operating manual dcat

Operating manual DCAT D y n am i c C on t a ct An g l e M e t e r a nd Te n s io m et e r

D:\Documents\Texte\Manuals\DCAT\DCAT_all\DCAT_302E.doc • 26.07.06

Operating manual Dataphysics DCAT 11 and DCAT 21 Version 3.02, English Firmware-Version, from 2.41 (DCAT 11); from 2.41 (DCAT 21) Software-Version from 2.5.1 Build 56 Release: March 2006 All Rights, also of translation reserved. No part of this document may be reproduced in any form (print, photocopy, microfilm or any other process) or be processed, multiplied or distributed by any electronic means without the prior written approval of DataPhysics. This does not affect the exceptions expressly stated in §§ 53, 54 UrhG. DataPhysics Instruments GmbH does not accept any kind of liability for technical or printing mistakes or defectiveness in this operating manual. We reserve the right to make changes to the content of this operating manual without prior announce-ment. The use of names, trade names, merchandise descriptions and such in this operating manual does not justify the assumption that such names may simply be used by anyone; often we are concerned with legally protected registered trademarks even if they are not marked as such. Text, graphics and layout Gerhard Maier Editorial office Dr. Wolfram Waibler, Nils Langer Printed in Germany © Copyright 2006 by DataPhysics Instruments GmbH, Filderstadt

® is a registered trademark of DataPhysics Instruments GmbH, Filderstadt

® IBM and IBM-PC are registered trademarks of International Business Machine Corporation

® Microsoft and Windows are registered trademarks of Microsoft Corporation DataPhysics Instruments GmbH Raiffeisenstraße 34 DE 70794 Filderstadt phone ++49 (0)711-770556-0 fax ++49 (0)711-770556-99 email [email protected]

DCAT

Operating manual DCAT 11 and DCAT 21

Content

1 Introduction 4 1.1 Compliance 4 1.2 Safety warnings 4 1.3 Detailed Security precautions 5 2 General Description 6 2.1 About this manual 6 2.2 Application 6 2.3 Features 7 2.4 Software SCAT 8 2.4.1 SCAT 31 8 2.4.2 SCAT 32 8 2.4.3 SCAT 33 9 2.4.4 SCAT 34 9 2.4.5 SCAT 35 9 3 Installation and setup 10 3.1 General preparations 10 3.2 Checklist of delivered items 11 3.3 Installation of the DCAT 12 3.3.1 Mounting of TV xx to a DCAT 12 3.3.2 Leveling the measuring device 13 3.3.3 Mechanical connection 13 3.3.4 Electrical connection 13 3.3.5 Installation of a liquid sample vessel 14 3.3.6 Installation of probe or sample holder 14 3.4 PC setup 14 3.5 Software setup 15 3.5.1 General 15 3.5.2 First setup of SCAT software 15 3.5.3 First start of the SCAT 16 3.5.4 Remove and Update of the SCAT software 16 4 General use of the software and the DCAT 17 4.1 General use of the software SCAT 17 4.1.1 Icons 17 4.1.2 Menu bar 17 4.2 Preparations 19 4.2.1 Preparation of the sample 19 4.2.2 Preparation of the probe 19 4.2.3 Setup of the measuring device 20 4.2.4 Device Settings 20 4.2.5 Options 20 4.2.6 Balance clamping 21 4.2.7 Syringe Database 21 4.2.8 Liquid Database 21 5 Single measurements 22 5.1 Surface Tension with a plate 22 5.1.1 Measurement with other plates 25 5.1.2 Evaluation of the SFT measurement with a plate 26 5.2 Surface Tension with a ring 27 5.2.1 Evaluation of the SFT measurement with a ring 32 5.3 Interfacial tension with a plate 34 5.3.1 Measurement with other plates 37 5.3.2 Evaluation of the IFT measurement with a plate 38 5.4 Interfacial tension with a ring 39 5.4.1 Measurement with the Pull method 43 5.4.2 Measurement with the Ring Push method 46 5.4.3 Evaluation of the IFT measurement with a ring 47

5.5 Dynamic Contact Angle 49 5.5.1 Evaluation of the Dynamic Contact Angle 53 5.5.2 Measurement with other sample holders 55 5.6 Powder Contact Angle 56 5.6.1 Evaluation of the Powder Contact Angle 60 5.7 Wetted length 62 5.7.1 Evaluation of the Wetted length 65 5.7.2 Measurement with other sample holders 67 5.8 Density of a liquid 68 5.8.1 Evaluation of the density of a liquid 71 5.9 Sedimentation 73 5.9.1 Evaluation of the sedimentation rate 76 5.10 Penetration 78 5.10.1 Evaluation of the penetration rate 81 6 Project 83 6.1 CMC increasing concentration 83 6.2 CMC reversed 90 7 Data Analysis 97 7.1 CMC Determination 97 7.2 Analysis of surface free energy 101 7.3 Result Collection 103 7.4 Adhesion 104 8 Optional accessory 105 8.1 Plates 105 8.2 Du-Noüy rings 105 8.3 Liquid Dispense unit LDU 105 8.3.1 LDU – control 106 8.3.2 LDU – connections 107 8.4 Kit for powder measurement PUR 11 108 8.5 Fiber holder FH 11 108 8.6 Single fiber holder FH 12 108 8.7 Plate options holder PSH 11 108 8.8 Options holder for films FO 11 109 8.9 Penetrometer probe PP 11 109 8.10 Sedimentation cone SC11 109 8.11 Density determination set DIS 11 109 8.12 Adapter for small sample vessels 109 8.13 Sample vessels GS 110 8.14 Diffusion reducers CP 110 8.15 Ring aligning tool R-AT 110 8.16 Inert gas appliance GTR 70 110 8.17 Non-magnetic liquid thermal unit TV 70-NM 111 8.18 Temperature control unit TEC 250/DCAT 112 9 Maintenance 113 9.1 General 113 9.2 Cleaning of instrument 113 9.3 Device not reacting 113 10 Appendix 114 10.1 Technical data 114 10.2 Terms of Guarantee 115 10.3 Requirements of the mains cable 116 10.4 Declaration of conformity 118

© DataPhysics Instruments GmbH, Filderstadt

1 Introduction

This manual is valid for the dynamic contact angle meters and tensiometers DCAT 11 and DCAT 21. If there is a difference in the use of the both type of instruments it will be noted. This manual contains important advises for use of the DCAT. Therefore it must always remain with the unit, especially if this is passed on to a third person!

1.1 Compliance Products tested and found to be in compliance with the requirements defined in the EMC standards defined by 89/336/EEC as well as Low Voltage Directive (LVD) 73/23/EEC can be identified by the CE label on the side of the unit. For any additional information refer to the Letter of Compliance that shipped with the unit (Declaration of Conformity).

1.2 Safety warnings Make sure you read and understand all instructions and safety precautions listed in this operating manual before installing or operating your unit. If you have any question con-cerning the operation of your unit or the information in this manual, contact your sales partner for assistance.

• Performance of installation, operation, or maintenance procedures other than those described in this manual may result in hazardous situation and may void the war-ranty.

• Never operate the unit for any purpose other than described in the operating manual.

• Do not use any accessories other than those supplied or approved by DataPhysics.

• You must not operate the unit if a fault is suspected.

• Ensure that all operators are fully trained in the correct use of this unit and have understood all safety precautions.

• Connect the power supply of the DCAT to a socket with protective plug reception only! Use a three-wire power cord. No other way of protective grounding is permitted!

• You must never open the casing of the power supply. The power supply can only be exchanged complete.

• The measuring results do not only depend upon the correct use and functioning of the unit, but may also be influenced by other factors. It is advised therefore, that the measuring results are plausibility tested before consequential actions are taken.

Introduction


In addition to the warnings listed above, warnings are posted throughout the manual. These warnings are designated by a STOP sign and with text highlighted in bold. It points out a hazard and calls attention to a procedure, practice, or the like, which, if not correctly performed or adhered to, could result in damage of the unit, injury or loss of life. Do not proceed beyond a WARNING sign until indicated conditions are fully understood and met.

The HINT sign points out a remark. It calls attention to any additional information which might be useful for the operator.

1.3 Detailed Security precautions Risk of contusion – Never bring any body parts between the movable parts of the unit.

Electrical connections – The unit must only be used with cables supplied by DataPhysics or our sales partner. All cable connections must only be closed or opened when the unit is switched off. Make sure that the voltage of the device corresponds to the power source.

Unpacking – Retain all cartons and packing material until the unit is operated and found in good condition. If the unit shows external or internal damage, or does not operate properly, contact the transportation company and file a damage claim. Under ICC regulations, this is your responsibility.

Lifting and transport – Great care must be taken when lifting or transporting the unit. Use proper ergonomic techniques and methods of lifting and carrying this unit.

General – The unit should not be used in areas with high electromagnetic fields as well as in areas with danger of explosion. When operating at high temperatures all inflammable materials must have a distance of minimum 1 meter to the unit. Use only original DataPhysics accessories and spare parts or parts approved from Data-Physics.

The DCAT must never be lifted by the windows, the sample stage or the

measuring system!


2 General Description

2.1 About this manual This manual describes the operating of the dynamic contact angle meter and tensiometer DataPhysics DCAT.

Make sure you have read and understood all instructions and safety precautions listed in this operating manual before installing or operating your unit. The installation should be carried out in the same order as described in this manual. If you have any question con-cerning the operation of your unit or the information in this manual, contact your sales partner for assistance.

2.2 Application The DCAT is used in research, development, production and quality control of surface active substances in

• paint and varnish industry varnish additives (defoamers, deaerators, slip additives)

• pharmaceutical industry wetting and dissolving of pharmaceutical powders, pills and capsule material in body liquids

• cosmetic industry washing and cleaning agents, bubble baths and crèmes

• textile industry wetting of single fibers and textile fabrics

General Description


2.3 Features

Fig. 1: DCAT 21 with LDU 2/2, Du Nöuy-ring RG 11 and software SCAT 33

The DCAT consists of the basic instrument with the following technical equipment: • High-precision electro dynamically compensated weighing system with automatic

calibrating function,

• Software-controlled motorized height positioning of the temperature controllable sample vessel with variable speed,

• Temperature controllable sample vessel with build-in Pt100 probe and magnetic stirrer for the sample vessel with diameters of 50, 70 or 100 mm

• DCAT 21: Automatic balance lock; DCAT 11 manual balance lock • Integrated measuring and control electronics with digital thermometer • Graphical display for weighing data, temperature and other measuring statuses • Serial RS 232C interface with PC connecting cable • Illuminated sample chamber with connection for inert gas • Pt100 temperature sensor for the installation in the temperature control unit • support for the attachment of a liquid dispensing tube

It is prepared for the installation of a liquid temperature control unit TV 50, TV 70 or TV 100 with integrated magnetic stirrer for mounting either of the sample vessels made of borosilicate glass (with diameters 50,70 or 100 mm).

Optional available in a Non Magnetic version with a temperature control unit TV 70 NM made of gold-plated brass with a removable micro-electronic stirrer system.

Fig. 2: DCAT 21 with Du Nöuy-ring RG 11


2.4 Software SCAT 2.4.1 SCAT 31

Software module Surface Tension

For the control of the test, the measurement and analysis of the surface and interfacial tensions

Measurement and analysis programs:

• Measurement of the static, time- and temperature-dependent surface and interfacial tensions of and/or between liquids according to the surface and interfacial tension of liquids according to the Du-Noüy ring method (to DIN 53915 & ASTM-971), the Wilhelmy plate and the wire hoop method, tension and pressure on the interface

• Ring tear-off test to determine the surface elasticity

• Automatic ring corrections according to Zuidema & Waters, Mason &Huh and Harkins & Jordan

• Access to the gas-, liquids- and solids data base

2.4.2 SCAT 32

Software module Contact Angle/Surface free energy

For the control of the test, the measurement and analysis of contact angles and the surface free energy


• Force-based measurement of the dynamic contact angle of prismatic and cylindrical solids (e.g. plates, films, rods and single fibers) as well as the wetted length according to the Wilhelmy method

• Adsorption measurement on powders and fiber bundles with the determination of the average contact angle according to the modified and the extended Washburn method

• Calculation of the surface free energy of solids and their components from measured contact angles with any number of test liquids, evaluation according to the methods of Fowkes (geometric mean), Wu (harmonic mean), Extended Fowkes (incl. hydrogen bonds), Zismann (critical surface tension), Owens-Wendt (dispersive & polar), van Oss & Good (acid-base theory), Neumann's Equation of State (EOS)


• Calculation of Work of Adhesion

General Description


2.4.3 SCAT 33

Software module CMC

For the automatically determination of the critical micelle formation concentration of surfactants (CMC)


• Fully automatic determination of the critical micelle formation concentration of surfactants (CMC) in forward & reversed mode

• Calculation of the minimum surface tension in case of synergistic effects of surfactant mixtures

• Calculation of the head space required by molecules on the surface

• Calculation of the free adsorption energy after Gibbs

• Calculation of the surface excess

• Automatic ring corrections according to Zuidema & Waters, Mason & Huh and Harkins & Jordan


• Control of the dosing devices LDU x/x and DO 665, DO 765 for additive and subtractive dosing

2.4.4 SCAT 34

Software module Liquid Density

For the control of the test, the measurement and analysis of density of liquids


• Determination of the density of liquids with the optional available density determination set DIS 11 (Part-No: 2000337)


2.4.5 SCAT 35

Software module Sedimentation/Penetration

For the control of the test, the measurement and analysis of sedimentation and penetration tests


• Determination of sedimentation rate

• Measuring of the yield forces on soft gels, pastes etc.

• Measuring of the penetration resistance and penetration rate



3 Installation and setup

Make sure you have read and understood all instructions and safety precautions listed in this operating manual before installing your unit. The installation should be carried out in the same order as described in the following pages.

3.1 General preparations Please open all packages on the designated openings. Avoid all damages to the packing material.

Keep the packing material for a later sending. The DCAT is best protected in the original packing!

Find yourself a comfortable working place where you want to set up your DCAT system with its peripheral equipment. We recommend a vibration free table for the DCAT. There should be sufficient room to set up the base unit, the substances to be measured and the peripheral equipment (e.g. printer, computer and thermostat).

For the connection of the DCAT power supply to the mains, you need a grounded mains socket with corresponding fuse protection (see technical data). You do require some additional sockets for the connection of the peripheral equipment.

Your working environment and the place where you store your DCAT mustn’t be extremely hot or extremely cold.

Also, avoid places in which the temperature and the atmospheric moisture greatly fluctuate.

Because the DCAT measures very small forces avoid places with vibrations (watch out for vibrations because of steps, close of doors …)!

Furthermore, make sure that the DCAT is not exposed to

• heavy dirt or dust

• direct sun shine

• objects which emit great heat (e.g. radiators)

• objects with a strong electromagnetic field (e.g. loud speaker, motors,...)

• liquids or corrosive chemicals (except in the measurement devices that are designed for it)

The instrument must be tempered to room temperature before you install and operate it (if it comes out of a cold ambient atmosphere watch out for condensed water).

Installation and setup


3.2 Checklist of delivered items Please check that all items of the delivery were unpacked and in good condition.

A standard DCAT delivery consists of:

• DCAT with a build-in optional liquid thermal chamber TV 50 / TV 70 / TV 70 NM / TV 100.

• power supply with a power cord

• serial cable to the PC

• bubble level

• operating manual

• software SCAT (control of instrument and measurement)

Optional available are:

• Du Nöuy-ring RG 11 and RG 10

• Wilhelmy plate PT 11, PT 10 and PT 9

• sample vessel of borosilicate glass available with diameters 50,70,100 mm

• accessories kit for measurements of powder PUR 11

• filter paper for PUR 11

• fiber holder FH 11

• Single fiber holder FH 12

• multiple single fiber holder FH 12

• special options holder for solids in plate form PSH 11

• special options holder for films FO 11

• density determination set DIS 11

• liquid dispense units

• a PC-system with MICROSOFT Windows XP® or 2000®

To run the software SCAT your PC must be able to run MICROSOFT Windows XP® or 2000® without failure. The following specifications are our recommendation for comfortable work with the SCAT:

• Pentium 4 processor with 2.0 GHz or more (Pentium 3 1 GHz)

• 256 MB RAM or more

• MICROSOFT Windows XP® or 2000® with Service Pack 3

• 17” color monitor (min 1024 x 768 Pixel)

• Windows conform printer.


3.3 Installation of the DCAT The Installation of the DCAT is described in the chapters below.

3.3.1 Mounting of TV xx to a DCAT

The TV XX is dismounted in delivery state to prevent mechanical damage by transport shocks.

Installation

1) Put the DCAT on the table. Connect the power supply.

2) Cut off the cable binder which holds the silicon tubes. Be careful not to damage the expansion bellows or the silicon tubes. Also never pull out the silicon tubes.

3) Switch on the DCAT.

4) Move up the stage to about position 70 mm (see display of

DCAT) by using the -switch.

5) Put the TV XX onto the stage with the connectors for the tubes to the back. Be very careful not to touch the options holder.

6) Fix the TV XX onto the stage with the four hex screws A; use the delivered Allan key wrench size 2.5 mm

7) Carry out a reference run for the stage by pressing the and

the down key simultaneously longer than 4 sec.

8) Fix the lift protection with the hex screw B using the delivered Allan key

9) Connect the built in PT 100 to the socket inside the DCAT.

10) Move up the stage to about position 60 mm

11) Put the silicone tubes over the corresponding connectors C on the TV XX.

12) Fix the tubes with the two delivered cable binders.

Fig. 3: Up- and down-switch on front panel

Back Front

A

Fig. 4: TV XX position on the lift Fig. 5: Screws to fix the TV XX onto the lift

B

Fig. 6: Fixing screw for protection cover Fig. 7: PT 100 connection

C

Fig. 8: Connection of the silicone tubes



3.3.2 Leveling the measuring device

The DCAT should be always leveled before you start to measure, because the built-in high precision balance works more accurate when leveled. In the delivery lot you will find a bubble level.

Put the bubble level onto the lower part of the housing (this part is adjusted parallel to the balance). The leveling could be carried out with the four height adjustable feet.

A proved way to level is to try it with only three feet (without the one in the left front). First turn all feet till the unit is on the lowest height, and then turns the left back foot down about two turns. Level the unit first with the right back foot. Now level it with the right front foot. Finally turn down the left front foot until it touches the base.

3.3.3 Mechanical connection

On the rear of the DCAT you can connect a liquid circulator bath to the both sockets LIQUID CIRCULATION. For this you can use the delivered quick couplings.

It is important to connect the circulator outlet to the socket LIQUID CIRCULATION IN.

3.3.4 Electrical connection

The DCAT uses an external power supply as power source. Connect the power supply to the socket DC-IN 12V on the DCAT. For the connection of the power supply to the mains, you need a grounded mains socket with corresponding fuse protection.

Connect the power supply to a socket with protective plug reception only! Use a three-wire power cord.

No other way of protective grounding is permitted!

All cable connections must only be closed or opened when the unit is switched off

The serial cable leads from the socket SERIAL PC on the DCAT to any free serial port (preferably COM 1) on the computer.

The socket SERIAL AUX is for the connection of additional units like the liquid dispensing unit LDU or the TC 250/DCAT.

The socket T2 is for the connection of a secondary PT 100 temperature probe.

Fig. 9: Rear view of DCAT


3.3.5 Installation of a liquid sample vessel

Fill the sample vessel with the desired liquid.

Move the sample stage down to its lowest position by using the -switch on the front

panel of the DCAT or the -icon in the SCAT software.

Insert the sample vessel carefully into the temperature controlled receptacle without touching the options holder.

3.3.6 Installation of probe or sample holder

The DCAT 21 has a build-in automatic options holder clamping, the DCAT 11 has a manual clamping.

If you want to analyze a liquid (e.g. detection of the surface tension or the density) or a solid (e.g. detection of the contact angle or the wetted length) you must install the probe or the sample into the options holder at the balance.

You must never touch the sample holder or the probe if the options holder is not fixed (closed clamp)!

If you use a Wilhelmy plate or a Du Noüy-ring as probe to measure, be sure that it is absolutely clean and not deformed.

A proved way to clean is to make them red-hot in a gas flame.

Insertion of the probe into the options holder of the balance:

• DCAT 11: Fix the clamp of the options holder by turning the knob A on the left side of the DCAT 11 clockwise. DCAT 21: Make sure that the options holder clamp is closed.

• Insert the probe carefully into the options holder.

• Close the doors of the sample room.

• DCAT 11: Release the options holder clamp by slowly screwing out the knob A on the left side of the DCAT 11 head anticlockwise. DCAT 21: The options holder clamp will be automatically released before the measurement starts.

3.4 PC setup Information for the setup of your computer system and Microsoft Windows 2000 or Windows XP you can take out of the particular documentation. The PC must be compliant to the EN60950.

A

Fig. 10: Manual clamping of the options holder at a DCAT 11

Fig. 11: Insertion of the probe



3.5 Software setup 3.5.1 General

The SCAT software is developed as a 32-bit application for MICROSOFT Windows XP® or 2000®.

MICROSOFT Windows XP® or 2000® should be already installed and must work on your computer before you can install the SCAT. You need Administrator rights to install any software; to execute the SCAT it is sufficient to have Power user rights on your local PC.

3.5.2 First setup of SCAT software

• Put the SCAT CD into your CD-ROM drive.

• If the SCAT Setup does not start automatically execute the file SetupMenu.exe onto your SCAT CD-ROM.

• First have a look to the READ ME file for latest information about the setup procedure.

• Execute the DAO setup. Only the JET-Engine (Jet 3.5) must be installed, the ODBC-drivers, and the optional components for accessing additional data formats are not necessary to run the SCAT.

• Execute the BDE Setup and follow the advices on screen.

• Execute the Setup SCAT and follow the advices on the screen. You have to accept the license agreement before the setup can be continued.

• Please enter the correct Full Name and Organization into the corresponding text boxes, if they are not already filled by the operating system.

• If more than one person should use the program we recommend selecting Anyone who uses this computer and not Only for me.

• The software key that you have to enter can be found onto the CD-ROM and on the CD inlay

• You can select the Destination folder. We recommend to use the default folder C:\Program files\dataphysics\. With Browse you can select another folder.

Fig. 12: Setup-Menu

Fig. 13: User information

Fig. 14: Software-Key

Fig. 15:Destination folder


3.5.3 First start of the SCAT

At the first start of the SCAT you need to choose the liquids database in the menu Select Database File. Please select the following database ...dataphysics\Scat\Liquids.mdb.

3.5.4 Remove and Update of the SCAT software

Before you can update the SCAT you have to remove the present version of the SCAT.

• Insert the new SCAT software CD in your CD- or DVD-drive.

• If the SCAT Setup does not start automatically execute the file SetupMenu.exe onto your SCAT CD-ROM.

• First have a look to the READ ME file for latest information about the setup procedure.

• Execute the Setup SCAT and follow the advices on the screen. Confirm uninstall SCAT from this computer to remove the present SCAT version.

• Now execute again the Setup SCAT to install the new SCAT software.

Fig. 16: Dialog Select database

Fig. 17: Remove of SCAT

General use of the software and the DCAT


4 General use of the software and the DCAT

To perform a measuring with the software SCAT for the DCAT is very easy, because the user will be guided through the whole measurement by a work flow assistant.

Start the software with a click to the -icon on your desktop.

If you hold the mouse-cursor longer than 1 second on an icon a short description in form of a bubble-help is showed.

4.1 General use of the software SCAT 4.1.1 Icons

The icons in the main window of the SCAT have the following meaning and function:

New (Ctrl+N) Opens the dialog for creating a new single

measurement window

Open(Ctrl+O) Opens a stored file

Save(Ctrl+S) Store the actual file. If it was not stored before you

will be asked to enter a filename

Cascade Lays all opened windows one on top of the other

Tile Horizontally Lays all opened windows next to each other

Tile Vertically Lays all opened windows one below the other

Stirrer Control Opens the dialog Stirrer Control

Liquid Dispenser Unit Opens the dialog Liquid Dispenser Unit

Move vessel down Moves the sample stage down to his lowest position

tare balance Tares the balance (sets the displayed weight to zero)

Temperatures log Opens the Temperature chart

TEC Ramp Edit Opens the TEC ramp editor

TEC control Opens the TEC control dialog

TEC Preferences Opens the dialog TEC Preferences

4.1.2 Menu bar

The Menu File is made up of

• New – Opens a new window for a measurement

• Open... – Opens a stored measurement file *.mea

Fig. 18: Icons

Fig. 19: Menu bar


• Reopen – To open one of the last six stored measurement file *.mea

• Save... – Stores the actual active measurement file (the Save As... dialog opens if the file is not stored before)

• Save As... – Opens the file save dialog to store the actual active measurement file under a definable name and into a selectable folder

• Save as Template... - Stores the actual active measurement file as a template (e.g. for CMC measurements. Every measurement file (*.MEA) can be stored as a template (*.TPL). All information, except the measurement data, are stored in a template. This means you can start a measurement directly after opening of a template (Menu File—New—Open Template...) without any further settings

• Print... – Prints the data and graph of the active measurement file

• Print Setup – Settings for the printer

• Exit – Ends the program

The Menu Window is made up of:

• Cascade - Lays all open windows one on top of the other

• Tile Horizontally - Lays all open windows next to each other

• Tile Vertically - Lays all open windows one below the other

• Minimize All – Minimizes all open windows

• Arrange All – Orders all open window to your selection (Cascade, ...)

• Show LDU Control – Opens the LDU dialog

• 1-x – Here you can select one of all open windows; the active is marked with a check

The Menu Setup is made up of:

• Device... – Settings for the PC and LDU/Dosimat connections and calibration of DCAT

• Options... – Settings fort he program start

• Show Balance Clamping... – Shows the actual position of the balance clamping

• Show Assistent – Deselect this to disable the workflow assistant

• Databases - To edit the liquids or syringe database

• Reference Vessel – Starts the reference run for the lift

The Menu Help contains the version information’s, the customer information, the Master ID, and the installed modules.

Fig. 20: Dialog Save as

Fig. 21: Menu - Window

Fig. 22: Menu - Setup



4.2 Preparations The measuring results do not only depend on the correct use and functioning of the measuring device and the software, but may also be influenced by other factors. It is advised therefore, that the measuring results are plausibility tested before consequential actions are taken.

Before you start a measurement have a look to the following points:

• What is the goal of the measuring series?

• How the samples will be prepared?

• Which test liquids or pieces will be used?

• How is the set-up of the measuring device?

A precise definition of the problem or the terms relieves the single-mindedly actions by the practical realization of an experiment.

4.2.1 Preparation of the sample

The preparation of the sample (solid surface, powder, fiber, liquid ...) is decisively important for the measuring results. Therefore be sure to treat the samples always the same way, unless you want to measure the different results of different sample treatments.

To avoid systematic errors it is absolutely necessary to prepare the sample and the probe always the same way.

4.2.2 Preparation of the probe

The selection of the probe arises from the measuring job as well as according to the tolerability to the sample. It must be noticed (or be tested) that the used probe neither reacts with the solid nor etches it or is absorbed. Care and cleanliness must be taken in filling the vessel with the liquids, especially if surface active substances (e.g. surfactants) will be used. Smallest contaminations can reduce the surface tension of liquids, especially of water.


4.2.3 Setup of the measuring device

The setup of the measuring device is, amongst others, important for reliable and reproducible results. Have a look to the following points:

• leveled and vibration-free stand

• calibration of the balance

• cleanliness of the probe (e.g. Wilhelmy plate or Du Noüy-ring)

4.2.4 Device Settings

Before you start the first measurement set up your measuring device. Open the menu Setup — Device... and select the COM-Port (serial port on the PC) where the DCAT and the Dosimat are connected to. If you have a LDU with installed refill valves RRS 11 you need to select

, because the DCAT is not able detect the valves automatically.

Reset Device Moves the sample stage to his lowest position and resets the internal position control.

Calibrate Balance Starts the integrated calibration function of the balance. With the DCAT 11 be sure that the balance clamp of the options holder isn’t fixed. The DCAT must stand vibration free and should be warm (switched on for min. 30 min) before starting the calibration. Under this good conditions a calibration should be done in max. 2 min.

Be sure that the balance clamping is open and avoid any vibrations during the calibration of the balance!

Temperature Sensor Select the sensor you want to use during the measuring. T1 is the sensor built-in to the TV xx and connected to the socket inside the measuring room. T2 is the sensor connected to the socket on the back of the DCAT. If you want to get the average of both sensors you have to select T1+T2.

4.2.5 Options

You can select the liquids database you want to use (Liquids.mdb or LiquidsEditable.mdb) and two options for program start and new measurement windows.

Reopen previous template on program start – Opens the last used template at program start.

Use previous measurement window size – Sets the last window size for a new measurement window.

Fig. 23: Dialog Setup — Device...

Fig. 24: Dialog Setup — Options...



4.2.6 Balance clamping

At a DCAT 21 you can reset the controller of the automatic balance clamping. Also the actual status of the clamp is indicated. You can use the slider to change the status of the balance clamping.

You must never touch the options holder or the probe if the options holder is not fixed (closed clamp)!

4.2.7 Syringe Database

In the syringe database you can select, edit or add the syringe type for the LDU. With Shift + Ins you can define new set of data. With Ctrl + Del you can delete data sets.

4.2.8 Liquid Database

The liquid database is a very helpful tool to obtain all the necessary parameters of the liquid used for the measuring. In the left part of window, you select the liquid and in the right part you get the parameters depending on the method you have selected with the tab ruler.

You can add or delete a complete row. If you want to edit one of the entries in the database you have to select .

Fig. 25: Dialog Setup — Show Balance Clamping…

Fig. 26: Dialog Setup — Edit Syringe Database…

Fig. 27: Dialog Setup — Liquid Database Edit


5 Single measurements

With the selection of a measuring method in the menu File—New—Single Measurement you open a new window in which you perform the measurement, the analysis and the presentation of the measured data. The appearance of this new window depends on the selected measuring method.

5.1 Surface Tension with a plate The measurement of the surface tension can be best done with a Wilhelmy plate (PT 11), made of platinum-iridium according to DIN 53914. It is also possible to measure with other probes in a Square, Circle, Ellipse or User defined form.

Before you use a plate to measure, be sure that it is absolutely clean and not deformed.

A proved way to clean a plate made of platinum-iridium is to make it red-hot

in a gas flame.

Never touch the hot plate with bare hands, use always heat-proof gloves!

To measure the surface tension the DCAT first detects the surface of the test liquid by moving the sample vessel with the liquid up until the balance detects a weight difference (because the probe is getting lighter when it dips into the liquid). This position of the stage is stored as the position where the plate meets the surface. The stage moves further up (this means the plate dips into the liquid) to the position you defined (immersion depth). The stage moves down to the stored position of the surface and wait until the stop criteria (sd smaller than) for the SFT is reached.

The dialog SFT Measurement is a tabbed dialog box. This means that the content of the box differs depending on which tab you have selected. The content also depends on the selected probe (ring, plate etc.). The area with the Start and the Stop button is always visible.

Sample Info In this tabbed dialog you can enter information about the test in plain text. This information will be stored together with the measurement results.

Fig. 28: Dialog File — New — Single Measurement...

Fig. 29: Dialog Sample Info

Single measurements—Surface Tension with a plate


TEC/TPC This tabbed dialog is used to enter special control parameters necessary for a test using the temperature controlled chamber TEC 250, but it can also be used without any connected controller.

Active TEC/TPC temperature start condition feature… This feature also works without a TEC, you can also use it when a liquid bath circulator controls the temperature in the sample vessel (normally measured with the built-in sensor T1). If you select the Temperature Sensor T2 be sure that it is connected and measures the desired temperature.

If the temperature difference dT will not be exceeded during the Time Interval and is also above the Start Threshold temperature, the measurement will start.

Setup In this tabbed dialog you can enter parameters required for the test. The parameters are depending on the used probe.

Testing Body You must enter the geometric dimensions of the cross section according to the shape of the used probe (testing body). The parameters for the three standard plates (normal PT 11, small PT 9 , and cylindrical PT 10) are already defined. For all other probes you have to define the parameters (see chapter 5.1.1 Measurement with other plates page 25).

Device

Motor Speed (Surf. Detection): Defines the speed of the lift motor in mm/s used when detecting the surface of the liquid.

Surface Detection Threshold: Defines the sensitivity threshold for the surface detection, this means the position of the lift, where the detected weight difference (because the probe is getting lighter when it dips into the liquid) exceeds this threshold, will be defined as the surface of the liquid.

If the sensitivity threshold for the surface detection is defined too large it could prevent that the surface will be detected, and that means that the

probe or the balance can be destroyed.

Samples/second: Defines how much measures were made within one second.

Immersion depth: Defines the immersion depth of the probe before the test.

Stop and Evaluation Cond.

Stop if sd is smaller than mN/m Stops the test when the standard deviation (sd) of the SFT is smaller than x mN/m over the last n measurement cycles. For this condition you can to select also the number of measurements to be taken into account.

Average last n measurements n=... If activated, an average over the last n surface tension measuring will be used for the above stop condition.

Start Starts the measurement and optionally the work flow assistant (if not deactivated in the menu Setup).

Fig. 30: Dialog TEC/TPC

Fig. 31: Setup for plate


The integrated work flow assistant will guide you in performing a surface tension measurement. You can disable the workflow assistant by de-selecting Show Assistent in the menu Setup or by selecting .

You have to carry out the following steps:

• DCAT 11: Fix the clamp of the options holder by turning the correspondent knob on the left side of the DCAT 11 clockwise. DCAT 21: Make sure that the options holder clamp is closed.

You must never touch the options holder or the probe if the options holder is not fixed!

• Open the housing of the DCAT.

• Move the sample stage down to its lowest position (use the -switch on the DCAT or the -icon in the SCAT software).

• Fill the sample vessel with the desired liquid.

• Insert the sample vessel carefully into the temperature controlled receptacle without touching the option holder.

• Put the clean probe (plate) into the options holder.

• DCAT 11: Release the options holder clamp by slowly screwing out the correspondent knob on the left side of the DCAT 11 head anticlockwise. DCAT 21: The options holder clamp will be automatically released before the measurement starts.

• Move the sample stage up (use the -switch on the DCAT) to some millimeters below the bottom of the probe.

• Start the SFT measurement (if you are sure that the probe is cooled down). The measurement is carried out automatically. You can stop the measurement at any time without loosing the so long measured data with a click on the Stop button.

Keep an eye on the complete measurement, especially at the start. Please check if the surface of the liquid is correctly detected. This will be visible by the

varying measuring value on the DCAT display and by the different lift speed.

If this isn’t the case stop the measurement immediately, because otherwise the probe can be destroyed.

• At the end of the measurement the options holder clamp must be closed: DCAT 11: Fix the clamp of the options holder by turning the correspondent knob on the left side of the DCAT 11 clockwise. DCAT 21: Make sure that the options holder clamp is closed.

• Save the measurement by selecting File – Save As... which opens the file save dialog to store the actual active measurement file under a definable name and into a selectable folder, or by selecting File –Save as Template... to store all information, except the really measurement data in a template. This means you can start a measurement directly after opening of a template (Menu File—New—Open Template...) without any further settings.

Fig. 32: Work Flow Assistant

Fig. 33: Insertion of probe

Fig. 34: Graph during the measurement

Single measurements—Surface Tension with a plate


5.1.1 Measurement with other plates

Measurements with a small plate (PT9) or a cylindrical plate (PT 10) will be carried out in the same manner than with the normal plate (PT11). Solely the geometric data has changed. The shape parameters for the standard probes Small (PT9) and Cylindrical (PT 10) are already filled in. For other non standard plates (Square, Circle, Rectangle, Ellipse or Cylindrical) you must enter the dimensions a and b or do and di; with User defined probes the Wetted Length.

Testing Body You must enter the geometric dimensions of the cross section according to the shape of the used probe (testing body).

Square You must enter the length a one side of the probe.

Circle You must enter the diameter d the circle shaped probe.

Rectangle You must enter the length a and the width b of the probe.

Ellipse You must enter the length a and the width b of the probe.

Cylindrical You must enter the inner di and the outer diameter do of the probe.

User defined You must only enter the Wetted Length of the probe.

Contact Angle: For others than the standard plates (made of platinum-iridium according to DIN 53914) you must enter the contact angle (of the probe).

Fig. 35: Geometry dimensions depending on the shape of the cross section


5.1.2 Evaluation of the SFT measurement with a plate

Graph In this tabbed dialog you define which curve you want to see in the graph. If you change the selection you must click on the button independent to actualize the graph. You can select one or more of

temperature (site 1) temperature probe in the receptacle temperature (site 2) temperature probe connected to the rear socket T2 SFT Surface tension weight Measured weight data

With a click on the button Appearance, or a right mouse-click into the graph you can adjust all necessary graph parameters in the tabbed dialog Graph Control.

X- and Y-Axis to define the Title, the Scale and the appearance Appearance to define the Title of the graph, the Colors of the Axes, the Background and the Grid, and the Font for the Title, Label and Caption. Data for the different data curves you can define the Title, the Line Style, the Symbol, and the colors. You can also change the label of the data curves in the field Change Title. The changed label will be shown in the dialog Graph and in the diagram.

Result In this tabbed dialog you can define the Fit Range of the curve by typing in the range (From: and To:) or click and hold the left mouse key to define the range; the calculation will be performed automatically. Press the <Shift>-key and click and hold the left mouse key to zoom in by pulling an ‘elastic band” with the mouse. To zoom out you must use the dialog Appearance.

Fig. 39: Example for a surface tension test with a Wilhelmy plate PT 11

If you type the range into the text fields From and To of the Fit Range, you have to click on the button Calculate to fit the curve and show the result (Surface Tension) with its standard deviation. You can easily find out the desired values in the status line part of the graph (the first value is the x-axis; here the position in mm, and the second value is the y-axis, here the weight in g).

Fig. 36: Tabbed dialog Graph

Fig. 37: Tabbed dialog Graph Control— X-Axis

Fig. 38: Tabbed dialog Graph Control—Data

Single measurements—Surface Tension with a ring


5.2 Surface Tension with a ring The measurement of the surface tension can be done with a standard Du-Noüy ring RG 11 or with the small Du-Noüy ring RG 10. These probes are made of platinum-iridium according to DIN 53914.

Before you use a ring to measure, be sure that it is absolutely clean and not deformed.

A proved way to clean a ring made of platinum-iridium is to make it red-hot

in a gas flame.

Never touch the hot ring with bare hands, use always heat-proof gloves!

To measure the surface tension the DCAT first detects the surface by moving the sample vessel with the liquid up until the balance detects a weight difference (because the probe is getting lighter when it dips into the liquid). Now the stage moves down until the balance detects a weight maximum, then up again to the position you defined (surface - immersion depth). This cycle of up- and down- movements will continue until the stop criteria for the SFT or the maximum number of cycles is reached.

The dialog SFT Ring is a tabbed dialog box. This means that the content of the box differs depending on which tab you have selected. The content also depends on the selected probe. The area with the Start and the Stop button is always visible.

Sample Info In this tabbed dialog you can enter additional information about the test. This information will be stored together with the measurement results.








Substances In this tabbed dialog you can enter the density of the upper and the lower phase by selecting the correct phase liquid in the list box. The density will be taken out of the liquids database. For certain liquids in the database the temperature coefficients for the different physical values are registered. For these liquids you can activate the automatic temperature correction of the necessary physical value (e.g. Density).

You can also enter additional parameters of the used liquid like Temperature, Concentration and Composition.

Upper Phase You can select a sample out of the integrated liquids database in the combo box; the corresponding density will be inserted in the text field below. You can also enter any other Text (e.g. MyOwnDesignedLiquid) and below you can enter the corresponding value of the density in g/cm3.

Lower Phase You can select a sample out of the integrated liquids database in the combo box; the corresponding density will be inserted in the text field below. You can also enter any other Text (e.g. MyOwnDesignedLiquid) and below you can enter the corresponding value of the density in g/cm3.

Please note that for a surface tension measurement the upper phase must be always Air.

Additional Data This data are not valid for the SFT measurement, they are only necessary for the CMC measurement.

Temperature Temperature of the liquid valid for the entered density.

Concentration Concentration of the liquid.

Concentr. B Concentration of the second liquid

Temperature use Here you can enter the temperature used to calculate the temperature corrected values of the density. A click to the button (if the button is selected it looks like pressed ) will use the temperature value of the actual selected sensor (see chapter

4.2.4 Device Settings page 20).

Fig. 43: Dialog Substances



Setup In this tabbed dialog you can enter parameters necessary for the test. The necessary parameters are dependent from the used probe (ring). For both rings, available at DataPhysics (RG 11 and RG 10), the parameters are already filled in. If you want to use another ring (with different geometries) you have to measure it carefully and to enter the corresponding values.

Ring Geometry

Wire radius The radius of the ring wire in mm (preset parameter).

Ring radius The radius of the ring in mm (preset parameter).

General

Immersion depth: Defines the immersion depth of the ring before the test.

Motor Speed (Surf. Detection): Enter the speed of the lift motor in mm/s used when detecting the surface of the liquid.

Motor Speed (Measurement): Enter the speed of the lift motor in mm/s used when measuring.


max. Number of Cycles: Defines the maximum number of measuring cycles (for each pull and push cycles). The measurement can stop before the defined cycles are finished, if you have also selected the ‘sd’ stop condition and it becomes true.

Average last n measurements n=... Builds an average over the last n surface tension measuring values (see Results dialog). Only this number of measurement values will be shown in the graph and the results table.

Stop if sd is smaller than mN/m Stops the test if the standard deviation (sd) of the SFT is smaller than x mN/m over the last n measurement cycles. For this condition you can to select also the number of measurements to be taken into account.

Sensitivity Thresholds

Surface Detection: Defines the sensitivity threshold for the surface detection, this means the position of the lift, where the detected weight difference (because the probe is getting lighter when it dips into the liquid) exceeds this threshold, will be defined as the surface of the liquid.



Fig. 44: Setup for ring


Maximum Detection: Defines the sensitivity threshold for the maximum detection. This means when the weight difference between the last found maximum value (of the generic data) and the actual measured value exceeds this threshold the last found maximum value will be defined as a maximum. After every maximum the direction of the lift will change (Push and Pull).

Load Defaults A click onto this button will restore all the default parameters for the selected ring

Calc. Settings In this tabbed dialog you can select and enter calculation parameters

Fitting Parameters

No. of Points: Defines the number of points used for fitting the maximum weight.

Corrections

Zuidema Waters For selecting automatic ring correction according to ‘Zuidema-Waters’

σ= a + bσ* + c[1 – exp(-dσ*)] Here you can define the correction parameters (a, b, c and d) yourself.

Perform Online Calculation Select this item to perform the calculation directly during the measurement (online); if not selected the calculation of the results will be done at the end of the test.

Load Defaults A click onto this button will restore all the default parameters for the selected ring in this tabbed dialog

Maximum DetectionThreshold of 8.0 mg

Time to reverse the rotating direction and restart the lift motor

Time to stop lift motor

+ Generic Measurings

Detected Maximum Weight on pulling the ring

time Fig. 45: Sensitivity threshold for the maximum detection

Fig. 46: Dialog Calc. Settings




The integrated work flow assistant will guide you in performing a surface tension measurement. With and without the work flow assistant you have to carry out the following steps:







• Put the clean probe (ring) into the options holder.



• Start the SFT measurement (not before the probe is cooled down). The measurement is carried out automatically. You can stop the measurement at any time without loosing the so long measured data with a click on the Stop button .

•



If this isn’t the case, for what reason so ever, stop the measurement immediately, because otherwise the probe can be destroyed.

• If you had select Perform Online Calculation all results will be presented on the graph during the measurement. If this is not selected you see no result data and no graph during the measurement. You can de-select Hide generic data in the tabbed dialog Graph to visualize the generic measuring data (weight) during the measurement.





• After the first measuring the actual measured temperature will be displayed in the dialog Temperature. Subsequently the displayed temperature is the average over all measured temperature values during the measurement.


• Save the measurement by selecting File – Save As... which opens the file save dialog to store the actual active measurement file under a definable name and into a selectable folder, or by selecting File –Save as Template... to store all information, except the really measurement data in a template. This means you can start a measurement directly after opening of a template (Menu File—New—Open Template...) without any further settings

5.2.1 Evaluation of the SFT measurement with a ring

Graph In this tabbed dialog you can select the data you want to plot in the graph. If you change the selection you must click on the independent to actualize the graph. You can select between

SFT/IFT Surface/Interfacial tension

SFT/IFT on pushing the ring [mN/m] Surface/Interfacial tension measured during the up-movement of the stage

SFT/IFT on pulling the ring [mN/m] Surface/Interfacial tension measured during the down-movement of the stage

maximum weight [g] Measured weight data

maximum weight on pushing the ring [g] Measured weight data during the up-movement of the stage

maximum weight on pulling the ring [g] Measured weight data during the down-movement of the stage

Hide generic data Uncheck this checkbox to display the raw (generic) data of the balance.

Fig. 50: Temperature display during the

measurement


Fig. 52: Tabbed dialog Graph Control

Fig. 53: Example of generic data of a ring measurement




X- and Y-Axis Here you can define the Title, the Scale and the appearance of both axes

Appearance Here you can define the Title of the graph, the Colors of the Axes, the Background and the Grid and the Font for the Title, Label and Caption.

Data For the different data curves you can define the Title, the Line Style and Symbol. You can also change the label of the data curves in the field Change Title. The changed label will be shown in the dialog Graph Control, in the dialog Graph and in the diagram.

Result In this tabbed dialog the two tables of the results (mass and SFT) by Pulling the Ring and Pushing the Ring were shown, and also the mean values over all included measuring values as well as the average value over both measuring rows. The number of the averaged values was defined in the Setup dialog. You can define which values were included into the fit of the surface tension result. To mask out a value which you don’t want to be included into the calculation, just click onto the time value (t [s]) in the result table. The time value of the masked out results will be set into parentheses. With a second click onto a masked (parenthesized) value it will be again included into the calculation.

Fig. 54: Example for a surface tension test with a Du-Noüy ring


5.3 Interfacial tension with a plate The measurement of the interfacial tension can be best done with ‘normal’ Wilhelmy plate PT 11, made of platinum-iridium according to DIN 53914. It is also possible to measure with the small plate PT 9 or other probes in a Square, Circle, Ellipse or User defined form.

Before you use a plate to measure, be sure that it is absolutely clean and not deformed.


in a gas flame.


The measurement of the interfacial tension (IFT) will be done in three steps. First the buoyancy of the probe in the liquid with the lower density is measured. In the second step the surface of the liquid with the higher density is detected. The third step is the real measurement of the interfacial tensions between the two not miscible liquids.

The dialog IFT Measurement is a tabbed dialog box. This means that the content of the box differs depending on which tab you have selected. The content also depends on the selected probe (ring, plate etc.). The area with the Start and the Stop button is always visible.





Setup In this tabbed dialog you can enter parameters necessary for the test. The necessary parameters are dependent from the used probe.

Testing Body The shape parameters for the standard probes Normal (PT11) and Small (PT9) are already filled in. For other non standard plates (Square, Circle, Rectangle, Ellipse or Cylindrical) you must enter the dimensions a and b or with User defined probes the Area and the Wetted Length.




Single measurements—Interfacial tension with a plate


Contact Angle: For others than the standard plates you must enter the contact angle (of the plate).

Device





Samples/second: Defines how much measures were made in one second.

Immersion depth: Defines the immersion depth of the probe before the test.


Stop if sd is smaller than mN/m Stops the test when the standard deviation (sd) of the SFT is smaller than x mN/m over the last n measurement cycles. For this condition you can to select also the number of measurements to be taken into account.

Average last n measurements n=... If activated an average over the last n surface tension measuring will be used for the above stop condition.

Start Starts the measurement and optionally the work flow assistant (if not deactivated in the menu Setup). The integrated work flow assistant will guide you in performing an interfacial tension measurement.

We recommend using the work flow assistant for the measurement of the interfacial tension.

The measurement of the interfacial tension (IFT) will be done in three steps. First Step Ι (buoyancy in the liquid with lower density)

Ι DCAT 11: Fix the clamp of the options holder by turning the correspondent knob on the left side of the DCAT 11 clockwise. DCAT 21: Make sure that the options holder clamp is closed.


Ι Open the housing of the DCAT.

Ι Move the sample stage down to its lowest position (use the -switch on the DCAT or the -icon in the SCAT software).

Fig. 58: Setup for plate



Ι For the first step of the interfacial tension measurement fill the sample vessel with the test liquid with the lower density. If you don’t know the density it can be measured separately with the DCAT. (see chapter 5.8 Density of a liquid page 68). The minimum filling height is 13 mm because the probe (in this example the standard plate) must dip totally into the liquid to measure the buoyancy correctly (also the force caused by the small liquid lamella on the rod).

Ι Insert the sample vessel carefully into the temperature controlled receptacle without touching the option holder.

Ι Put the clean probe (plate) into the options holder.

Ι DCAT 11: Release the options holder clamp by slowly screwing out the correspondent knob on the left side of the DCAT 11 head anticlockwise. DCAT 21: The options holder clamp will be automatically released before the measurement starts.

Ι Move the sample stage up (use the -switch on the DCAT) to some millimeters below the bottom of the probe.

Ι Start the first step of the IFT Measurement (not before the probe is cooled down). The measurement is carried out automatically. You can stop the measurement at any time without loosing the so long measured data with a click on the Stop button .




Ι At the end of the first step the options holder clamp should be closed: DCAT 11: Fix the clamp of the options holder by turning the correspondent knob on the left side of the DCAT 11 clockwise. DCAT 21: Make sure that the options holder clamp is closed.



Ι Take the probe (plate) out of the options holder, clean it thoroughly

Ι Take the sample vessel out and clean it very thoroughly if you want to use it for the second step again (we recommend to use a new clean sample vessel for the second and third step of the IFT measurement)

Second Step ΙΙ (surface detection of the liquid with higher density)

ΙΙ For the second step of the interfacial tension measurement fill the sample vessel with the test liquid with the higher density. If you don’t know the density it can be measured separately with the DCAT. (see chapter 5.8 Density of a liquid page 68). The minimum filling height is 13 mm.

ΙΙ Insert the sample vessel carefully into the temperature controlled receptacle without touching the option holder.

Liquid oflower density

Fillingheight

Standard PlatePT 11

small bouyancy and wetting forces

Fig. 60: Buoyancy of the probe


Fig. 62: Work Flow Assistant ‘End of first step”

Fig. 63: Work Flow Assistant ‘Start of second

step”

Single measurements—Interfacial tension with a plate


ΙΙ Put the cleaned probe (plate) into the options holder.

ΙΙ DCAT 11: Release the options holder clamp by slowly screwing out the correspondent knob on the left side of the DCAT 11 head anticlockwise. DCAT 21: The options holder clamp will be automatically released before the measurement starts.

ΙΙ Move the sample stage up (use the -switch on the DCAT) to some millimeters below the bottom of the probe.

ΙΙ Start the second step of the IFT Measurement (not before the probe is cooled down). The measurement is carried out automatically. You can stop the measurement at any time without loosing the so long measured data with a click on the Stop button .

ΙΙ At the end of the second step the lift will stand still at the position where the probe has met the surface of the liquid

ΙΙ Open the housing of the DCAT.

Third Step ΙΙΙ (interfacial tension measurement between the both liquids)

ΙΙΙ For the third step of the interfacial tension measurements leave the sample vessel with the test liquid (with the higher density) inside the DCAT. Stack up (fill in very carefully without mixing) the second liquid with the lower density onto the first with the higher density. The minimum filling height of the second liquid is 12 mm.

Do not touch the options holder or the probe!

ΙΙΙ Start the IFT Measurement. The measurement is carried out automatically. You can stop the measurement at any time without loosing the so long measured data with a click on the Stop button .

ΙΙΙ At the end of the measurement the options holder clamp must be closed: DCAT 11: Fix the clamp of the options holder by turning the correspondent knob on the left side of the DCAT 11 clockwise. DCAT 21: Make sure that the options holder clamp is closed.

ΙΙΙ Save the measurement by selecting File – Save As... which opens the file save dialog to store the actual active measurement file under a definable name and into a selectable folder, or by selecting File –Save as Template... to store all information, except the really measurement data in a template. This means you can start a measurement directly after opening of a template (Menu File—New—Open Template...) without any further settings.

5.3.1 Measurement with other plates

Measurements with a small plate (PT9) or any other prismatic probe will be carried out in the same manner than with the normal plate (PT11). Solely the geometric data has changed. For all non standard probes (Square, Circle, Rectangle, Ellipse or Cylindrical) you must enter the dimensions a and b or do and di; with User defined probes the Area and the Wetted Length.

Lamella

Liquid ofhigher density

Standard PlatePT 11

Surface

Fig. 64: Surface detection of second liquid

Fig. 65: Work Flow Assistant ‘Start of third step”

Lamella



Standard PlatePT 11

Interface

small bouyancy and wetting forces

Fig. 66: Interfacial tension detection



5.3.2 Evaluation of the IFT measurement with a plate

Graph In this tabbed dialog you define which curve you want to see in the graph. If you change the selection you must click on the button independent to actualize the graph. You can select one or more of

temperature (site 1) temperature probe in the receptacle temperature (site 2) temperature probe connected to the rear socket T2 IFT Interfacial tension weight Measured weight data


X- and Y-Axis to define the Title, the Scale and the appearance Appearance to define the Title of the graph, the Colors of the Axes, the Background and the Grid, and the Font for the Title, Label and Caption. Data for the different data curves you can define the Title, the Line Style, the Symbol, and the colors. You can also change the label of the data curves in the field Change Title. The changed label will be shown in the dialog Graph Control, in the dialog Graph and in the diagram.

Result In this tabbed dialog you can define the Fit Range of the curve by typing in the range (From: and To:) or click and hold the left mouse key to define the range; the calculation will be performed automatically. Press the <Shift>-key and click and hold the left mouse key to zoom in by pulling an ‘elastic band” with the mouse. To zoom out you must use the dialog Appearance.

Fig. 71: Example for an interfacial tension test with a Wilhelmy plate

If you type the range into the text fields From and To of the Fit Range, you have to click on the button Calculate to fit the curve and show the result (Surface Tension) with its standard deviation. You can easily find out the desired values in the status line part of the graph (the first value is the x-axis, here the position in mm, and the second value is the y-axis, here the weight in g).


Fig. 69: Tabbed dialog Graph Control— X-Axis

Fig. 70: Tabbed dialog Graph Control—Data

Single measurements—Interfacial tension with a ring


5.4 Interfacial tension with a ring The measurement of the surface tension can be done with a standard Du-Noüy ring RG 11 or with a the small Du-Noüy ring RG 10. These probes are made of platinum-iridium according to DIN 53914.

Before you use a ring to measure, be sure that it is absolutely clean and not deformed.


in a gas flame.

Never touch the hot ring with bare hands, use always heat-proof gloves!

The measurement of the interfacial tension (IFT) can be done in two different ways:

You should use the Pull method if the liquid with the higher density has the higher surface tension.

You should use the Push method if the liquid with the higher density has the lower surface tension.

If you want to approve the surface tension of your test liquid you can measure it with a standard Wilhelmy plate(see chapter 5.1 page22) or a with a standard Du-Noüy ring (see chapter 5.2 page 27). If you don’t know the density you can measure it with the density determination set DIS 11. (see chapter 5.8 page 68).

The dialog SFT Ring is a tabbed dialog box (same dialog as for the surface tension measurement). This means that the content of the box differs depending on which tab you have selected. The content also depends on the selected probe. The area with the Start and the Stop button is always visible.

Sample Info In this tabbed dialog you can enter additional information about the test. This information will be stored together with the measurement results.







Substances In this tabbed dialog you must enter the density of the upper and the lower phase by selecting the correct phase liquid in the list box. The density will be taken out of the liquids database. For some liquids in the database the temperature coefficients for the different physical values are registered. For these liquids you can activate the automatic temperature correction of the necessary physical value (e.g. Density).

You can also enter additional parameters of the used liquid like Temperature, Concentration and Composition.

Upper Phase (liquid with the lower density) You can select a sample out of the integrated liquids database in the combo box; the corresponding density will be inserted in the text field below. You can also enter any other Text (e.g. MyOwnDesignedLiquid) and below you can enter the corresponding value of the density in g/cm3.

Lower Phase (liquid with the higher density) You can select a sample out of the integrated liquids database in the combo box; the corresponding density will be inserted in the text field below. You can also enter any other Text (e.g. MyOwnDesignedLiquid) and below you can enter the corresponding value of the density in g/cm3.

Additional Data This data are not valid for the IFT measurement, they are only necessary for the CMC measurement.







Fig. 75: Dialog Substances



Setup In this tabbed dialog you can enter parameters necessary for the test. The necessary parameters are dependent from the used probe (probe). For both rings available at DataPhysics (RG 11 and RG 10) the parameters are already filled in. If you want to use another ring (with different geometries) you have to measure the geometry data carefully and to enter these data into the edit fields.

Ring Geometry

Wire radius The radius of the ring wire in mm(preset parameter).

Ring radius The radius of the ring in mm (preset parameter).

General

Immersion depth: Defines the immersion depth of the ring before the test.




max. Number of Cycles: Defines the maximum number of measuring cycles (for each pull and push cycles). The measurement can stop before the defined cycles are finished, if you have also selected the ‘sd’ stop condition and it gets true.

Average last n measurements n=... Builds an average over the last n surface tension measuring values (see Results dialog). Only this number of measurement values will be shown in the graph and the results table.

Stop if sd is smaller than mN/m Stops the test when the standard deviation (sd) of the SFT is smaller than xx mN/m over the last n measurement cycles. For this condition you can to select also the number of measurements to be taken into account.

Sensitivity Thresholds

Surface Detection: Defines the sensitivity threshold for the surface detection, this means the position of the lift, where the detected weight difference (because the probe is getting lighter when it dips into the liquid) exceeds this threshold, will be defined as the surface of the liquid.



Fig. 76: Setup for ring


Maximum Detection: Defines the sensitivity threshold for the maximum detection. This means when the weight difference between the last found maximum value (of the generic data) and the actual measured value exceeds this threshold the last found maximum value will be defined as a maximum. After every maximum the direction of the lift will change. (Push and Pull).

Load Defaults A click onto this button will restore all the default parameters for the selected ring

Calc. Settings In this tabbed dialog you can select and enter calculation parameters

Fitting Parameters

No. of Points: Defines the number of points used for fitting the maximum weight.

Corrections

Zuidema Waters For selecting automatic ring correction according to ‘Zuidema-Waters’

σ= a + bσ* + c[1 – exp(-dσ*)] Here you can define the correction parameters (a, b, c and d) yourself.

Perform Online Calculation Select this item to perform the calculation directly during the measurement (online); if not selected the calculation of the results will be done at the end of the test.

Load Defaults A click onto this button will restore all the default parameters for the selected ring in this tabbed dialog

Maximum DetectionThreshold of 8.0 mg

Time to reverse the rotating direction and restart the lift motor

Time to stop lift motor

+ Generic Measurings

Detected Maximum Weight on pulling the ring

time Fig. 77: Sensitivity threshold for the maximum detection

Fig. 78: Dialog Calc. Settings



5.4.1 Measurement with the Pull method

The measurement of the interfacial tension (IFT) with the pull-method will be done in three steps. First the buoyancy of the ring in the liquid with the lower density is measured. In the second step the surface of the liquid with the higher density is detected. The third step is the real measurement of the interfacial tensions between the two not miscible liquids.

You should use the Pull method only if the liquid with the higher density has also the higher surface tension, otherwise the ring could be damaged.



First Step Ι (buoyancy in the liquid with lower density)

Ι DCAT 11: Fix the clamp of the options holder by turning the correspondent knob on the left side of the DCAT 11 clockwise. DCAT 21: Make sure that the options holder clamp is closed.

You must never touch the options holder or the ring if the options holder is not fixed!



Ι For the first step of the interfacial tension measurement fill the sample vessel with the test liquid with the lower density. If you don’t know the density it can be measured separately with the DCAT. (see chapter 5.8 Density of a liquid page 68). The minimum filling height is 5 mm because the ring must dip totally into the liquid to measure the buoyancy correctly (also the force caused by the small liquid lamella on the both holding rods).

Ι Insert the sample vessel carefully into the temperature controlled receptacle without touching the option holder.

Ι Put the clean ring into the options holder.



Surface Ring

Fig. 80: Buoyancy of the ring


Ι DCAT 11: Release the options holder clamp by slowly screwing out the correspondent knob on the left side of the DCAT 11 head anticlockwise. DCAT 21: The options holder clamp will be automatically released before the measurement starts.

Ι Move the sample stage up (using the -switch on the DCAT) to some millimeters below the bottom of the probe.

Ι Start the first step of the IFT Measurement (not before the ring is cooled down). The measurement is carried out automatically. You can stop the measurement at any time without loosing the so long measured data with a click on the Stop button .



If this isn’t the case, for what reason so ever, stop the measurement immediately, because otherwise the ring can be destroyed.

Ι At the end of the first step the options holder clamp should be closed: DCAT 11: Fix the clamp of the options holder by turning the correspondent knob on the left side of the DCAT 11 clockwise. DCAT 21: Make sure that the options holder clamp is closed automatically.



Ι Take the ring out of the options holder, clean it thoroughly

Ι Take the sample vessel out and clean it very thoroughly if you want to use it for the second step again (we recommend to use a new clean sample vessel for the second and third step of the IFT measurement)

Second Step ΙΙ (surface detection of the liquid with higher density)

ΙΙ For the second step of the interfacial tension measurement fill the sample vessel with the test liquid with the higher density. If you don’t know the density it can be measured separately with the DCAT. (see chapter 5.8 Density of a liquid page 68). The minimum filling height is 13 mm.

ΙΙ Insert the sample vessel carefully into the temperature controlled receptacle without touching the option holder.

ΙΙ Put the cleaned ring into the options holder.

ΙΙ DCAT 11: Release the options holder clamp by slowly screwing out the correspondent knob on the left side of the DCAT 11 head anticlockwise. DCAT 21: The options holder clamp will be automatically released before the measurement starts.

Fig. 81: Insertion of ring

Fig. 82: Work Flow Assistant ‘End of first step”

Fig. 83: Work Flow Assistant ‘Start of second

step”



ΙΙ Move the sample stage up (use the -switch on the DCAT) to some millimeters below the bottom of the ring.

ΙΙ Start the second step of the IFT Measurement (not before the rig is cooled down). The measurement is carried out automatically. You can stop the measurement at any time without loosing the so long measured data with a click on the Stop button .

ΙΙ At the end of the second step the lift will stand still at the position where the ring has met the surface of the liquid.

ΙΙ Open the housing of the DCAT.

Third Step ΙΙΙ (interfacial tension measurement between the both liquids)

ΙΙΙ For the third step of the interfacial tension measurements leave the sample vessel with the test liquid (with the higher density) inside the DCAT. Stack up (fill in very carefully without mixing) the second liquid with the lower density onto the first with the higher density. The minimum filling height of the second liquid is 12 mm.

Do not touch the options holder or the ring!

ΙΙΙ Start the IFT Measurement. The measurement is carried out automatically. You can stop the measurement at any time without loosing the so long measured data with a click on the Stop button .

ΙΙΙ At the end of the measurement the options holder clamp must be closed: DCAT 11: Fix the clamp of the options holder by turning the correspondent knob on the left side of the DCAT 11 clockwise. DCAT 21: Make sure that the options holder clamp is closed.

ΙΙΙ Save the measurement by selecting File – Save As... which opens the file save dialog to store the actual active measurement file under a definable name and into a selectable folder, or by selecting File –Save as Template... to store all information, except the really measurement data in a template. This means you can start a measurement directly after opening of a template (Menu File—New—Open Template...) without any further settings.


Ring

Surface

Fig. 84: Surface detection of second liquid

Fig. 85: Work Flow Assistant ‘Start of third step”


Lamella

Interface


Ring

Fig. 86: Interfacial tension detection



5.4.2 Measurement with the Ring Push method

The measurement of the interfacial tension (IFT) with the push-method will be done in only one step.

You should use the Push method only if the liquid with the higher density has the lower surface tension, otherwise the ring could be damaged.



The integrated work flow assistant will guide you in performing an interfacial tension measurement. With and without the work flow assistant you have to carry out the following steps:


You must never touch the options holder or the ring if the options holder is not fixed!



• Fill the sample vessel first with the test liquid with the higher density and the lower surface tension. Stack up (fill in very carefully without mixing) the second liquid with the lower density and the higher surface tension onto the first one. We recommend the minimum filling height is 5 mm for both liquids.


• Put the clean ring into the options holder.


• Move the sample stage up (use the -switch on the DCAT) to some millimeters below the bottom of the ring.

• Start the IFT Measurement (not before the probe is cooled down). The measurement is carried out automatically. You can stop the measurement at any time without loosing the so long measured data with a click on the Stop button .








• If you had select Perform Online Calculation all results will be presented on the graph during the measurement. If this is not selected you see no result data and no graph during the measurement. You can de-select Hide generic data in the tabbed dialog Graph to visualize the generic measuring data (weight) during the measurement.

• After the first measuring the actual measured temperature will be showed in the dialog Temperature. Subsequently the displayed temperature is the average over all measured temperature values during the measurement.



5.4.3 Evaluation of the IFT measurement with a ring

Graph In this tabbed dialog you can select the data you want to plot in the graph. If you change the selection you must click on the independent to actualize the graph. You can select between

SFT/IFT Surface/Interfacial tension

SFT/IFT on pushing the ring [mN/m] Surface/Interfacial tension measured during the up-movement of the stage

SFT/IFT on pulling the ring [mN/m] Surface/Interfacial tension measured during the down-movement of the stage

maximum weight [g] Measured weight data

maximum weight on pushing the ring [g] Measured weight data during the up-movement of the stage

maximum weight on pulling the ring [g] Measured weight data during the down-movement of the stage



measurement





X- and Y-Axis You can define the Title, the Scale and the Appearance of both axes

Appearance You can define the Title of the graph, the Colors of the Axes, the Background and the Grid and the Font for the Title, Label and Caption.


Result In this tabbed dialog the two tables of the results (mass and SFT) by pulling and pushing the ring were shown, and also the mean values over all included measuring values as well as the average value over both measuring rows. The number of the averaged values was defined in the Setup dialog. You can define which values were included into the fit of the surface tension result. To mask out a value which you don’t want to be included into the calculation, just click onto the time value (t [s]) in the result table. The time value of the masked out results will be set into parentheses. With a second click onto a masked (parenthesized) value it will be again included into the calculation.


Fig. 94: Example of generic data of a ring measurement

Fig. 95: Example for a interfacial tension test according to the Push method

Single measurements—Dynamic Contact Angle


5.5 Dynamic Contact Angle The measurement of the contact angle can be done with prismatic and cylindrical samples according to the Wilhelmy method and with a known test liquid..

To measure the contact angle the DCAT first detects the surface by moving the sample vessel with the liquid up until the balance detects a weight difference (because the probe is getting lighter when it dips into the liquid). This position of the stage is stored as the position where the probe meets the surface. The stage moves further up to the position you defined (immersion depth). Now the stage moves down to the stored position of the surface. This will be repeated as often you had defined before by ‘Number of Cycles’.

If you want to approve the purity of your test liquid you can measure the surface tension of the liquid with a standard Wilhelmy plate (see chapter 5.1 page

22) or a with a standard Du-Noüy ring (see chapter 5.2 page 27)

The dialog ‘Dynamic Contact Angle’ is a tabbed dialog box. This means that the content of the box differs depending on which tab you have selected. The content also depends on the selected sample geometry.

Sample Info In this tabbed dialog you can enter information about the test. This information will be stored together with the measurement results.







Setup In this tabbed dialog you have to enter the parameters necessary for the test. The necessary parameters are dependent from the used sample (probe).

Testing Body You must enter the geometric dimensions of the cross section according to the shape of the used sample

Square You must enter the length a one side of the sample.

Circle You must enter the diameter d the circle shaped sample.

Rectangle You must enter the length a and the height b of the sample.

Ellipse You must enter the length a and the height b of the sample.

Cylindrical You must enter the inner di and the outer diameter do of the sample. This probe form is not good suitable for IFT measurements.

User defined You must enter the Area and the Wetted Length of the sample.

Device


Motor Speed (Measurement Adv.): Enter the speed of the lift motor in mm/s used when measuring the advancing contact angle.

Motor Speed (Measurement Rec.): Enter the speed of the lift motor in mm/s used when measuring the receding contact angle.


If the value for the Surface Detection Threshold is defined too large it could prevent that the surface will be detected, and that means that

the probe, the sample or the balance can be destroyed.

Immersion depth: Defines the immersion depth of the probe before the test starts.

Number of Cycles: Determines the number of measuring cycles.

Wait between Cycles: Determines the waiting time in seconds between two consecutive measuring cycles.

Samples/second Measuring values per second in Hz.

Fig. 98: Geometry dimensions depending on the shape



Liquid In this tabbed dialog you can select the used test liquid from the liquid database or, if you want to use another test liquid –not included in the database– you have to add it first to the liquid database or you must enter the Density, the Surface Tension and the Viscosity manually. For some liquids in the database the temperature coefficients for the different physical values are registered. For these liquids you can activate the automatic temperature correction of the necessary physical value (e.g. Density).




The integrated work flow assistant will guide you in performing a dynamic contact angle measurement. With and without the work flow assistant you have to carry out the following steps:


You must never touch the options holder or the sample if the options holder is not fixed!





• Put your sample – held in a special sample holder (e.g. PSH 11 a special sample holder for solids in plate form) – into the options holder.


• Move the sample stage up (use the -switch on the DCAT) to some millimeters below the bottom of the sample.

• Start the contact angle measurement. The measurement is carried out automatically. You can stop the measurement at any time without loosing the so long measured data with a click on the Stop button .

Fig. 99: Selection of the used test liquid


Fig. 101: Insertion of special options holder for solids in plate form (PSH 11)





• The results will be presented on the graph during the measurement.


• After the first measuring the actual measured temperature will be shown in the dialog Temperature also. Subsequently the displayed temperature is the average over all measured temperature values during the measurement.




measurement



5.5.1 Evaluation of the Dynamic Contact Angle

Graph In this tabbed dialog you can define which curve you want to see in the graph. If you change the selection you must click on the independent to actualize the graph. As independent (X-axis) you can select time or position. You can select for the independent time

temperature (site 1) temperature probe in the receptacle T1

temperature (site 2) temperature probe connected to the rear socket T2

and for the independent position

weight (advancing)(cycle #) Measured weight data on pushing the sample for measuring cycle # (where # is the number of the measuring cycle)

weight (receding)(cycle #) Measured weight data on pulling the sample for measuring cycle # (where # is the number of the measuring cycle)

Only the curves selected here will be shown in the Graph. All the not selected cycles will be pre-set in parentheses in the Results dialog.

Fit Range Here you can enter the range in which the curve for the advancing and for the receding contact angle will be fitted. To define the range for both Advancing and Receding Cycles together click and hold the left mouse key and pull an ‘elastic band” with the mouse. To define the fit range for the Advancing and the Receding Cycles separately by entering the values for the position into the edit fields From and To. You can easily find out the desired values in the status line part of the graph (the first value is the x-axis, here the position in mm, and the second value is the y-axis, here the weight in g).

Zoom the graph Press the <Shift>-key and click and hold the left mouse key to zoom in by pulling an ‘elastic band” with the mouse, or enter the values for the axes manually in the dialog Appearance. To zoom out you must use the dialog Appearance.


X- and Y-Axis You can define the Title, the Scale and the appearance






Result In this tabbed dialog you can re-calculate the contact angle with a click to the button Calculate.

All the cycles of the dynamic contact angle measurement will be shown as a table. With a click on the cycle number the corresponding cycle will be not longer included into the calculation of the contact angle and his number was set in parentheses.

For every measured cycle you will find an own row in the table sorted after Advancing and Receding; the columns are titled with:

cycle Consecutive numbering of the measuring cycles

CA Contact angle in degrees

CA (±) Standard deviation of the contact angle in degrees

from Start value of the Fit Range defined in the dialog Graph

to End value of the Fit Range defined in the dialog Graph

N Number of values defined by the fit range in the dialog Graph

Ch2/N Statistical deviation over the measuring points

RQ Regression coefficient (RQ = 1 is ideal)

Fig. 106: Example for a measurement of dynamic contact angle on a solid body



5.5.2 Measurement with other sample holders

Special options holders are available for a wide range of samples. For all samples you have to enter the dimensions of the cross section into the tabbed dialog Setup.

Solid samples in plate form can be measured with the special options holders PSH 11. You have to determine the cross section geometry of your sample very precise, or you have to measure the ‘Wetted Length’ before you can detect the dynamic contact angle.

Solid samples in film form can be stretched in the special options holder FO 11. If it is not possible to determine the cross section geometry of your film sample, because it is too wavy, it is better to measure the ‘Wetted Length’.

The FH 11 is a special options holder to determine the wetting behavior (dynamic contact angle) of adsorbing materials like powders, pigments, fibers and fiber bundles. Fill your sample as homogeneous as possible into the holder, to get a reproducible filling. Because it is nearly impossible to detect the cross section geometry of a sample like a fiber bundle you have to measure the wetted length before. You should clean the FH 11 very thoroughly before you use it to measure. A proved way to do this is the following procedure:

• Wash it with a solvent suitable for the beforehand used test liquid.

• Wash it with distilled water.

• Dry it for one hour at 100 °C.

• Wash it with hexane.

• Dry it again for one hour at 100 °C.

If necessary first put a filter paper (FP 12) into the bottom screw cap A to prevent that the small holes clogs up. Screw on the cap A. Fill in a defined portion of your sample (e.g. a fiber bundle). Screw on the cap B with the piston C in his uppermost position. Compress the sample by screwing in the piston C. If you want to measure a series of measurements it is very important to fill in always the same amount of the sample as homogeneous as possible and to compress it equally. You must carry out the filling very thoroughly, because small differences in the packing density cause big differences in the penetrability.

Please note that the screw cap of the FH 11 has a left handed thread.

Single fibers can be glued to the single fiber holder FH 12. Because the detection of the surface is not very precise or impossible when measuring very thin fibers (with very small buoyancy) it is better to use as much fibers as you can glue to the holder without producing a lamella between two neighboring fibers. If the fibers are from a well defined cross section (e.g. cylindrical) you can calculate and enter the complete wetted length. At natural fibers or fibers with not determinable geometry you have to measure the wetted length before. The single fiber or the bunch of fibers must hang vertical to the surface of the test liquid.

Fig. 107: Sample holders PSH 11 and FO 11

A

B

C

Fig. 108: Sample holder Fh 11 and FH 12


5.6 Powder Contact Angle The contact angle measurement according to Washburn is done by the capillary rise of a liquid into a porous medium implies the replacement of the solid-air interface by a solid-liquid interface.

The measurement of the contact angle of powders can be done with the accessories kit for measurements of powder samples PUR 11. To measure the contact angle of powder in the PUR 11 you must know the capillary constant C which is a material factor (mainly dependent on the porous architecture of the powder). This constant can be measured in a first step using a total wetting liquid e.g. n-Hexane. (because of the low surface tension of 18 mN/m this liquid builds a contact angle of 0° to the powder).

The measurement o the powder contact angle consists of two tests. The first is for the detection of the capillary constant C and the second the contact angle analysis with a test liquid.

A strict powder packing control with a reproducible procedure is absolute essential because you cannot re-use the same powder packing (used to measure factor c) for the measurement with another liquid.

• Put a filter paper (FP 11) into the glass tube (GT 11) to prevent that the glass frit (sintered permeable glass filter) on the bottom of the tube clogs up.

• Fill in the powder –by use of a balance– in equal portions.

• After every addition compress the powder by tapping the tube on the table.

If you want to measure a series of measurements it is very important to fill in always the same amount of powder and to compress it equally. You must fill the tube very thoroughly, because small differences in the packing density cause big differences in the penetrability.

It is also essential that the glass tube is absolutely clean. A proved way to do clean is the following procedure:

• Wash it with acetone.


• Dry it one hour at 100 °C.

• Wash it with n-hexane.

• Dry it again one hour at 100 °C.

To measure the powder contact angle the DCAT first detects the surface by moving the sample vessel with the liquid up until the balance detects a weight difference (because of the buoyancy) greater than the defined surface detection threshold. Now the powder in the glass tube will be wetted by means of the capillary forces.

If you want to approve the cleanliness of your test liquid you can measure the surface tension of the liquid with a standard Wilhelmy plate(see chapter 5.1

page22) or a with a standard Du-Noüy ring (see chapter 5.2 page 27)

The dialog Powder Contact Angle is a tabbed dialog box. This means that the content of the box differs depending on which tab you have selected.


Single measurements—Powder Contact Angle






Setup In this tabbed dialog you can enter parameters necessary for the test.

Test Liquid The Density, Viscosity and Surface Tension of the liquid must be known before the contact angle can be calculated. You can select a sample out of the integrated liquids database in the combo box; the corresponding density, viscosity and surface tension values will be inserted in the text fields below. You can also enter any other Text in the combo box (e.g. MyOwnDesignedLiquid) and below you have to enter the corresponding values for the Density in g/cm3, the Viscosity in mPas and the Surface Tension in mN/m.

Device Setup




sample (the glass tube) or the balance can be destroyed.




Fig. 111: Setup for powder contact angle


Schedule In this tabbed dialog you can enter a time dependent sampling rate for the test and you can define that the measurement stops only by user interaction. The BEGIN and the END row are always there. With a right mouse click you can insert (Insert Row) and delete additional rows (Delete Row). The new inserted row will be placed above the actual marked row.

t/s Enter the time value at the selected point of reference.

Freq/s^-1 Enter the sampling frequency at the selected point of reference.

Time Units Select a time unit for the time table and the graph below. If you change the time unit already entered values will be converted.

Wait for user interaction to end Select this if you will stop the measurement manually.


The integrated work flow assistant will guide you in performing a powder contact angle measurement. With and without the work flow assistant you have to carry out the following steps:





• Fill the sample vessel with the desired liquid (in the first step n-Hexane for the determination of the c factor).


Fig. 112: Schedule for powder contact angle

measurement



• Insert the special adapter (PUR 11) –with the mounted filled glass tube– into the options holder.








Fig. 114: Graph during the determination of the capillary constant with n-Hexane

• After the first measuring the actual measured temperature will be showed in the dialog Temperature also. Subsequently the displayed temperature is the average over all measured temperature values during the measurement.



Fig. 113: Insertion of special adapter PUR 11


measurement


• Open a second measuring window and repeat the whole measuring cycle with a second glass tube (with the same powder), but now with the test liquid instead of the calibration liquid (n-Hexane).

5.6.1 Evaluation of the Powder Contact Angle

Graph In this tabbed dialog you can define which curve you want to see in the graph. If you change the selection you must click on the independent to actualize the graph. As independent (X-axis) you can select time or position. You can select for the independent time





Only the curves selected here will be shown in the Graph.

Fit Range Here you can enter the range in which the curve for the contact angle will be fitted. To define the range click and hold the left mouse key and pull an ‘elastic band” with the mouse or enter the values for the position into the edit fields From and To. You can easily find out the desired values in the status line part of the graph (the first value is the x-axis, here the time in s, and the second value is the y-axis, here the weight in g or the weight2 in g2).

Show squared values Select this to display the measured data in squared values. This is very helpful because the area where the capillary constant (with n-Hexane) and the contact angle (for the test liquid) should be fitted is nearly linear when displayed as

squared values (weight2 over time). As shown in the graphs below it is easier to select the fit range in squared values.

Fig. 117: Graph with normal values Fig. 118: Graph with squared values Zoom the graph Press the <Shift>-key and click and hold the left mouse key to zoom in by pulling an ‘elastic band” with the mouse, or enter the values for the axes manually in the dialog Appearance. To zoom out you must use the dialog Appearance.




With a click on the button Appearance, or a right mouse-click into the graph you can adjust the graph parameters in the tabbed dialog Graph Control.



Data For the different data curves you can define the Title, the Line Style and Symbol. You can also change the label of the data curves in the field Change Title (here for example ‘Silica 60 in n-Hexane’ instead of the standard label). The changed label will be shown in the dialog Graph Control, in the dialog Graph and in the diagram.

Result In this tabbed dialog you can determine the c-factor by using a totally wetting liquid like n-hexane or you can calculate the result (contact angle). To determine the capillary constant c of the measured powder you must select

Calibrate now, assuming a contactangle of 0° before you click to the Calculate-button.

For the next measurement cycle with your real test-liquid you must un-check this checkbox and you must enter the capillary constant c to calculate the contact angle.


Fig. 120: Example for the c-factor of powder with n-Hexane

Fig. 121: Example for a measurement of powder with water


5.7 Wetted length The measurement of the wetted length is necessary if you cannot determine the wetted length of your sample (prismatic or cylindrical) you use to measure the contact angle.

The wetted length can be measured using a total wetting liquid (with low SFT) such as n-Hexane. Using a total wetting liquid one can suppose that the contact angle is zero. Knowing the surface tension of this test liquid (n-Hexane) it is possible to determine the

wetted length by measuring the wetting force.

To measure the wetted length the DCAT first detects the surface by moving the sample vessel with the liquid up until the balance detects a weight difference (because the test piece is getting lighter when it dips into the liquid). This position of the stage is stored as the position where the test piece meets the surface. The stage moves further up to the position you defined (immersion depth). Now the stage moves down to the stored position of the surface. This will be repeated as often you had defined before by ‘Number of Cycles’.

If you want to approve the purity of your test liquid you can measure the surface tension of the liquid with a standard Wilhelmy plate (see chapter 5.1 page

22) or with a standard Du-Noüy ring (see chapter 5.2 page 27)

The dialog ‘Wetted length’ is a tabbed dialog box. This means that the content of the box differs depending on which tab you have selected. The content also depends on the selected sample geometry.

Sample Info In this tabbed dialog you can enter information about the test. This information will be stored together with the measurement results.





wetted lenghth

Fig. 123: Wetted length


Single measurements—Wetted length


Setup In this tabbed dialog you have to enter the parameters necessary for the test.




If the value for the Surface Detection Threshold is defined too large it could prevent that the surface will be detected, and that means that

the probe, the sample or the balance can be destroyed.

Immersion depth: Defines the immersion depth of the probe before the test starts.

Number of Cycles: Determines the number of measuring cycles.

Wait between Cycles: Determines the waiting time in seconds between two consecutive measuring cycles.

Samples/second Measuring values per second in Hz.

Liquid In this tabbed dialog you can select the used test liquid from the liquid database or, if you want to use another test liquid –not included in the database– you have to add it first to the liquid database or you must enter the Surface Tension and the Contact Angle manually. For some liquids in the database the temperature coefficients for the different physical values are registered. For these liquids you can activate the automatic temperature correction of the necessary physical value (e.g. Density).




The integrated work flow assistant will guide you in performing a dynamic contact angle measurement. With and without the work flow assistant you have to carry out the following steps:

Fig. 125: Setup for dynamic contact angle

Fig. 126: Selection of the used test liquid



You must never touch the options holder or the sample if the options holder is not fixed!





• Put your sample – held in a special sample holder (e.g. PSH 11 a special sample holder for solids in plate form) – into the options holder.








• After the first measuring the actual measured temperature will be shown in the dialog Temperature also. Subsequently the displayed temperature is the average over all measured temperature values during the measurement.




Fig. 128: Insertion of special options holder for solids in plate form (PSH 11)




5.7.1 Evaluation of the Wetted length

Graph In this tabbed dialog you can define which curve you want to see in the graph. If you change the selection you must click on the independent to actualize the graph. As independent (X-axis) you can select time or position.

You can select for the independent time





weight (receding)(cycle #) Measured weight data on pulling the sample for measuring cycle # (where # is the number of the measuring cycle)

Only the curves selected here will be shown in the Graph. All the not selected cycles will be pre-set in parentheses in the Results dialog.










Result In this tabbed dialog you can re-calculate the contact angle with a click to the button Calculate.

All the cycles of the wetted length measurement will be shown as a table. With a click on the cycle number the corresponding cycle will be not longer included into the calculation of the contact angle and his number was set in parentheses.

For each measured cycle you will find an own row in the table sorted after Advancing and Receding; the columns are titled with:

cycle Consecutive numbering of the measuring cycles

l / mm Wetted length in millimeter

l (±) Standard deviation of the wetted length

from Start value of the Fit Range defined in the dialog Graph

to End value of the Fit Range defined in the dialog Graph

N Number of values defined by the fit range in the dialog Graph

Ch2/N Statistical deviation over the measuring points

RQ Regression coefficient (RQ = 1 is ideal)

Fig. 132: Example for a measurement of the wetted length



5.7.2 Measurement with other sample holders

Special options holders are available for a wide range of samples. For all samples you have to enter the dimensions of the cross section into the tabbed dialog Setup.

Solid samples in plate form can be measured with the special options holders PSH 11. You have to determine the cross section geometry of your sample very precise, or you have to measure the ‘Wetted Length’ before you can detect the dynamic contact angle.

Solid samples in film form can be stretched in the special options holder FO 11. If it is not possible to determine the cross section geometry of your film sample, because it is too wavy, it is better to measure the ‘Wetted Length’.

The FH 11 is a special options holder to determine the wetting behavior (dynamic contact angle) of adsorbing materials like powders, pigments, fibers and fiber bundles. Fill your sample as homogeneous as possible into the holder, to get a reproducible filling. Because it is nearly impossible to detect the cross section geometry of a sample like a fiber bundle you have to measure the wetted length before. You should clean the FH 11 very thoroughly before you use it to measure. A proved way to do this is the following procedure:

• Wash it with a solvent suitable for the beforehand used test liquid.


• Dry it one hour at 100 °C.

• Wash it with hexane.

• Dry it again one hour at 100 °C.

If necessary first put a filter paper (FP 12) into the bottom screw cap A to prevent that the small holes clogs up. Screw on the cap A. Fill in a defined portion of your sample (e.g. a fiber bundle). Screw on the cap B with the piston C in his uppermost position. Compress the sample by screwing in the piston C. If you want to measure a series of measurements it is very important to fill in always the same amount of the sample as homogeneous as possible and to compress it equally. You must carry out the filling very thoroughly, because small differences in the packing density cause big differences in the penetrability.

Please note that the screw cap of the FH 11 has a left handed thread.

Single fibers can be glued to the single fiber holder FH 12 or FH 13. Because the detection of the surface is not very precise or impossible when measuring very thin fibers (with very small buoyancy) it is better to use as much fibers as you can glue to the holder without producing a lamella between two neighboring fibers. If the fibers are from a well defined cross section (e.g. cylindrical) you can calculate and enter the complete wetted length. At natural fibers or fibers with not determinable geometry you have to measure the wetted length before. The single fiber or the bunch of fibers must hang vertical to the surface of the test liquid.

Fig. 133: Sample holders PSH 11 and FO 11

A

B

C

Fig. 134: Sample holder FP 11 and FH 12


5.8 Density of a liquid The measurement of the density will be done with the density determination set DIS 11 (Part. No. 2000337) and the optional software SCAT 34.

The density determination set DIS 11 is consisting of one probe made of pure silicone and one special holder for it made of Platinum-Iridium.

Before you use the DIS 11 to measure, be sure that it is absolutely clean and not deformed.

A proved way to clean the holder made of platinum-iridium is to make it red-

hot in a gas flame.

Never touch the hot holder with bare hands, use always heat-proof gloves!

To measure the density the DCAT first detects the buoyancy of the holder in the liquid. In the second step the density of the liquid is detected using the silicone probe.

The dialog Density of a liquid is a tabbed dialog box. This means that the content of the box differs depending on which tab you have selected. The content also depends on the selected probe (ring, plate etc.). The area with the Start and the Stop button is always visible.








Single measurements—Density of a liquid



Probe properties You must enter the volume and the mass of the silicone probe. The density of the silicone probe of the DIS 11 is 2,329 g/cm3 at 20°C. The density for other temperatures can be calculated as follows: ρ (T) = ρ • (20°C) • [1 - 3 • 4.2 • 10-6 • (T – 20)]

Volume You must enter the volume of the silicone probe (1.35034 cm3)

Mass You must enter the mass of the silicone probe ( 3.14633 g)

The button will be not available until the volume and the mass are entered.

Device

Immersion depth: Defines the immersion depth of the probe





Wait time after immersion: Defines the time between immersion and start of the measurement.

Average time: Defines how long the measurement of the density will last (all measurements taken in this time will be averaged).

Additional Data This data are not valid for the density measurement, they are only necessary for the CMC measurement.




Fig. 138: Setup for density



The integrated work flow assistant will guide you in performing a density measurement. You can disable the workflow assistant by de-selecting Show Assistent in the menu Setup or by selecting .

With and without the work flow assistant you have to carry out the following steps:


You must never touch the options holder or the holder if the options holder is not fixed!



• Fill the sample vessel with the liquid to be tested.


• Put the clean holder into the options holder.


• Move the sample stage up (use the -switch on the DCAT) to some millimeters below the bottom of the holder.

• Start the measurement of the buoyancyof the holder (not before the holder is cooled down). The measurement is carried out automatically. You can stop the measurement at any time without loosing the so long measured data with a click on the Stop button .



If this isn’t the case, for what reason so ever, stop the measurement immediately, because otherwise the holder can be destroyed.


• Put the clean silicone probe into the special holder.

• DCAT 11: Release the options holder clamp again by slowly screwing out the correspondent knob on the left side of the DCAT 11 head anticlockwise. DCAT 21: The options holder clamp will be automatically released again before the measurement will be continued.


Fig. 140: Insertion of holder


Single measurements—Density of a liquid



• Save the measurement by selecting File – Save As... which opens the file save dialog to store the actual active measurement file under a definable name and into a selectable folder, or by selecting File –Save as Template... to store all information, except the really measurement data in a template. This means you can start a measurement directly after opening of a template (Menu File—New—Open Template...) without any further settings.

5.8.1 Evaluation of the density of a liquid

Graph In this tabbed dialog you define which curve you want to see in the graph. If you change the selection you must click on the Independent to actualize the graph. For the Dependent you can select one or more of

temperature (site 1) temperature probe in the receptacle temperature (site 2) temperature probe connected to the rear socket T2 maximum weight Measured weight data




X- and Y-Axis to define the Title, the Scale and the appearance Appearance to define the Title of the graph, the Colors of the Axes, the Background and the Grid, and the Font for the Title, Label and Caption. Data for the different data curves you can define the Title, the Line Style, the Symbol, and the colors. You can also change the label of the data curves in the field Change Title. The changed label will be shown in the dialog Graph and in the diagram.

Press the <Shift>-key and click and hold the left mouse key to zoom in by pulling an ‘elastic band” with the mouse. To zoom out you must use the dialog Appearance.



Result In this tabbed dialog you can define the

Fig. 143: Example for a density measurement

If you type the range into the text fields From and To of the Fit Range, you have to click on the button Calculate to fit the curve and show the result (Surface Tension) with its standard deviation. You can easily find out the desired values in the status line part of the graph (the first value is the x-axis, here the position in mm, and the second value is the y-axis, here the weight in g).

Single measurements—Sedimentation


5.9 Sedimentation The analysis of the sedimentation rate will be done with the sedimentation cone SC 11 (Part. No. 2000444). Before you use the sedimentation cone be sure that it is absolutely clean and not deformed.

A proved way to clean a sedimentation cone is to dip it

into 30% sulphuric acid and afterwards wash with water.

Be very carefully when working with strong acids. Risk of chemical burn!

Please wear always adequate protection gloves and clothing. Please watch the corresponding material safety data sheets!



Active TEC/TPC temperature start condition feature… This feature also works without a TEC, you can also use it when a liquid bath circulator controls the temperature in the sample vessel (measured with the built-in sensor T1 by default). If you select the Temperature Sensor T2 be sure that it is connected and measures the desired temperature.






Probe properties You must enter two geometric values of the sedimentation cone. The values for the cone SC 11 are the default values.

Outer Diameter You must enter the diameter of the cone in mm (16.5 mm)

Inner Diameter You must enter the diameter of the rod in mm (1.2 mm)

Measurement settings

Duration of stirring: Defines how long the magnetic stirrer is switched on

Wait time after stirring: Defines the time before the measurement starts after the end of the stirring period

Immersion depth: Defines the immersion depth of the cone


Surface Detection Threshold: Defines the sensitivity threshold for the surface detection, this means the position of the lift, where the detected weight difference (because the cone is getting lighter when it dips into the liquid) exceeds this threshold, will be defined as the surface of the liquid.


cone or the balance can be destroyed.

Stirring rate: Defines the rotational speed of the stirrer in % of the maximum speed

Sedimentation Rate – Filter The filter is a sliding window evaluating the mid point of a parabola at each point. Taking the first derivative of the parabola gives the sedimentation rate.

Filter strength The window size of the filter can be adjusted using the slider Filter strength. The maximum value is half the total number of points. The more points the smoother the curve of the filtered values.

Calculation Click to recalculate the values.

Fig. 146: Setup for sedimentation cone SC 11



Schedule In this tabbed dialog you can enter a time dependent sampling rate for the test and you can define that the measurement stops only by user interaction. The BEGIN and the END row are always there. With a right mouse click you can insert (Insert Row) and delete rows (Delete Row). The new inserted row will be inserted above the actual row.

t/s Enter the time value at the selected point. The unit depends on the selected Time Units below.

Freq/s^-1 Enter the sampling frequency at the selected point. The unit depends on the selected Time Units below.


Wait for user interaction to end Select this if you want to stop the measurement manually.


The integrated work flow assistant will guide you in performing a sedimentation measurement. You have to carry out the following steps:





• Fill the sample vessel with the desired sample.


• Insert the sedimentation cone (SC 11) into the options holder.



• Start the sedimentation measurement. The measurement is carried out automatically. You can stop the measurement at any time without loosing the so long measured data with a click on the Stop button .

Fig. 147: Schedule for sedimentation measurement

Fig. 148: Insertion of sedimentation cone SC 11




If this isn’t the case, for what reason so ever, stop the measurement immediately, because otherwise the cone and balance can be destroyed.




5.9.1 Evaluation of the sedimentation rate

Graph In this tabbed dialog you can select the data you want to plot in the graph. If you change the selection you must click on the independent to actualize the graph. As independent (X-axis) you can select only time.



weight Measured weight data

Filtered Weight Smoothed weight data

Sedimentation Rate / g/cm2s Calculated sedimentation rate (deduced out of the filtered data)


Zoom the graph Press the <Shift>-key, click and hold the left mouse key to zoom in by pulling an ‘elastic band” with the mouse, or enter the values for the axes manually in the dialog Appearance. To zoom out you must use the dialog Appearance.

Fig. 149: Graph during sedimentation test





X- and Y-Axis You can define the Title, the Scale and the Appearance



With the Sedimentation Rate - Filter (see Setup) you can smooth the curve of the Filtered Weight and the curve sedimentation rate.


Abb. 152: Curves of filtered weights with filter values of 300, 5000 and 12000 and the deduced sedimentation rates


5.10 Penetration The analysis of yield forces on soft gels, pastes etc. could be done with the penetration cone PP 11 (Part. No. 2000445). Before you use the penetration cone be sure that it is absolutely clean and not deformed.

A proved way to clean a penetration cone is to dip it

into 30% sulphuric acid and afterwards wash with water.

Be very carefully when working with strong acids. Risk of chemical burn!

Please wear always adequate protection gloves and clothing. Please watch the corresponding material safety data sheets!







Single measurements—Penetration


Setup In this tabbed dialog you can enter parameters required for the test. These parameters are depending onhe used probe.

Probe properties The probe properties are predefined because the penetration test can be carried out only with the penetration cone PP 11.

Measurement settings


Surface Detection Threshold: Defines the sensitivity threshold for the surface detection, this means the position of the lift, where the detected weight difference (because the cone is getting lighter when it dips into thesample) exceeds this threshold, will be defined as the surface of the sample.


cone or the balance can be destroyed.

Diving speed: Defines the speed of the penetration

Immersion depth: Defines the immersion depth of the cone

Penetration Rate - Filter The filter is a sliding window evaluating the mid point of a parabola at each point. Taking the first derivative of the parabola gives the penetration rate.

Filter strength The window size of the filter can be adjusted using the slider Filter strength. The maximum value is half the total number of points. The more points the smoother the curve of the filtered values.

Calculation Click to recalculate the values.

Schedule In this tabbed dialog you can enter a time dependent sampling rate for the test and you can define that the measurement stops only by user interaction. The BEGIN and the END row are always there. With a right mouse click you can insert (Insert Row) and delete rows (Delete Row). A new row will be inserted above the actual row.

t/s Enter the time value at the selected point of reference. The unit depends on the selected Time Units below.

Freq/s^-1 Enter the sampling frequency at the selected point of reference. The unit depends on the selected Time Units below.


Wait for user interaction to end Select this if you want to stop the measurement manually.

Fig. 155: Setup for penetration cone PP 11

Fig. 156: Schedule for penetration measurement



The integrated work flow assistant will guide you in performing a penetration measurement. You have to carry out the following steps:





• Fill the sample vessel with the desired sample.


• Insert the penetration cone (PP 11) into the options holder.



• Start the penetration measurement. The measurement is carried out automatically. You can stop the measurement at any time without loosing the so long measured data with a click on the Stop button .



If this isn’t the case, for what reason so ever, stop the measurement immediately, because otherwise the cone can be destroyed.

Fig. 157: Insertion of penetration cone PP 11

Single measurements—Penetration





5.10.1 Evaluation of the penetration rate

Graph In this tabbed dialog you can select the data you want to plot in the graph. If you change the selection you must click on the independent to actualize the graph. As independent (X-axis) you can select only time.



weight Measured weight data

Filtered Weight Smoothed weight data

Penetration Rate / g/cm2s Calculated penetration rate (deduced out of the filtered data)






Data For the different data curves you can define the Title, the Line Style and Symbol. You can also change the label of the data curves in the field Change Title . The changed label will be shown in the dialog Graph Control, in the dialog Graph and in the diagram.

Fig. 158: Graph during penetration test




With the Penetration Rate - Filter (see Setup) you can smooth the curve of the Filtered Weights and the curve penetration rate.

Fig. 161: Curve of filtered weight and the deduced penetration rate

Project—CMC increasing concentration


6 Project

All tests which are done fully automated in measurement series including the data analysis will be defined as a project. The project includes all the definitions required to control the DCAT and the LDU xx (Liquid Dispense Unit), to run the tests and to analyze the measured data.

There are two projects available:

CMC increasing concentration The automatic measurement of the CMC (Critical Micelle formation Concentration) by increasing the concentration of the surface active substance (surfactant).

CMC reversed The automatic measurement of the CMC (Critical Micelle formation Concentration) by decreasing the concentration of the surfactant.

To detect the CMC ‘hands-off’ you need an additional liquid dispense unit such as the LDU xx or a Dosimat. Please refer to the corresponding manual for the use of a Dosimat.

6.1 CMC increasing concentration The critical micelle formation concentration is the characteristic concentration of a surfactant solution, at which the molecules of the surface active agent starts to build agglomerates (micelles) standing a kinetic equilibrium with the remaining single molecules of the solution; in crossing the CMC as a phase transition point, the slopes of several physical properties as a function of concentration changes their values, particularly the surface and interfacial tension show an inflexion point at the CMC.

The detection of the CMC by increasing the concentration will be done using a series of surface tension measurements on the same sample but with increasing concentration. The concentration can be increased manually by a precise pipette or automatically by a LDU xx or a Dosimat.

For the detection of the CMC we recommend to use a Wilhelmy plate (PT 11), made of platinum-iridium according to DIN 53914. The use of other probes is optional.

Before you use a probe for analysis, be sure that it is absolutely clean and not deformed.


in a gas flame.


The first step to detect the CMC is to measure the surface tension of the receiver liquid (e.g. water). Normally the parameters of the receiver liquid are well known so this first surface tension value can show if the receiver liquid is pure and/or the probe is clean. The process sequence of each particular SFT measurement is the same as in the above described single measurements.

Fig. 162: Dialog File — New — Project ..


The dialog CMC increasing concentration is a tabbed dialog box. This means that the content of the box differs depending on which tab you have selected.


Setup In this tabbed dialog you must enter information about the project.

Print measurement reports Mark this check box to print every single SFT measurement report.

Print final reports Mark this check box to print the final CMC report.

Original Liquid Here you must enter parameters for the receiver liquid.

Liquid: You can select a receiver liquid out of the integrated liquids database in the combo box; the corresponding density and molar mass will be inserted in the text field below. If the receiver liquid is not in the database you can enter the name directly into the combo box and below the corresponding values of the density in g/cm3 and of the molar mass in g/mol. Furthermore you have the possibility to enter additional liquids to the database.

Concentration of Liquid A (or B) initially contained in vessel: If the receiver liquid in the vessel still contains an initial amount of the surfactant to add.

Volume: The amount of receiver liquid actually contained in the vessel at the start of processing in ml.

Capacity of vessel: The maximum capacity of the vessel in ml.

Solution to add Here you must enter parameters for the surfactant you want to add.

Liquid A (or B): You can select a liquid out of the integrated liquids database in the combo box; the corresponding density and molar mass will be inserted in the text field below. If the liquid you want to add is not in the database you can enter the name directly into the combo box and below the corresponding values of the density in g/cm3 and of the molar mass in g/mol. Except of the case where a constant concentration of liquid B for a two component CMC will be used, only either ‘Concentration of Liquid A initially contained in vessel’ or ‘Concentration of Liquid B initially contained in vessel’ must be entered.

Concentration (Liquid A or Liquid B): Concentration of surfactant in the liquid to add.

General Parameters Here you can set general parameters valid for the whole CMC project.

Units: The units for all concentrations to be given in can be set globally by selecting from the following drop down combo box. If values for concentrations already exist they are converted to the new units afterwards. Also the values in the measurement table (TAB ‘Measurement’) are converted.

Fig. 163: Dialog Setup



Available units are: mol/l, mmol/l, µmol/l, g/l, mg/l, µg/l, µl/l, ml/l, l/l, mol/mol, mmol/mol, µmol/mol, g/g, g/kg, and ppm.

Stirrer Here you define the stirring time (Stirr Time:) in s, the speed of the magnetic stirrer (Stirr Rate:) in % of the maximum speed, and the time to wait (Wait:) in s before the next SFT measurement will start.

Variation of Concentration Here you define which dosing system will be used.

Manual (Liquid A) With this variation you must add the amount of surfactant necessary for the next step manually a with precise pipette.

LDU slot A Use of the surfactant in the LDU A for increasing the concentration.

LDU slot B Use of the surfactant in the LDU B for increasing the concentration.

Dosimat (Liquid A) Use of the surfactant in the dosimat for increasing the concentration.

LDU slot A / B (B const. c) Use of the surfactant from the LDU A for increasing the concentration and the concentration in the sample vessel of the surfactant from LDU B will be hold constant. This is used to examine synergistic effects.

Liquid Extraction In this tabbed dialog you can enter parameter for the liquid extraction.

Use upper and lower limits for CMC and reversed CMC Mark this check box if you want to activate this function.

Vessel – fill level limits Enter the upper limit and the lower limit between the liquid level will be hold.

Extraction by liquid suction

Manual With this variation you must extract the necessary amount of surfactant manually with a precise pipette.

LDU slot A Use of the LDU A to extract the solution.

LDU slot B Use of the LDU B to extract the solution.

Dosimat Use of the dosimat to extract the solution.

Stirring before extraction Here you define the stirring time (Stirr Time:) in s the speed of the magnetic stirrer (Stirr Rate:) in % of the maximum speed and the time to wait (Wait:) in s before extracting.

Method

Keep fill-level constant at maximum fill-level reached Select this to keep the fill level constant at the maximum (by extracting the same amount which will be added in the next step).

Reduce to minimum fill level before dispensation Select this to keep the fill level constant at the minimum.

Fig. 164: Dialog Liquid Extraction


Measurement In this tabbed dialog you define the series of single SFT measurements, the volumes to add to reach the next concentration step, and if necessary the volumes to extract. These rows will be auto-matically calculated and filled in by the concentration wizard. The template used for the single SFT measurement will be selected in the TAB File Directories.

Delete Table Click this button to delete the complete table.

Wizard Click this button to open the Concentration Wizard.

Lowest Concentration: Defines the lowest concentration resp. the start concentration.

Highest Concentration: Defines the end concentration.

Steps: Number of steps (increasing the concentration)

Fixed concentration Liquid B: Defines the constant concentration of Liquid B in the solution in the sample vessel.

Scale You can select a linear or a logarithmic scale.

Start first measurement without dosing Mark this check box to start the first SFT measurement with the start concentration, useful to check the purity of the receiver liquid.

Fill levels viz. In this tabbed dialog the fill levels will be displayed in a graph.

show intermediate fill levels Mark this check box to show also the levels before extraction.

In the context menu (right mouse click) you can export the Fill-Level map to Clipboard, as DIB file (Device Independent Bitmap graphic), and as JPG file and set the properties of the graph:

General Here you can set the layout parameters for the graph of the Fill-Level map.

Scaling Here you can set the scaling for the Fill-Level map.

Fig. 165: Dialog Measurement

Fig. 166: Dialog Concentration Wizard

Fig. 167: Context menu Properties — General

Fig. 168: Fill-Level map

Fig. 169: Context menu Properties — Scaling



File Directories In this tabbed dialog you define the directories and the files for the results and the templates.

Output of Results: Define a directory and a root file name (the step no, e.g.003, were added automatically) to store the data.

Single Measurement Template: Define a template-file for the single SFT measurements.

Data Analysis Template: Defines a template file for the data analysis.

Start Click this button to start the complete CMC project.

Stop Click this button to stop the complete CMC project.

Pause Click this button to pause the execution of the CMC project.

Defining and starting a CMC project

• Select an existing measurement template for the single SFT measurements ‘File directories’ or define a new one by saving either a Wilhelmy plate measurement or a Du-Noüy ring measurement as a measurement template.

• Define a CMC result template file.

• Setup the CMC project parameters.

• Define a measurement sequence in terms of concentrations at each step in ‘Measurement’ using the Wizard.

• Check your settings under fill levels and limit the fill levels if necessary.





• Connect all the tubes and the three-way valve TWV (see chapter 8.3.2 LDU – connections

page 107).

• Fill the bottles with the liquid you need to increase or decrease the concentration (e.g. solution with surfactant and water).

• Fill the dosing syringe (e.g. the delivered standard syringe DS 500/GT) manually with

the liquid of the bottle without any air bubbles and fix it in the ES 11. Use the or

the key on the ES 11 to move the piston holder to clamp the piston.

Fig. 170: Dialog File Directories


• Get rid of all air bubbles in the just filled dosing device (Slot A or Slot B). We recommend the following procedure:

1) Put a waste vessel into the DCAT, and place the needle of the dosing tube DT 500/04 (Valve/Syringe — DCAT) and the end of the rinse-tube DT 500/16 (connected to the right side of the TWV) into the waste vessel.

2) Open the LDU control .

3) Switch the TWV to the rinse-tube (right side)

4) Start purging the system with a click to the Purge Button.

5) Shortly before the syringe is empty (the piston of the ES 11 reaches his upper position) switch the TWV to the valve (left side).

6) When the syringe is empty (the piston of the ES 11 reaches his lower position) switch the TWV to the rinse-tube (right side).

7) Repeat the steps 1 to 6 until no air bubbles are visible in the syringe or the tubes. When all air bubbles are out of the system you can stop the purging and switch the TWV to the valve (left side).

8) Fix the needle of the dosing tube DT 500/04 (Valve/Syringe — DCAT) inside the DCAT to the TH 70 or TH 50 (Tube Holder).

9) Remove the waste vessel.

• Fill the sample vessel with the receiver liquid (e.g. water).


• Put the clean probe (e.g. Wilhelmy plate) into the options holder.



• Start the CMC measurement with a click to the button in the dialog ‘File directories’. The measurement is carried out automatically. You can stop the measurement at any time without loosing the so long measured data with a click on the Stop button .

Keep an eye on the first whole measurement especially at the start. Please check if the surface of the liquid is correctly detected. This will be visible by the



The CMC project will carry out the pre-defined number (steps) of single SFT measurements on the same sample (receiver liquid) but with an increasing concentration (as defined in the dialog ‘Measurement — Concentration Wizard’). The concentration will be increased (manually or automatically by a LDU or a Dosimat) before the respective single SFT measurement will start. Every single SFT result will be stored and printed (if selected) at the end of the respective measurement.

To syringe

Right side to drain syringe

to waste

Left side to fill syringe from bottle

Fig. 171: Use of the TWV




• The following procedure will be carried out for every single step of the CMC project: 1) Optional the pre-calculated amount of liquid will be extracted from the sample

vessel, after the liquid was mixed for the defined time (see dialog Liquid Extraction).

2) The pre-calculated amount of liquid A (and if selected also of liquid B) will be added. When the variation Manual (Liquid A) was selected you will be prompted to add the calculated amount of liquid A.

3) The magnetic stirrer will mix the liquid in the vessel for the defined time.

4) After the wait time the sample stage will move up.

5) The measurement of the SFT will be done.

6) During the single SFT measurement the results will be shown in a graph.

7) The results will be stored in a result file. To the defined name the step number will be added automatically (e.g. cmc-test003.mea).

8) The results (SFT) were entered in the data table of the analysis window.

9) The sample stage will move down.

These steps (1 – 9) will be repeated until all defined single SFT measurement steps are done.

• At the end of the CMC project the options holder clamp has to be closed: DCAT 11: Fix the clamp of the options holder by turning the correspondent knob on the left side of the DCAT 11 clockwise. DCAT 21: Make sure that the options holder clamp is closed.

• Clean the complete dosing system (syringe, tubes, valves, bottle, and vessel) very thoroughly before you use it again. An easy way to clean is to exchange the bottle with the liquid A (or B) with a bottle containing a pure solvent and purge the system.

Fig. 173: Graph during single SFT measurement

Fig. 174: Results and graphic in the data analysis window


6.2 CMC reversed The critical micelle formation concentration is the characteristic concentration of a surfactant solution, at which the molecules of the surface active agent starts to build agglomerates (micelles) standing a kinetic equilibrium with the remaining single molecules of the solution; in crossing the CMC as a phase transition point, the slopes of several physical properties as a function of concentration changes their values, particularly the surface and interfacial tension show an inflexion point at the CMC.

The detection of the CMC by decreasing the concentration will be done using a series of surface tension measurements on the same sample but with decreasing concentrations. The concentration can be decreased manually by a precise pipette or automatically by a LDU xx or a Dosimat.

For the detection of the CMC reversed we recommend to use the small Du-Noüy ring (RG 10), made of platinum-iridium according to DIN 53914 and the special sample vessel GS CMC. The use of other probes is optional.

Before you use a probe for analysis, be sure that it is absolutely clean and not deformed.


in a gas flame.


The first step to detect the CMC is to measure the surface tension of the liquid in the vessel (e.g. high concentration of surfactants in water). The process sequence of each particular SFT measurement is the same as in the above described single measurements.

The dialog CMC reversed is a tabbed dialog box. This means that the content of the box differs depending on which tab you have selected.


Project—CMC reversed


Setup In this tabbed dialog you must enter information about the project.

Print measurement reports Mark this check box to print every single SFT measurement report.

Print final reports Mark this check box to print the final CMC report.

Original Liquid Here you must enter the parameters for the receiver liquid.

Liquid (Surfactant): You can select the liquid in the vessel out of the integrated liquids database in the combo box; the corresponding density and molar mass will be inserted in the text field below. If the liquid in the vessel is not in the database you can enter the name directly into the combo box and below the corresponding values of the density in g/cm3 and of the molar mass in g/mol. Furthermore you have the possibility to enter additional liquids to the database.

Concentration of Liquid (Surfactant) initially contained in vessel: The initial amount of the surfactant in the liquid in the vessel.

Volume: The amount of liquid actually contained in the vessel at the start of processing in ml.

Capacity of vessel: The maximum capacity of the vessel in ml.

Solution to add Here you must enter parameters for the solution you want to add. You need to specify a solution to add even in the case of the reversed CMC, because the concentration together with the density and molar mass of that liquid are parameters for the concentration initially in the liquid, even if you add a liquid with concentration zero.

Solvent: You can select a liquid out of the integrated liquids database in the combo box; the corresponding density and molar mass will be inserted in the text field below. If the liquid you want to add is not in the database you can enter the name directly into the combo box and below the corresponding values of the density in g/cm3 and of the molar mass in g/mol.

Concentration: Concentration of the surfactant in the solution to add.

General Parameters Here you can set general parameters valid for the whole CMC project.

Units: The units for all concentrations to be given in can be set globally by selecting from the following drop down combo box. If values for concentrations already exist then they are converted to the new units. Also the values in the measurement table (TAB ‘Measurement’) are converted. Available units are: mol/l, mmol/l, µmol/l, g/l, mg/l, µg/l, µl/l, ml/l, l/l, mol/mol, mmol/mol, µmol/mol, g/g, g/kg, and ppm.

Stirrer Here you define the stirring time (Stirr Time:) in s the speed of the magnetic stirrer (Stirr Rate:) in % of the maximum speed and the time to wait (Wait:) in s before the next SFT measurement will start.

Fig. 175: Dialog Setup


Variation of Concentration Here you define which dosing system will be used.

Manual (Solvent) With this variation you must add the amount of solvent necessary for the next step manually a with precise pipette.

LDU slot A Use of the solvent in the LDU A for decreasing the concentration.

LDU slot B Use of the solvent in the LDU B for decreasing the concentration.

Dosimat (Liquid A) Use of the solvent in the dosimat for decreasing the concentration.

Liquid Extraction In this tabbed dialog you can enter parameter for the liquid extraction.

Use upper and lower limits for CMC and reversed CMC Mark this check box if you want to activate this function.

Vessel – fill level limits Enter the upper limit and the lower limit between the liquid level will be hold.

Extraction by liquid suction

Manual With this variation you must extract the necessary amount of surfactant manually with a precise pipette.

LDU slot A Use of the LDU A to extract the solution.

LDU slot B Use of the LDU B to extract the solution.

Dosimat Use of the dosimat to extract the solution.

Stirring before extraction Here you define the stirring time (Stirr Time:) in s the speed of the magnetic stirrer (Stirr Rate:) in % of the maximum speed and the time to wait (Wait:) in s before extracting.

Method

Keep fill-level constant at maximum fill-level reached Select this to keep the fill level constant at the maximum (by extracting the same amount which will be added in the next step).

Reduce to minimum fill level before dispensation Select this to keep the fill level constant at the minimum.

Measurement In this tabbed dialog you define the series of single SFT measurements, the volumes to add to reach the next concentration step, and if necessary the volumes to extract. These rows will be automatically calculated and filled in by the concentration wizard. The template used for the single SFT measurement will be selected in the TAB File Directories.

Delete Table Click this button to delete the complete table.

Wizard Click this button to open the Concentration Wizard.

Lowest Concentration: Defines the lowest concentration resp. the end concentration.

Highest Concentration: Defines the highest concentration resp. the start concentration.

Fig. 176: Dialog Liquid Extration

Fig. 177: Dialog Measurement



Steps: Number of steps (decreasing the concentration)

Scale You can select a linear or a logarithmic scale.

Start first measurement without dosing Mark this check box to start the first SFT measurement with the start concentration.

Fill levels viz. In this tabbed dialog the fill levels will be displayed in a graph.

show intermediate fill levels Mark this check box to show also the levels before extraction.

In the context menu (right mouse click) you can export the Fill-Level map to Clipboard, as DIB file (Device Independent Bitmap graphic), and as JPG file and set the properties of the graph:

General Here you can set the layout parameters for the graph of the Fill-Level map.

Scaling Here you can set the scaling for the Fill-Level map.

File Directories In this tabbed dialog you define the directories and the files for the results and the templates.

Output of Results: Define a directory and a root file name (the step numbers, e.g.003, were added automatically) to store the data.

Single Measurement Template: Define a template-file for the single SFT measurements.

Data Analysis Template: Defines a template file for the data analysis.

Start Click this button to start the complete CMC project.

Stop Click this button to stop the complete CMC project.

Pause Click this button to pause the execution of the CMC project.

Fig. 178: Dialog Concentration Wizard

Fig. 179: Fill-Level map

Fig. 180: Context menu Properties — General

Fig. 181: Context menu Properties — Scaling

Fig. 182: Dialog File Directories


Defining and starting a CMC reversed project

• Select an existing measurement template for the single SFT measurements ‘File directories’ or define a new one by saving either a Wilhelmy plate measurement or a Du-Noüy ring measurement as a measurement template.

• Define a CMC result template file.

• Setup the CMC project parameters.

• Define a measurement sequence in terms of concentrations at each step in ‘Measurement’ using the Wizard.

• Check your settings under fill levels and limit the fill levels if necessary.





• Connect all the tubes and the three-way valve TWV (see chapter 8.3.2 LDU – connections

page 107).

• Fill the bottle with the liquid (e.g. water) you need to decrease the surfactant concentration.

• Fill the dosing syringe (e.g. the delivered standard syringe DS 500/GT) manually with

the liquid of the bottle without any air bubbles and fix it in the ES 11. Use the or

the key on the ES 11 to move the piston holder to clamp the piston.

• Get rid of all air bubbles in the just filled dosing device (Slot A or Slot B). We recommend the following procedure:

1) Put a waste vessel into the DCAT, and place the needle of the dosing tube DT 500/04 (Valve/Syringe — DCAT) and the end of the rinse-tube DT 500/16 (connected to the right side of the TWV) into the waste vessel.

2) Open the LDU control .

3) Switch the TWV to the rinse-tube (right side)

4) Start purging the system with a click to the Purge Button.

5) Shortly before the syringe is empty (the piston of the ES 11 reaches his upper position) switch the TWV to the valve (left side).

6) When the syringe is empty (the piston of the ES 11 reaches his lower position) switch the TWV to the rinse-tube (right side).

7) Repeat the steps 1 to 6 until no air bubbles are visible in the syringe or the tubes. When all air bubbles are out of the system you can stop the purging and switch the TWV to the valve (left side).

To syringe

Right side to drain syringe

to waste

Left side to fill syringe from bottle

Fig. 183: Use of the TWV



8) Fix the needle of the dosing tube DT 500/04 (Valve/Syringe — DCAT) inside the DCAT to the TH 70 or TH 50 (Tube Holder).

9) Remove the waste vessel.

• Fill the sample vessel (e.g. GS CMC) with the surfactant solution.


• Put the clean probe (e.g. small Du-Noüy ring RG 10) into the options holder.



• Start the CMC measurement with a click to the button in the dialog ‘File directories’. The measurement is carried out automatically. You can stop the measurement at any time without loosing the so long measured data with a click on the Stop-button .

Keep an eye on the first whole measurement especially at the start. Please check if the surface of the liquid is correctly detected. This will be visible by the



The CMC project will carry out the pre-defined number (steps) of single SFT measurements on the same sample (surfactant solution) but with a decreasing concentration (as defined in the dialog ‘Measurement — Concentration Wizard’). The concentration will be decreased (manually or automatically by a LDU or a Dosimat) before the respective single SFT measurement will start. Every single SFT result will be stored and printed (if selected) at the end of the respective measurement.

• The following procedure will be carried out for every single step of the CMC project: 1) Optional the pre-calculated amount of liquid will be extracted from the sample

vessel, after the liquid was mixed for the defined time (see dialog Liquid Extraction).

2) The pre-calculated amount of solvent will be added. When the variation Manual (Solvent) was selected you will be prompted to add the calculated

amount of solvent.

3) The magnetic stirrer will mix the liquid in the vessel for the defined time.

4) After the wait time the sample stage will move up.

5) The measurement of the SFT will be done.

6) During the single SFT measurement the results will be shown in a graph.

7) The results will be stored in a result file. To the defined name the step number will be added automatically (e.g. cmc-test003.mea).

8) The results (SFT) were entered in the data table of the analysis window.

9) The sample stage will move down.

Fig. 184: GS CMC


Fig. 186: Graph during single SFT measurement


These steps (1 – 9) will be repeated until all defined single SFT measurement steps are done.

• At the end of the CMC project the options holder clamp must be closed: DCAT 11: Fix the clamp of the options holder by turning the correspondent knob on the left side of the DCAT 11 clockwise. DCAT 21: Make sure that the options holder clamp is closed.

• Clean the complete dosing system (syringe, tubes, valves, bottle, and vessel) thoroughly before you use it again. An easy way to clean is to purge the system.

Fig. 187: Results and graphic in the data analysis window

Data Analysis—CMC Determination


7 Data Analysis

7.1 CMC Determination The analysis of a CMC project will be done in the CMC Determination Window.

You open a new one with the menu File — New — Data Analysis — CMC Determination. This window is divided in two parts, the graphic and the data part.

In the graphic part of the window the measured data will be displayed and on the left side of the window you find the icons for analyzing the CMC.

draw line c < CMC Click this icon and draw with the mouse cursor (first

click defines the first point of the straight line the second click the second one) a ‘best fit straight line’ for the part of the SFT curve smaller than the CMC (before the kink in the curve).

draw line c > CMC Click this icon and draw with the mouse cursor (first

click defines the first point of the straight line the second click the second one) a ‘best fit straight line’ for the part of the SFT curve higher than the CMC (after the kink in the curve). If the second point of this line is set the results will be calculated.

select range c < CMC Click this icon and define the range for the part of

the SFT curve smaller than the CMC (before the kink in the curve).

Fig. 188: File — New — Data Analysis — CMC Determination

Fig. 189: Measurement data and graphic


select range c > CMC Click this icon and define the range for the part of the SFT curve higher than the CMC (after the kink in the curve). If this second range is set the results will be calculated.

auto fit Click this icon to determine the CMC automatically.

clear marks Click this icon to clear all defined marks (lines or

ranges).




Data For the different data curves you can define the Title, the Line Style and Symbol. You can also change the label of the data curves in the field Change Title . The changed label will be shown in the dialog Graph Control, in the dialog Graph and in the diagram.

The data part of the window is a tabbed dialog box. This means that the content of the box differs depending on which tab you have selected.


Data In this tabbed dialog you see all the SFT results with additional data (concentration, temperature, and added volumes) in a table form. You can define which rows were included into the fit of the CMC. To mask out a row which you don’t want to be included into the calculation, just click onto the number cell in the result table. The number of the masked out results will be set into parentheses. With a second click onto a masked (parenthesized) number it will be again included into the calculation.

Fig. 190: Graph of CMC Determination

Fig. 191: Dialog Data

Data Analysis—CMC Determination


Preferences In this tabbed dialog you can select preferences for the analysis.

Calc. Settings Here you define calculation setting.

No. of Stochiometric Units Chose between non-ionic surfactants (1) and ionic surfactants (enter 2)

Temperature Select the temperature you want to use.

Options Here you can activate different options.

Auto Calculation Activate this check box for automatically determine the CMC.

Assume constant SFT for c > CMC Activate this check box to assume that the SFT is constant after reaching the CMC.

Hide Error Bars Activate this check box to disable error bars in the graph.

Change substance properties… Click this button to change the substance properties.

Results In this tabbed dialog you can seethe results of the analysis.

Surface Parameters

CMC The Critical formation concentration.

∆G Gibbs free energy of adsorption ∆G = RT ln⎝⎜⎛

⎠⎟⎞CMC

molarity of solvent

Γ surface excess Γ = - 1

RT dσ

dlnc for non-ionic surfactants

Γ = - 1

2RT dσ

dlnc for ionic surfactants

A Surface Area of surfactant molecule A = 1

ΓNA (NA = 6.022 1023 mol-1)

Also the temperatures will be displayed.

Fig. 192: Dialog Preferences

Fig. 193: Dialog Results


Substances In this tabbed dialog you can enter parameters of the substances and select the unit for the concentration.

Solvent: You can enter the Name, Molar mass, Density, and Start Concentration (for liquid A and B) of the solvent (receiver liquid).

Surfactant: You can enter the Name, Molar mass, Density, and Start Concentration for the surfactant solution.

Surfactant B with constant conc.: You can enter the Name, Molar mass, Density, and Start Concentration for the surfactant B whose concentration was hold constant during the CMC project.

Initial volume in vessel: Volume of the receiver liquid in the sample vessel at the beginning of the project.

Fig. 194: Dialog Results

Data Analysis—Analysis


7.2 Analysis of surface free energy The calculation of the surface free energy of solids will be done in the SE Surface Energy Window. You can open a new SE Analysis window with the menu File — New — Data Analysis — SE Analysis. The layout of the window depends on the selected calculation method. You can select one of the following methods in the menu Method. The given applications and examples are meant as a rule. A more detailed investigation of the applicability for the analyzed system might be necessary.

Fig. 195: File — New — Data Analysis — SE Analysis

Table : Application examples for different analysis methods

Method Information Min. No. of Fluids

Application Examples

Zisman critical surface tension 2 non-polar solids PE, PTFE, waxes Fowkes disperse parts of surface energy 1 non-polar systems PE, PTFE, waxes OWRK (Owens-Wendt-Rabel and Kaelble)

disperse and polar parts of surface free energy

2 universal polymers, aluminum, coatings, varnishes …

Extended Fowkes disperse, polar and hydrogen parts of surface free energy

3 specific questions of surface properties

plasma or corona treated polymers

Wu (Harmonic Mean)


2, at least one polar fluid

low energetic systems

organic solutions, polymers, organic pigments

Acid-Base Theory disperse, acid and base parts of surface free energy

3 specific questions of surface properties

biological system

Equation of State theory

surface free energy 1 universal polymers, aluminum, coatings, varnishes …

Schultz 1 (Polar Drop Phase)


2 high energetic system

metal, glass

Schultz 2 (Polar Bulk Phase)


2 high energetic system

polymers, aluminum, coatings, varnishes …


With the Browse... button you can select the liquid database.

Select the liquid you had measured the contact angle in the combo-box Liquid or type in the name and the parameters of the surface tension and their components if not found in the liquid database. Now you must enter the measured contact angle manually.

The choice of liquids depends on the selected analysis method. Only if all necessary parameters for the analysis method are available in the database the liquid is available in the combo-box Liquid.

With the + button you add the liquid with his SFT (and its components) and the con-

tact angle to the liquid list. If you have entered the minimum number of liquids (see table above) you can calculate the surface free energy (and its components) by a click on the Calculate-button. The calculate button is set inactive if any of the necessary data is missing. After the calculation is finished, the surface free energy and a corre-sponding graph is displayed

Fig. 196: Dialog SE – Surface Energy

Data Analysis—Result Collection


7.3 Result Collection To compare results from different measurements you can use the Result Collection window. Open a new window with the menu File — New — Data Analysis — Result Collection.

You can transfer data to a Result Collection Window by selecting the data in the tabbed dialog ‘Graph’ in every single measurement window and then choose ‘Transfer to active Result Collection Window’ from the context menu.

The Result Collection Window is divided in a data part (with a table) and the graph part.

You can delete rows from the table in the context menu.

You can adjust the layout of the graph with a right mouse click in the context menu Properties:

General In this dialog you can define the Form, the Fill Color and Size of the measuring points and the Border and Line Color and Weight for the intermediate lines for the graphic for every curve.

Scaling In this dialog you can define the scaling parameters for the graph.

Labels In this dialog you can enter the labels for the graphic.

Fig. 197: Export of data to active Result Collection

Fig. 198: Export of data to active Result Collection

Fig. 199: Context menu Properties General

Fig. 200: Context menu Properties Scaling


7.4 Adhesion The analysis of the work of adhesion (wetting envelope) will be done in the Adhesion Window.

Open a new window with menu File — New — Data Analysis — Adhesion.

Find below a working example for input of data using the default settings under parameters:

Two liquids ‘Red Ink’ (Liq. 1) and ‘Blue Ink’ (Liq. 2) are analyzed depending on the surface energy of the solid. You can verify in the diagram that both liquids are close to the optimum line and both within the tolerance lines, but the red ink is beyond the 30°-wetting envelope whereas the blue ink is within the 0°-wetting envelope, i.e. that the blue is totally spreading.

The optimum line corresponds to the minima of the iso-lines of the adhesion work, i.e. on the optimum line are those points where the liquid’s surface tension has a minimum respectively the polar contribution of a liquid that is where the

adhesive force has a maximum. For a full discussion see our application note 14 ‘Determination of the maximum adhesion work of certain liquids’

The procedure for getting a diagram like the above is the following:

• Input of the parameters of the solid surface (Surface Energy an its dispersive and polar parts)

• Input of at least one liquid to analyze (if more rows are present than needed, and then delete the needless rows by selecting ‘Delete rows’ in the context menu).

• Press ‘Calculate’

If you want to analyze more liquids than rows are displayed, then insert rows at first by using the context menu.

You may change the appearance of the diagram by right clicking in the diagram for popping up the menu ‘Properties’. You can change for example the symbol for the liquids by dropping down the combo box ‘Curve No.’ and choose ‘Liquids’. Then select a form, the colors and the size of the new symbol and press ‘Apply’.

Fig. 201: Data and graphic of Work of Adhesion

Fig. 202: Context menu Edit

Fig. 203: Context menu Properties…

Optional accessory


8 Optional accessory

8.1 Plates PT 11 – Wilhelmy plate for the measurement of surface and interfacial tension (Part. No. 2000323) according to DIN 53914 made of Platinum-Iridium (Length: 10 mm, Width: 19.9 mm, Thickness: 0.2 mm)

PT 9 – Wilhelmy plate for the measurement of surface and interfacial tension (Part. No. 2000446) according to DIN 53914 made of Platinum-Iridium (Length: 10 mm, Width: 9.95 mm, Thickness: 0.2 mm)

PT 10 – Cylindrical plate for 0.2 ml sample volume for the measurement of surface and interfacial tension (Part. No. 2000324) made of Platinum-Iridium (Inner diameter: 6.2 mm, Outer diameter: 6.6 mm, Cylinder height: 10 mm)

8.2 Du-Noüy rings RG 11 – Du-Noüy ring for the measurement of surface and interfacial tension (Part. No. 2000321) according to DIN 53914 made of Platinum-Iridium (Height: 25 mm, ∅: 18.7 mm, Thickness:0.37 mm)

RG 10 – Du-Noüy ring for down to 0.2 ml sample volume for the measurement of surface and interfacial tension (Part. No. 2000322) made of Platinum-Iridium (Height: 6 mm, ∅: 10 mm, Thickness: 0.3 mm)

8.3 Liquid Dispense unit LDU Accessory for the precise dosing of liquids into the sample vessel of the DCAT, e.g. for concentration rows, as well as for the automatic, software controlled refilling or rinsing of the dosing syringes. Motor-driven and software controlled, connectable to the Dynamic Contact Angle Measuring Device/Tensiometers DCAT 11 and DCAT 21.

Four different types of the LDU are available:

• LDU 1/0 (Part. No. 2000440) with one ES 11

• LDU 2/0 (Part. No. 2000467) with two ES 11

• LDU 1/1 (Part. No. 2000468) with one ES 11 and one RRS 11

• LDU 2/2 (Part. No. 2000469) with two ES 11 and two RRS 11

The electronic syringe module ES 11 includes one gastight 500 µl precision syringe DS 500/GT and one dosing tube DT 500/04 (Valve/Syringe — DCAT)

The refill and rinse system RRS 11 includes the electronic valve, one dosing tube DT 200/04 (Valve — Syringe), two dosing tube DT 500/16 (Valve — Bottle) and one Three-Way Valve TWV-LDU (very useful to drain air bubbles).

Fig. 204: PT 9; Pt 11 and Pt 10

Fig. 205: DIS 11; RG 11 and RG 10

Fig. 206: LDU 2/2


Attachments for the LDU

ES 11 - Electronic syringe unit for LDU (Part. No. 2000443)

DT 200/04 – PTFE dosing tube Valve — Syringe(Part. No. 8001405)

DT 500/04 - PTFE dosing tube Valve/Syringe — DCAT (Part. No. 8001404)

DT 500/16 - PTFE dosing tube Valve — Bottle (Part. No. 8001406)

DS 1000/GT - 1000 µl precision syringe DS 1000/GT (Part. No. 6000006)

DS 500/GT - 500 µl precision syringe DS 500/GT (Part. No. 6000005)

TWV-LDU Three-way valve for LDU (Part. No. 8003182)

The LDU is designed for the precise dosing/siphon of liquids into/from the sample vessel of the DCAT, e.g. for concentration rows, the CMC determination as well as for the automatic, software controlled refilling or rinsing of the dosing syringes.

The left ES 11 (and his refill valve) is called Unit A in the software SCAT and the right (the second one) is called Unit B.

8.3.1 LDU – control

The control of the LDU will be done with software SCAT in the dialog LDU .

Unit A or B In this both tabbed dialog you can enter the dosing parameters. For use with the CMC project you have to define only the dosing rate and the refill rate, the rest will be adjusted automatically by the wizard.

Syringe Type: You can select a syringe type out of the integrated syringe database in this list box; the corresponding fill volume will be shown in the text field on the right.

Auto Refill: Select this check box if you want the syringe to be refilled automatically.

Dosing Rate: Set the dosing rate by moving the slider left and right or by entering a value.

Refill Rate: Set the refill rate by moving the slider left and right or by entering a value.

Actions:

Add Defines the dispense or reverse dispense volume to be added in ml.

reversed Select to reverse the switching behavior of the valve and therewith it will reverse dispense instead of dispense.

A click on the Start button will dispense or reverse dispense (suck off) the defined value.

Refill A click on the Refill button will refill the syringe. Necessary if the ‘ Auto Refill’ is disabled or you want to dispense a special amount without refilling in between.

Run Continuous will dispense continuously the syringe until the Stop button is clicked.

Reset Syringe moves the piston holder of the selected electronic syringe module (A or B) to his lowest position (maximum filling volume) and resets the internal position

DT200/04 DT 500/04

DT500/16 TWV

Fig. 207: Attachments for LDU x

For second ES 11

For second RRS 11Syringe

DCAT

Bottle

Unit A

Fig. 208: LDU 1/1

Fig. 209: Dialog LDU – Unit A

Optional accessory


control. It is recommended to remove the syringe before resetting the syringe position.

Maintenance In this tabbed dialog you can control the LDU for each Slot A (Unit A) and Slot B separately.

Valve

Connect to Reservoir Switches the syringe to the bottle.

Connect to Sample Switches the syringe to the DCAT.

Purge Continuously drain (valve switched to sample) and refill (valve switched to reservoir) the syringe. This is useful to clean the complete system (valve, tube and syringe) or to get it free of air bubbles.

Refill To completely fill the syringe out of the reservoir.

Reset Syringe To reset the ES 11.

8.3.2 LDU – connections

All cable connections must only be closed or opened when the DCAT is switched off

• Connect the LDU with the delivered cable (marked LDU) to the socket SERIAL AUX on the back of the DCAT.

• Connect the electronic syringe module (or both) ES 11 to the front side of the LDU as shown in the figure beside.

• Mount the three-way valve TWV to the dosing syringe.

• Attach the tube DT 200/04 (Valve — Syringe) to the Syringe connector and to the left side of the TWV.

• Attach the Luer-lock side of the tube DT 500/04 (Valve/Syringe — DCAT) to the DCAT connector and fix the side with the needle inside the DCAT to the TH 70 or TH 50 (Tube Holder).

• Attach the first tube DT 500/16 (Valve — Bottle) to the Bottle connector and dip the other side into the bottle.

• Attach the second tube DT 500/16 (Valve — Bottle) as a rinse-tube to the right side of the TWV and dip the other side into a waste container (e.g. GS 50).

Fig. 210: Dialog LDU - Maintenace

DCAT

TC 250

Fig. 211: Back view of LDU

Syringe

DCAT

Bottle DCAT

Syringe

Bottle

Fig. 212: Connections to the valves

To syringe

DT 500/16to waste

DT 200/04from valve

Fig. 213: Connections to the TWV


8.4 Kit for powder measurement PUR 11 Accessories kit for the measurement of the contact angle of powder samples and for the measurement of adsorption and wetting behavior of powder samples (Part. No. 2000333) only useable with the optional software SCAT 32.

Consisting of one special adapter made of aluminum for the DCAT 11/21 and one sample vessel made of glass

Additional available for use with the PUR 11:

GT 11 (Part. No: 2000436 ) Set of five sample vessels made of glass for the measurement of adsorption and wetting behavior of powder samples

FP 11 (Part. No: 2000406 ) Filter paper for GT 11; Set with 100 pieces

8.5 Fiber holder FH 11 Fiber holder to determine the wetting behavior of adsorbing materials like powders, pigments, fibers and fiber bundles (Part. No. 2000408) only useable with the optional software SCAT 32.

Consisting of one special adapter hard gold-plated

Additional available for use with the PUR 11:

FP 12 (Part. No: 2000409 ) Filter paper for FH 11; Set with 100 pieces

8.6 Single fiber holder FH 12 Fiber holder to determine the wetting behavior of wettable materials like single fibers or hairs (Part. No. 2000441) only useable with the optional software SCAT 32.

Consisting of one special adapter

Additional available for use with the FH 12:

8.7 Plate options holder PSH 11 Special options holder for solids in plate form, to determine the wetting behavior of wettable materials like solids in plate form (Part. No. 2000407) only useable with the optional software SCAT 31 and SCAT 32.

Consisting of one special adapter made of aluminum

Fig. 214: FH 11 + PUR 11 with GT 11

Fig. 215: FO 11 and PSH 11

Optional accessory


8.8 Options holder for films FO 11 Special options holder for solids in film form, to determine the wetting behavior of wettable materials like solids in plate form (Part. No. 2000335) only useable with the optional software SCAT 31 and SCAT 32.


8.9 Penetrometer probe PP 11 Special probe for determine yield forces on soft gels, pastes etc. (Part. No. 2000445) only useable with the optional software SCAT 35.


8.10 Sedimentation cone SC11 Special probe for use in particle size and sedimentation rate analysis (Part. No. 2000444) only useable with the optional software SCAT 35.


8.11 Density determination set DIS 11 Special probe for the determination of the density of liquids (Part. No. 2000337) only useable with the optional software SCAT 34.

Consisting of one probe made of silicone and one special holder for it made of Platinum-Iridium.

8.12 Adapter for small sample vessels Special adapters for small sample volumes to measure with small probes like the Wilhelmy plate PT 9, the cylindrical plate PT 10 or the Du-Noüy ring RG 10.

ADAPT 70 – Adapter (Part. No. 2000331) for GS 50 and SV 10 to be hold in the temperature controlled receptacle TV 70 made of aluminum

ADAPT 50 – Adapter (Part. No. 2000453) for and SV 10 to be hold in the temperature controlled receptacle TV 50 made of aluminum

SV 10 – Sample vessel for small sample volumes to measure with small probes like the Wilhelmy plate PT 9, the cylindrical plate PT 10 or the Du-Noüy ring RG 10 (Part. No. 2000454) for GS 50 and SV 10 to be hold in the temperature controlled receptacle TV 70 made of aluminum

Fig. 216: PP 11 and SC 11

Fig. 217: DIS 11

Fig. 218: ADAPT 70 and 50 with SV 10


8.13 Sample vessels GS Sample vessels made of borosilicate glass or PTFE to measure in the temperature controlled receptacle TV 70, TV 50, TV 100 or TV 70-NM.

GS 50 – Set of 6 sample vessels made of borosilicate glass (Part. No. 2000325) ∅ 50 mm

GS 50P –One sample vessels made of PTFE (Part. No. 2000404) ∅ 50 mm





8.14 Diffusion reducers CP Cover plates for the sample vessels made of temperature resistant plastics (POM polymer) to reduce the diffusion.

CP 50 –One set of cover plates (Part. No. 2000328) ∅ 50 mm



8.15 Ring aligning tool R-AT Ring aligning tool for reorienting the Du-Noüy ring RG 11 (Part. No. 2000332) made of aluminum.

8.16 Inert gas appliance GTR 70 Special sample vessel made of borosilicate glass to measure in the temperature controlled receptacle TV 70 or TV 70-NM under inert gas atmosphere.

Consisting of one special sample vessel made of borosilicate glass and cover plates with inert gas connector

Fig. 219: Sample vessels and diffusion reducer

Optional accessory


8.17 Non-magnetic liquid thermal unit TV 70-NM Optional non magnetic liquid thermal unit TV 70/NM for factory-made installation in a DCAT 11 or DCAT 21. Connectable to a liquid bath circulator (like the cryostat F25 ME)

Consisting of: • Thermal chamber for mounting the optional sample vessel GS 70 • one sample container, diameter 70 mm made of borosilicate glass • Housing of MES 21 • Micro-Electronic Stirrer MES 21 (Super flat removable magnetic stirrer without any

motor), sealed and chemical resistant

Technical data: • Temperature range: -10 ...130 °C • Heat up and cool down rate and accuracy of the temperature is depending on the

thermostat • Mounting for sample vessels: 70 mm diameter • Removable Micro-Electronic Stirrer with continuous speed control • Material:

- Chamber made of brass, hard gold-plated - Sealing made of Viton - Housing of Micro-Electronic Stirrer made of POM polymer

• Weight: 1.0 kg

Fig. 220: TV 70-NM


8.18 Temperature control unit TEC 250/DCAT Electrical temperature control unit – Only usable in combination with the DCAT 21 (Not with the DCAT 11). For measurements below or above room temperature, e.g. for measuring of resins, hot melt adhesives and solders, as well as under protective at-mosphere. Needs the temperature controller TC 250. The temperature setting can be done manually or software controlled. All software dependent functions in combination with the optional software packages SCAT xx only.

Features of the TEC 250/DCAT

• Thermal chamber with two fixed and two removable windows made of special optical glass

• Connector for inert gas

• Two resistance thermometers Pt 100 as measuring and control sensor

• Exchangeable sample vessel made of aluminum

• Temperature range: Room temperature...250 °C; ±0.2 K

• Heating rate: 1 K/s

• Diameter of sample container: 50 mm

• Weight: 1.0 kg (without controller)

Installation –Move the lift of the DCAT 21 to his lowest position (with the down key ). Open both plastics doors of the DCAT 21 completely. Insert the TEC 250/DCAT into the TV 70 (it fit only into the TV 70 not in another receptacle). If you want to measure the temperature in the vessel you can connect the Pt 100 plug to the rear of the DCAT 21. Connect the connection cable and the temperature sensor to the corresponding sockets on the TC 250. Connect the inert gas onto the back of the TEC 250/DCAT.

Operation – The manual temperature setting will be done directly on the temperature controller TC 250. Below the display with the actual value and the setting value, there are three silicone rubber buttons. The left button is for selecting the operation mode and to program and is normally out of function. The button will increase and the button will decrease the set temperature (if you press it longer the change of the set value becomes faster and faster). Before you start with the measurement be sure that the desired temperature is balanced. Insert the test liquid into the sample vessel and then the sample vessel into the receptacle of the TEC 250/DCAT. Now you can perform the measurement in the usual way.

An active red alarm LED it indicates that the controller states an irregular condition and is switching of the heating power. If you have eliminated the fault (e.g. a senor break), you need to reset the controller by switching off and on.

Some accessible surfaces can become very hot. Therefore, please wait until the system has cooled down sufficiently and the temperature allows you

to touch the system without danger, or use specific hand protectors.

Fig. 221: TEC 250/DCAT with accessories

Fig. 222: TC 250

A1 A2 PV °C °F

SV

OUT

Fig. 223: Build in temperature controller KS 20i

Optional accessory


9 Maintenance

9.1 General The DCAT is continuously rated.

Internal work on the unit must only be done when the power supply is disconnected and the mains cable has been pulled out!

If the unit has a fault, please turn to the service departments of our representations or to ourselves directly at:

DataPhysics Instruments GmbH Raiffeisenstraße 34

D-70794 Filderstadt

Tel. ++49 (711) 770556-0 Fax ++49 (711) 770556-99 email [email protected]

9.2 Cleaning of instrument The coat of varnish of the DCAT is resistant to the most common solvents and weak acids, except the both windows. To clean the housing, use a dry, clean, soft, and fluffiness cloth. With heavy dirt on the housing, use a neutral cleaning liquid on a soft cloth.

Do not use any chemical products like strong solvents or acids to clean the housing. Make sure that no liquids get into the inside of the housing (for example by means of the connecting socket on the side of the DCAT). This leads to the destruction of the unit and can lead to a hazardous short circuit. The windows are made of plastics and must only be cleaned with water or a special plastic cleaner.

9.3 Device not reacting If it happens that the DCAT doesn’t react at all, please switch off the DCAT check all cable connections and carry out a Reset by pressing both keys on the DCAT simultaneously. In the display should appear the word Reset instead of Idle.

If the DCAT doesn’t react at all please consult your sales partner.


10 Appendix

10.1 Technical data

Measuring range contact angle • 0...180°; ± 0.01°( at 90° will be no wetting force)

Measuring range surface tension

• DCAT 21: 1…1 000 mN/m; ± 0.0o1 mN/m

• DCAT 11: 1…1 000 mN/m; ± 0.01 mN/m

Measuring rate • max. 30 weighing values per second; for adsorption measurement: max. 50 weighing values per second

Weighing range • 10 µg...210 g

Lifting speed • DCAT 21: 0.7 µm/s...500 mm/min

• DCAT 11: 2 µm/s...60 mm/min in measuring mode; 400 mm/min rapid travel for init mode

Position resolution • DCAT 21: 0.1 µm

• DCAT 11: 1 µm

Lifting range • DCAT 21: 105 mm

• DCAT 11: 74 mm

Sample size • max. weight: approx. 200 g

• max. diameter/length: approx. 80 mm / DCAT 21/11: 110 mm/90 mm

• min. fiber diameter approx. 10 µm (approx. 3 µm with special receiver)

Temperature range • -10…130 °C

Temperature measurement • 2 Pt100 input channels with -60...450 °C (Pt100 optional), 0.01 K resolution; 1/3 DIN IEC 751 (± 0.03 %), class B

Receptacle for sample vessel • optionally 50 mm, 70 mm or 100 mm diameter

Size of instrument (LxWxH) • . DCAT 21: 340 x 230 x 565 mm

• . DCAT 11: 340 x 230 x 500 mm

Weight • . DCAT 21: 25 kg

• . DCAT 11: 23 kg

Power supply • 100 … 240 VAC; 50 … 60 Hz; 55 VA

Appendix


10.2 Terms of Guarantee DataPhysics guarantees the faultless functioning of this unit provided it is used and serv-iced appropriately and is connected and handled in accordance with these operating instructions.

The guarantee is for two years from the date of delivery.

The place of the guarantee fulfilling is the respective representative or DataPhysics in Filderstadt, Germany

All guarantee and damage claims of the customer are forfeited if he has improperly treated the supplied unit or has supplemented or worked on it or given it to a third party for subsequent reconditioning without our prior approval.

DataPhysics entire liability and your exclusive remedy shall be at DataPhysics option, either a) return of the price paid or b) repair or replacement of the unit that does not meet DataPhysics limited guarantee and is returned to DataPhysics together with a copy of the receipt. This limited guarantee is void if failure of the unit has resulted from acci-dent, abuse, or misapplication. Any replacement delivery will only be warranted by Data-Physics for the remainder of the original guarantee period or 30 days, whichever is longer.

DataPhysics disclaims all further warranties with respect to the unit, and the accompa-nying manuals and written materials.

DataPhysics and its suppliers shall not be liable for any damages whatsoever (including, without limitation, damages for loss of business profits, business interruption, loss of business information, or other pecuniary loss) arising from the use or inability to use this DataPhysics product, even if DataPhysics has been advised of the possibility of such dam-ages. In any case, DataPhysics entire liability shall be limited to the amount actually paid by you for this product. This limitation does not apply to damages which were caused by DataPhysics on intent or by gross negligence. Likewise, claims remain unaffected which are based on mandatory legal rules regarding product liability.

Furthermore, the guarantee conditions of the ‘General conditions of supply for products and services of the electrical industry’ of the ‘Zentralverband Elektrotechnik- und Elek-tronikindustrie (ZVEI) e. V., Stresemannallee 19, D-60596 Frankurt am Main’apply.


10.3 Requirements of the mains cable The power supply of the DCAT 21 enable operation at a voltage supply with 90 … 264 Volts Alternating Current (43 … 60 Hz).

The mains cable delivered with your DCAT 21 may not meet the requirements of the coun-try in which you are using the system.

You must, without fail, use a mains cable which meets the requirements of the relevant country or the local Electricity Board.

The following information explains the requirements which are to be taken into account when choosing a mains cable.

General information

∗ The mains cable must be permitted (authorized) for the country in which it is used.

∗ The mains cable should be at least 2m and at most 3m long.

USA and Canada

∗ The mains cable must have the UL release and the CSA certificate

∗ For the cable, the following minimum requirements apply:

− No. 12 AWG; 3.2 mm2; outer 10.9 mm2

− Type SV or comparable

− 3 phase

∗ The cable must have a nominal current-carrying capacity of at least 20 A.

∗ The mains plug must be shock proof plug of the type NEMA 5-15P (15A, 125V) or NEMA 6-15P (15A, 250V).

Other countries

∗ The connectors of the mains cable must carry the approval certificate of the respec-tive country (see table below):

BSI (Great Britain) NEMKO (Norway)

CEBEC (Belgian) OVE (Austria)

DEMKO (Denmark) SEMKO (Sweden)

EANSW (Australia) SETI (Finland)

IMQ (Italy) SEV (Switzerland)

KEMA (Netherlands) UTE (France)

VDE (Germany)

∗ The cable must be a three-phase HAR cable of the type HO5VV-F3 with a minimum

phase-diameter of 2.5 mm2 .

∗ The mains cable must have a minimum current-carrying capacity of 20 A and accord-ing to the country, have a nominal voltage of 125 V or 250 V Alternating current.

Appendix


Japan

In Japan the following cable types and connected loads are required:

∗ All parts of the cable (cable, box, and plug) must have the trademark and the registry number according to the Japanese Dentori Law.

∗ The following minimum requirements apply to the cable:

− 3.2 mm2

− Type VCT or VCTF

− 3 phase

∗ The cable must have a nominal current-carrying capacity of at least 20 A

∗ The mains plug must be a 2 pin shock-proof plug according to the Japanese Industrial Standard (15A, 125V).


10.4 Declaration of conformity

EG-KONFORMITÄTSERKLÄRUNG DECLARATION OF CONFORMITY DÉCLARATION DE CONFORMITÉ

Wir bestätigen, daß das Produkt / We confirm that the product / Nous confirmons que le produit

Dynamic Contact Angle Meter and Tensiometer DCAT 11 and DCAT 21

den Schutzanforderungen entspricht, die in der EU-Richtlinie 89/336/EWG zur Angleichung der Rechtsvorschriften der Mitgliedsstaaten über die Elektromagnetische Verträglichkeit festgelegt sind. / is in conformity with the EC directive 89/336/E.E.C. according to the Electromagnetic Compatibility. / est conforme aux obligations de protection définies dans la directive C.E. 89/336/C.E.E. pour une harmonisation des prescriptions des états membres relatives à la compatibilité électromagnétique.

Diese Erklärung gilt für alle Exemplare, die nach den anliegenden technischen Unterlagen - die Bestandteil dieser Erklärung sind - hergestellt werden. / This declaration is valid for all products which are produced in accordance with the technical documentation which is part of this declaration. / Cette déclaration est valable pour tous les exemplaires qui ont été fabriqués selon les documents techniques ci-joints faisant parties intégrantes de cette déclaration.

Zur Beurteilung des Erzeugnisses hinsichtlich der Elektromagnetischen Verträglichkeit wurden die folgenden Vorschriften angewendet: / For verification of conformity with regard to Electromagnetic Compatibility the following standards are applied: / Pour la vérification du produit en regard de la compatibilité électromagnétique, les prescriptions suivantes ont été appliqués:

• EN 50081-1 (1992) Fachgrundnorm Störaussendung (Wohnbereich)

Generic emission standard, residential environment

Norme générique émission, environnement résidentiel

• EN 50082-1 (1993) Fachgrundnorm Störfestigkeit (Wohnbereich)

Generic emission standard, residential environment

Norme générique émission, environnement résidentiel

Diese Erklärung wird verantwortlich für den Hersteller: / This declaration is given under sole responsibility of: / Cette déclaration engage le constructeur:

DataPhysics Instruments GmbH

Raiffeisenstrasse 34

D-70794 Filderstadt

abgegeben durch: / from: / émis par:

Herrn /Mr. /M. Torsten Holz

Entwicklungsleiter / Development Manager / Directeur développement

D-70794 Filderstadt 03 - 09 - 1999 Unterschrift / Signature

V is it us i n th e I nt e r n et u n d e r ht t p : / / w ww .d a t a p h y s i cs .d e

DataPhysics Instruments GmbH • Raiffeisenstraße 34 • D-70794 Filderstadtphone ++49 (0)711 770556-0 • fax ++49 (0)711 770556-99 email [email protected] • internet http://www.dataphysics.de

Tech

nica

l inf

orm

atio

n in

this

docu

men

t is s

ubje

ct to

chan

ge.

Copy

right

© 19

98 D

ataP

hysi

cs In

stru

men

ts G

mbH

, Fild

erst

adt.

i

s a re

gist

ered

trad

emar

k of

Dat

aPhy

sics I

nstr

umen

ts G

mbH

. TD

/DC

AT-

3.0

/E

Y o u r s a l e s p a r t n e r :