Sigma Tensiometers - rheology.cn · Sigma Tensiometers handle them all with ease ... IEC 60422. Sigma 702ET is user friendly and reli-able, requiring no pre-vious knowledge of in-terfacial

Sigma Tensiometers

Excellence in Surface Chemistry

Modular Tensiometer SystemSigma 700Sigma 701Sigma 702Sigma 702ETSigma 703D

From demanding R&D appli-cations to routine measure-ments, educational teachingand industrial QC use – TheSigma Tensiometers handlethem all with easeSurface Tension (ST), Interfacial Tension (IT),Dynamic Contact Angle (DCA) and Critical MicelleConcentration (CMC) are extremely sensitiveindicators when studying surface and interfacialproperties of liquids as well as interactionsbetween liquids and solids. Precise characterizationof material surfaces and understanding interactionsof liquid systems play a vital role in the develop-ment of new, better performing products withenhanced qualities. ST, IT, DCA, and CMC providevital information in the measurement of adhesion,material solubility, biocompatibility, lubricity ofsolid surfaces as well as wetting, washability,spreading, and adsorption of liquids.

Applications• Surfactants, Soaps & Detergents• Emulsions• Polymers-Plastics• Pharmaceuticals• Sprays, Paints & Coatings• Paper, Film & Ink Products• Cosmetics• Textiles• Food Industry• Surface Treatments• Cleanliness• Transformer Oils

Sigma – Modular SurfaceTension/Contact Angle System

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Sigma 703DA manually operated computer controlled ten-siometer designed for educational, industrial andother multiple user applications. The sigma 703Dcan measure ST and IT quickly and easily, theresults displayed on the large LC-display. Theonly difference compared with 702 is the manualsample stage. The best choice for occasional testsand QC use.

Modularity is the Key

Sigma 700/701/702/703TensiometersThe Sigma Tensiometer models are designed tomeet the diverse needs of a modern surface che-mistry laboratory. Whether your application is inquality assurance at a production line, in edu-cating future surface scientists, or in a demand-ing R&D project – the Sigma 700 series offer anideal solution to meet your measurement needs.

Sigma 700A basic tensiometer for determination of ST, IT,DCA, CMC and other standard measurementsby ring or plate methods. Because of its extendedweight range microbalance, the Sigma 700 fits avariety of rugged industrial applications and R&Dmeasurements as well as powder testing, density,and wettability.

Sigma 701A multi-purpose, high-performance tensiometerfor applications in industry, R&D and education.Due to its modularity and balance sensitivity itallows for DCA of single fiber and many otherhigh precision measurements.

Sigma 702A stand-alone tensiometer for measuring surfaceand interfacial tension in situations requiring highsensitivity and simple operation. The large LCDdisplay and touchpad keyboard enable easyoperation without external PC. The option ofconnecting to an external PC and/or serial printerenables reliable data storage and simple reporting.

Sigma 702ETA dedicated tensiometer for measuring theinterfacial tension of transformer oils accordingto ASTM D971 andIEC 60422. Sigma 702ETis user friendly and reli-able, requiring no pre-vious knowledge of in-terfacial tension measu-rement. The step-by-stepinstructions on the largeLCD display ensure fail-safe measurement everytime!

Measuring Unit – Sigma 700/701

Stand-alone Sigma 702

Sigma 700/701 Unique Features

• Large working space – wide opening doors• Dispenser and inert-gas ports• LED illumination of measuring compartment• Built in stirrer – no moving parts – no magnetic

field during measurement• Built in connectors for temperature

and pH sensors• Auto-locking & auto-calibrating microbalance

(Sigma 700)• Super-sensitive fiber range balance for standard

and single-fiber measurements (Sigma 701)• Static charge eliminator• High speed/extended length movement

of sample stage• Large and heavy sample measuring capability• Thermal separation space between balance and

measuring compartment• Removable measuring compartment for

customized future measuring options such asLangmuir studies, high temperature applications,

bursting membrane tests and X-Y sample positioning

• Enlarged pull-down sub-window for on-line viewing of selected data

• Optional synchronized dual dispenser softwarefor dilution CMC measurements of highly

concentrated solutions

Touchpad for manual system operations without PCcontrol. On-off status light, up-down stage movementbutton, stirrer and measuring chamber light buttons.Solvent proof design for easy cleaning.

All measuring chamber surfaces are specially coated to resistcorrosive liquids and allow easy cleaning. Thermoplastic wa-ter jacket for better sample liquid temperature control andelimination of heat loss. Cool surface for worker safety. Rubberbellows for liquid spill protection of the stage shaft and electronics.

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Measuring Unit, Modules andAccessoriesModularity makes it possible to tailor the instru-ment's hardware, software, and performance tomeet your exact measurement needs. The Sigma700/701 design philosophy is straight forward – thedesired instrument set-up is built around theMeasuring Unit of the Sigma 700/701 by using avariety of software and hardware add-on modulesand accessories. The Sigma 700/701 tensiometersare similar and both are compatible with all thesystem modules and accessories. Only the micro-balance and intended use differentiate the Sigma700 and 701. The Sigma 702 and 703 tensiometersare stand-alone manually operated digital tensio-meters and compatible with most of Sigma 700System accessories.

Sigma 700The Sigma 700 is a complete, ready to use tensio-meter. It uses the latest advances in precision mic-robalance technology. Special attention is paid tothe ergonomic and user-friendly design. The Mea-suring Unit is the main building block of the systemthat can be tailored to meet your exact needs.

First determine what needs to be measured andany special conditions that will affect your measu-rement. Then choose which software modules andaccessories are needed to accomplish your task.

Accessory modules are easily mounted into theMeasuring Unit and plug-and-play software modulescan be operated by anyone with WindowsTM

experience. Once the system requirements havebeen decided, KSV will assemble the Sigma 700 anddeliver it in a ready-to-use condition. It possible forthe customer to take the instrument directly fromits shipping crate and put it to use. Setting up thesystem, running test experiments, and analysing thedata are all covered with step-by-step instructions. The comprehensive operation and installationmanual ensures smooth, trouble free set-up of theinstrument and software.

Because of its wide weight range and auto-calibrating microbalance, the Sigma 700 is wellsuited for DCA measurements of large and heavysolid and powder samples. It can run two dispen-sers simultaneously for CMC measurements. FullPC control over all system functions makes it possibleto carry out long measurements without operatorintervention during the test – saving time and freeingthe operator to concentrate on other tasks.

Measuring Unit

Application SpecificSoftware Modules

Surface/Interfacial Tension Dynamic Contact Angle

Critical Micelle Concentration Adsorption, Powder Wettability

Sigma 701The Sigma 701 is a multipurpose tensiometerbased on the Sigma 700 technology and designbut equipped with a different microbalanceoptimized for a different range of applications. Itexpands from a basic tensiometer to a fullyequipped R&D grade high performance instrumentcapable of handling most of the known surfacechemistry measuring methods. It can run twodispensers simultaneously for CMC measurementsand the high resolution balance makes it possibleto measure single fibers only a few microns indiameter. The Sigma 701 is an excellent tool forthose looking for a high performance, easy touse, standard tensiometer as well as for anyonelooking for exacting performance and precisionin higher end applications.

Sigma 702 and Sigma 703DDesigned for educational, industrial and routineQC use, the Sigma 702 and 703D take the leadin ease of use and versatility of applications. Theyoffer immediate access to the Surface Tension orInterfacial Tension measurements which are aprerequisite in random fast measurements orwhen ST/IT needs to be measured occasionally.For further information ask for a separatebrochure or go to the KSV web site atwww.ksvltd.com.

Sigma 702ETSigma 702ET is a dedicated tensiometer formeasuring the interfacial tension of transformeroils according to ASTM D971 and IEC 60422.

Sigma 700/701 Performance• Surface and interfacial tension measurements

push and pull modes by ring. Correctioncalculation by Huh & Mason (Harkins & Jordan,Zuidema & Waters and others supplied.)

• Dynamic advancing and receding contact anglemeasurements (DCA)

• Contact angle of powders and single fibers• Automatic critical micelle concentrations (CMC)

determination• Surface energy and adsorption measurement• Density of liquids and sedimentation

Sigma 700/701Modules and AccessoriesSoftware Modules

• ST/IT Module – surface/interfacial tension

• DCA Module – dynamic contact anglemeasurement/single fiber wettability

• CMC Module – for critical micelle concentration

• PW Module - wettability of powders and

disperion sedimentation

• DEN Module – liquid density determination

Accessories• Thermostatic jacket for sample liquid• Temperature control with temperature probe• pH probe• Du Nouy rings – Wilhelmy plates• Auto dispenser (up to two dispensers)• Water bath circulators• Consumables, glassware• Sample holders – for various types of

solid samples• Density ball• Certified calibration kit

Sigma 700/701 Features• Full computer control and automatic operation of all measuring modes• Wilhelmy plate or Du Nouy ring method• Ultra-sensitive or extended-range balance, two choices to best suit your application• Software controlled sample temperature control

and stirring – constant or ramp temperaturecontrols

• Direct reading of sample temperature• Fully automatic dispenser for CMC or

dilution measurements• Automatic calculation of ring correction values• Informative on-line graphic presentation• Data export to spreadsheet programs, Excel,

Origin, PlotIT etc• Small sample vessels and measuring probes

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PC Software Sigma 700/701

KSV´s Sigma 700/701 is run by a powerful Win-dowsTM software written in C++. The point-and-click format of the software using drop-downmenus, buttons, and icons is easily leaned by allusers. The software included with the instrumentallows the user to perform a variety of pre-programmed experiments which can be modifiedto particular needs. A wide range of data pointsand measurement parameters are stored in adatabase and can easily be retrieved and analyzedlater or alternatively exported to another datareduction software.

Standard program include:

• Surface and Interfacial tension• Dynamic Advancing and Receding Contact

Angles (DCA)• Powder Wettability (contact angle of powders)• Single Fiber Wettability• Critical Micelle Concentration (CMC)• Adsorption Behavior of Solids• Surface Free Energy of Solids (Fowkes, Wu,

Acid-Base)• Critical Surface Tension (Zisman)• Wetted Length of Solids• Density of Liquids

The major parts of the program are the MainMenu, Experimental Setup, Experiments

of the software is the Main Menu from whichall other sections and programs can be accessed.

The Experimental setup includes informationthat is specific to each measurement. Once anexperiment has been chosen, the various infor-mation and parameters are entered in theExperimental Setup. This helps to keep thedata organized and makes it easier to search fora specific measurement afterwards.

The actual performance of the Experiments(Surface/Interfacial Tension, Contact Angle, CriticalMicelle Concentration, Absorption, for example)occurs after the Experimental Setup has beenfilled out and the materials for the experimentare in place. Once the final experimental controlshave been chosen the experiment is started. Theexperiment will then continue unsupervised untilcompletion.

After an experiment has been performed youcan return to the data for further analysis in theData Reduction and Analysis section. Afterselecting an experiment the data for that experi-ment will be displayed. There is an option ofviewing and editing the Experimental setupwhich can be very helpful if the data producedshould be recalculated based on new informationabout the materials involved. A variety of graphsfor your data can be displayed and printed.Calculation of additional results and export ofdata can be done.

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Main Menu Experimental setup

Du Nouy ringmethodThis method measures the maxi-mum weight of the liquid lifted bya ring which is pulled out of a liquidsurface or interface. The force (F)required to lift the ring is relatedto the surface tension (s) by the expression s =kF. The factor (k) derives from the capillarypressure across the curved surface of the liftedliquid. The factor (k) depends on the geometricaldimensions of the ring and on the contact anglebetween the ring surface and the liquid. Reliablemeasurements can generally be made only if thering is completely wetted by the liquid, i.e. contactangle equals to zero. Precise determination of themaximum force is achieved by repeatedly risingand lowering the ring close to the rupture ofliquid lamella hanging from the ring. Just beforethe rupture the lamella force applied on the ringdecreases dramatically. The balance detects thisforce change and lowers immediately the ring toeliminate lamella rupture.

Measuring Process1.The ring is above the surface and

the balance is zeroed2.The ring touches the surface and gets wetted

resulting in some positive force3.Negative force is applied on the ring when it

is pushed through the surface into the liquid4.Some positive force will remain because of the

wetting of the vertical supports of the ring5.When pulled out of the liquid (by lowering

the sample cup) the upper surface of the ringtouches the liquid surface and the force startsto increase. This is because the surface tensionof the liquid tries to prevent the ring frompenetrating its surface.

6.The liquid is attached to the ring while pullingit up until the maximum force (7) is reached. At this point the volume of the liquid pulled up by the ring is also at its maximum causing the ring to detach from the liquid.

7.The maximum force needed to pull the ring from the liquid is proportional to the surface tension of the liquid. The greater the force needed the greater is the surface tension.

Wilhelmy PlatemethodIn this method, the weight of the liquidlifted when a plate is withdrawn throughthe surface is measured. This weightincreases to some maximum valuewhich, provided that the plate is com-pletely wetted by the liquid and that the loweredge of the plate is at the same level as the flatsurface, equals the surface tension times the lengthof the contact line between the plate and the li-quid. In order to ensure the complete wetting theplate is usually made of micro-roughened platinum.

Static measurementThe sample surface is lifted until it contacts thelower edge of the plate. The wetting or capillaryforce pulls liquid up on the surface of the plateuntil equilibrium is reached.

Dynamic measurementsThe plate is completely immersed into the liquidand then withdrawn through the surface until themaximum force is reached. In order to achieve aprecise determination of the maximum the plateis not detached from the surface but repeatedlylowered and pulled back to the maximum.

Surface and interfacialtension measurements

Force

Time

12

34 5

6

7 8

5 6 7 8

1 2 3 4

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CMC measurement

Dynamic ContactAngle measurement

Measurement of dynamic contact angles providesinformation on the properties of surfaces such asporosity and homogeneity, surface topographyand reactivity. The contact angle is the anglebetween the tangent to the liquid surface and theliquid/solid surface at the point of liquid/solidcontact. The method is based on the Wilhelmyplate principle where the solid sample is held bythe electro balance and then pushed into or pulledfrom the substance. Therefore the measured forceacting on the sample alternates depending ondirection of the movement. The force differencesobtained are directly proportional to the diffe-rences is contact angle. As the solid samplepenetrates into the liquid an advancing contactangle is determined while pulling the sample fromthe liquid provides receding contact angle infor-mation.

The progress of the experiment is shown grap-hically with the x-axis representing the immersiondepth and the y-axis the force. The contact anglesare calculated from the force versus depthinformation.

The structure of surfactant molecules can beclearly divided into polar and non-polar parts. Asa result, dissolved surfactants tend to concentrateat the solution surface so that the part of themolecule least compatible with the solvent orientsitself away from the solution.

Even at quite low total concentrations the sur-factants form a fairly densely packed monolayer atthe surface. This results in a rapidly decreasing sur-face tension. Above a certain concentration, calledthe critical micelle concentration, CMC, thesurfactant molecules form large aggregates, micel-les, in the solution. Above the CMC the surfacetension is almost independent of the bulk con-centration because virtually all additional surfac-tant forms micelles. Hence, the value of the CMC,which is characteristic for a given surfactant, canbe determined by measurement of surface tensionas a function of concentration. The Sigma softwaretotally automates the CMC measurements.

Powder wettabilitymeasurementWettability of powders e.g., determination ofcontact angles and surface free energies ofpowders is performed according to the Washburnmethod. The powder is packed in a glass vesselwith a fine sinter glass porous bottom, or metalvessel with filter paper in the bottom allowingliquid penetration but preventing the powder tofall through. As soon as the bottom touches theliquid surface the liquid penetrates and absorbsinto the powder resulting in wetting of the powder.Change of weight as function of time is measured.

Single fiber contact anglemeasurementBecause of the super-sensitive balance of theSigma 701 the dynamic contact angle of singlefibers or fiber bundles can be measured.

Density measurementLiquid density is measured with a density kit. Aglass density probe with known volume is hungfrom the balance hook and immersed into theliquid to be measured. The force needed to holdthe probe at a constant depth in the liquid is thenrecorded. The software automatically calculatesthe density of the liquid using the principle ofArchimedes.

Software

Test report sheet for three different powders.

Test report sheet for DCA of clean and dirty hair.

Screen showing density measuring result.

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Surface/Interfacial Tension

Dynamic Contact Angle

Critical Micelle Concentration

Compliance toStandards and Norms

The Sigma 700 covers most of the known forcebalance methods in today’s modern surfacechemistry laboratory while meeting the inter-national standards set by ISO and ASTM.

ISO 6889 IT – oil/waterISO 6295 IT of liquid filmsISO 1409 ST by ring for polymers

and plasticsISO 304 ST of surface active films

by drawing up liquid filmsISO 4311 CMC of anionic and non-ionic

surface active agents byplate, stirrup or ring

DIN 53914 Du Nouy ringDIN 53993 Interfacial tension

ASTM D 1590 ST of waterASTM D 1417 ST of synthetic rubber latices

ASTM D 1331 ST/IT of Surface activeagent solutions

ASTM D 971EN 14370JIS K2241IEC 60422 IT of oil/ water by

Du Nouy ring

Special application exampleLangmuir films – Forhighly accurate Langmuirfilm measurements, suchas dilational rheologicalstudies, the measuringchamber of the Sigma 700and 701can be removed,and replaced by a smallLangmuir trough – theKSV MiniMicro.

Balance specificationsSigma 700 (extended range balance)Measuring range 0.001 - 2000 mN/mResolution withstandard probe 0.001 mN/mMaximum load 210 gWeighing resolution 0.01 mgForce resolution 0.1 μNContact angle range 0-180Contact Angle resolution 0.01°Automatic calibration and locking

Sigma 701 (super sensitive balance)Measuring range 0.01 - 1000 mN/mResolution standard probe 0.001 mN/mMaximum load (701) 5 gWeighing resolution 0.01 mgForce resolution 0.01 μNContact angle range 0-180Contact Angle resolution 0.01°

Sigma 701F (available by special request)Specially designed for single fiber measurementsResolution 0.0001 mN/mMaximum load 3 gWeighing resolution 0.001 mg

Sigma 700/701Measuring Unit specificationsStage speed 0.01 - 500 mm/min(others by request)

Stage positioning resolution 0.015 μm

Computer interface USB(RS232 as option)

Temperature rangeThermoplastic water jacket -10 ... 80°CStainless steel water jacket -10 ... 150°CElectronically heated jacket room temp.

up to 250°C(others by request)

Size 24 x 33 x 62 cm(D x W x H)

Weight 20 kg

Power supply 85-264 VACFrequency 47-440 Hz

SigmaSpecifications

Sigma 702, 702ET and 703D SpecificationsMaximum balance load 5 gWeighing resolution 0.01 mgMaximum surface/interfacialtension 1000 mN/mResolution 0.001 mN/mDensity range 1-2200 kg/m3

Stage speed 0.01 -500 mm/min (Sigma 702 & 702ET only)

Stage position resolution 0.3 μm (Sigma 702 & 702ET only)

Size 24 x 33 x 62 cm(D x W x H)

Weight 20 kgPower supply 85-264 VACFrequency 47-440 Hz

Sigma 700/701 Software ModulesS700 ST/IT softwareS701 DCA softwareS702 CMC softwareS703 Density softwareS704 Powder Wettability and

Sedimentation Software

Sigma 700/701 accessoriesT705 Thermostatic vesselT706 Magnetic stirrerT708 Computerized temperature

controllerT101 Dispenser for CMC measurementsT102 Bath/circulator PC operatedT102USB RS232/USB adapterT103 Bath/circulator manually controlledT104 Sample Vessel 70 mmT105 Sample Vessel 50 mmT106 Du Nouy ring Pt-Ir-ringT106B Calibration Certificate

for Du Nouy ringT107 Wilhelmy Plate PtT107A Certificate for Wilhelmy plate

dimensionsT107B Platinum RodT108 Ring re-form toolT108A Ring re-form serviceT109RF Sample holder for rigid and

flexible platesT111 Sample holder for fibersT112 Powder wettability measuring deviceT113 Density kitT115 Gas phase temperature controllerT117 Certified Calibration WeightT117A Calibration Certificate for

Du Nouy ringT117B Certified calibration kitT118 pH meterT119 Sedimentation kitT130 Computer with software installed

SigmaSpecifications (cont.)

Tel. +358-9-5497-3300Fax +358-9-5497-3333e-mail: [email protected]

KSV Instruments LtdHöyläämötie 700380 HelsinkiFINLAND

Tel. +1-800-280 6216+1-203-268-1745

Fax +1-203-459-0437e-mail: [email protected]

KSV Instruments Inc.P.O. Box 192Monroe, CT 06468USA

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The CompanyKSV Instruments Ltd is a leading global provider of routine,research and characterization instruments for surface chemistryand Langmuir-Blodgett film applications. Our headquarters arein Helsinki, Finland and we have offices in North America andSweden and trained representatives throughout the world.

InterfacialCharacterizationWith Sigma tensiometers and CAM Drop Shape Analysiscontact angle meters and their various modifications KSVcovers most of the known interfacial measurement techniques. All instruments utilize the latest technological advances inmeasurement of surface/ interfacial tension of liquids as wellas contact angles and surface free energies.

Langmuir FilmPreparation andCharacterizationRanging from manual, educational instruments to fully equippedhigh performance R&D grade multi/alternating layer LB-troughsKSV offers the widest range of Langmuir systems in the world.KSV’s BAM (Brewster Angle Microscope) and ISR (InterfacialShear Rheometer) are used for characterization of Langmuirand LB films in a wide variety of nanotechnology, biology andmolecular engineering applications.

Dip CoatingA wide variety of dip-coaters for exacting applications, fromsingle manual dippers to automatic multiple dipping devices.

Process ControlKSV makes a range of at-line (AL) and on-line (OL) processcontrol tools for monitoring surface tension, temperature, pH,viscosity and conductivity. An option also exists for automaticdosing of surfactants.