DSA4. Software for Drop Shape Analysis. User manual part 1: Installation, introduction, working in standard mode V2.0-02

Transcription

1 DSA4 Software for Drop Shape Analysis User manual part 1: Installation, introduction, working in standard mode V KRÜSS GmbH, Hamburg

2

3 Contents page 1 Contents 1 Introduction Standard mode Expert mode Explanation of symbols Technical customer service Installation Note Carrying out the installation General information on using the program Selecting program functions Context menus Keyboard control Starting the program Selecting standard or expert mode Introduction to the DSA4 software Explanation of terms The program desktop Overview Tabs in the video and results window Control Panel (CPanel) Command icons Main toolbar Toolbar above the CPanel Keyboard control of the instrument Illumination List of shortcut keys General measurement and data processing procedure Measurement Data processing The Control Panel (CPanel) Tasks... 25

4 page 2 Contents 5.2 Overview General use of the software Entering values Saving settings Image settings (O-Con tab) Sample table positioning (Axes tab) Sample table control Saved sample table positions (Set as ) Axis movement modes Initialising an axis Speed of movement (Velocity) Axis options (Options) Syringe selection and dosing Dosing mode and dosing volume Filling a syringe Emptying, rinsing and resetting syringes (Tools) Needle positioning (N-Pos) Automatic needle positioning (auto scan) Saving needle positions Information applicable to all measuring methods Starting and stopping measurements Starting a complete measurement sequence Starting an evaluation of the live image or a loaded image Individual evaluation Video image options and image setup Switching between live image and still image Saving and loading an image Adjusting the focus with the help of the Focussing Assistant Criteria for a good drop image Defining the evaluation range (Region of Interest; ROI) Measuring and contour lines Lines used for Sessile Drop and Pendant Drop Lines used only for Sessile Drop Lines used only for Pendant Drop Preparing a contact angle measurement Selecting the drop type Selecting the method for analysing the drop contour... 48

5 Contents page Positioning and lens settings Adjusting the dosing (for software-controlled dosing unit only) Measurement sequence settings (Mode tab) Start Measurement Drop deposition (Deposition) Choosing between measurement and video recording (Measurement Mode) Measurement period and measurement rate Determining the baseline (Baseline, Detection) Choosing the drop liquid to be used Using the Height-Width (Manual) method Special features of Captive Bubble measurements Preparing a surface tension and interfacial tension measurement Selecting the drop type Determining the needle diameter Measurement sequence settings (Mode tab) Start Measurement Choosing between measurement and video recording (Measurement Mode) Measurement period and measurement rate Entering the needle diameter Entering the density Positioning and lens settings Depositing drops Determining the scale of the image Excluding the upper part of the drop contour Recording, playing back and evaluating video Recording during a measurement sequence Frame rate and recording time Start options Manual recording Saving a video Saving a video retrospectively Saving the video automatically Loading a video Playing back a video Evaluating a video Preliminary settings Starting the evaluation... 70

6 page 4 Contents 10 Managing unsaved measurement data (Results Monitor) Creating series of measurements When starting an MT or SDM When starting an image or video evaluation For a single image measurement Changing the displayed table columns Changing for the current software session only Changing permanently Copying the contents of a table to the clipboard Mean value calculation Displaying charts (RTPlotView) Selecting series of measurements Changing the axis assignment Show legend Displaying diagram in a new window Saving measured data in the database The results database (Results-DB-Explorer) Database structure Database management Creating a new database Opening a database Workspaces Creating a workspace Copying a project to a Workspace Managing Workspaces Moving a measurement to another project Projects and measurements Editing a project Displaying measurements Changing the liquid entry for a measurement retrospectively Exporting all measurements for a project Charts Creating a chart Changing the scale Buttons on the chart toolbar Creating a report General report options (Report Settings tab)... 89

7 Contents page Incorporating a chart (Chart Selection tab) Changing displayed table columns (Table Properties tab) Creating a report Evaluations Information for all evaluation methods Selecting measurement series Changing the displayed table columns Settings for calculating mean values and eliminating outliers Report of an evaluation Calculating the surface free energy Entries and selection options (CA tab) Result (Result tab) Liquid data (IFT tab) Wetting Envelope tab Mean values of contact angle for several drops (Value Analysis) Carrying out the Value Analysis Creating a chart (Chart tab) The substance database Opening the substance database Substance database structure Substance list Substance data Entries for interfacial and surface tension data (IFT-Items) Creating a new database entry Editing your own database entry Deleting your own database entry Creating a new IFT-Item System Settings and Miscellaneous Connector assignment; environment and system parameters (General tab) Changing the connector assignment for instrument components Environmental and system parameters (General Parameters area) Dosing unit options (Dosing tab) Syringe position assignment for software-controlled multi-dosing units Setting the image size and frame rate (Camera tab) Camera module for IEEE-1394 interface Camera module CF322x (high-speed option)

8 page 6 Contents 14.4 Various presets (Miscellaneous) Automatically load last open database on program start Saving / exporting messages automatically Switching prompts on and off Special instrument components Tilting tables Safety information for the internal tilting table Controlling and programming the tilt Dosing and starting the measurement Video evaluation for the PA3240/4240 internal tilting table DSA100M (Micro): Sample table control and dosing Controlling the PS3240 sample table Controlling a Piezo dosing unit DS Adjusting the humidity for HC Appendix I Entering the syringe dimensions for disposable syringes II List of quantities which can be displayed in the Results Monitor

9 SPA C SPA C SPAC SPAC Two-part manual for standard and expert mode SPAC SPAC SPAC SPAC SPA C SPA C SPAC SPAC Ref erence to oth er manuals You will find the necessary information relating to all the activities to be undertaken directly at the measuring instrument in the supplied measuring instrument manual. These r ange from set-up and installation via preparation for the measurement and preparation of the sample to maintenance and care. The DSA4 software functions which are used for the TVA100 top view distance measuring instrument are described in the TVA100 manual. SPA C SPA C SPAC SPAC Introduction page 7 1 Introduction The DSA4 software is the control and data management software for your contact angle measuring instrument. This manual describes the functional scope in standard mode. The DSA4 software can be used in standard mode or in expert mode. A two-part manual has been produced accordingly. Part 1: Installation, introduction, working in standard mode Part 2: Working in expert mode, DSA mapping editor, theory The description of expert mode is based on the standard mode. If you want to work in expert mode, please read Part 1 of the manual first and then Part 2. References to chapters and pages in the other manual refer to Version of the manual Standard mode A measurement in standard mode involves the manual or software-controlled dosing of a single drop with subsequent analysis and evaluation of the drop shape. In order to evaluate several measurements (e.g. for the calculation of mean values or surface energy), these are saved manually in a common project. Working in standard mode is suggested when The measuring instrument is mainly fitted with manual components. The nature of the sample, the problems and the measurement parameters change frequently Expert mode A measurement in expert mode can involve fully automatic, programmed measuring sequences with almost any number of drops and up to 8 test liquids. Working in expert mode is suggested when The measuring instrument is mainly fitted with software-controlled components. The nature of the sample, the problems and the measurement parameters recur frequently. Contact angle mapping of a sample is to be carried out.

10 page 8 Introduction 1.2 Explanation of symbols Certain symbols, which indicate the function of a text passage, are used in KRÜSS manuals: Information and tips Warning sign. For your own safety, please observe the sections marked with this symbol.! Important information, which if ignored can lead to measuring errors, loss of data or undesirable behavior of the software or the measuring instrument. Hints and tricks, information and explanations. Troubleshooting rectify or remove undesirable behavior of the software or the measuring instrument. Glossary - explanation of technical terms and terms used in the software or in the manual. Note which instrument or software components are required to use the functions described in the concerning chapter. Instructions Individual handling instructions. 1. Handling sequence, Step Handling sequence, Step Handling sequence, Step Structural assistance List of aspects. Reference to passages in this manual or other manuals.

11 SPA C SPA C SPAC SPAC SPA C SPA C SPAC SPAC Introduction page 9 Typography Terms and text citations from the software user interface are typographically emphasized. The names of keys of the computer keyboard are written between the symbols < >. Example: Press the <Esc> key. 1.3 Technical customer service If problems should occur when working with your KRÜSS product please consult the technical customer support at KRÜSS GmbH. You can contact them at: KRÜSS GmbH Technical customer support Tel: / Fax: / info@kruss.de

12 page 10 Installation 2 Installation You can skip this chapter if the software has already been installed by a KRÜSS engineer. For installing the DSA4 Mapping Editor please read Chapter 17.1 in the manual for expert. 2.1 Note! If a frame grabber board is used, it must be fitted and the driver must be installed before installing DSA4. A driver must also be installed for an IEEE-1394 camera ( Refer to instrument manual). 2.2 Carrying out the installation 1. Close all running applications with the exception of Explorer. 2. Insert the DSA4 CD. Open the DSAsetup directory. Start the Setup.exe program. 3. Welcome window and copyright information. Click Next. 4. Version information. Click Next. 5. Confirm the licence conditions. In order to continue you must accept the licence conditions with Yes. 6. Enter your user name under Name and your company name under Company. Click Next. 7. The registration data will be shown again for checking. Confirm with Yes or correct the entry with No. 8. Confirm the proposed installation directory with Next (recommended) or choose a different directory using Browse. 9.a Selecting the installed frame grabber or IEEE-1394 camera.

13 Installation page 11 9.b Selecting the camera type. This step is only necessary if a Falcon frame grabber is used. The standard camera type is T1C. This setting should only be changed if you use a camera that you have not obtained from KRÜSS. 10. Enter the name of the program folder as it is to appear in the Windows Start menu. The recommended folder name is: Drop Shape Analysis [DSA4]. 11. Check all the listed data and close the installation with Next. 12. Optionally: If you have selected the IEEE-1394 option in step 9, a dialogue box will appear to enable you to open a README file. Place a tick in the checkbox if you want to read the README file. In this case, close the subsequent page with Next. Otherwise, complete the installation with Finish. 13. Optionally: If you did not select the IEEE-1394 option in step 9, the computer must be restarted before the program is started for the first time. If this is not to take place automatically at the end of the installation then select the option No, I will restart my computer later. 14. Complete the installation with Finish.

14 SPA C SPA C SPAC SPAC SPA C SPA C SPAC SPAC SPA C SPA C SPAC SPAC page 12 General information on using the program 3 General information on using the program 3.1 Selecting program functions Context menus Many functions are assigned to so-called context menus. A context menu is opened with the right-hand mouse button. It contains menu entries that are required in connection with the particular screen element that has been clicked on Keyboard control Keys and key combinations are available for controlling motorised instrument components. You will find a list of the key commands on P Starting the program! The instrument must be connected up and switched on before starting the program. Some functions are only accessible when DSA4 finds the appropriate device components. Double-click on the desktop icon or select Drop Shape Analysis in the Windows start menu. Licensing A dialog for selecting a license file appears after the first software startup. Insert the mini CD provided. Select the root directory of the mini CD. Select the file DSASP.DAT. Click on OK. The product key will be copied into the installation folder of the DSA4 software.

15 SPA C SPA C SPAC SPAC SPA C SPA C SPAC SPAC SPA C SPA C SPAC SPAC General information on using the program page 13 You may quit the selecting dialog with Cancel and then run the DSA4 software with limited functionality. In this case you can carry out licensing subsequently with the help of the menu item Help Set License File. Note concerning the video image When the program starts, no camera is found and no video image is displayed: Check that the camera has been connected correctly ( Refer to instrument manual). IEEE-1394 cameras: Check that, as intended, the IEEE-1394 driver was installed before the IEEE-1394 card was fitted. Otherwise follow the instructions in the appendix of the instrument manual. 3.3 Selecting standard or expert mode Selecting the mode when starting the program for the first time When the program is started for the first time, a dialogue box will open for selecting the mode. Select the required mode. The selected mode will be opened every time the program is restarted. The selection dialogue box will not appear again. Changing the mode after the program has been started for the first time 1. Select Tools Run Mode from the menu. 2. Select the required mode. 3. Close the DSA4 software and then restart it. The selected mode will be opened every time the program is restarted.

16 SPA C SPA C SPAC SPAC page 14 Introduction to the DSA4 software 4 Introduction to the DSA4 software 4.1 Explanation of terms Sessile Drop: A drop lying on the surface of the solid for measuring the contact angle. Captive Bubble: An air bubble beneath a solid body in a liquid for measuring the contact angle. Pendant Drop: A drop hanging from a needle in a surrounding phase (a gas or another liquid) for determining the interfacial or surface tension from the drop shape. CPanel: Control Panel. Dialogue box for controlling software-controlled instrument components and for parameterizing and programming a measurement. 4.2 The program desktop Overview Menu bar Toolbars Video and results window Instrument control and measurement (CPanel) Measurement sequence event report Status line

17 SPA C SPA C SPAC SPAC SPA C SPA C SPAC SPAC Introduction to the DSA4 software page 15 Desktop elements can be hidden or shown with the View menu. The appearance of the desktop depends on the settings which were active when the program was last exited Tabs in the video and results window The video and results window on the left-hand side contains five tabs: ImageView Display of the video image and the measuring and contour lines used for a measurement Definition of the drop type and the measuring method with the help of the context menu Loading, playing back and evaluating videos

18 page 16 Introduction to the DSA4 software Results monitor Tabular presentation of measurement results before evaluation Transfer to a database with the help of the context menu RTPlotView (1 and 2) Diagrammatic presentation of measurement results before evaluation

19 SPA C SPA C SPAC SPAC SPA C SPA C SPAC SPAC Introduction to the DSA4 software page 17 Results-DB-Explorer Creation, presentation and administration of results databases Surface energy calculation Statistical evaluation Creation and printing of reports Control Panel (CPanel) Software-controlled instrument components are controlled by means of the Dosing, NPos, O-Con and Axes tabs ( Chapter 5). If certain software-control components are not available, the corresponding tabs will be inactive. Measurement settings are made on the Mode tab.

20 SPA C SPA C SPAC SPAC page 18 Introduction to the DSA4 software 4.3 Command icons The command icons are located in the main menu bar and in a menu bar above the CPanel. You can change the displayed buttons and toolbars from the toolbar context menu Main toolbar Button Function Creates a new results database Opens a file of the active window type Saves the contents of the active window Changes background settings for the measurement and system settings Opens the substance database (liquids, solids, gases). Switches between live image (left) and snapshot (right) Generates a snapshot Resets the timer to 0 (reset timer) Opens the Focussing Assistant Determines the image scale (pixels/mm) Determines and displays the baseline (for test measurements) Determines the drop shape according to the currently set analysis method (for test measurements) Single image analysis (for test measurements) Evaluates the live image or a loaded image with the current settings in the ImageView window and the CPanel or starts a video recording when this option is set

21 Introduction to the DSA4 software page 19 Video functions Button Function Record a video Play back a video Stops recording, playback or evaluation of a video Jump to the last Frame Jump to the first Frame Evaluate a video Toolbar above the CPanel Button Function Only active in expert mode: Create a new measurement template file (MT-file) Save the current measurement settings Change additional measurement settings Start a measurement sequence Liquid dosing according to the settings in the CPanel Reverse syringe plunger (reduce drop) 4.4 Keyboard control of the instrument For controlling, the referring software-controlled components (axes, dosing unit, optics) are required. Illumination and all motorised components of the instrument can be controlled directly via the keyboard. The <Ctrl> key is used in combination with a letter key to switch between the components to be controlled. The toolbar shows the item currently under key control. In most cases, control is carried out with <Ctrl> and the <Page Up>and <Page Down>keys.

22 page 20 Introduction to the DSA4 software Illumination The illumination is changed in single steps. The control key must be pressed several times. <Ctrl> + <i>: Switch to illumination control ("i" for "illumination") <Ctrl> + <Page Up>: brighter <Ctrl> + <Page Down>: darker List of shortcut keys Component Switch Control x-axis <Ctrl> + <x> <Ctrl> + <Page >: right <Ctrl> + <Page >: left y-axis <Ctrl> + <y> <Ctrl> + <Page >: back <Ctrl> +<Page >: front z-axis <Ctrl> + <v> <Ctrl> + <Page >: top <Ctrl> + Page >: bottom Syringe <Ctrl> + <s> <Ctrl> + <Page >: top <Ctrl> + <Page >: bottom : left : right Illumination <Ctrl> + <i> <Ctrl> + <Page >: light <Ctrl> + <Page >: dark Zoom <Ctrl> + <z> <Ctrl> + <Page >: larger <Ctrl> + <Page >: smaller Focus <Ctrl> + <f> <Ctrl> + <Page >: larger <Ctrl> + <Page >: smaller

23 Introduction to the DSA4 software page General measurement and data processing procedure This chapter describes the general working procedure. For the detailed procedure, please read Chapter 5 to Measurement 1. The Drop Type and the drop shape analysis method (Comp. Method) are selected in the context menu for the ImageView window. 2. Settings for the planned management are made in the Mode tab of the CPanel. Selected drop type Sessile Drop Mode tab Settings Drop deposition Data recording rate and measurement start options Baseline determination options Specification of the liquid used

24 page 22 Introduction to the DSA4 software Selected drop type Pendant Drop Mode tab Settings Measurement start and data recording rate options Specification of the density for the drop phase and the surrounding phase Specification of the needle diameter 3. Measuring instrument components are positioned and adjusted manually or with the help of other tabs in the CPanel: Measuring method Contact angle measurement with Sessile Drop Positioning/Settings Sample table position Syringe selection and needle positioning Drop volume, dosing mode and dosing rate Brightness, focus, zoom, camera settings Surface tension measurement with Pendant Drop Syringe selection and needle positioning Manual dosing of the drop (as a rule) Brightness, focus, zoom, camera settings 4. Further steps for surface tension measurements are carried out in the ImageView window: Setting of measuring lines for evaluation ranges, for determining the scale and for analysing the drop shape Scale determination 5. The measurement is started by means of the button. Message boxes showing the manual steps that may be required appear during the measurement.

25 Introduction to the DSA4 software page Data processing The results are initially displayed in the Results Monitor tab in the video and results window. Saving measurements in a database The data are copied to a database using the context menu in the Results Monitor (Store into DB).

26 page 24 Introduction to the DSA4 software Evaluating and managing results The results are evaluated and managed in the Results-DB-Explorer. The following options are available: Calculate surface energy (for contact angle) Carry out a statistical evaluation (Value Analysis) Create and print measurement reports

27 The Control Panel (CPanel) page 25 5 The Control Panel (CPanel) 5.1 Tasks The CPanel is intended for the following tasks in standard mode: Controlling instrument components If your instrument has no motorised components then only the illumination can be controlled from the CPanel. Making measurement settings and starting measurements The Mode tab which is required for measurement settings is described in Chapters 7 and 8 in the description of the individual measuring methods. 5.2 Overview Tab Functions Restriction Dosing Syringe selection, dosing mode, dosing rate, filling options For software-controlled dosing systems only, otherwise inactive N-Pos Horizontal and vertical needle position, saving of positions For software-controlled dosing systems only, otherwise inactive Axes Sample table control, movement mode, movement speed For software-controlled axes only, otherwise inactive

28 page 26 The Control Panel (CPanel) Tab Functions Restriction O-Con Brightness, focus, zoom, camera settings, image evaluation settings Focus and zoom for software-controlled lenses only, otherwise inactive Mode Measurement sequence settings, definition of evaluation parameters, decision between online measurement and video recording Only available in standard mode 5.3 General use of the software Entering values Click in the text box for the parameter, the value of which you want to change. Change the value with the help of the two cursor keys < > and < > or by entering a number. Numerical entries in the CPanel must be confirmed with <Return> Saving settings All settings that are required for a measurement are stored in a standard measurement template (Default-MT). Click on the button above the CPanel to save the changes.

29 The Control Panel (CPanel) page Image settings (O-Con tab) IEEE-1394 Falcon frame grabber Illum. Intensity: Brightness of the illumination Zoom: Magnification (only with software-controlled optics) Focus: Image sharpness (only with software-controlled optics) Brightness/Contrast: Brightness and contrast settings for the camera image. These values should not be altered; the image brightness should be controlled via the illumination unit. Shutter (IEEE-1394 camera only): Exposure time. The amount of light falling on the camera chip for each individual image depends on this value.! The frame rate reduces for longer exposure times. Gain (IEEE-1394 camera only): Amplification of the image signal. With short exposure times, the brightness of the image can be increased by means of the Gain.! The signal gain also increases the image noise. If possible, try to increase the brightness of the image by means of the illumination. Gradient Threshold (standard mode only): Minimum greyscale difference for detecting the drop shape and the baseline. The default value (see illustration) can usually be retained. The value can be reduced if the shape or baseline is not detected correctly.

30 SPA C SPA C SPAC SPAC page 28 The Control Panel (CPanel) 5.5 Sample table positioning (Axes tab) Software-controlled axis or axes The x-position (left-right), the y-position (front-back) and the z-position (up-down) of the sample table are controlled via the Axes tab of the CPanel.! Before using the axes you must make sure that no objects are located within the range of movement of the axes or in the vicinity of the guide rail Sample table control Keyboard control If the Axis tab is active then the x-, y- and z-axes can be controlled directly via the keyboard. Sample table direction Key To the right (x-coordinate increases) To the left (x-coordinate decreases) To the back (y-coordinate increases) To the front (y-coordinate decreases) Upwards (z-coordinate increases) Downwards (z-coordinate decreases) Page Up Page Down Cursor Cursor Cursor Cursor

31 The Control Panel (CPanel) page 29 Menu control The left drop-down menu is used for selecting an axis and for storing standard sample table positions. The right drop-down menu is used for selecting the movement mode and contains control options Saved sample table positions (Set as ) The following sample table positions can be saved: Parking Position: The basic position before and after a measurement. Stand-by Position: Table stand-by position during a measuring sequence. Deposition Position: The position of the sample table when the drop is in contact with the surface.

32 page 30 The Control Panel (CPanel) All Positions: The sample table position is assigned to all three saveable positions. The position is not only saved for the currently selected axis, but also for all available axes. Activating the saved sample table position directly (Go to) Select the required position under Go to (see above). Using positions for an MT (expert mode only) Please refer to Chapter 10 in the expert mode manual for how to use the positions for an MT Axis movement modes Continuous / Manual: Continuous movement. The movement is started with the arrow buttons Up and Down and stopped by clicking on the same button. Up and Down refer to the change in the coordinates of the particular axis and not to an up or down movement.

33 The Control Panel (CPanel) page 31 Range: Moves the axis between two defined coordinates. The selected axis will first move to the coordinate from and then to the second coordinate set under to. The movement is triggered with Go and cancelled with Stop (the button label changes) Initialising an axis The selected axis is moved to its zero position and initialised with Reset Zero Position Speed of movement (Velocity) You can choose between three different speeds for the axis movements, Slow, Normal and High. The setting applies to each axis separately Axis options (Options) The settings under Step mode are not yet effective.

34 SPA C SPA C SPAC SPAC page 32 The Control Panel (CPanel) Fine adjustment of the velocity A fine adjustment of the axis velocity can be carried out under Speed. This setting corresponds to the three speed stages (see above). Moving back to the start position in the Range mode When the option Back to begin position in case of Range mode is selected the appropriate axis will move back to the starting position set under from after the sample table has reached its target position. 5.6 Syringe selection and dosing Software-controlled dosing unit Keep your hands away from the range of movement of the needles. Otherwise, this may result in injury. The choice of syringe and control of the dosing process are carried out using the Dosing tab on the CPanel. The left-hand drop-down menu is used for selecting a dosing syringe and for setting filling options.

35 The Control Panel (CPanel) page 33 The number of syringes shown depends on the instrument s equipment. The item labelled (M) represents a manually operated syringe. The right-hand drop-down menu is used for selecting the dosing mode. In standard mode, the settings (dosing mode, volume) apply to all syringes. The text boxes below the menus are used for entering volume target values. Dosing is started in the selected mode by means of the button. Dosing is reversed by means of the button. The level in the selected syringe is shown under Fill Status. The dosing rate is adjusted under Rate. A good guide for this value is µl/min. For more viscous liquids (e.g. glycerol) the rate should be reduced slightly Dosing mode and dosing volume Information on dosing volume! In the case of a software-controlled dosing system with a disposable syringe, the changed dimensions of the syringe must be entered so that the required volume can be dispensed correctly. Please read Chapter I in the appendix.

36 page 34 The Control Panel (CPanel) Selecting the dosing mode and specifying the volume There are six dosing modes available for controlling the dosing process. These can be assigned to each syringe separately. Manual: Dosing takes place as long as the or button is kept pressed. Volume: The volume entered under Liq. Vol. will be dosed. Continuous: Dosing is initiated by clicking the or button and stopped by clicking it again. Volume Range: A drop will first be generated with the volume entered on the left and then increased or reduced to the volume shown on the right. Volume Oscillation: A drop will first be generated with the volume entered on the left. This mean volume will then be increased and decreased alternatingly by the volume entered on the right. Volume Loop: A drop will first be generated with the volume entered on the left and then increased or reduced to the volume shown on the right. In a third step the drop will then be set to the volume entered at the bottom left. With the last three dosing modes, a dedicated dosing speed can be assigned to each step.

37 The Control Panel (CPanel) page Filling a syringe Select the Refill Refill Now option in the left-hand drop-down menu. Once filling has been initiated, the Break Refill option will be active and can be used to stop the filling process. Refill speed You can select one of three filling speed steps under Refill Refill Speed.

38 page 36 The Control Panel (CPanel) Emptying, rinsing and resetting syringes (Tools) Large volumes of liquid are transported with some of the Tools functions. Place a collection vessel below the needle. Emptying and rinsing the syringe The current syringe can be rinsed with the Squeeze command. The syringe will be continuously emptied and refilled until the Squeeze process is terminated by pressing the <ESC> key. Switching the valve Toggle Switch Syringe Valve switches the dosing valve in order to rinse the length of tubing between the storage bottle and the syringe. When dosing, the liquid will then not be transported to the needle, but back into the storage bottle (or waste vessel). Resetting the syringe The selected syringe is reset with Reset Syringe. This option is required when installing the instrument ( Refer to instrument manual).

39 The Control Panel (CPanel) page Needle positioning (N-Pos) Software-controlled dosing unit Keep your hands away from the range of movement of the needles. Otherwise, this may result in injury. The sliders show the current position and can also be used for control. Keyboard control is used for fine adjustment of the needle position. Keyboard control If the N-Pos tab is active then the positions can be controlled directly via the keyboard: Needle movement Key down fast down up fast up top position bottom position to the left to the right Cursor Page Up Cursor Page Down Home End Cursor Cursor

40 page 38 The Control Panel (CPanel) Automatic needle positioning (auto scan)! If the needle is not detected, it can be moved too far down and hit the sample. Before using auto scan move the needle down to check that the needle appears in the live image. Adjust the focus and brightness if necessary. Click on the button. The needle will be positioned by image recognition so that the tip of the needle appears centrally at the top of the image. Stop the search process by clicking again Saving needle positions Saved needle positions are used for measurements with automatic drop deposition ( Chapter 7.5.2). The following needle positions can be saved: Parking Position: Starting position of the needle before and after a measurement. Stand-by Position: Stopping position of the needle during a measuring sequence. Deposition Position: Needle position when contact is made between drop and surface.

41 The Control Panel (CPanel) page 39 Max. Limiting Position: Lower position limit below which the needle must not go when moving to the sample position under automatic control (Auto Delivery; P. 53). The positions are saved separately for each available needle. Moving directly to saved positions Press the <Ctrl> key. The inscription on the buttons will change to Goto. Click on the Goto button for the required saved position.

42 SPA C SPA C SPAC SPAC page 40 Information applicable to all measuring methods 6 Information applicable to all measuring methods This chapter describes program functions which are required both for contact angle measurements and for measuring the surface and interfacial tension. 6.1 Starting and stopping measurements Starting a complete measurement sequence A complete measurement sequence is started with the button. Automatic control of instrument components may also be included in the measuring sequence. The measurement is stopped with <Esc> Starting an evaluation of the live image or a loaded image An evaluation of the live image or a loaded image is started with the button ( Chapter 6.2.2). Settings for controlling instrument components are not used. The measurement is stopped with <Esc>. When the measuring sequence involves a video recording, the initiates the start of recording. button Individual evaluation Individual evaluations can be carried out on the live image or on a loaded image for test purposes with the help of three buttons on the toolbar. Button Function Determines and displays the baseline Determines the drop shape Individual image evaluation using the set method 6.2 Video image options and image setup Switching between live image and still image The camera icon on the toolbar indicates the current video image status: Green lens : live image

43 Information applicable to all measuring methods page 41 Grey lens : still image: The mode is changed by clicking the button Saving and loading an image Saving 1. Switch the video image status to still image. 2. Select Save as from the context menu in the ImageView window. 3. Select the required path. Enter the required file name. Click OK. Loading Select Open from the context menu in the ImageView window. Select the required file. Click OK. SPA C SPA C SPAC SPAC

44 page 42 Information applicable to all measuring methods Adjusting the focus with the help of the Focussing Assistant! The Focussing Assistant cannot be used if displayed objects (drops or needles) appear too small in the image. Click on the button. Adjust the focus so that the Median field appears green and displays the highest possible value Criteria for a good drop image Attention should be paid to the following criteria when adjusting the drop image settings: With contact angle measurements, the drop should be as wide as possible and, with SFT measurements, should appear as high as possible in the image. The image should be well illuminated but not overexposed. Interference from external light should be avoided. The drop shape should be shown as sharply as possible. Use the manual aperture on the measuring instrument if the top edge of the drop is overexposed.

45 SPA C SPA C SPAC SPAC Information applicable to all measuring methods page Defining the evaluation range (Region of Interest; ROI) Region of Interest, ROI: Area of the image which is used for the evaluation. Defining the ROI serves to avoid interference outside that part of the image which is relevant to the measurement.! Measurement errors will occur if relevant parts of the image lie outside the ROI. The illustrations in this section show the ROI using the example of a surface tension measurement. Depiction of the ROI in the video image A coloured, rectangular frame which represents the ROI appears in the video image. If the boundary lines of the ROI cannot be seen, they are located at the edge of the image. Changing the size Click on the boundary line to be moved while holding the <Shift> key pressed. The mouse pointer will appear as a double arrow. Move the boundary line to the required position.

46 page 44 Information applicable to all measuring methods Changing position Click on the ROI while holding the <Shift> and <Ctrl> keys pressed. The mouse pointer will appear as cross hairs with arrows. Move the ROI to the required position. Saving the ROI 1. Select Update SDM Settings from the video image context menu. 2. Expert mode only: Click on the button. 3. Click above MT-Explorer. In expert mode, the ROI is saved separately for each SDM. SPA C SPA C SPAC SPAC

47 Information applicable to all measuring methods page Measuring and contour lines As part of a drop shape analysis, contour lines, which display the contours determined from the image analysis and, if available, calculated contours, appear in the drop image Lines used for Sessile Drop and Pendant Drop The illustrations in this section show lines referring to contact angle measurements. Optically determined contour: red contour line around the drop. The contour line should correspond as closely as possible to the visible outline. If this is not the case, take the following actions: Try to increase the contrast. Reduce the value of the Gradient Threshold in the O-Con tab of the CPanel.

48 page 46 Information applicable to all measuring methods Calculated contour: Green contour line, the shape of which corresponds to the chosen measurement and evaluation method (e.g. elliptical in the case of the Tangent 1 contact angle evaluation method). The green contour line should correspond as closely as possible to the red line. If this is not the case, choose an evaluation method in which the assumed contour shape corresponds more closely to the actual contour Lines used only for Sessile Drop Baseline: Boundary line between drop profile and the solid surface. Horizontal or curved line which runs transversely through the image. The baseline can be determined automatically or set manually.

49 Information applicable to all measuring methods page 47 Contact angle: Tangent to the calculated contour line at its point of intersection with the baseline Lines used only for Pendant Drop a) b) a) Measuring lines for determining the scale of the image: two horizontal lines which are set manually. b) Measuring line to preclude the contact region between needle and drop: a horizontal line which is set manually.

50 page 48 Preparing a contact angle measurement 7 Preparing a contact angle measurement This chapter describes the preparation of a contact angle measurement. Please read: Chapter 6.1 on starting the prepared measurement Chapter 10.6 on saving the measurement data in a database 7.1 Selecting the drop type Select Drop Type Sessile Drop from the context menu in the ImageView window. 7.2 Selecting the method for analysing the drop contour Select Comp. Method from the menu. Select the required method. For the background to the methods, please read Chapter 18 in the manual for expert mode. For information on the Top View Distance method, please read the manual for the TVA100 top view contact angle measuring module.

51 Preparing a contact angle measurement page 49 Meaning and use of methods Tangent - 1 Assumed contour shape Elliptical arc Recommended measuring range 10 to 120 Dynamic measurement possible Symmetrical drop shape required Yes No. However, in the case of severe asymmetry (e.g. measurement with a tilting table), Tangent - 2 is recommended. Tangent - 2 Assumed contour shape No prior assumption (polynomial fit) Recommended measuring range 10 to 180 Dynamic measurement possible Symmetrical drop shape required Yes No Circle and Height-Width Assumed contour shape Circular arc Recommended measuring range 0 to 20 Dynamic measurement possible Symmetrical drop shape required No Yes Laplace-Young Assumed drop shape Flattened curve with different curvature at every level due to the inherent weight of the drop Recommended measuring range 20 to 180 Dynamic measurement possible Symmetrical drop shape required No Yes

52 page 50 Preparing a contact angle measurement 7.3 Positioning and lens settings Variations from the following procedure may be necessary, as needle and sample table positions as well as the lens often have to be adjusted alternately. 1. Set the zoom to the minimum value. 2. Set the angle of inclination of the camera to 2. The viewing angle can be increased if detection of the boundary line between drop and solid is poor. 3. Set the illumination to medium brightness. 4. Place the sample on the sample table. Raise the sample table until the sample appears in the bottom third of the camera image. 5. When using a multiple dosing unit, select the required syringe. 6. Position the sample table or the sample horizontally so that the needle is above the required measuring position. 7. Lower the needle until it is just above the sample. For automatic measurements, define the position as the Deposition Position. Move the needle to the top edge of the image and define the position as the Parking and Stand-by Position. Move the needle back to the Deposition Position. 8. Adjust the zoom so that the image of the needle takes up % of the image width.

53 Preparing a contact angle measurement page Adjust the focus so that the needle is shown as sharply as possible. For how to use the Focussing Assistant, please read P Adjusting the dosing (for software-controlled dosing unit only) Software-controlled dosing unit 1. Select the Dosing tab in the CPanel. 2. Select the required dosing mode. If Manual dosing mode is selected, a message box for carrying out the manual dosing will appear during the measurement. 3. Enter the required dosing volume or volume steps. 4. Enter the required dosing rate or rate steps.

54 page 52 Preparing a contact angle measurement 7.5 Measurement sequence settings (Mode tab) Start Measurement Manual: After starting the measuring sequence with the button, all steps are carried out (manually or automatically) until the dispensed drop is displayed in the video image. The image evaluation is then carried out manually with the help of the or buttons. At start of deposition: The measurement is started as soon as dosing begins. This option is normally used for dynamic measurement with the Continuous, Vol. Range, Vol. Oscillation and Vol. Loop dosing modes. Once deposition is finished: The measurement is started as soon as dosing is complete. This option is normally used for static measurements with the Manual and Volume dosing modes.

55 Preparing a contact angle measurement page Drop deposition (Deposition) Manual: Manual movement of the needle. A message box with a request to position the needle appears during the measurement. The measuring sequence is resumed by pressing Continue. Teach-in Software-controlled dosing unit The needle moves to the position defined as the Deposition Position. When dosing is complete or when the measuring time has expired, it moves to the Parking Position. Auto Delivery Software-controlled dosing unit The needle moves to a suitable dosing position using image recognition.! Before carrying out the measurement, select the lower position limit for the needle (Max. Limiting Position; Chapter 5.7.2) to prevent the needle from hitting the sample if the surface is not detected correctly Choosing between measurement and video recording (Measurement Mode) Choose whether a measurement is to be taken (On-Line Computation) or whether a video is to be recorded during the sequence. Please read Chapter 9 for recording, playing back and evaluating videos.

56 page 54 Preparing a contact angle measurement Measurement period and measurement rate Measure each: Time between image evaluations. Until: Total duration of the measurement. You can switch between seconds and minutes in the drop-down menu on the right-hand side Determining the baseline (Baseline, Detection) Baseline: The baseline is the boundary line between the surface of the solid and the drop. contact angle θ baseline The following options are available: Automatically determined linear baseline The baseline is not determined automatically with the Height-Width (Manual) method ( Chapter 7.6). The baseline must be positioned manually together with the other lines of the rectangle. Manually defined linear baseline

57 Preparing a contact angle measurement page 55 Manually defined curved baseline The curved baseline cannot be used together with the Height-Width (Manual) contact angle method ( Chapter 7.6). With the manual options, a message box with a request to define the baseline appears during the measurement: The measuring sequence is resumed by pressing Continue. Automatically determined linear baseline The baseline can be determined automatically under the following conditions: High-contrast image with clearly visible phase contact boundary Contact angle less than 90 In expert mode, the baseline can also be determined automatically when contact angles of greater than 90 are expected ( Chapter 13.2 in the manual for expert mode). Manually defined linear baseline The baseline appears as a blue line in the ImageView window

58 page 56 Preparing a contact angle measurement When the appropriate message box appears, move the baseline to the required position with the mouse or the cursor keys < > and < >. If necessary, adjust the slope of the baseline with the cursor keys < > (left side down) and < > (right side down). Double-clicking on the baseline will align it horizontally. Manually defined curved baseline With a curved baseline the only contact angle methods possible are Tangent 1 and Circle. Three points define the degree of curvature of the curve. Use the mouse to place the two outer points on the phase contact points of the drop. Match the curvature to the curvature of the surface using the middle point. To change the height of the curve, move the mouse pointer onto the curve outside the three curvature points and move it with the mouse Choosing the drop liquid to be used With a single-dosing unit, the required liquid is selected in the Mode tab and remains assigned to the syringe until a new liquid is selected. With a multi-dosing unit, the liquid selected in the Mode tab is not saved when a syringe is changed. In order to find the required standard liquid when a syringe is changed, liquids can be assigned to syringes in the default measuring template (Default-MT).

59 SPA C SPA C SPAC SPAC Preparing a contact angle measurement page 57 Assignment via the Mode tab The liquid used is displayed in the Liq. Ass. text box. 1. Click on the button. The database for test liquids will open. 2. Select the required liquid from the left-hand list. Click on Name in the column header to sort the entries alphabetically. If the liquid used is not in the database, a new database entry must be created ( Chapter 13.3). 3. If the contact angle of the liquid is to be used for calculating the surface energy, select the required entry for surface tension and interfacial tension from the IFT Properties list. For many liquids, several entries exist with data from different literature sources. A note as to which method of surface energy calculation the liquid is suitable for will be found in the Mtd column. 4. Click OK. SPA C SPA C SPAC SPAC

60 page 58 Preparing a contact angle measurement Assignment in the default measuring template 1. Select Tools System Settings from the menu. Select Syringe Assignment from the list in the structure tree on the left. 2. Select the line for the syringe to which you want to assign a liquid. 3. With the help of the test liquids database, select the required liquid with the button as described in the previous section. 4. Repeat Steps 2 and 3 for all existing syringes. 5. Click. Click on the button above the CPanel to save the changes. 7.6 Using the Height-Width (Manual) method With the Height-Width (Manual) method, a rectangle is positioned around the drop contour with the help of the mouse. Starting the image evaluation If the measurement is to be started manually, then the image evaluation is started with the or button. If the measurement is to be started automatically, then the image evaluation is carried out in the course of the programmed measuring sequence. In both cases, a message box opens with a request to position the lines of the rectangle.

61 Preparing a contact angle measurement page 59 Carrying out a manual image evaluation Define the baseline. The baseline cannot be determined automatically with the Height-Width (Manual) method. If a measuring sequence is started with the Linear/Manual baseline option, then the message box for defining the baseline appears first. The baseline defined by this means is used for the rectangle to be positioned. Position the other three sides of the rectangle using drag-and-drop. The left hand and right hand side must pass through the three-phase contact points. The top side must pass through the apex. 7.7 Special features of Captive Bubble measurements For information on sample preparation, dosing the air bubble and setting up the image, please read the manual for the ST10 sample holder set. Select Drop Type Captive Bubble from the context menu in the ImageView window.

62 page 60 Preparing a contact angle measurement Recommended settings and start options The manual option should be selected under Deposition in the Mode tab in the CPanel. Dosing should be carried out manually. In most cases, the baseline must be defined manually. The measurement should be carried out using the button for serial measurements. The measured angle is already the complementary angle between the liquid and the solid (180 minus the bubble contact angle), meaning that this does not have to be calculated first.

63 Preparing a surface tension and interfacial tension measurement page 61 8 Preparing a surface tension and interfacial tension measurement The preparation of a surface tension or interfacial tension measurement is described in this chapter. Please read: Chapter 6.1 on starting the prepared measurement Chapter 10.6 on saving the measurement data in a database 8.1 Selecting the drop type Select Drop Type Pendant Drop from the context menu in the ImageView window. 8.2 Determining the needle diameter! A special dosing needle with a larger diameter is used for pendant drop measurements. The needle used for contact angle measurements is not suitable. Needles with metal Luer-Lock connector: NE23, 24, 28, 29, 31, 32, 33, 34 The diameter of the specified needles is determined by KRÜSS and is noted on the packaging.

64 page 62 Preparing a surface tension and interfacial tension measurement A hole in the shaft indicates the point on the diameter at which the measurement was carried out. The needle must be inserted into the dosing unit so that the hole lies on the optical axis. Other needles Place the needle in the dosing unit. Determine the outside diameter of the needle perpendicular to the optical axis to an accuracy of 1/100 mm, e.g. with the help of a micrometer. The diameter should be measured just above the tip because this section is used for image scale determination. 8.3 Measurement sequence settings (Mode tab)

65 SPA C SPA C SPAC SPAC SPA C SPA C SPAC SPAC SPA C SPA C SPAC SPAC SPA C SPA C SPAC SPAC SPA C SPA C SPAC SPAC Preparing a surface tension and interfacial tension measurement page Start Measurement Manual: After starting the measuring sequence with the button, all steps are carried out (manually or automatically) until the dispensed drop is displayed in the video image. The image evaluation is then carried out manually with the help of the or buttons. when dosing stops: The measurement is started as soon as dosing is complete. when dosing starts: The measurement is started as soon as dosing begins Choosing between measurement and video recording (Measurement Mode) Choose whether a measurement is to be taken (On-Line Computation) or whether a video is to be recorded during the sequence. Please read Chapter 9 for recording, playing back and evaluating videos Measurement period and measurement rate Measure each: Time between image evaluations. Until: Total duration of the measurement. You can switch between seconds and minutes in the drop-down menu on the right-hand side Entering the needle diameter Enter the needle diameter ( Chapter 8.2) under needle diameter.

66 page 64 Preparing a surface tension and interfacial tension measurement Entering the density Enter the density of both phases in the Mode tab of the CPanel: the density of the drop liquid under liquid the density of the surrounding phase under surr. phase For surface tension measurements the density of the gas is entered here. 8.4 Positioning and lens settings 1. Set the angle of inclination of the camera to Fill the syringe with the liquid under investigation. Place the syringe in the manual dosing system or in the manual position of the multi-dosing system. 3. Set the illumination to medium brightness. 4. Move the needle to the top center of the video image.! The needle should be as near to vertical as possible. 5. Adjust the zoom so that the image of the needle takes up 10 to 20% of the image width. 6. Adjust the focus so that the needle is shown as sharply as possible. For how to use the Focussing Assistant, please read P. 42.

67 Preparing a surface tension and interfacial tension measurement page Depositing drops Deposit a suspended drop which is as large as possible. The drop can be produced in a glass cuvette in order to prevent movement. If necessary, the bottom of the cuvette can be filled with sample solvent in order to avoid evaporation. 8.6 Determining the scale of the image 1. Readjust the focus if necessary. 2. Drag and drop the two upper measuring lines so that they include part of the needle tip in the image. It is possible that not all measuring lines will be seen if they are located at the top edge of the image. 3. Click on the button. The scale of the image will be calculated and displayed above the ImageView window.! The zoom and focus must not be changed after the scale of the image has been determined.

68 page 66 Preparing a surface tension and interfacial tension measurement 8.7 Excluding the upper part of the drop contour The upper part of the drop contour is distorted due to the contact with the needle. This area is excluded from the measurement with the help of the third measuring line. Drag and drop the bottom measuring line so that it lies below the part of the drop contour which is distorted by contact with the needle.

69 Recording, playing back and evaluating video page 67 9 Recording, playing back and evaluating video Instead of evaluating the video image in an online measurement, it is possible to record a video. Online measurement at the same time as recording a video is not possible. 9.1 Recording during a measurement sequence Settings for a measurement sequence with video recording can be made in the Mode tab of the CPanel. Select Video Recording in the Measurement Mode drop-down list box. The contents of the Mode tab will change: Frame rate and recording time Enter the required frame rate (individual images/second) in the fps text box. Enter the required recording time in the during text box. The size of the video file is given by the product of the frame rate and the recording time Start options The Start Measurement drop-down list box includes options for starting the video recording. Sessile Drop Pendant Drop

70 page 68 Recording, playing back and evaluating video Start dependent on dosing at start of deposition (Sessile Drop) or when dosing starts (Pendant Drop): Start recording when drop dosing starts once deposition is finished (Sessile Drop) or when dosing stops (Pendant Drop): Start recording when drop dosing stops Start with the help of a trigger on trigger line: Start recording when a change in the greyscale values is registered at a defined height in the image, e.g. when the needle penetrates. Move the bottom blue line to the required height in the video image. 9.2 Manual recording Recording with the video settings in the Mode tab can be started manually. The following settings are used: fps during Start Measurement Starting recording Click on one of the buttons or. Stopping recording prematurely Click on the button. 9.3 Saving a video When the video recording is complete, a dialogue box for saving the video will appear. Select the required path and file name. Click OK. After saving, the video will be displayed in the ImageView tab.

71 Recording, playing back and evaluating video page Saving a video retrospectively If you close the dialogue box for saving the video with Cancel, the video will initially remain in the working memory. To save the video retrospectively: Select Save Video from the context menu in the ImageView window.! When DSA4 is closed or when a new video is recorded, the video in the working memory will be lost Saving the video automatically For how to save videos automatically, please read Chapter in the Expert Mode manual. 9.4 Loading a video 1. Select Open from the context menu in the ImageView window. 2. Select the Video Documents (Avi) option in the File type drop-down list box. 3. Select the required file. Click Open. 9.5 Playing back a video Video playback buttons Button Function Play Stop Jump to the last Frame Jump to the first Frame Scrollbar below video image <Frame > <Frame > Set required frame to next frame to previous frame

72 page 70 Recording, playing back and evaluating video 9.6 Evaluating a video Preliminary settings Select the drop type that was used for the video ( P. 48 or 61). Define the evaluation range ( Chapter 6.3). For Sessile Drop 1. Select the required method of drop shape analysis ( Chapter 7.2). 2. Select the required method of determining the baseline ( Chapter 7.5.5). If a manual method for determining the baseline is chosen, a request to define the baseline will appear when the video evaluation starts. 3. Select the liquid that was used for the video ( Chapter 7.5.6). For Pendant Drop 1. Enter the density for the drop phase and the surrounding phase ( Chapter 8.3.5). 2. Enter the diameter of the needle that was used for the video ( Chapter ). 3. Determine the scale for the image ( Chapter 8.6) Starting the evaluation Define the Frame at which the evaluation is to start with the help of the slider at the bottom edge of the ImageView window.

73 SPA C SPA C SPAC SPAC Recording, playing back and evaluating video page 71 You can move forwards and backwards in single steps with the <Page Up> and <Page Down> keys. Click on the button. The video will be evaluated frame by frame starting with the selected Frame. The results will appear in the Results Monitor ( Chapter 10). Stopping the evaluation prematurely Click on the button.

74 SPA C SPA C SPAC SPAC SPA C SPA C SPAC SPAC SPA C SPA C SPAC SPAC page 72 Managing unsaved measurement data (Results Monitor) 10 Managing unsaved measurement data (Results Monitor) The results of a measurement are first collected in the Results-Monitor. The Results-Monitor is a data table in which all available data are listed for each individual measuring point of the generated measurement series. The data can be assessed in the table and in two charts (RTPlotView). To save in the results database (Results-DB), please read Chapter For the meaning of the quantities that can be displayed please read appendix II Creating series of measurements When starting an MT or SDM If the Results-Monitor is empty, a new series of measurements will be generated when a measurement sequence is started ( button). If there are already data in the Results-Monitor, a dialogue box for handling the existing data will open when a measurement sequence is started: Save the current data into database (RDB): A dialogue box for saving the data in the Results Monitor will open ( Chapter 10.6). Empty results buffer (data will be deleted): The data in the Results Monitor are deleted.! The deleted data are not moved to the recycle bin, but deleted immediately. Continue buffering: A new series of measurements is generated.

75 SPA C SPA C SPAC SPAC Managing unsaved measurement data (Results Monitor) page When starting an image or video evaluation A new series of measurements is created when an image evaluation is started ( button) or when a video evaluation is started ( button) For a single image measurement If the Results-Monitor is empty, a new series of measurements will be generated when a single image measurement is started ( button). The series of measurements will be named Orphan. If the dispensing liquid or the evaluation method is changed, a new series of measurements is also generated. If there are already data in the Results-Monitor and if the dispensing liquid has not been changed, the results of a single image measurement will be attached to the last series of measurements generated. Generating a new series of measurements manually If data from the single image measurement are not to be attached to an existing series of measurements, a new series of measurements can be generated manually. Select Add new Measurement from the Results-Monitor context menu.

76 page 74 Managing unsaved measurement data (Results Monitor) 10.2 Changing the displayed table columns Changing for the current software session only Select Options from the Results-Monitor context menu. All displayable measured quantities will be found in the left-hand list and those already displayed in the right-hand list. Select the required quantity and transfer it from one list to the other with the help of the arrow buttons. Click OK Changing permanently 1. Select Tools System Settings from the menu. Select Presentation/Report from the list in the structure tree on the left. 2. To select the quantities to be displayed, proceed as described in the previous section. 3. Click Finish when the selection is complete. 4. Click on the button above the CPanel to save the changes.

77 Managing unsaved measurement data (Results Monitor) page Copying the contents of a table to the clipboard Mark the content to be copied using the mouse. Select Copy from the context menu for the marked range. The copied content can be copied from the clipboard into another program (e.g. Excel) Mean value calculation The top line of a series of measurements marked with SUM contains the arithmetic mean values for each parameter of a measurement series. The mean value is calculated automatically when a series of measurements is generated. Updating mean values If you add data to a measuring series or if you retrospectively change the mean value options, then the mean value calculation must be updated. Select Update from the context menu in the SUM line.

78 page 76 Managing unsaved measurement data (Results Monitor) 10.5 Displaying charts (RTPlotView) The data from the Results-Monitor are displayed in the two charts RTPlotView-1 and RTPlotView Selecting series of measurements All series of measurements in the Results-Monitor are displayed as standard. To change the selection, proceed as follows: 1. Select Options from the context menu for the required chart. All displayable series of measurements will be found in the left-hand list and those already displayed in the right-hand list. 2. Remove the All new created MSTs entry with the help of the arrow button. 3. Select the series of measurements to be shown or hidden and transfer it from one list to the other with the help of the arrow button. Click OK.

79 Managing unsaved measurement data (Results Monitor) page Changing the axis assignment Changing for the current software session only 1. Select Options from the context menu for the required chart. Select the Chart Axes Settings tab. 2. Select the measured quantity which you want to assign to one of the axes from the list. 3. Select the required axis with the Set as X or Set as Y1 button. Click OK. You can use a second y-axis by selecting the use Y2-axis option. Changing permanently 1. Select Tools System Settings from the menu. Select Presentation/Report from the list in the structure tree on the left. Select the Chart tab. 2. Select the chart for which you want to change the axis assignment from the top drop-down list box. 3. To make the axis assignment, proceed as described in the previous section.

80 page 78 Managing unsaved measurement data (Results Monitor) 4. Click Finish when the assignment is complete. 5. Click on the button above the CPanel to save the changes Show legend Click on the button above the chart. The legend is shown at the right-hand side of the chart Displaying diagram in a new window Open the context menu of the tab for the required diagram. Select the menu item Release. Re-integrating the window Click on the symbol for closing the window Saving measured data in the database The required series of measurements are copied from the Results-Monitor into the database. Further steps, such as the calculation of the surface energies or the creation of measurement reports, are carried out here. If no database is available or if the data are to be copied to a new database, please read Chapter Select the series of measurements to be transferred by setting or removing the ticks in the checkboxes.

81 SPA C SPA C SPAC SPAC Managing unsaved measurement data (Results Monitor) page Select the Store into DB command from the Results-Monitor context menu. 3. If a database has not yet been opened, a dialogue box for selecting a database will appear. Select the required database. Click OK. 4. A dialogue box for saving the measured data will appear. Saving as a new project in an existing Workspace: Mark the required Workspace ( icon). Click Select. Saving in an existing project: Mark the required project ( icon). Click Select. Saving in a new workspace: Click New Workspace. Overwrite the text New Workspace with the required name. Click Select.

82 page 80 The results database (Results-DB-Explorer) 11 The results database (Results-DB-Explorer) Data are managed and evaluated in Results-DB-Explorer: Creating charts and reports Carrying out a value analysis Calculating the surface energy 11.1 Database structure The database is arranged as follows: Workspace Project Measurement (Measurement; single drop) Report Values Chart Report (Value Analysis; SFE; Mapping Analysis) Only reports of evaluations can be stored in the DB. Reports of measurements can only be printed or exported. Deleted database items are initially stored in the Recycle Bin they can be permanently deleted. from where

83 The results database (Results-DB-Explorer) page Database management Creating a new database Select File New from the menu. Select the required directory. Enter the required file name. Click OK Opening a database Select File Open from the menu. Select the required database. Click OK Workspaces Creating a workspace Select the Create new Workspace command from the database context menu. The new Workspace will appear in the structure tree. Overwrite the text New Workspace with the required name Copying a project to a Workspace Select Add Existing Project from the context menu of a Workspace.

84 page 82 The results database (Results-DB-Explorer) Select the required project. Click OK. Projects can only be copied from one Workspace to another within one and the same database Managing Workspaces The context menu for a Workspace contains items for managing the workspace: Rename Workspace: Rename the Workspace. Delete Workspace: Move the Workspace to the Recycle Bin. Edit Details: Write or modify memo text Moving a measurement to another project Select Cut from the context menu of the measurement to be moved. Select Paste from the context menu of the destination project Projects and measurements Measurements are assigned to a Project when they are saved in the Results-DB.

85 The results database (Results-DB-Explorer) page Editing a project Select the project to be edited. Information relating to the project will appear on the right-hand side in the Project tab. Changing solid or bulk phase The solid or bulk phase can only be changed retrospectively in standard mode. Click on the appropriate Edit Parameter button for the phase to be changed (solid: Substrate Phase; bulk phase: Environment Phase). The following dialogue box will appear: Enter the name and the missing data or the data to be changed for the respective phase. Click OK. Changing information text Click on the button. Enter the required text. Click OK.

86 page 84 The results database (Results-DB-Explorer) Displaying measurements The results of a measurement are listed under Values. Changing the displayed table columns 1. Click Grid Settings. All displayable measured quantities will be found in the left-hand list and those already displayed in the right-hand list. 2. Select the required quantity and transfer it from one list to the other with the help of the arrow buttons and. 3. The order of the columns from left to right is defined by the order of the items in the Displayed Columns list. Use the arrow buttons and to change the order.

87 The results database (Results-DB-Explorer) page Changing the liquid entry for a measurement retrospectively In two cases it is necessary to change the liquid entry retrospectively: When the liquid assigned to a measurement is not the same as the liquid actually used. When not all the liquid data required for a surface energy calculation are available or if other data are to be used. The liquid entry can only be changed retrospectively in standard mode. Procedure Select the measurement to be edited. Click on the Measurement tab. button in the Enter the name and the missing data or the data to be changed for the liquid. Click OK. You can select the required substance from the substance database with the button ( Chapter 7.5.6).

88 page 86 The results database (Results-DB-Explorer) Exporting all measurements for a project 1. Select Export to from the context menu for the required project. 2. Click Open. Select the required path for the export file. Click OK. 3. Select the required file format from the Format drop-down list box. Click OK Charts Creating a chart 1. Select New Chart from the context menu of the Values entry for the required measurement.

89 The results database (Results-DB-Explorer) page Enter the required name. 3. Click Add Series. Select the required quantities for the X and Y-axis from the Axis X and Axis Y drop-down list boxes. Selecting further quantities for the Y-axis You can select further quantities for the Y-axis in the same chart with Add Series. Only one quantity can be selected for the X-axis. You can remove a quantity which has been assigned to the Y-axis with Remove Series. Showing and hiding legends The legend can be shown and hidden with Show legend Changing the scale 1. Click on the button. The following dialogue box will appear: 2. Select one of the tabs Axis X or Axis Y to change the scaling for the corresponding axis. 3. Enter the start value under Begin from and the end value under End by. 4. Enter the required distance between the graduation marks under Step. 5. If required, select a logarithmic scaling and enter the base for the logarithm. 6. Click OK.

90 page 88 The results database (Results-DB-Explorer) Buttons on the chart toolbar Buttons for outputting a chart Button Function Storing as a graphic file Opening the print dialogue Print preview Buttons for viewing a chart Button Function Selection of the chart type (e.g. x-ydiagram, bar chart) Selection of the colour palette Showing / hiding legend Toggle 3D view Tools for notes and marks

91 The results database (Results-DB-Explorer) page Creating a report Reports can be created from measurements or from evaluations ( Chapter 12). Select Create Report from the context menu for the required Measurement or Values entry in the database structure tree General report options (Report Settings tab) Entering a title Enter the required title under Title. Selecting the character set and font colour Select the required character set under Select. Select the required font colour under Color. Incorporating a logo Click Open. Select the required file. Click OK. Files with bmp, jpg or gif format can be incorporated. Select the Show Logo option.

92 page 90 The results database (Results-DB-Explorer) Incorporating a chart (Chart Selection tab) Select the Add Chart to Report option. Incorporating an existing chart Select the Use Existing Chart option. Select the Name of the required chart from the drop-down list box. Incorporating a new chart Select the Create New Chart option. Proceed as described in Chapter The design options described in Chapter are not available when creating a chart in the Chart Selection tab Changing displayed table columns (Table Properties tab) Please read the description for the display of columns under the Values structure tree entry on P. 84 for how to proceed. In addition, you can select the quantity used for sorting the table under Sort Table by.

93 The results database (Results-DB-Explorer) page Creating a report Click Create Report. A dialogue box with report options will appear. After setting the options described below, the report is created by pressing Start. Printer selection The printer which has been set as the default printer is shown under Print Target. To select a different printer, click Change. Select the required printer. Click OK. Preview Open the Direct to drop-down list box. Select the Preview option.

94 SPA C SPA C SPAC SPAC page 92 The results database (Results-DB-Explorer) Selecting the format for outputting the report as a file An output format for saving the report to file can be selected in the Direct to dropdown list box. Settings for the respective format can be made with the Options button. With the graphical output formats and with HTML, an image file is produced for each page. Charts cannot be output with pure text formats. Defining the page ranges The pages of the report to be output can be selected under Options.

95 Evaluations page Evaluations The context menu for a project in the Results-DB includes three options for evaluating data: Calculate SFE: Calculation of the surface energy from contact angle data Value Analysis: Statistical evaluation of several measurements of the project Mapping Analysis: Display of contact angle as a function of sample position How to carry out and evaluate a mapping measurement is described in Chapter 17 of the expert mode manual Information for all evaluation methods Selecting measurement series A series of measurements usually consists of several image evaluations for a single drop. However, individual image evaluations for several drops may also have been combined to form one series of measurements (e.g. in the TVA100). Select the measurement series which are to be used for the calculation with the help of the checkboxes in the top list. A Value Analysis can only be carried out for measurements with the same liquid.

96 page 94 Evaluations Changing the displayed table columns Please read the description for the display of columns under the Values structure tree entry on P. 84 for how to proceed. In addition, you can select the quantity used for sorting the table under Sort Table by Settings for calculating mean values and eliminating outliers The evaluation is carried out based on mean values of contact angle for the individual series of measurements.! The settings for forming the mean value which have been made for one evaluation method (selected measurements and options) are adopted for the other evaluation methods. The mean value over all the series of measurements for the same liquid can also be used when calculating the surface energy ( Chapter12.2.3). The mean value is not taken from the Results-Monitor but recalculated using the settings made here. Choosing a series of measurements and individual measurements Mark the series of measurements for which the mean value calculation settings are to be changed. Select the individual measurements which are to be included in the mean value for the particular series of measurements. Options for forming the mean value Averaging: Use of the arithmetic mean or median. Calculate Value: Use of the left (CA Left) or right contact angle (CA Right) or the mean of the two (CA Mean).

97 Evaluations page 95 Confidence Interval: Confidence interval. Only values which lie within the percentage selected in the drop-down list box are used in the mean value calculation. The multiple of the standard deviation (SD) resulting from the given percentage is shown on the right. With Don t Apply all the values will be used for the calculation. Based on: Selection of the quantity to which the confidence interval is to refer Report of an evaluation Adding charts to the report Select the Add Chart to Report option. Incorporating a logo Please read P. 89. Preview or print Click Show Report. For information on the print and preview options, please read Chapter Saving a report in the project With the surface energy calculation, the report cannot be saved until the preview has been opened. Click Create Report.

98 page 96 Evaluations 12.2 Calculating the surface free energy Select Calculate SFE from the context menu for the required project Entries and selection options (CA tab) Selecting the calculation method For the theory behind the calculation methods, please read Chapter 18 in the manual for expert mode. Select the required calculation method from the SFE Calculation Method drop-down list box. The following table shows the minimum number of contact angle test liquids which are required for the calculation and which liquid data must be available: Method Equation of State (EOS) 1 Zisman 2 Liquids required Fowkes 2 with pol/disp. data

99 Evaluations page 97 Method Liquids required Wu Ow/We/Ra/Kae Schultz-1 (not for TVA100) Schultz-2 (not for TVA100) Ext. Fowkes Acid-base 2 with pol/disp. data 2 with pol/disp. data 2 drops liquid + one surrounding phase 1 drop liquid + 2 surrounding phases 3 with HH bridge data 2 with acid-base data Performing the calculation! The entries and options in the IFT tab affect the calculation ( Chapter ). Select the measurements which are to be used for the calculation with the help of the checkboxes in the left-hand list. Click Result (Result tab) The result is displayed in the Result tab. With some calculation methods, a chart is also displayed. To add the chart to the report, Select the Add Result Chart to Report option.

100 page 98 Evaluations An error-weighted calculation can be carried out for some calculation methods with the help of the Error-weighted option. Here, mean values of contact angle with a higher standard deviation are used with lower weighting in the result. With some calculation methods, a Wetting Envelope can be displayed in an additional tab ( Chapter ) Liquid data (IFT tab) Data table: The table shows the chemical and physical data of the liquid which has been used for the measurement marked on the left-hand side. You can change the values, for example to use data from another literature source. Mean Contact Angle of Substance: Mean value of the contact angle over all drops of liquid. Use "Mean Contact Angle of Substance" for Calculation: If this option is selected, then the mean value over all series of measurements of the same liquid is used for the calculation. Otherwise, the data of each individual series of measurements are used in the calculation.

101 Evaluations page Wetting Envelope tab For the interpretation and theory behind the Wetting Envelope, please read Chapter 18 in manual for expert mode. Calculating the Wetting Envelope Click on the button. The diagram shows a plot of the polar component against the dispersive component of the surface tension. Liquids within the envelope wet the solid completely. Adding the wetting envelope to the report Select the Add Wetting Envelope Chart to Report option Mean values of contact angle for several drops (Value Analysis) Mean values of contact angle for measurements of several drops of the same liquid can be calculated with the Value Analysis Carrying out the Value Analysis Select Value Analysis from the context menu for the required project. Please read Page 94 for settings relating to the calculation of mean values and elimination of outliers.

102 SPAC SPAC SPAC SPAC page 100 Evaluations Creating a chart (Chart tab) Selecting measurements Several measurements can be selected for displaying in the chart when carrying out a Value Analysis. All displayable measurements will be found in the left-hand list and those already displayed in the right-hand list. Select the required measurement and transfer it from one list to the other with the help of the arrow buttons and. Assigning axes Select the required quantities for the X and Y-axis from the Axis X and Axis Y drop-down list boxes.

103 The substance database page The substance database Chemical and physical data of liquids, solids and gases are stored in the substance database. The liquid used for carrying out a contact angle measurement is selected with the help of the substance database. If the liquid used is not in the database, a new database entry must be created ( Chapter 13.3) Opening the substance database The substance database can be opened in two ways: With the button in the Mode tab of the CPanel. With the button in the main menu bar Substance database structure Substance list The substances entered in the database are listed on the left-hand side. Selecting a substance for viewing Click on the required substance. Sorting the list alphabetically Click on Name in the column header.

104 page 102 The substance database Substance data The physical data which have been entered for the selected substance will appear at the top right Entries for interfacial and surface tension data (IFT-Items) IFT-Item: Entry with interfacial and surface tension data for the selected substance database entry. The data stored in IFT-Items are transferred when the liquid is selected and are used, for example, for calculating the surface energy. Several IFT-Items can be stored for one substance entry. The IFT-Items available for the selected substance are listed at the bottom right Creating a new database entry 1. Select Substance Add a New Substance from the menu. A dialogue box for creating the new substance entry will appear. 2 Click Next.

105 The substance database page Enter the required substance data. The name must be specified. All other data are optional. Top text box: Name of substance Memo: Information relating to the database entry CAS-No: Chemical Abstracts Service Number; CAS registration number for the substance. Density: Density of the substance in g/ml. Viscosity: Viscosity in Pas. Temp. Coef (1/K): Thermal coefficient of expansion. State: Drop-down list box for specifying the aggregate state: Liquid, Solid or Gas Editing your own database entry Only your own database entries can be edited. Select the required database entry. Select Edit Edit from the menu.

106 page 104 The substance database 13.5 Deleting your own database entry Only your own database entries can be deleted. Select the required database entry. Select Edit Delete from the menu Creating a new IFT-Item Select the database entry for which a new IFT-Item is to be created. Click on the open. button. A dialogue box with two tabs will General Properties tab For the background to the entries, please read Chapter 18 in the manual for expert mode. Method: Method of calculating the surface energy for which the entry is suitable or recommended. Standard Deviation: Standard deviation for the respective entries. IFT / SFT (Total): Surface/interfacial tension Dispersive: Dispersive component of surface/interfacial tension Polar / Acid-Base: Polar component of surface/interfacial tension H-H: Proportion of hydrogen bridge bonding interactions in the total polar component

107 SPA C SPA C SPAC SPAC The substance database page 105 Acid: Acid component of the polar interactions according to the Lewis acidbase model Base: Base component of the polar interactions according to the Lewis acidbase model Extra Information tab Env. Phase: Environment phase. When entering an interfacial tension, the second liquid phase must be selected here. Memo: Information relating to the IFT-Item. Ref.-Temp.: Reference temperature for the data. Reference: Source of the data. The Add button is inactive. It is currently only possible to select from existing source information.

108 page 106 System Settings and Miscellaneous 14 System Settings and Miscellaneous System settings can be carried out under Tools System Settings and Tools Miscellaneous on the menu.! KRÜSS recommends that the settings above System Settings and Miscellaneous should not be changed in standard mode Connector assignment; environment and system parameters (General tab) Select Tools System Settings from the menu Changing the connector assignment for instrument components Selecting a serial interface Select the serial interface of the computer to which the instrument has been connected in the DSA100 drop-down list box. Selecting the connector for the temperature sensor Select the connector which is used for connecting the temperature sensor to the measuring instrument in the Temperature Sensor drop-down list box ( Refer to instrument manual). The option ET... at the bottom is intended for the following purposes: Measurements with a thermostat chamber TC40 Measurements with a high-temperature furnace with DSA HT

109 System Settings and Miscellaneous page Environmental and system parameters (General Parameters area) Earth s Acceleration of Gravity: Local value of the Earth's acceleration due to gravity. The Earth's acceleration due to gravity is used in the calculation of the surface tension in the pendant drop measurement. Aspect Ratio: The length/width ratio of the pixels for image presentation.! For components supplied by KRÜSS, the value of must not be changed under any circumstances Dosing unit options (Dosing tab) Syringe position assignment for software-controlled multi-dosing units The basic DSA4 settings are the same as those described in the measuring instrument manual. For this reason, it is not usually necessary to make any changes here. The number of syringes in the dosing unit is selected in the top drop-down menu. In the drop-down menu beneath it, the positions A-H of the needle selector are assigned to the syringe numbers (1-8 and M). Please read the measuring instrument manual for information on the needle selector positions and the syringe numbering.

110 page 108 System Settings and Miscellaneous 14.3 Setting the image size and frame rate (Camera tab) If a camera with a Falcon frame grabber is installed, it is not necessary to make any alterations in the Camera tab Camera module for IEEE-1394 interface Settings must be made in two tabs in order to set the frame rate and obtain a proper image: Shutter and Gain on the O-Con tab of the CPanel. The settings for Brightness and Contrast usually have no effect when working with an IEEE-1394 camera. Image size (resolution) and image area with the help of the Camera Setup button on the Camera tab in System Settings.

111 SPA C SPA C SPAC SPAC System Settings and Miscellaneous page 109 Setting the resolution (image size and area) As a rule, the image height (Y-Size) is changed in order to achieve a higher frame rate. An appropriate adjustment of the width (X-Size) is also possible. The position of the visible area (X-Pos and Y-Pos) can be defined in order to ensure that the object is located within the measured area. Proposed settings The Gain should be set as low as possible for the respective frame rate. The settings listed in the following table are only guidelines. Other combinations of values for the Shutter and Gain as well as the resolution are possible. CF30 Frame rate Resolution Shutter (at medium zoom) Gain (at medium zoom) 79 fps 656x fps 656x fps 656x fps 656x fps 656x fps 656x

112 page 110 System Settings and Miscellaneous CF31/3216/4016 Frame rate Resolution Shutter Gain 25 fps 780x fps 780x fps 780x fps 780x fps 780x fps 780x CF3217 with standard optics CM3210 Frame rate Resolution Shutter Gain (at medium zoom) 202 fps 640x fps 640x fps 640x fps 640x fps 640x fps 640x CF3217 with microscope optics CM CM3253 Frame rate Resolution Shutter Gain (at medium zoom) 202 fps 640x fps 640x fps 640x fps 640x fps 640x fps 640x

113 System Settings and Miscellaneous page 111 Explanation of the parameters Mode: Various predefined camera settings can be selected here. For DSA4 we recommend the Scalable Modes which can be used to vary the image size. With the other Modes, the frame rate can be reduced at full resolution; however this is not sensible in most cases. Alterations on the tab are assigned to the currently selected scalable mode and saved in this mode. This means that you can define various scalable modes with your own standard settings. Speed: This value defines the bit transmission rate for the IEEE-1394 bus (maximum 800 Mbit/s); this setting should not be altered. X-Size; X-Pos: Width and horizontal position of the image. If the image width (X-Size) is reduced then the horizontal position of the visible area of the image can be defined with X-Pos. Y-Size; Y-Pos: Height and vertical position of the image. If the image height (Y- Size) is reduced then the vertical position of the visible area of the image can be defined with Y-Pos. Packet: Size of the data packet during transmission.! Set the maximum value. Otherwise the speeds given in the tables above will not be reached. Checking the frame rate The current frame rate is shown in the status bar at the bottom right. However, after it has been reset it takes some time for the new value to be shown. To have the current value indicated immediately after making a change you can close and re-start DSA4.

114 page 112 System Settings and Miscellaneous Camera module CF322x (high-speed option) 1. Select the Camera tab under System Settings. 2. Select the Customized option in the Format drop-down list box. 3. A prepared DCF-file, which assigns the desired frame rate in DSA4, can be loaded with the button. The files are located on the DSA4 CD-ROM under Cameras/ P1H/DCF. 4. In a second step, settings must be made in the PFRemote camera software (see below). The best way to do this is to copy the DCF files from the DSA4 CD-ROM to the DSA4 installation folder. The image height is reduced in order to achieve a higher frame rate.

115 System Settings and Miscellaneous page 113 Decoding the file name The file name contains information about the settings for the camera: The first part (x fps) specifies the desired frame rate. The second part (x lines) indicates the height of the resulting video image (in lines). The third part (x us) corresponds to the exposure time in µs. The fourth part (gain x) specifies the gain. Camera Settings in the PFRemote program The settings for the camera are made in the PFRemote program. After installing the frame grabber and the camera, this will be found in the Windows Start menu ( Instrument manual).! Adjust the parameters in PFRemote to the values indicated in the DCF file name. Please do not change any parameters other than those shown below: Exposure/Trigger tab: Set the Exposure time to the value indicated in the DCF file name. Window tab: Set the window height H to the value indicated for lines in the DCF file name.

116 page 114 System Settings and Miscellaneous Special tab: Set the Gain to the corresponding value in the DCF file name Various presets (Miscellaneous) Preliminary settings for data management and prompts can be made under Miscellaneous in the structure tree Automatically load last open database on program start Select the General tab. Select the Load the last used Results-Database option Saving / exporting messages automatically Select the Results Management tab. Activating save Select the Yes, automatically after option. each measurement (SDM) option: Saving takes place when a measurement is completed on a single drop (SDM).

117 System Settings and Miscellaneous page 115 complete measurement (MT) option: Saving takes place when all SDMs of an MT are complete. The difference between these two options is only relevant in expert mode. Save options prompt me for selecting Workspace and Project: When this option is selected, a selection dialogue box for the Workspace and the project appears before automatic saving takes place. clear data after being saved into Database successfully: When this option is selected, the measurement data are deleted from the Results-Monitor after automatic saving has taken place. Exporting data automatically Data can be exported automatically as a CSV file.! Only the columns which appear in the results monitor are exported. Select the export Results-Data to option. Select the required directory by means of the button. The file name will be assigned automatically in the following form: MT-Name_SDM-Name_DateYYYY-MM-DD_TimeHH-MM-SS.csv Switching prompts on and off Select the Prompt-Dialog Management tab.! The prompts which appear by default (see figure above) interrupt the sequence for essential user intervention. They should only be switched off in exceptional cases (e.g. in DSA4 remote mode).

118 page 116 System Settings and Miscellaneous Selectable prompts Checkbox Prompt Default setting Prompt for Sample Position: Measurement Prompt for Needle Position: Standby Prompt for Needle Position: Deposition Prompt for Needle Position: Parking Prompt for Setting Baseline Prompt for Creating a New Measurement Series Request to position the sample Request to set the needle standby position Request to set the needle deposition position Request to set the needle parking position Request to set the baseline manually Query as to whether a new series of measurements is to be generated in the results monitor when important measuring parameters are changed (e.g. when changing the test liquid). If this option is not selected, a new series of measurements will be generated without prompting. Prompt appears Prompt does not appear Prompt appears Prompt does not appear Prompt appears Prompt does not appear

119 Special instrument components page Special instrument components 15.1 Tilting tables! Please refer to the safety information in the instrument manual regarding the control of the PA3220 external tilting table Safety information for the internal tilting table! If the needle is positioned too low, the tilting table can hit the needle when it moves. Procedure for manual dosing unit Position the dosing unit so that the needle lies outside the range of movement of the tilting table. Procedures for software-controlled dosing unit In Continuous/Manual mode (see below): Position the dosing unit so that the needle lies outside the range of movement of the tilting table. In Range mode (see below): The needle moves automatically to the Standby position before the tilting table moves. Define a Standby position ( Chapter 5.7.2) for the needle outside the range of movement of the tilting table Controlling and programming the tilt Select the Axes tab in the CPanel. Select the Tilting Table option from the lefthand drop-down menu. The Parking, Stand-by and Deposition positions are not used for the tilting table.

120 page 118 Special instrument components Movement mode Select the required movement mode in the right-hand drop-down menu. Continuous or Manual: Continuous movement. The movement is started with the arrow buttons Up and Down and stopped by clicking on the same button. In this mode, you can set the table at a required angle directly by entering it in the text box and confirming with <Return>. Range: The tilting table moves between two fixed tilting angles. The tilting table first moves to the angle under from and then to the second angle set under to. The movement is triggered with Go and cancelled with Stop (the button label changes).

121 Special instrument components page 119 Speed of movement (Velocity) You can choose between three different speeds for the tilting table movement, Slow, Normal and High. Resetting to the starting position (initialisation) Select Reset Zero Position from the right-hand drop-down menu Dosing and starting the measurement Automatically linking a measurement or video recording to the tilting table movement The measurement or video recording can only be linked to the tilting table movement in the Range mode. Online measurements are not possible with the PA3240/4240 internal tilting table. A video of the tilting process must always be recorded for the measurement. When high image rates are used for the video recording, the live image may be deactivated. Select Options from the right-hand drop-down menu. Select the Extra Parameters tab.

122 page 120 Special instrument components Invoke measurement at begin of rotation: The measurement or video recording starts as soon as the from position selected in Range mode has been reached. Stop measurement at the end of rotation: The measurement or video recording is stopped when the to position selected in Range mode has been reached. Combining with the Mode tab of the CPanel Measurements with the tilting table can be combined with the measurement start options in the Mode tab of the CPanel ( Chapter 7.5). In doing so, dosing will be carried out using the settings under Deposition. When the Invoke measurement tilting table option is selected, the selection under Start Measurement in the Mode tab has no significance. In all cases, the measurement or video recording is not started until the tilting table moves. When the Invoke measurement tilting table option is deactivated, a measurement or video recording can be carried out with the settings in the Mode tab without moving the tilting table. Starting a video recording manually When the Invoke measurement tilting table option is deactivated, the video recording can be started at any time by means of the button. The Video Recording option in the Mode tab of the CPanel must also be selected. When the button in the Mode tab is clicked, the time required for the tilting table movement in Range mode is calculated automatically and used as the recording time. The recording time is updated if the tilting table settings are changed. The Continuous mode can also be used for the tilting table movement when recording a video manually.

123 Special instrument components page Video evaluation for the PA3240/4240 internal tilting table When measuring with the internal tilting table, the respective tilting angle must be taken into account in the evaluation of every image. Video images are therefore evaluated differently from other measuring methods. Load the video to be evaluated ( Chapter 9.3.2). Activating video evaluation Select Working with ITT (Internal Tilting Table) in the video window context menu. Setting breakpoints for the baseline The baseline is different for every single image. In order to be able to evaluate the whole video, the progression of the baseline height and slope is determined with the help of breakpoints. For this purpose, the baseline for at least five images of the video is defined by the user. For information on navigating within the video, please read Chapter 9.5. For information on determining the baseline, please read Chapter The baseline can often be determined automatically for a table which has not yet been tilted. When the table has been tilted, it must be defined manually.

124 page 122 Special instrument components 1. Select the first frame in the video. Determine the baseline. 2. Select Set Baseline Guide in the video window context menu. 3. Select the last frame in the video. Determine the baseline. Select Set Baseline Guide from the menu once more. If the drop leaves the image during the video: Set up the last frame in which the drop still appears completely in the frame. The original line is rotated through the tilting angle corresponding to the frame by double-clicking on the baseline. The height can then be defined and the baseline slope finely adjusted.

125 Special instrument components page Repeat the procedure for at least three further frames which are spaced so as to divide the range between the first and last selected frame as equally as possible. 5. Select Apply Baseline Analysis Results in the video window context menu. The progression of the analysed baseline will be saved and used for each subsequent video evaluation. Carrying out an evaluation Select the required method of drop shape analysis ( Chapter 7.2). Only the Tangent-1 or Tangent-2 methods should be used due to the asymmetry of the drop when tilted. Carry out the video evaluation as described in Chapter 9.6. Deleting breakpoints and analysed baseline progression Select Remove Baseline Guide in the video window context menu.

126 page 124 Special instrument components 15.2 DSA100M (Micro): Sample table control and dosing The DSA100M comes with an optional sample table PS3240 and a piezo dosing unit Controlling the PS3240 sample table The PS3240 micro-step sample table has an x-axis and a y-axis. The axes are controlled in the same way as the standard axes with the difference that the range is limited to 50 mm but the position can be accurately controlled to 1 µm Controlling a Piezo dosing unit DS3234 For controlling a dosing unit DS3232, please read the concerning manual of the accessory. Meaning of the parameters Drops are produced by applying a current of defined voltage and duration to the piezo element. The drop size results from the parameters set for drop creation. Voltage: The strength of a single pulse is given by the voltage entered. Period [µs]: For several drop (Drop Count > 1) the Period sets the time distance between the start of a pulse and the start of the following one.

127 Special instrument components page 125 Pulse [µs]: Length of a single pulse. The pulse cannot be longer than the period length. Drop Count: Number of drops produced. Is linked to the number of pulses, i.e. the number of periods. Schematic presentation of the parameters Voltage Pulse Period Drop Count Notes concerning settings and dispensing Higher viscosities require an increased voltage. To obtain small volumes, the pulse width can be reduced. However, it may then be necessary to increase the voltage. If no drop is produced, this may be because the voltage is too low. If the drop splashes or sprays, this may be because the voltage is too high. To find the dosing position in the image ( DSA100M manual), it is helpful to set the dosing mode to Continuous. The continuous liquid stream produced in this way is easier to find.

128 page 126 Special instrument components Guide values determined by KRÜSS Liquid Water Diiodomethane Voltage [V] Period [µs] 10,000 10,000 Pulse [µs] Adjusting the humidity for HC10 When the HC10 humidity chamber is connected to the measuring instrument, a separate tab with the title Mix is displayed for controlling the humidity. Notes on use! Make sure that the storage tank for the chamber is always at least one-third full of distilled water ( Refer to instrument manual). Wait before starting the measurement until the humidity inside the chamber has reached the desired value. Variations of a few percentage points about the setpoint are normal. Currently, it is only possible to read out the temperature inside the chamber with the help of an external sensor. Desired and actual value The desired value for the Humidity is entered in percent. The actual value measured by the humidity sensor inside the chamber is shown in the status line.

129 Appendix page 127 Appendix I Entering the syringe dimensions for disposable syringes Procedure 1. Select Tools System Settings from the menu. Select Syringe Assignment from the list in the structure tree on the left. 2. Select the line for Syringe 1. Click on the button. The following dialogue box will appear: 3. Enter the dimensions according to the following table. Click on OK. Dimensions Syringe Volume (Max. capacity) Inside diameter (Hube diameter) Height of syringe scale (Piston stroke length) SY20/22 (glass syringe) SY3601 (disposable syringe) 500 µl mm 60.0 mm 1000 µl mm 57.7 mm For other syringes, the dimensions must be determined by the user.