Surface Smoothness Test for Power Cable Semi-Conductive ...

dec 11 - mar 12

[email protected] 1 www.rheologysolutions.com

• Industry Applications

Surface Smoothness Test forPower Cable Semi-ConductiveCompounds (Semicons)

Mechanical imperfections protruding from thesemi-conductive surface into the insulation(protrusions) amplify electrical stresses inproportion to the size and sharpness of theprotrusions, thereby promoting tree growth(Figure 1) in the insulation and premature failureof the cable. Acceptable cable life can only beachieved with smooth interfaces and low ion/lowsulphur containing semi-conductive formulations,as shown in Figure 2.

The performance of a conductive black in asemicon application is therefore a function of thephysical cleanliness of the conductive blackand the quality of its dispersion. Dispersion is,in turn, influenced by the conductive blackmorphology, the pellet quality, the semiconformulation and the compounding technology. Theconductive black loading has also an influence onthe results. Often, the higher the loading (for thesame black), the better the surface smoothness.Indeed, if the loading is increased, the shear

during the mixing is also intensified and thus,the dispersion can be improved. The surfacesmoothness test measures the sum of theseeffects.

The surface smoothness test involves thecontinuous extrusion of a formulated semicontape (polymer filled with conductive black)through a die, under controlled extrusionconditions, to achieve a constant thickness.An on-line camera coupled to a computersimultaneously registers images of the extrudedtape surface and performs the imageanalysis. The result is a detailed description ofthe number of defects by size and by shape.

The system can detect protrusion, fish eyes,black spots, holes and others inhomogeneities,putting them into 10 freely definable class sizes.The quality of the resolution depends on the usedoptics being the standard resolution 18μm.

A full copy of this application paper is availableby quoting OCS010. �

Figure 1: Growth of vented water trees Figure 2: Effect of surface smoothnesson cable life

Figure 3: Previous extrusion of semicon tapes tothe on-line image analysis

• In This IssueSpecific Industry Key

Pg. 2, 5, 8, 10, 11,12, 13, 16 & 17

Pg. 1, 3, 4, 14,15 & 16

Pg. 17

Pg. 10 & 17Pg. 10, 14 & 17

Pg. 5 & 6

Pg. 6, 7, 9,17 & 18

See AllIndustries

www.rheologysolutions.comdec 11 - mar 12

2

• In This Issue:

Technical Papers

17 Rheological Investigation of StarchSwelling, Gelatinisation andRetrogradation

18 Investigating Mixtures Of Poloxamer17 Investigating the Influence of Sodium

Chloride on the Gel Point of PoloxamerFormulations

18 Monitoring the Output ofPharmaceutical Hot Melt Extruders

News & Views

07 Article – Continuous Granulation –Opportunities to Increase Efficiency inPharmaceutical Production

07 Pharmaceutical Melt Extrusion - MostFrequently Asked Questions

10 Missed an Issue of RheoTalk

08 Viscometer & Rheometer Calibrations2012

14 Schleibinger Update14 Optical Control Systems 2012 Exhibitions05 Applications Laboratory

Product News & IndustryApplications

09 Conical Micro-Compounder for HotMelt Extrusion

03 Online Polymer Analysis in BorealisGroup

01 Surface Smoothness Test for PowerCable

04 Online Measurement of Contaminantson Polymer Pellets

05 New UV Module for UV CuringMeasurements

06 Viscometers – A Brief Overview02 Refrigerated Circulator Available

for 48 hour Delivery10 Viscometer for Mining & Construction

Materials

11 Product Reports

11 Double Gap Geometry

11 Sample Hoods

12 Normal Force Option

12 Exchangeable plates

13 Temperature Control Unit Peltier

Cylinder

11 Spectroscopical Insight

13 Adapters

13 Flexible Holder

16 New Literature

16 Modular Universal Rheometer

16 Refrigerated & Heated Bath

Circulators

17 Process Viscometers

15 Literature

16 Film & Liquid Optical Testing Systems

15 Extrusion – Cast & Blown Film Lines

15 Pellet & Powder Optical Testing

Systems

• Product News

Cool Tech Plus Recirculating Bath Circulators $3,990* (Delivered in 48 hours- Stock available)

With the calendar year ending, this isyour chance to place your order forthe current calendar year.

We are pleased to advise that we now hold stockof these circulators and are able to ship one toyou within 48 hours of receipt of your purchaseorder. Contact us for a formal quotation.

Max: flow rate 17 L

Max: pressure 300 mbar

Temperature range -28ºC to 100ºC

Dimensions (HxWxL) mm 711 x 273 x 483

Cooling capacity 320W @ 20ºC

Bath capacity 6 to 10L

Work area (DxWxL) mm 204 x 173 x 129

New weight 36 kg

Order no: 152528101

* Excluding GST ** Delivery $125 plus GST

Looking for something else?Rheology Solutions are able to offer you the mostflexible, cost-effective temperature controlsolutions for a multitude of applications across:• Pharmaceutical • Petrochemical • Food & Beverage • BioTech• Analytical Instruments • Chemical • Laboratory Equipment • QA/QC• Research & Development

The range covers: • Refrigerated Bath Circulators • Recirculating Chillers• Software Options • Heating Bath Circulators • Water Recirculators• Extensive Range of Accessories • Ultra Low Refrigerated Circulators• Open Bath Circulators

If you would like to discuss your application andtemperature control requirements, please contactour office 03 5367 7477 or email [email protected]�

[email protected] 10-mar 11

3


Online Polymer Analysis in Borealis: a Step Change in Process & Quality Control

Manufacturers today need to makeever improving products even faster.

At Borealis they help their customers meet thesecontinuously higher market demands by pushingthe boundaries of our polymers. But they do morethan that: higher quality demands also require atrue step change in quality control.

In traditional quality control, process variation ofpolymer properties is tracked by checking theregular final blend and through process and spotsampling. With the increase in throughput andmore stringent consistency requirements, thisapproach has reached its limits. Today, Borealismonitors the main quality properties online:tacticity indicators (xylene solubles, heptaneinsolubles, decaline solubles), copolymer contentfor polypropylene (PP), density for polyethylene(PE), gels and contaminants determination andrheological properties.

The choice for online technology is a consistentstrategy in Borealis plants and joint ventures, withthe following OCS solution already implemented:• online gels and contaminants determination

(OCS, Germany).

Gel and Contaminants MeasurementsDetermining the level of gel (or fish eyes) and/ormicro-contaminations are crucial qualityparameters for the Borealis Film and Wire & Cable businesses.

The analyser house in Schwechat for the LD3 and4 reactors

Pellet Contamination and AppearanceBorealis uses the PA66 from OCS for qualitycontrol and online instrumental pellet analysis. Ithas allowed us to standardise the reportingof pellet shape and size throughout all locations.

The online application is used in Wire & Cable tooptimise production cycles and will be installed from the start-up in our new PP plant in

Burghausen. The software stores defects anddeviations in pellet size or shape, so they can beused for reference to allow faster trouble-shootinglater.

A typical particle size distribution

The FSA100, developed by OCS, is a modularinspection system for use in laboratories andonline in production. The film quality is assessedopto electronically with high resolution linecameras and the appropriate illuminationtechnology.

A higher resolution on the camera, a calendarunit, a marking unit and a cutting/sorting devicetake quality control a huge step forward. Thesystem is used in Film & Fibre plants as well asfor measuring the cleanliness of insulationmaterial in Wire & Cable.

Because the concept is modular, it allowsdifferent equipment like APLAIRS (FTIR), thicknessmeasurement, gloss measurement or hazemeasurement to be used in an integrated waywithin the system. �

The cleaning of an extruder and the returnto a high purity level

A selection of contaminants identified by thepellet analyser

A full copy of this application paper is availableby quoting OCS011.

www.rheologysolutions.comdec 10-mar 11

4


Online Measurement of Contaminantson Polymer Pellets

Figure 3: Level of contaminants, productioncampaign with shower of contaminants

Figure 4: Level of contaminants before extruder stop

Figure 5: Level of contaminants after extruderstart up

Figure 6: Level of contaminants during transition

Picture 1: Online Polymer Analysis installation, Schwechat line A & B

Online equipment (from OCS GmbH) installed atBorealis line A and B is as follows:• PA66, consisting of PS25C (pellet

contamination) and PSSD (pellet shapeand size)

• FSA100, CR8, ME20/26V2, gel andcontamination on film

• APLAIRS, FTIR density and additive analysison film

• PTS, pellet transport system

Pellets pass through the PS25C and are analysedwith a 3-CCD chip colour camera, the defects aredivided into colour classes and size classes.A contaminant is defined as a moving defectwhich is detected at least three times whilstpassing through the viewing field of the camera.All detected contaminants are shown as mosaics(see figure 1) to which size and spectrum arelinked (see figure 2).

Using the spectral information shown in figure2 a user defined colour class can be made fromany detected contaminant.

For our purposes the longest elongation isreported for the size classes of the contamination.

Figure 1: The detected contaminants are shownas mosaics

Figure 2: Colour spectrum and size data from acontaminant

Figure 3 shows the level of contaminants duringa production campaign with a shower ofcontaminants. Due to this high amount ofcontaminants only for a short period of time it is necessary to down-grade the whole lot.By means of a fast online detection ofcontaminants it is possible to cut out the poorquality product by changing the production silo.

Online detection of contaminants is also usefulto optimise the way of running the plant. It is

possible to visualise the impact of different plantoperations on the level of contaminants. Figure 4and figure 5 show the developing of the level ofcontaminants during an extruder cleaningprocedure before shut down and after start up ofthe production extruder. Figure 6 shows the effectof extruder cleaning during a transition. �

A reprint of this application paper is availableby quoting OCS012.


5

• Product Report

New UV Module for UV Curing Measurements

In many industrial segments theuse of UV curing materials for theprocessing or application of paints,inks, adhesives, coatings, etc. is ofgreat importance.

This technology combines environmental andeconomical advantages with improved productfeatures:• Higher throughput in production processes

thanks to faster curing• Higher profitability because of less required

space in manufacturing plants, no need forpost-treatment of exhaust fumes and noneed for Ex-protection

• Solvent-free products for environmentalfriendly processes and improved workingsafety

• Optimised product features, including abetter corrosion and abrasion protection,better chemical resistance and betterformability

For measurements on UV curing materials a newmodule for the HAAKE MARS rheometer platformhas been developed. This module consists of anupper shaft with an integrated mirror and anexchangeable quartz glass plate, as well as aholder for a collimator plus light guide, which ismounted to the HAAKE MARS measuring head.

The UV light beam of a commercially availablelight source, first bundled by the collimator andthen reflected by the mirror, is directed into thesample vertically from above through the quartzglass plate.

The quartz glass plate is the upper plate of aplate / plate measuring geometry, whereas the

lower plate is part of a standard temperaturecontrol module, this allows for a temperaturecontrol of the sample within a wide temperaturerange.

Quartz glass plates with diameters of 8 and20mm are available for the adaption to thedifferent viscosities and G moduli of the samples.The quartz glass plates are available in twodifferent versions: a circular model, which needsa separate clamp ring made of stainless steel, asa simple low-cost version as well as a one pieceglass model with integrated clamping surface.

A selection of different standard temperaturemodules for plate/plate measuring geometries(TM-XX-P) using different technologies like aPeltier-element, electrical-heating plus liquidcooling or a circulator, are available to cover awide range of temperatures and applications.Alternatively the new UV module can becombined with the (temperature controlled)Rheonaut module for simultaneousmeasurements of rheological properties and FTIRspectra to investigate structural changes withinthe sample.

The use of the optional available sample hood isrecommended for measurements beyond ambientconditions. This hood is made out of Teflon andcan be used for temperatures up to 240ºC.

Using the HAAKE RheoWin rheometer softwarefully automated measuring and evaluationroutines can be created including an automatictriggering of the UV light source. Especially forvery fast curing materials a new measuring mode- the so-called FastOSC for oscillatory tests – has been developed. FastOSC offers a dataacquisition rate of 500 Hz (i.e. one data point per2 ms) independent of the oscillation frequency.�

HAAKE MARS III configuration for UV curingmeasurements including temperature control

Measuring geometry and adapter for mounting& adjusting the collimator & light guide

A copy of this product report (including orderinginformation) is available by quoting P-037.

• Company News

Applications Laboratory

Specialist contract testing services are availableand contracts can be tailored to suit discrete testsor protracted testing requirements involving aseries of tests over a period of weeks or months.

Rheology Solutions has invested in a fullyequipped applications laboratory to further

increase the level of customer focus andapplication support. The appointment of tworheologists and the upgraded laboratory facilitieshas proved to be a great asset to new andexisting customers. These initiatives are providinga valuable resource to the growing customer basewithin the field of rheology and materialcharacterisation. The key areas we service are:• Contract testing of customer samples and

products

• Technical support for new and existingRheology Solutions customers

• Customer method development & validation• Customer training covering rheology theory

and practice• Development and facilitation of rheology

seminars and workshops �

For further information contact us either by phone 03 5367 7477 or [email protected].


6

• Application Focus

Viscometers – A Brief Overview

Following is a brief overview on theThermo Scientific HAAKE range ofviscometers. These are suitable forpaints, inks, food, cosmetics and or oil samples.

HAAKE Falling Ball Viscometer type CFalling ball viscometer for accurate viscositymeasurements of transparent Newtonian liquidsand gases in a wide temperature range (new: upto 150ºC). It meets the requirements of theGerman DIN 53015 as well as ISO 12058standards.

HAAKE Falling Ball Viscometer type C

HAAKE Viscotester 1 plus & 2 plusSmall, battery-operated rotational viscometer,suitable for quick, reliable tests and comparativemeasurements for quality control applications.Easy to use due to the digital display and one-button operation.

HAAKE Viscotester 1 plus & 2 plus

HAAKE Viscotester C, D & ERotational viscometer for comparativemeasurements in quality control according torecognised standards such as ISO 2555.Extended measuring range thanks to the smallsample and low viscosity adapters as well as theHAAKE RheoWin software for automated jobroutines.

HAAKE Viscotester C, D & E

HAAKE Viscotester 550Modular rotational viscometer for the rheologicalcharacterisation of low up to high viscosesamples. A wide range of absolute and relativemeasuring geometries can be used with built injob routines or with the HAAKE RheoWinsoftware.

HAAKE Viscotester 550

HAAKE RheoWinIndividually configurable measuring andevaluation software for automated job routines.Pre-defined elements for beginners and additionalmodules for experts or to help meet the FDArequirements.�

“Here I am! Just waiting and resting” Marshal“I'm ready... do you want me to come to you?” Evie


7

• Application Focus

Pharmaceutical Melt Extrusion Most Frequently Asked Questions

As more knowledge on meltextrusion is developed anddiscovered by pharmaceuticalscientists worldwide, people who are new to the arena are facedwith similar questions.

In the Thermo Scientific Melt Extrusion - FAQpage, they address and comment on some ofthe most frequently asked questions. Followingis a copy of the details that they provide atwww.thermoscientific.com/mc_pharma

FAQ 5: I have bubbles in my extrudate. Dothey matter and where do they come from?

We assume here that the target was not to obtaina foam by adding foaming agents to theformulation and so the answer to the firstquestion is: Yes, bubbles matter, because theycan lead to a different mechanical characteristicsof the extrudate as well as bubbles could meanthe result of an non-optimised process as it willbe discussed below.

Where do they come from? This can havedifferent causes.1. With feeding in materials, air was pulled in

and could not leave in the feeding zone. Thiscan happen with micronised materials

especially if the material tends to stick. Also ifliquids are fed in and some gases aredissolved in the liquid these gases could bereleased in the extruder. As long as oxygen orother gases does not mean a harm to theformulations ingredients, this is no problemand can be overcome by optimisation offeeding zone and/or by opening the ventingport.

2. If a component of the formulation ishygroscopic and it is fed non-conditioned (i.e. dry air) or in pre-dried condition, thisabsorbed moisture can be released attemperatures above boiling point as vapourwhich form the bubbles in the extrudate then.Since liquids like e.g. water acts asplasticiser they can be a problem if includeduncontrolled or not-considered in theformulation. If a substance in yourformulation would be unstable in humidcondition this moisture would mean aproblem. The problem can be avoided byopening the venting port to remove the watersteam and by using dry products. In generalit is important to not expose hygroscopiccomponents to high moisture.

3. Bubbles could mean a degradation of one ormore components. If decomposition occursby unfavorable process conditions you needto optimise your process. With the meltextrusion process it is possible to have verygentle conditions which allow you to handleeven heat-sensitive substances. If

decomposition of a component is caused bychemical incompatibility or by a chemicalreaction with another component you need tooptimise the formulation.

Please feel free to contact Thermo Fisher if youfind bubbles in your extrudate. They will help youin solving this problem.

Coming up soon:

FAQ 6: How can an API be stabilised in theamorphous state for the complete shelf-lifeperiod of a drug?

Questions 1 – 4 were published in the previousissue of RheoTalk.• FAQ 1: What is Melt Extrusion?• FAQ 2: How can I ensure the content

uniformity of my active pharmaceuticalingredient?

• FAQ 3: How can I apply Cremophor* as aplasticiser even though it is in a paste form?

• FAQ 4: What is our recommendation in termsof a direct up-scaling from a small-scale to aproduction-scale cGMP?

* Cremophor is the registered trademark of BASF Corp.

To access all the pharmaceutical melt extrusionmost frequently asked questions log ontowww.thermoscientific.com/mc_pharma�

• News & Views

Continuous Granulation - Opportunities to Increase Efficiency in Pharmaceutical Production

The particle size enlargement by granulation isoften used in the manufacturing of tablets andcapsules. The efficiency of a traditional batchprocess can improve considerably if the wholeprocess of tablet manufacturing is converted intoa continuous process. Granulation isimportant here, as this influences thecompressibility and the release profile of thedrug, as well as the quality of the final product.

Read more on the method for the continuousgranulation that allows the user to adapt itsexisting processes while simultaneously designingnew developments.�

A copy of this paper is available by quotingHA050.

The paper was published in the PharmaBio World. www.pharmabioworld.com

Thermo Scientific Pharma 16 TSE with feeder


8

• News & Views

Viscometer & Rheometer Calibrations 2012

Why re-calibrate?The accuracy of the electronic components usedin all instruments drifts over time. The effects oftime in service as well as environmentalconditions add to this drift. As time progresseschanges in component values cause greateruncertainty in your measurements. At some pointin time, the drift causes the instrumentsuncertainty to become undefined, meaning themanufacturer can no longer predict theuncertainty and guarantee measurement results.To resolve this issue instruments must becalibrated at regular intervals as defined by themanufacturer.

Calibration is the comparison of an instrumentsperformance to a standard of known accuracy.The result of a calibration may be documentationshowing the deviation of a measurement from theknown standard or it may also include adjustingthe instruments measurement capability toimprove accuracy.

The goal of calibration is to quantify and improvethe 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 turn around from the time it arrives in ouroffice and we will contact you to confirm receiptof equipment 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

contact in the coming weeks to arrange andfinalise your booking.

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 16th January 2012• New South Wales

Week commencing 13th February 2012• South Australia & Tasmania

Please contact our office to arrange a time• Western Australia

Scheduled for mid November 2012

The pricing for calibrations that are conducted inour office or link in with the scheduled interstateschedule in 2012 are based on Melbournemetropolitan rates as follows:

HAAKE RheoScope 1* $ 1,675.00

HAAKE RheoStress 50* $ 1,275.00

HAAKE RheoStress 600* $ 1,275.00

HAAKE RheoStress 6000 $ 1,275.00

HAAKE RotoVisco 1 $ 1,675.00

HAAKE RheoStress 1 $ 1,675.00

HAAKE ViscoTester 550 $ 895.00

HAAKE MARS $ 1,675.00* Denotes the model has been discontinued by the manufacturer

Notes:• Melbourne metropolitan customers can have

their HAAKE instrument calibrated at anytime on site.

• Victorian customers (non metropolitan) can

arrange 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.

• The manufacturer guarantees that spareparts for all old units will be available for atleast seven years from the date the modelwas discontinued.

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• and 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, spare parts can beobtained from us at any time.


9

• Product News

Conical Micro-Compounder for Hot Melt Extrusion Built to GMP Standards

When developing new drugs,shortening time-to-market andreducing waste of expensiveAPI’s and overall developmentcosts provide a distinctcompetitive advantage.

Hence, quick and early assessment of newAPI/excipient formulations is critical. The ThermoScientific Pharma mini HME allows users toidentify the right drug candidates for hot meltextrusion by compounding as little as 3 grams ofmaterial.

Materials• Pharmaceutical ingredients (API’s)• Excipients• Medical polymers• Drug delivery systems• Soft gels

Applications• Hot melt extrusion• Medical devices• Implants• Controlled drug release• Handling and processing of highly potent

API’s in a glovebox

Thermo Scientific Pharma mini HME

Thermo Scientific Pharma mini HME screwcomponents

The challengeHot melt extrusion and continuous processing canlead to speedier formulation development andcost efficient production. But in development ofnew drugs, users are still faced with severalchallenges. Due to very expensive and hencelimited quantities of API, finding the rightAPI/excipient formulation and testing if thisformulation is the right candidate for hot meltextrusion can be difficult. In this phase, the healtheffects of a new API are often not clear. Thereforeit can be necessary to run such trials in a laminarflow or glovebox.

On the other hand, new special implants designedfor controlled drug release are produced in suchsmall dimensions that a delivery rate of onlya few grams per hour is required to establish amicro production line.

The solutionWith the Pharma mini HME, we offer a microtwin-screw compounder which requires as littleas 3 grams of total material to identify the rightdrug candidates for hot melt extrusion. Thecompounder with conical co- or counter-rotatingscrews is designed to minimise waste and reducedowntime necessary for cleaning.

The product contact parts can be easily removedand cleaned using a washing machine and anautoclave. But even washing the product contactparts by hand is simple due to rounded edges andminimised screw threads and crevices. To reducethe risk of cross-contamination and cleaningdowntime to a minimum, additional sets ofproduct contact parts are available.

All parts are designed and manufactured to alloweasy handling as well as quick assembling anddisassembling, even with gloves in containmentsolutions such as a laminar flow box or aglovebox. This containment solution is also

supported by the very small footprint of thePharma mini HME and the separate touch screencontrol which offers the same look and feel as thelarger Thermo Scientific Pharma twin-screwextruders. The IP 54 rating and the fanless designallow the operator to spray-wash the Pharma miniHME to bind powdery excipients and API’s.

The conical screw design offers the advantage ofreducing total volume and extra pressure build upat the screw tips to extrude a uniform materialwith constant output rates. In addition, the conicaldesign offers the best mixing capability on such asmall scale and allows the Pharma mini HME tooperate without the use of expensive and sensitivefeeding devices.

In combination with the integrated feed portcooling and an optional continuous force feeder,the Pharma mini HME can be used as continuoussmall scale compounder to prepare samples forclinical trials or for micro production of medicaldevices and implants as drug delivery systems.The shape of the extruded material can becontrolled by adding various die sections.�

Technical Specifications

Motor power 400 W

Speed range 10…360 min-1

Max. torque 5 Nm / shaft

Power supply 230 V ± 10 %, 50/60 Hz

Design Conical co-/counter rotating

Max. temperature 280ºC

Heating time (22º - 170ºC)

< 10 Minutes

Volume 3 g (4 ml)

Screws Co- or counter rotating,pharma grade stainless steel 1.4112 (440 B)

Barrel High performance / pharma grade stainless steel M340


10

• Product NewsThe Ideal Controlled Rate Viscometerfor Mining & Construction Materials

ApplicationThe measurement of the flow properties ofmineral slurries and construction materials is ofpractical interest in a broad spectrum ofapplications. Especially the quantitativeknowledge of the yield stress which is exhibitedby these materials is very important to improvetheir storage, processing and transportationproperties.

SetupThe Thermo Scientific HAAKE Viscotester 550 isespecially designed for Quality Controlapplications. It is a suitable instrument for quickand reliable tests and comparative viscositymeasurements, which are important for theprediction of flocculation or aggregation ofmineral slurries and enhancement of materialproperties.

All measurement results like the viscosity, shearstress, shear rate, yield point and the sampletemperature are shown on the digital LED display.

The Thermo Scientific HAAKE Viscotester 550 canbe used as a stationary laboratory viscometer oras a portable unit. The well known “Boger –

method“ (J. of Rheol., 27(4), 321-349 (1983)),for measuring the yield stress value using a vanegeometry rotating at a very low angular speed,isintegrated in the instrument firmware. The yieldstress value provides valuable information aboutthe force required to start the movement(rotation) of impellers or rakes immersed in aslurry or suspension.

For running measurements and data evaluationthe instrument can also be connected to a PCand operated with the HAAKE RheoWin software,the universal software for all Thermo Scientificviscometers and rheometers. For measuring yieldstresses using a vane rotor the HAAKE Viscotester550 is available in a “ready-to-go“ packagedelivered in a stable carrying case and consistingof the base unit together with a powersupply, a vane rotor FL 100, a universal cardancoupling for E, FL and RS sensors and the HAAKERheoWin software.

Advantages at a glance• Robust and reliable rotational viscometer for

use with predefined internal routines or withthe HAAKE RheoWin software

• Easy to use as handheld or standaloneinstrument

• Precise measurements of viscosity incontrolled rate (CR) mode

• Yield stress measurement using the Bogervane method

• Viscotester 550 Slurry package�

Thermo Scientific HAAKE Viscotester 550

• News & ViewsMissed an Issue of RheoTalk?

All issues of RheoTalk are available on ourwebsite www.rheologysolutions.com/news/newsletters/ as a PDF file. The Rheology SolutionsNewsletter was created in 1999 specifically forAustralian customers and interested parties. Theconcept of this newsletter is to provide an updateand overview of news and informationcovering Australian Seminars, Industry SpecificApplication Reports, Product Launches, NewAppointments and General Product Information.

A Biennial RheoTalk PDF version is availablecommencing with 2005 - 2006. The concept ofthe cumulative issue is to provide industries witha complete index that categorises the contentsinto specific industry related information.

The industry classifications used are:• Building & Construction Industries• Chemical & General Manufacturing Industries• Food Industries• Mineral Slurries• Pharmaceutical, Cosmetics & Allied Industries• Polymer Industries• Surface Coatings Industries�


11

• Product Reports & Information

Spectroscopical Insight into Rheology

Suitable for Thermo ScientificHAAKE MARS

With the Rheonaut a compact module has beendeveloped* to investigate structural changes of amaterial on the molecular level using FT-IRspectroscopy.

With the patented Rheonaut module a standardFT-IR spectrometer with side port and the ThermoScientific HAAKE MARS rheometer is coupled toform one measuring unit.

The Rheonaut technology enables a new level of understanding of rheological properties andprocesses, which depend on changes on themolecular structure. On the one hand,deformations and orientations of moleculesas function of shear can be monitored. On theother hand the insitu-spectroscopy enablesthe investigation of chemical reactions in themeasuring gap such as chemical or thermalcuring of polyurethane (PU)- or epoxy-adhesives.�

A copy of this Product Information sheetis available by quoting P-033.

Image: Rheonaut module

• Product Reports & InformationDouble Gap Geometry for Pressure Cell

Suitable for Thermo Scientific HAAKEMARS & Thermo Scientific HAAKERheoStress rheometers

A new measuring geometry for the pressure cellD400/300, which extends the measuring rangedown to lower viscosities, is now available. Thisdouble gap cylindrical geometry PZ DG 34 Ti, asschematically illustrated in Fig. 1, consists of two

parts. The inner part - designed as an insert – isat the same time the bottom lid of the pressurecell and is equipped with two ports: One port forfilling the sample into the cell and one port foradapting a temperature sensor to monitor thetemperature of the sample during themeasurement.�


Fig. 1: Double gap geometry


New Series of Sample Hoods with Integrated Solvent Trap for Plates/Cones and Cylinders

Suitable for Thermo Scientific HAAKEMARS & Thermo Scientific HAAKERheoStress rheometers

A new series of universal sample hoods weredesigned for the HAAKE rheometers for use incombination with parallel plate, cone & plate andcoaxial cylinder geometries.

The use of a hood is recommended formeasurements at temperatures beyond ambientconditions, when an inert gas atmosphere isrequired or in order to prevent solvent loss.�


Image: Sample hood made of glass


12


Normal Force Option

• Product Reports & InformationExchangeable Lower Plates for Temperature Module


For cone/plate as well as plate/plate measuringgeometries it is important that the effectivediameter of the lower plate matches the diameterof the upper plate in order to achieve correctmeasurement results.

For the HAAKE MARS III temperature modulesmatching lower plates are available for all upperplates and cones (diameters 8 to 60 mm). Thestandard plates are made out of stainless steel.Inexpensive disposable plates made out ofaluminium, as well as plates with differentsurfaces (smooth, serrated, sand blasted) areavailable also. Customised versions are availableon request.�

A copy of this Product Report is availableby quoting P-029.

Temperature module with plate/plate measuring geometry and one half of a sample hood (made of POM: 222-1903) with integrated solvent trap

Suitable for Thermo ScientificHAAKE CaBER 1

The capillary breakup technique as used in theextensional rheometer Thermo Scientific HAAKECaBER 1 is a powerful tool to determine theextensional properties of fluids by measuring thedecline of the diameter of a stretched fluidfilament, which is narrowed down by the capillaryforce as a function of time. For certain sampleshowever, the physical properties of the sample,e.g. a specific sample structure or the lack of asubstantial surface tension, limit the use of thistechnique. In order to be able to measure theextensional properties of such samples with theCaBER 1 a different measuring approach isneeded.

With the normal force option, a compact modulehas been developed to investigate the normal forces that arise in the fluid filament during the

Schematic view of the experimental setup

initial stretching. Any existing CaBER 1 instrumentcan be equipped with this sensor.�

A copy of this Product Report is availableby quoting P-034.


13


Flexible Holder


An infinitely adjustable holder which can beattached to the optional mounting rods isavailable for the rheometer platform MARS.Individual components with a weight up to 4 kgcan be mounted and optimal adjusted with thisholder. A camera (e.g. FOculus type) for example,

can be used to observe the sample during ameasurement. The camera focusing on themeasuring gap provides images, which can bestored along with the rheological data in therheometer software RheoWin for further analysisof the measuring data.�


Image: Thermo Scientific HAAKE MARS III withmounted camera to the rear side

• Product Reports & InformationAdapters for ExtendingViscosity Measuring Range

Suitable for Thermo ScientificHAAKE Viscotester

The rotational viscometers HAAKE Viscotester C,D and E are described in the standard ISO 2555.The model C is suitable for the simple, fast andexact manual measurement of the viscosity andthe model D for routine measurements of theviscosity with data transfer. The expert model E

enables automatic measurements of flow curveswith PC connection. All 3 models are available intwo versions: whereas the ’’L’’-version is suitablefor measurements on low and medium viscosesamples, the ’’R’’-version can be used formedium and higher viscose materials.�


Image: Adapter with temperature vessel andconnections for circulator


Temperature Control Unit Peltier Cylinder

Suitable for Thermo Scientific HAAKEMARS & Thermo Scientific HAAKERheoStress 6000

A new Peltier temperature control unit for coaxialcylinder geometries as well as plates and coneshas been developed to complemented the seriesof temperature control modules for the ThermoScientific HAAKE MARS and HAAKE RheoStress6000 (and its predecessor 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.�


Image: Peltier temperature module for cylinders(left) and with built-in insert for plate and conegeometries (right), insert as well as plate andcylinder

geometries


14

• News & Views

An Update from Optical Control Systems (OCS)

During 2012, OCS will beparticipating at the followingexhibitions.

If you are in the area then it is worth a visit to theexhibition and their stand. The equipment on thestand is fully operational scanning samples.�

ExpansionTo improve their service and shorten the deliverytimes, Schleibinger Gerate is expanding theirfacilities by three fold. After several monthsorganising the government licenses etc, the planis to celebrate the opening of their new officesand workshop in January 2012.

2012 Conference & Exhibition ScheduleDuring 2012 Schleibinger will be participating inthe following conferences:• Shotcrete Conference 2012, January 12th-

13th, 2012, Alpbach, Austria• 21st Conference "Rheology of Building

Materials" February, 29th and March, 1st,2012, Univ. of Applied Science Regensburg,Germany

• 2nd International Conference onMicrostructure Related Durability ofCementitious Composites, April, 11th - 13th,2012, Amsterdam, Netherlands

• 1st International Congress on Durability ofConcrete - ICDC 2012, June, 18th - 21st,2012, Trondheim, Norway

• 18th Ibausil, International Conference OnBuilding Materials, September, 12th - 18th,2012, Weimar, Germany - one of the mostimportant conferences in the world!

NEW – The Rheometer for Fresh Concrete& MortarThe Schleibinger Viskomat XL, Rheometer forMortar and Fresh Concrete up to 8 mm andmore, grain size is based on 20 years experiencewith rheometers for mortar and fresh concrete. Itfills the gap between the Viskomat NT for mortarand paste with a specimen volume of 360 ml andthe concrete rheometer BT2 with a samplevolume of 20l. The operation principle of theViskomat XL is the same as for the Viskomat NT.A probe measures the torque while the specimenvessel rotates. An additional scraper cleans thewall of the vessel.�

Image: Schleibinger Viskomat XL Rheometer

OCS 2012 Exhibition Schedule

Name Month Dates Town Country Web Addressof Exhibition

Interplastica January 24th-27th Moscow Russia www.interplastica.de

Plast India February 1st-6th New Delhi India www.plastindia.org

ArabLab March 26th-29th Dubai UAE www.arablab.com

Chinaplas April 18th-21st Shanghai China www.chinaplasonline.com

NPE April 1st-5th Orlando USA www.npe.org

Plast Milan May 8th-12th Milan Italy www.plastonline.org

Achema June 18th-22nd Frankfurt Germany www.achema.de

• News & Views

An Update from Schleibinger Gerate

Optical Control Systems - In House Seminar will be runningin Germany in either May or June 2012.

The seminar is called "On-Line Inspection and Control."

Contact Rheology Solutions at [email protected] to register your interest in receiving further information. We will keep you posted as soon

as the dates and seminar content is finalised and provided from OCS.


15

• Product Brochures

Extrusion – Cast & Blown Film Lines

Optical Control Systems offer an extensive rangeof products specifically for R&D, QC, Lab & On-line applications for the polymer industry.

The brochure includes full product informationand specifications on the following products:• Measuring Extruder• Chill Rolls & Winder Unit• Cast Film Lines• Blown Film Lines• Pelletiser• Calender/Tape Test equipment• Filter Test System

This range of products is tailored to the needs ofR&D and QC for laboratory and on-lineapplications and will provide you with:• improvement of quality through elimination

of non-standard products

• competitiveness by QC automation • accurate and consistent automatic grading • reduction of customer returns and complaints• increased line speed and throughput where

manual inspection is a limiting factor –perfect for on-line and laboratory applications

• efficient, objective and reproducible laboratory evaluation

• optimised quality • increased competitiveness by automated QC• precise and consistent quality evaluation • faster inspection • reproducible operation settings • precise control of haul-off and winding

motors • fully automated control of haul-off and

winding tension • maintenance free • designed for 24/7 continuous operation. �

A copy of the product brochure is availableon request.

• Product Brochures

Pellet & Powder Optical Testing Systems

A range of powder and pellet optical testingsystems are available from Optical ControlSystems that provide information oncontamination and discolouration in productsamples or on line throughout production.

The brochure provides full product informationand specifications on the following products:• High Speed Pellet Scanning Systems –

with a throughput up to 200 kg/hr or material throughput up to 400 kg/hr

• Contamination Detection - for pellets with colour scanning systems

• Contamination Detection - for powder with colour scanning systems

• Pellet Size and Shape Distribution System• Pellet Analyser - for contamination analysis

plus shape, size and distribution system• Colour Measurement System – for automatic

colour measurement of plastic granules

This range of products are tailored to meet theoptical control needs of pellets and powders usedwithin polymer industries for QC & R&D withinthe laboratory and on-line applications and willprovide you with:• accurate and continuous automatic analysis • 24 hour on-line production surveillance • trend analysis parallel to production • logging of the production process accurate

and consistent automatic grading • reduction of customer returns for complaints • quality increase • scrap – sub standard product minimising • transition time reduction as all values are

permanently available • cost savings • optimising product sequences. �



16

• New Product Brochures

Thermo Scientific HAAKE RheoStress 6000

The updated brochure is now available on theThermo Scientific HAAKE RheoStress 6000. Thebrochure details the history of the development ofthe rheometer and the key design features andbenefits.

The information in the brochure includes:• full product specifications• software features including customisation

function

• temperature modules • measuring geometries • application solutions • application oriented accessories

The HAAKE RheoStress 6000 has applicationssolutions specific for:• paints, inks & coatings • food • petrochemicals • polymers• pharmaceuticals & cosmetics. �


• New Product Brochures

Refrigerated & Heated Bath Circulators

The Thermo Scientific refrigerated and heatedbath circulator brochure provides 26 pagespacked with everything that you will need to knowto decide on the right temperature control systemto meet your application requirements.

The brochure includes the following sections andinformation:• frequently asked questions

• immersion circulator comparison table• specifications for heated immersion

circulators • specifications for refrigerated and heated

bath circulators • ultra low temperature refrigerated bath

circulator specifications • heated bath circulators specifications • accessories.�


• Product BrochuresFilm & Liquid Optical Testing Systems

A range of film and liquid optical testing systemsare available from Optical Control Systems thatprovide information on contamination andimpurities in product samples.

The brochure provides full product informationand specifications on the following products:• Film Testing Systems – surface inspection

system for use in laboratories and production

• Sample Testing Systems – a bench unit for laboratories for inspection of transparent and non transparent surfaces

• Multiple Plaque Analyser – table unit to detect impurities on the surface of several plaques

• Liquid Analyser – for counting and classifying contaminations in transparent liquid substances. �



17

• Application Articles

Investigating the Influence of Sodium Chloride on the Gel Point of Poloxamer Formulations by Means of Oscillatory Temperature Sweeps

Different liquid pharmaceutical applicationsrequire a defined gel formation at temperatures ofthe human body. Poloxamers such as 188 or407 offer this characteristic behaviour, whereasboth sol/gel transition temperature and gel

strength are affected by various parameters (e.g.poloxamer concentration in the aqueous system).

It has been described in literature that additivessuch as active ingredients are influencing the gelsystem as well. This may lead to a quite complexgel system. From the rheological point of view,oscillatory temperature sweeps have to beapplied for its characterisation.

The aim of this work was the rheologicalcharacterisation of aqueous solutions ofpoloxamer mixtures holding different amounts ofsodium chloride as model substance. Particularfocus was laid on gel point temperature andstrength of the formed gel.�

A copy of this Application Note is availableby quoting V-253.

• New Product BrochuresProcess Viscosity Measurement Solution

A new brochure on the Viscotronics range ofprocess viscometers from Marimex is nowavailable.

The brochure provides a detailed overview on theentire range of process viscometers. It includesinformation on the operating principle of the

viscometers, the technology and full productspecifications and overview on each of theproducts in the range.

Additionally, information and specifications isprovided on the transmitters and accessoriesthat are available.�



Rheological Investigation of Starch Swelling, Gelatinisation & Retrogradation using a Rheometer with Starch Pasting Cell

Starch is a very important natural material for thefood, adhesive, pharmaceutical and buildingmaterials industry. Its unique properties andlow price make starch a widely used material forvarious applications. Most common is its use asthe main component of flour in bread, otherbakery products and pasta. As a thickening agentfor liquid formulations like soups, sauces orcreams, as an adhesive in glues or even as acarrier in pharmaceutical applications, starchplays a key role in developing and improving avariety of products.

In production processes it is extremely importantto ensure consistent quality and production rates.Because starch is a natural product it has tobe precisely characterised in the incoming goodscontrol and throughout the whole productionprocess. This application note will focus on therheological characterisation of starch swelling,gelatinisation and retrogradation.�


Further information is available by contacting Rheology Solutions:

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

RHEO457


Monitoring the Output of Pharmaceutical Hot Melt Extruders with Near-infrared Spectroscopy

Recent drug discovery has been characterised byhigh throughput screening technologies thatmake a wide variety of candidates available.Although the number of new drugs available isgreat news in a therapeutic sense, it hasdrawbacks in that many of the new chemicalentities have solubility issues. This can lead toproblems with formulation with regard to thebioavailability of the active pharmaceuticalingredient (API).

Overcoming these issues is of prime importanceto maintaining a healthy pipeline of new drugsubstances. One solution is through novelformulation techniques such as hot melt extrusion(HME). Using the HME technique, the drugs arecombined with thermoplastic polymers attemperatures in the general range of 50 to180ºC. The extruder can be set to different

temperatures and has several sections that maybe configured for different functions of melting,mixing, sequential addition of formulationconstituents and vacuum venting.

Currently the use of HME is increasing due to anumber of advantages:• formulation of products with improved

solubility and bioavailability, thus reducingdosing intervals for the patient

• formulations allow taste masking of APIs• the continuous technology is reproducible

avoiding batch-to-batch variability• as a continuous process, it allows lower cost

manufacturing due to reduced operationsteps and smaller volumes of materials inuse

• creates thermodynamically stable solidsolutions which can deliver improvedtemperature and mechanical stability of theproduct

• amenable to in-line monitoring

Understanding the interactions betweenformulation characteristics and the extrudermechanisms is important to process efficiency.This note shows some basic research on theinfluence of screw speed and the throughput rateon the blend uniformity of an extrudate.

The use of near-infrared (NIR) spectroscopy forthe analysis of active ingredients inpharmaceutical formulations is well known.Increasingly, with the advent of process analyticaltechnology (PAT) and quality by design (QbD), NIRis being used to monitor processes on-line or in-line due to its unique advantages. The techniqueis non-destructive, has excellent signal-to-noiseratios and can use fibre optics to take samplingto the process. NIR spectroscopy is an idealchoice to monitor the output of a hot meltextruder.�

A copy of this Application Note is availableby quoting 51836.


Investigating Mixtures of Poloxamer 188 & 407Regarding their Gel Point and Rheological Characteristics of the Gel by Means ofOscillatory Measurements

Poloxamer 407 is a standard surfactant for liquidpharmaceutical applications. As regards specificdosage forms it is suggested to use thetemperature initiated gel formation properties ofthis product to achieve high viscosities (e.g.contact with the skin of the human body).

Depending on the active pharmaceuticalingredient, high poloxamer concentrations are

necessary for solubilisation. However, the sol/geltransition temperature of an aqueous poloxamer407 solution depends on its concentration. Ahigher poloxamer concentration lowers the gelpoint temperature (GPT). This can be a problemand may raise the need for an adjustment. Earlierinvestigations showed that poloxamer 188 offereda distinctively higher GPT than poloxamer 407.

The aim of this study was the rheologicalcharacterisation of the gel formation dynamics ofaqueous solutions containing mixtures of the

poloxamers 188 and 407. For the investigationoscillatory testing was applied. Particular focuswas laid on GPT and strength of the formed gelto answer the question to which extend thoseparameters can be tailored to the regardingapplication by mixing poloxamers with differentmolecular weights.�


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