5

• News & Views

K show overview - Dusseldorf, Germany

24 - 27 May 2011

Ausplas 2011Melbourne, Victoria

Visit Rheology Solutions on Stand no: 844

We will have 18m2 to showcase the latest andnewest products from Thermo Scientific andOptical Control Systems (OSC).

The instruments from OCS will be operational andwe will be offering sample testing. Furtherinformation will be provided closer to theexhibition.

If you are interested in having optical scanningconducted on your sample or product, contact usto discuss your requirements.

www.ausplas.com

Ausplas is Australia's national trade exhibition forthe plastics processing industry. It has been heldevery three years since the early 80's, with thelast event having taken place in October 2008.In a significant new development, Ausplas will co-locate with two other major manufacturingindustry trade exhibitions, Austech and NationalManufacturing Week.•

polymer industries

polymer industries

For more than 40 years, K hasbeen and still is the biggestinternational trade fair for plasticsand rubber, and takes place onceevery three years.

The leading raw material producers, processingcompanies and machinery manufacturers offer anoverview of the latest technical developments,procedures and techniques, of currentconstruction methods and future trends.

The plastics industry is one of the most innovativesegments of the world economy and plastics areseen as the material of the 21st century. Majoradvances in products and processes - plasticsare key.

In 2007, Rheology Solutions visited the K Showand spent time on both the exhibition stands ofThermo Scientific and Optical Control Systems(OCS). This year, we did not attend as one of the nearly 250,000 visitors. We are pleased toprovide you with an overview of what was on their stands.

At the K Show this year, Thermo Scientificwere in hall 10, Stand B59 and showcased an extensive range of products specific to the polymer industry. This included:

• Injection moulding machine that offersefficient sample preparation - ThermoScientific HAAKE MiniJet

• Measuring mixers and extruders that allowthe user to gain insight into their processes -Thermo Scientific HAAKE PolyLab OS. Fromsample batches of 50 grams up to outputs of10 kg/h, the bench mounted 16 mm ThermoScientific EuroLab XL twin-screw extruder isthe complete compounding and samplepreparation system

• Rheometers and viscometers that offer acomprehensive application solution specificfor industry applications - Thermo ScientificHAAKE MARS III and HAAKE RheoStress 6000

• Micro-compounding with a micro-conicaltwin-screw compounder for compoundingand processing of small sample volumes -Thermo Scientific HAAKE MiniLab

Optical Control Systems (OCS) were in hall 10,Stand E21 and this year their exhibition highlightswere:• Newly developed PS400C - pellet scanning

system for defect detection (50/100ºm) andsorting in normal production up to 800 kg/hrincluding mixing ratio determination andspecially suited for super-transparentgranules

• Three extrusion lines (cast, blown andcalendar/tape test line) with several controlsystems: APLAIRS® (FT-IR Spectrometer),Film Scanning Systems, Thickness - Glossand Haze measurements

• Process Melt Rheometer - OP5• Pellet Anayser - PA66• Pellet Transport System - PTS •

Specifications

Accel 250LC Accel 500LC

Heating Capacity

50Hz at 20ºC 2 kW 2 kW

Cooling Capacity at 20ºC 250 Watts 500 Watts

Working Temperature Range -10ºC to 80ºC -10ºC to 80ºC

Temp Stability +/- 0.1ºC +/- 0.1ºC

Force Pump

Maximum Flow 17 lpm 17 lpm

Maximum Pressure 300 mbar (4.4 psi) 300 mbar (4.4 psi)

Force/Suction Pump

Maximum Flow 21 lpm 21 lpm

Maximum Pressure 805 mbar (11.7 psi) 805 mbar (11.7 psi)

Reservoir Volume 2.8 litres 2.8 litres

Unit Weight 30 kg 30 kg

Physical Dimensions (HxWxD)

Centimeters (cm) 62 x 23.2 x 48.7 62 x 23.2 x 48.7

Voltage Options

220-230V/50Hz Available Available

Compliance UL/RoHS UL/RoHS

Features & Benefits

Feature Benefit

Small foot-print 62 x 23.2 x 48.7cm

Internal Reservoir Reduces evaporation concerns of open bath design

Easy to use, fluid fill, drain Fill the unit, drain the unit, and view the fluid level with& site tube line the same tube line

Full range cooling feature Limits power consumption for efficient operation

Pump speed control Allows the user to set the pump speed at either 50% or 100% for tighter control

Energy Savings Feature Limits power consumption for efficient operation

Multi Lanhuage HMI Offers the option of English, French or German on the display

USB Port/RS232 Communication Provides digital communication for remote operation(otional) and monitoring


6

• Product News

New laboratory chiller

all industries

Heat and cool external applicationswith a temperature range of -10°Cto +80°C and either a 250W or500W cooling capacity.

The Thermo Scientific Polar Series of chillers area versatile and economical option for laboratorycooling and heating needs. Its bathless designminimises the evaporation of temperature fluidduring daily use.

Applications• Analytical equipment• Chromatography• Electrophoresis• Laser diode cooling• Various research applications •

The Polar Series Laboratory Chiller is ideal tocontrol temperatures within a variety oflaboratories within the following industries:Pharmaceutical, Biotechnology, AcademicResearch, Food and Beverage, Chemical andPetrochemical.


7

• News & Views - Service and calibration program 2010 - 2011

Viscometers and rheometers - why check calibration?

all industries

The accuracy of the electroniccomponents used in allinstruments drifts over time. The effects of time in service aswell as environmental conditionsadd to this drift.

As time progresses changes in component valuescause greater uncertainty in your measurements.At some point in time, the drift causes theinstruments uncertainty to become undefined,meaning the manufacturer can no longer predictthe uncertainty and guarantee measurementresults. To resolve this issue instruments must becalibrated at regular intervals as defined by themanufacturer.

A calibration check is the comparison of aninstruments performance to a standard of knownaccuracy. The result of a calibration check may be documentation showing the deviation of ameasurement from the known standard or it may also include adjusting the instrumentsmeasurement capability to improve accuracy (re-calibration).

The goal of a calibration check is to quantify and improve the measurement accuracy of your instrument.

The benefits of maintaining properly calibratedequipment include:• Reduced measurement errors• Consistency between measurements• Increases in production yields• Assurance you are making accurate

measurements

Rheology Solutions recommends that youperiodically calibrate your hardware to ensuremeasurement accuracy and to keep yourinstrument operation in peak precision.

CalibrationsTo minimise the cost to our customers, weconduct scheduled annual calibrations interstate,however if you wish your rheometer or viscometercalibrated outside of the set program, pleasephone or email our Administration Manager,Jackie at [email protected] andshe will either organise your HAAKE equipment tobe sent to our office or put you on the list for asite visit to coincide with the schedule. Allequipment received for calibration will have a 48hours turnaround from the time it arrives in our

office. We will contact you to confirm receipt ofequipment and date for return despatch.

Calibration letters have been sent out to thosecustomers that have previously had their HAAKEequipment calibrated by us. We will be in contactin the coming weeks to arrange and finalise yourbooking.

If you have not received a calibration letter fromus and require your instrument calibrated, pleasecontact our office to arrange your booking.

Interstate calibration schedule• Queensland

Week commencing 10th January 2011• New South Wales

Week commencing 7th February 2011• South Australia

Week commencing 7th March 2011• Western Australia

Planned Mid November 2011• Tasmania

Please contact our office to arrange a time

The pricing for calibrations that are conducted inour office or link in with the scheduled interstateschedule in 2010/2011 are based on MelbourneMetropolitan rates as follows:

HAAKE MARS $ 1,650.00

HAAKE RheoScope 1 $ 1,650.00

HAAKE RheoStress 6000 $ 1,650.00

HAAKE RheoStress 1 $ 1,650.00

HAAKE RotoVisco 1 $ 1,250.00

HAAKE ViscoTester 550 $ 825.00

Notes:• Melbourne metropolitan customers can have

their HAAKE instrument calibrated at anytime on site.

• Victorian customers (non metropolitan) canarrange for calibration of their instrument atany time or when the next scheduledcalibration is due by contacting our officedirect.

• Prices exclude GST, and any parts requiredfor instrument repairs.

• Multiple unit calibrations are priced on asliding scale if they are serviced at the sametime. Prices are available on request.

All calibrations are completed by our ServiceEngineer who is factory trained at themanufacturers. A calibration certificate is providedas verification.

As part of the calibration our Service Engineer will• check and adjust the high sensitive

measuring head to plate geometry• calibrate all physical measurement

parameters according to standards• maintain all moveable parts• ensure your rheometer is in its optimal

condition

If any parts are required in order to repair anyinstrument found to be faulty, these will beordered directly from our suppliers, which cantake four - six weeks to arrive. When the partsare on hand the repair can be finalised. We willnotify you of timing and request that you pleasebe patient if this is the case.•

Quotes for all repairs and spare parts can beobtained from us at any time.


8

• News & Views

Commercialisation Australia funding announcement

all industries

Rheology Solutions is pleased toannounce that we have securedFederal Government fundingthrough CommercialisationAustralia (Early StageCommercialisation), from theDepartment for Innovation,Industry, Science and Research.

Rheology Solutions is commercialising a novelOnline Rheometer (OLR), developed by the CSIRO

for on-line process control. We will develop in-the-pipe instrumentation that delivers continuousreal-time data, to maintain better quality controlfor production processes.

We will use the Commercialisation Australia fundsto accelerate the on-going prototype and pre-production software and instrument design andconstruction, and for the construction of an in-house pipe-loop for rapid, iterative, applications-based testing of the new prototypes and software.

On the 15th October, 2010, Minister Kim Carrannounced that 22 Australian researchers,

individuals and businesses would share in fundingof over $8 million to help transform their projectsinto commercial successes*.

Rheology Solutions looks forward to working withour partners to develop a valuable resource forAustralian and international processingbusinesses.•

* Minister Carr's announcement:http://minister.innovation.gov.au/Carr/Pages/STRENGTHENINGOURECONOMYTHROUGHCOMMERCIALISATION.aspx

• Technical Papers

Accurate temperature control for the separation of solvents from liquid samples

AbstractAs a widely used technique, the separation of onecomponent from a liquid sample is integral to themedicinal chemistry, pharmaceutical,chromatography and petrochemical fields.However, achieving such separations in a fast andaccurate manner can prove problematic.Traditionally, this process has been timeconsuming and requires evaporator apparatus,e.g., rotary evaporators along with highly precisetemperature control to ensure that the separatedsolvent is in fact the component of interest. Awide range of heated and cooled ThermoScientific water baths and chillers are available,including re-circulating chillers, which can beused to effectively maintain the precisetemperatures during exothermic and endothermicstages of compound separation.

IntroductionTemperature control is an important issue acrossmany different research processes, fromchromatography and drug development topetrochemical and materials manufacturing. Thisis because the speed and accuracy of manychemical reactions, including changes of state,are affected by temperature alterations and oftenhave an optimal temperature. By using a watersource that is not temperature controlled,conditions are not accurately optimised tomaximise experimental efficiency. As a result,methods of temperature control are extremelyimportant in ensuring data precision. One suchtechnique in which temperature control isextremely important is the separation of a specificsolvent from a liquid sample.

In both chromatography and counter-currentdistribution, the rapid quantitative recovery of asolute from a large liquid volume can beproblematic. Chemical analysis studies often relyon the separation of solvents for the identificationof various components of both natural andartificial materials. Such identification can lead to:the detection of: (1) contaminants in wastewater(2) radiopharmaceuticals for therapy anddiagnosis (3) mutagenesis in areas ofpetrochemical contamination (4) identificationand/or refinement of potential pharmaceuticals.•

Thermo Scientific HAAKE ThermoFlex 5000

A full copy of this application note is available byquoting AN-SP-10-1. . 1.0.0

surface coatings industries

polymer industries

pharmaceutical, cosmetic& allied industries



9


Presented at the WA rheology conference,rheology for practical applications on 17 November 2010

all industries

The one day seminar covered awide range of materials processingapplications.

Keynote lectures were given on the flow ofmineral slurries by Professor Paul Slatter (RMIT),the rheometry of mixtures by Andrew Chryss(CSIRO) and the characterisation of materials formedical applications by Dr Michael Glinsky(CSIRO CEO Science Leader).

www.csiro.au/events/Rheology-Seminar.html

Oscillatory squeeze flow forprocess rheometryPresented by Dr Pradipto Bhattacharjee, SeniorScientist, Online Rheometer Group, RheologySolutions.

AbstractDifficulties in measuring viscoelastic properties offluids during processing contribute towards a

significant proportion of manufacturing loss inindustries. While a number of instruments existfor making on-line viscoelastic measurements,relating the measurement from these instrumentsto the material properties measured in laboratorybased instruments often becomes difficult. TheOnline Rheometer (OLR) discussed here usesoscillatory squeeze flow and a well defineddeformation field to measure viscoelastic materialproperties that are identical to those measured inthe laboratory. This makes the rheometer and theassociated technique advantageous for someprocessing conditions and industries. Thepresentation provided an overview of oscillatorysqueeze flow rheometry and highlighted itsapplication for on-line rheometry. Somepreliminary experimental measurementsperformed in realistic processing environmentswill be presented and the advantages andlimitations in comparison with existing techniqueswill be discussed.

Keywords: on-line rheometry, oscillatory squeezeflow, measurements, viscoelasticity.•

• Article

Standard search for specks... film inspection

Film inspection systems areincreasingly becoming an essentialpart of production lines.

They monitor the film web in transmitted light (inthe case of transparent and translucent films) orreflected light (opaque films). A combination ofboth illumination arrangements is possible whennot only transparent but also opaque films aremade or processed on the same installation.

Modern systems detect surface defects such asspecks, gels, black specks, fish eyes, coating

tears, streaks, flow lines, and insects. Theoperator can program the types of defect into thesystem which will then automatically determinethe corresponding criteria for classifying them.

However, the user needs to specify the defect sizeand the frequency threshold which triggers analarm. This should logically be done inconsultation with the end customer.

Definition: Specks and their causesSpecks are small film inhomogeneities that arecharacterised by their area (size in transmittedlight) and their elevation above the film surface.

However, defects, such as specks, are not definedin any ISO or DIN standard, nor are there anyclear rules on what constitutes scrap, etc. Theonce widely used statement “my film has nospecks” is now outdated. Specks occur in all films

and are an unavoidable outcome of theproduction process and the properties of thepolymer. Specks, as it were, are only a matter ofresolution.

Film manufacturers know from experience thatthe reasons for such defects can be broken downas follows:

• Extrusion line (non-optimal screw geometry,deposits, etc) 20%

• Raw material (impurity, cross-links, etc) 25%• Production process (wrong temperature

parameters, non-optimal purging, etc) 15%• Pellet transport, external and internal

(contamination of silo trucks, PE abrasions,etc) 40% •

A full copy of this article is available by quotingOCS009

food industries

polymer industries



10


Filter Pressure Value (FPV) Test, a new standard to examine master batches, white and carbon black colourants

For quite a period screen life tests for rating thequality and dispersibility tests of colourants inpolymer melts have been performed. But thecomparison of those test were poor. The newstandard EN 13900-5 describes now a procedurewhich increases the comparability of those tests.

On one hand this standard describes which kindof extruder, melt pump, sieves and beaker platehave to be used and on the other hand thecomposition of mixture, the test routine and theevaluation is described. One parameter, the FilterPressure Value - FPV - describes the quality anddispersion of the pigments. Due to standarisedquality control, an improvement of the product ispossible. Also the ranking of the same products

from different vendors by comparing the FPVresults is now easier. The use of the FVP test tocheck raw materials ensures the quality of yourproducts and the up time of screen changers ismore predictable.•

A copy of this report is available by quoting LR-49


Understanding temperature control in bioreactor systems

AbstractMicrobiologists, biochemists, and chemicalengineers need to cultivate organisms in a highlycontrolled manner. As such, bioreactors have

become integral to the pharmaceutical, food, andchemical industries. In order to successfully fulfillexperimental requirements, suitable conditionsand parameters must be provided, which includeaccurate temperature control, i.e., heating andcooling.

IntroductionThe environmental conditions of a bioreactor,including gas flow rates, temperature, pH,dissolved oxygen levels, and agitation rate needto be closely monitored and controlled in order toprovide optimal growth conditions. As one of the

key variables, temperature must be tightlyregulated to ensure reliable and consistent data isobtained across the many different processes thatuse bioreactors. This is because a single batchcan require both heating and cooling, with tighttemperature control and rapid ramping across abroad temperature range. Even singletemperature batches can require both heating(endothermic) and cooling (exothermic) reactionsto maintain a stable and accurate temperature.•

A ful copy of this application note is available byquoting AN-SP-10-2. 1.0.0

food industries



polymer industries


What happens when rheological properties change?

AbstractTo gain information about the reactions for certainchanges in rheological properties, a module forthe HAAKE MARS is available. It combines atemperature control unit for cone/plate- andplate/plate-geometries with a state of the artmicroscope. The RheoScope module is presented

and example data from different applications isshown.

IntroductionRheology is a “macroscopic” method, which tellsus how a material behaves under given conditionsbut never tells us why. For an understandingabout the reasons why a certain behaviouroccurs, we need to combine rheology with a“microscopic method” able to look into thestructure of the material.

Examples for such techniques complementingrheological measurements are GPC, thermalanalysis, FT (IR) or microscopy. Running two

independent measurements on differentinstruments, however, doubles instrument timeand measuring time and often leaves a bit of adoubt whether the sample and its treatmentbefore measuring have been exactly the same.

The double effort of time and resources can beavoided by running two different methods on thesame sample simultaneously, testing itsmacroscopic and microscopic properties. The tworesulting data sets can easily be correlated sincethey have been collected at the same time on thesame sample. •

A full copy of this application note is available byquoting V-228

food industries

surface coatings industries



11

• New Product Brochure

Thermo Scientific HAAKE PCR620

The Process Control RheometerHAAKE PCR 620 is a twin-pumpbypass rheometer that providesonline rheological measurementsof melt index and viscosity inpolymer industries.

With more than 200 installations around theworld, the HAAKE PCR has helped to improve customers’ product quality.

Applications• Online melt index measurement• Online viscosity measurement

Materials• Polypropylene (PP)• Polyethylene (LDPE/HDPE/LLDPE)• Polyester (PET)• Ethylene Vinyl Acetate (EVA)• Polymethyl-methacrylate (PMMA)• Polystyrene (PS)• Polyamide / Nylon (PA)• Polycarbonate (PC) •

polymer industries


Thermo Scientific HAAKE PCR630

The Process Control RheometerHAAKE PCR 630 is the latestgeneration of innovative processtechnology for online rheologicalmeasurements of melt index andviscosity.

It measures the melt index as standard ASTMloads and still maintains a minimal lag time which

remains almost constant over the melt indexmeasurement range. The slit die pressure controlfeature allows it to operate at pressures abovethe process pressure, thereby ensuring operationin the linear region of the transducers andpreventing out-gassing.

This also allows to cover a wide melt indexrange and follow transitions with a singledie, eliminating costly and trouble some diechanges common to other systems.•

polymer industries


Comprehensive materialcharacterisation for polymers

No matter what stage of thepolymer's life cycle, a range ofinstruments are available to enablemeasurements and small scaleproduction for a variety of specificrequirements.

The brochure has four sections incorporating asection on service. The product sections are asfollows:

• R&D of new polymers• Lab scale processing, pilot plant & small

scale production• Quality control

The instruments span the complete life cycle of apolymer: from the development of a polymer inthe laboratory to the pilot plant where smallbatches of test materials are compounded, toonline quality control in production, to processingsmall quantities of special polymers orcomposites.•

polymer industries


12


Thermo Scientific Viscometer

This new product brochureprovides an overview on thebasic principles of rheology,highlighting the differencesbetween rotational or falling ballviscometers, showcasing theThermo Scientific HAAKEViscometer range.

The brochure provides a summary page thatdetails the type of measurement, and the DIN andor ISO standards the viscometers comply to.

Basic principles in rheology -Selecting a viscometer

ViscometryViscometers determine the flow behaviour offluids. Viscosity describes a material property

which is dependent on different parameters suchas mechanical stress and strain, time as well astemperature and other ambient conditions.

Flow behaviourIn rheology we differentiate between so-calledNewtonian and non-Newtonian materials.Newtonian materials are characterised by aviscosity which may depend on temperature butis independent of the shear rate (and shearstress). Yet the viscosity of non-Newtonianmaterials depends on the shear rate. For mostnon-Newtonian materials the viscosity decreaseswith increasing shear rate. This behaviour iscalled shear-thinning, or pseudoplastic. A materialin which viscosity increases at increasing shearrates is called shear-thickening or dilatant.

Materials that do not flow until the applied shearstress surpasses a certain value are said to havea yield-stress.•


Best quality control for thepetrochemical industry

polymer industries

Plastics have becomeindispensable nowadays, and theareas of application are constantlybroadened. The level of therequirements has risen in equalmeasure.

The industry demands for high quality rawmaterial, that needs appropriate “online controls”to guarantee best properties for the fields ofpolymerisation, processing and application.Therefore it is essential that the extrusion processis checked for function and documented, as thepolymer film should be clear of contamination andgels. It is important to detect inhomogeneties assoon as possible so the cause can be eliminatedat an early stage of the process.

The rheological behaviour of the polymer melt isdefined by the molecular structure and allowsconclusions to the extrusion process.The quality of the granules, eg. the size andshape, has an influence on the pneumaticconveyance and of course also on the material

flow in the feeding process and extruder duringhigh performance extrusion.

For further processing the frequency and size ofgels and black specks in the film must bedetermined. These affect the optical appearanceof the film and reduce the mechanical stabilityand ability for treatment eg. printing, laminatingetc.

The surface quality is also an important QCcriterion when producing glossy and transparentfilms. Most thermoplastic material containsadditives for processing and preservation, thecontent of which has to be analysed duringquality inspection.

Optical Control Systems (OCS) has developed amodular conception of testing systems andoptions devices which can be combined according to requirements:• Pellet/powder purity• Size & shape distribution• Gels & contamination• Additives measurement• Rheology• Haze, gloss, thickness measurement• Pellet transport system

With these instruments all quality controlrequirements in modern plastic production andplastic conversion are fulfilled, offering tools forflawless history taking of all optical parametersfor effective process control and for root causeanalysis, treating and solid tests for processimprovements. •

all industries


13

• Product News

Temperature control unit peltier cylinder - a new dimension in performance, ease of use and flexibility

all industries

A new Peltier temperature controlunit for coaxial cylinder geometriesas well as plates and cones hasbeen developed to complementedthe series of temperature controlmodules for the Thermo ScientificHAAKE MARS and HAAKERheoStress 6000 (and itspredecessor models).

The module fulfills the highest requirements withregards to performance as well as handling. Themodule can be adapted to the rheometer withinseconds thanks to quick fit couplings, self-centering and auto-recognition.

This Peltier temperature control unit is suitable forfast temperature changes with temperaturegradients up to 40 K/min in a temperature rangebetween -40°C up to 200°C.

For temperature different to room temperatureusing a sample hood is recommended in order toensure an homogeneous temperature distributionwithin the measuring gap and avoidingcondensation or ice formation at lowertemperatures.

The Peltier cylinder is optimised for an easy insertof the measuring geometry as well as its quickand fast removal for cleaning. A wide range ofcoaxial cylinder geometries are available such asgeometries acc. to DIN 53019 (also as disposableversion), Mooney Ewart, double gap cylinder orvane rotors for relative measurements.

Plates and cones extend the application range ofthe Peltier temperature control unit. An insert withoptimised mass and material (Ampcoloy) isavailable in the function of a lower measuringplate, ensuring fast heat transfer in a temperaturerange between -20°C up to 180°C. •

Peltier temperature module for cylinders (left) and with built-in insert for plate and cone geometries(right), insert as well as plate and cylinder geometries


Modular rheometer platformfor individual demands

The HAAKE MARS III brochure nowincludes the addition of a newcustom combined measuringmethod - the innovative applicationsolutions such as the patentedRheonaut technique that offers yousimultaneous rheological and FT-IRspectrocopical measurements withthe Rheonaut compact module.

The Thermo Scientific HAAKE MARS III is one of the most modular high-end rheometerplatforms in its class. The innovative HAAKEMARS III system was designed for flexibility and meets the most demanding requirements in research and development with an architecturethat permits integration of custom modules.The concept is designed to meet today's andfuture rheology needs while protecting prioraccessory investments.•

polymer industries


14

• Product News & Industry Applications

Temperature control baths to suit your industry and applications

all industries

TemperatureControlBaths.comoffers the best selection oftemperature control productswithin Australia. This website isdedicated to the temperaturecontrol products portfolio fromRheology Solutions.

The range includes solutions for heating andcooling applications that provide the most flexible,cost effective temperature control solutions for amultitude of industries and uses.

These include:• analytical instruments • biological• biotechnology • chemical• environmental • food & beverages• laboratories • manufacturing• packaging • petrochemical• pharmaceutical • printing• process • QA & QC• raw materials • universities• research & development

Some 100 products are itemised on this websiteacross 12 category types (Accessories/Options,Baths, Cryostats, Fogging Tester, Heat Exchanges,Heating Bath Circulators, Immersion Circulators,Laboratory Chillers, Open Bath Circulators,

Process Chillers, Refrigerated Bath Circulators,Shaking Water Baths) and each product has fulltechnical specifications.•

Visit www.temperaturecontrolbaths.com.

Cool Tech Plus Refrigerated Bath Circulator• Max: flow rate: 17 L• Max: pressure: 300 mbar• Temperature range: -28ºC to 100ºC• Dimensions: 711 x 273 x 483 (HxWxL) mm• Cooling capacity: 320W @ 20ºC• Bath capacity: 6 to 10L• Work area: 204 x 173 x 129 (DxWxL) mm• Net weight: 36 kg• Order no: 152528101

Looking for something else?Rheology Solutions are able to offer you the most flexible, cost-effective temperature control solutionsfor a multitude of applications. Contact us now to discuss your application and temperature controlrequirements and we will recommend the product to meet your single or multiple equipment orapplication temperature control requirements.

(*) Price excludes GST and local delivery. 48 hours delivery from receipt of purchase order.

$3990DELIVERED

IN 48 HOURS*


15

• New Product

The Schleibinger viskomat XL, rheometer for mortar and fresh concrete up to 8 mm grain size

Based on 20 years experience with rheometers for mortar andfresh concrete, Schleibinger hasdeveloped a new instrument called viskomat XL.

It fills the gap between the viskomat NT formortar and paste with a specimen volume of 360ml and the concrete rheometer BT2 with asample volume of 20l. The principle of operationof the viskomat XL is nearly the same as for theviskomat NT. A mixer formed probe measures thetorque, while the specimen vessel rotates and anadditional scraper cleans the wall of the vessel.

Very dynamic speed rangeThe speed - 0.001 to 100 rpm in both directions,clockwise or counter clockwise. The speed may

be defined in several steps, as a linear increaseor decrease of speed. As an option also anoscillating or a logarithmic mode is possible.

High torque rangeThe viskomat XL has a torque range from 0..500Ncm with a resolution of 0.05 Ncm and accuracybetter then 0.2 Ncm. Optionally a sensor with atorque range up to 1000 Ncm and a accuracy of0.8 Ncm can be installed.

Temperature controlTemperature control is achieved by using adouble wall specimen container, with a circulatingcooling liquid. The specimen temperature ismeasured with a RTD mounted inside the shaft ofthe probe.

High time resolutionThe sampling rate can be set from 0.005s ..1min. Shear Stress Control Mode (optional) allows

you to run the viskomat XL with a shear stresscontrolled mode. The torque is preset over time,and the speed is automaticly controlled to achievethe predefined torque.

SoftwareThe viskomat XL is controlled with a built incomputer or via a network interface. TFT screen,keyboard and mouse are included.

DimensionsHeight 1320mm, width 315 mm, depth 410mm(without safety cabinet), Height 1320mm, width400 mm, depth 510mm, with safety cabinet.

Delivered with 3.5l vessel, online display with TFTscreen, 4 USB-ports, keyboard mouse, incl. 1meas. beaker, 1 double wall vessel incl. valves for temperature control, 1 probe for concrete and mortar, maximum grain size 6..8 mm,user manual. •

construction & building industries

The Viscomat XL is the first oscillating fresh concreterheometer on the market

Technical Data

Application rheometer for mortar paste and fresh concrete up to 6..8mm

Net. Size (h x w x d) 1320 x 315 x 410 mm (without safety cabinet)

Specimen volume 3.5l, inner diameter 165mm,height 175mm, other sizes on request

Motor speed range 0.001..100 rpm

Motor torque 1200 Ncm

Motor angle measurement better ± 0.05°accuracy

Measuring torque range ±0..500 (1000*) Ncm

Measuring torque resolution 0.05 (0.2*) Ncm

Measuring torque accuracy 0.2 (0.8*) Ncm

Temperature sensors RTD PT100 1/10 DIN B

Cooling and heating double wall vessel

Controller extra cabinet, 110..230V, 50..60Hz, 800W

Controller interfaces 4 x USB, 1 x network

User interface colored screen with online graphic,TFT-screen, keyboard mouse, no external computer necessary

Interfaces ethernet /TCP/IP for control and data recording

Weight including electronic and safety cabinet ca. 120 kg

Safety cabinet, with security switches included

Further information is available by contacting Rheology Solutions:

Telephone: 03 5367 7477 Email: [email protected]: 03 5367 6477 Web: www.rheologysolutions.com

RHEO439

• Product Review

Film Surface Analyser - FSA100

FSA100 is a modular surfaceinspection system for use inlaboratories and production.

The film quality is assessed optoelectronicallythrough the use of high resolution line camerasand the appropriate illumination technology. Themeasurement data are stored in an inspectionreport so that later analysis is possible at anytime.

The modular concept permits the use of differentcamera and illumination constellations and cantherefore be optimally used for transparent, dyedand nontransparent plastic films.

In addition to the recognition and classification ofdefects, the system can also be used for analysis,recording, archiving and documentation purposes.Every defect detected is transferred with thedefect image to the measurement protocoltogether with its feature vector (position, size,shape...).

Performance features

• Modular architecture - Simple possibility ofadaptation

• Operation - Menu-guided Windows desktopwith individual window representation

• Optimum lighting technology - Use ofspecial lighting techniques (filters, diffusers)depending on the material to be inspected

• Real-time defect analysis - Rapidevaluation and representation of themeasurement results in various ways. Tablewith size classes, time history, mosaic view,grades graphics ....

• Table view - Tabular display (absolute, perm, total defect area etc. and trend display) asa function of defect size and type

• Mosaic view - Continuous display of thedefects detected as real images (display ofdefect sections)

• Time history - Graphic representation of thedefect classes detected as a function of time,length or parcels

• Easy teach-In classification - Defects areautomatically classified by their featuresthanks to the use of intelligent fuzzytechnology

• 3D defect analysis - High-performancesoftware tool for improved image analysis

• Transparency measurement - Fortransmittance measurements, onlinedetermination of the absolute and relativetransparency values

• Process synchronisation - Linking of theinspection system to external equipment, e.g.link to industrial data acquisition system orSAP

• Interfaces for external equipment -APLAIRS, thickness measurement, glossmeasurement, haze measurement, labelprinter...

• Open database - The protocol data can beconverted into all common file formats(Access, Excel ...)

Fields of application

• Transparent materials - (LLDPE, LDPE,HDPE, PC, PS, PET …)

• Non-transparent materials - (rubber ordyed plastics etc.)

Types of defects

• Contamination• Gels• Fibres• Foreign particles• Black specks• Holes •

food industries

polymer industries



News & Views Expanded contract testing · PDF fileInstruments & equipment in ... ambient - +400°C (electrical temperature ... measurements for polymeric materials has mostly....

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