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1. Introduction

The KSV QCM-Z500 microbalance is a computer controlled quartz crystal

microbalance based on impedance analysis for determining the frequency (f)and the quality of resonance (Q) of quartz crystals in a gaseous or liquidenvironment. In other words, the QCM-Z500 microbalance is a mass sensingdevice with the ability to measure very small changes in mass on a quartzcrystal resonator in real-time.

The KSV QCM-Z500 microbalance can measure the quality factor (Q),dissipation (D) and different harmonics of the quartz crystal giving additionalinformation on the state of the layer adsorbed to the quartz crystal surface.

The KSV QCM-Z500 microbalance includes the main electronics unit with

built-in impedance analyzer software, a measuring chamber for fluid phases,quartz sensor crystals with a variety of optional coatings and a Windowsbased program to control it all. A temperature control unit can be supplied ifrequired.

The KSV QCM Impedance Analyzer software included with this instrumentallows the easy operation of the experiments, which can be modified to anyneeds. The data is stored on the hard drive in a database and can beretrieved for analysis later. The data files can easily be exported in a variety offormats if another data reduction software is preferred.

1.1 Purpose of This Manual

This manual describes all the necessary steps to get the QCM-Z500microbalance instrument operational, starting from the mechanical setup andthrough software installation, calibrating the instrument, makingmeasurements and finally analyzing the data obtained. Please read thismanual carefully before using the KSV QCM-Z500 microbalance and keep itavailable to ensure the maximum performance of the instrument.

1.2 MaintenanceThe hardware of the QCM-Z500 microbalance is manufactured to the highestquality standards and when used properly it should yield a trouble-free use fora long time. There are no specific maintenance requirements or proceduresfor the instrument that can be taken in order to prevent breakdowns. If theinstrument is set up and used as described in this manual only parts exposedto normal wear and tear might need to be exchanged.

WARNING! The original mains cables of the instrument and the computermust always be used and connected to a grounded wall socket. Ungrounded

wall sockets may cause dangerous voltages between the instrument, thecomputer and the real ground.

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1.3 Physical Description

The KSV QCM-Z500 microbalance consists of the main electronics unit and ameasurement chamber, optionally a temperature control unit as well. Themain electronics unit is the most central part of the KSV QCM-Z500microbalance, it is in fact a Linux based computer with factory-installedsoftware. It takes care of the communication between the measurementchamber and the data collecting computer through a local area networkconnection.

Figure 1.1:The axial measurement chamber (left) and the main electronicsunit.

The axial flow measurement chamber is the standard chamber and isspecially designed to ensure the best performance of the instrument byproviding a controlled environment for the quartz sensor crystal during themeasurements. It contains a temperature loop in which the sample fluid canbe thermostated before it flows into the actual measuring chamber or into thewaste channel. The tubing of the temperature loop is made of Viton, seesection 11. Appendix A - Chemical Compatibility of Viton of this manual for

details on the chemicals that can be used with Viton.

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1.3.1 Main Electronics Unit

The main electronics unit is a computer that sends and receives data from themeasurement chamber. It connects to the measurement chamber with a 3-pinD-connector located on its front panel. A local area network is used to connect

to the computer running the experiment, the network cable socket is locatedon the back panel. A power supply is also necessary, both 110-120VAC and220-240VAC can be used but check that the fuse is on the correct settingbefore connecting to the mains (see section 3.1 Mechanical Installation).

Figure 1.2: Connections of the QCM-Z500 microbalance main electronicsunit.

1) Fuse 4) Network connection port tocomputer (RJ-42)

2) Power connection and On / Offswitch

5) Com port (RS-232, not for usewith the TCU)

3) Connection port to measuringchamber (3-pin)

6) Reset button

NB) The Com port (number 5 in figure 1.2) at the back of the main electronicsunit is used onlyfor loading the internal Linux program at the factory and notfor use with the Temperature Control Unit (TCU)!

At the top of the front panel there is a green LED lamp which blinks when theinstrument is turned on whilst the internal operating system loads. This LEDwill blink for about 1 minute. When the LED light stops blinking the Linuxoperating system has been loaded and the main electronics unit is ready formeasurements.

The reset button (#6 in figure 1) reboots the main electronics unit.

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The internal components of the QCM-Z500 main electronics unit are shown infigure 1.3 below.

Figure 1.3:The internal components of the main electronics unit.

1) Power switch and Fuse 6) A/D-converter card

2) Transformer 7) Oscillator card 2

3) Fan 8) Oscillator card 1

4) Connection port to computer (RJ-42)

9) Detector card

5) Com port (RS-232, not for usewith the TCU)

10) Processor board

1.3.2 Axial Flow Measurement Chamber

The measurement chamber is where the actual experiment takes place.There are several models available of which the axial flow measurementchamber is the standard one. Common to all is that a quartz crystal is cleanedand placed inside so that it rests on two electrodes. The electrodes providealternating current that causes the crystal to move due to the piezoelectriceffect inherent in quartz crystals. A fluid can flow across one side of thecrystal.

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Figure 1.4:The axial flow measurement chamber.

The name of the axial flow measurement chamber comes from the way thefluid moves through the unit. The inlet tube is at the top of the instrument, andthe fluid flows down through a thermostation loop to either the crystal itself inthe measuring chamber and then out or out directly (used for cleaning thetubing between samples).

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Figure 1.5:Flow direction of the sample in the axial flow measuring chamber.

The volume of the temperature loop is around 3 ml, and the volume neededfor flushing the actual measuring chamber is 1 ml. The flow direction of thefluid is controlled by a three-way valve. All parts of it in contact with the fluidsample are made of acid resistant stainless steel except the o-rings holdingthe crystal sensor, the tubing used in the temperature loop and the outletsfrom the measurement chamber which are all made of Viton. The o-rings andtubing can be easily exchanged to another material if needed, Viton has beenchosen because of its high resistance to organic solvents. The actualmeasuring chamber is made of Teflon (PTFE) in order to meet the chemicalcompatibility standards and for ease of cleaning. The main body of themeasurement chamber is made of aluminum to maximum heat transfer.

Figure 1.6:Main components of the axial flow measuring chamber.

1) Upper module 5) Temperature control socket

2) Lower module 6) Grounding for crystal surface

electrode

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3) 3-way valve control knob 7) Upper outlet for Bypass tube

4) Heat sink 8) Lower outlet for Chamber tube

The axial measurement chamber also includes the sample inlet and the 3-pinD-connector socket on the lower module which links the measurement

chamber to the main electronics unit. The detailed components of the uppermodule (#1 in figure 1.6) of the axial flow measuring chamber are shownbelow.

Figure 1.7: Components of the upper module of the axial flow measuringchamber.

1) Fitting 11) 3-way valve

2) Crystal 12) Crystal chamber body

3) Teflon crystal holder 13) Centering pin

4) Center tube 14) Crystal support body5) Knob 15) Crystal support nut

6) Flange bearing 16) Thermostation spiral block

7) Viton O-ring 17) Thermostation outer block

8) Viton O-ring 18) Shaft

9) Viton O-ring 19) Upper module cover

10) Crystal support spring-loadedpins

20) Top plate

The detailed components of the lower module (#2 in figure 1.6) components

are shown below.

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Figure 1.8: Components of the lower module of the axial flow measuringchamber.

1) Circuit board module 6) Bottom plate

2) Grounding for crystal surfaceelectrode

7) Lower module cover

3) Temperature control socket 8) Heat sink

4) Peltier element 9) Lower thermostation block

5) Rubber feet 10) Centering pin

1.3.3 Quartz Crystal Sensors

The quartz crystal sensor is the heart of the instrument. The standardfundamental frequency of the crystals delivered with the QCM-Z500microbalance is 5 MHz, although crystals with up to 50 MHz can be used withthe instrument. KSV Instruments can also provide crystals with a fundamentalfrequency of 10 MHz. The electrodes on the crystals are made of gold andhave a keyhole configuration where the contacts for the electrodes are on the

same side. The electrode in contact with the sample fluid is grounded andmuch larger in order to make sure that the processes taking place on thequartz crystal surface are as similar as possible over the entire surface.

The gold surface of the electrodes can easily be modified for specialapplications or needs, for example by self-assembled monolayers, LBdeposition, spin coating, vapor deposition etc.

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Figure 1.9: The quartz crystal electrodes and quartz crystals with differentcoatings.

Apart from the standard gold-coated sensor crystals KSV Instruments canprovide a variety of other surfaces upon request, these include:

Metals: Ag, Al, Ca, Cr, Cu, Li, Mg, Ni, Sn, Pt

Inorganic: ITO, LiF, MgF2, SiO, SiO2, TiO2, ZnS, Ti3NO

Polymers: PANi, Teflon, PMMA, PS, PC, PE, PP, AKD

The standard crystal sensor has a fundamental frequency of 5 MHz, adiameter of 14 mm and a gold coating. Other frequencies and coatings can beobtained by request.

1.3.4 Optional Temperature Control Unit

The standard axial flow measuring chamber always contains the Peltierelement (#4 in figure 1.8), the heat sink (#8 in figure 1.8) the temperaturesensor inside the thermostation block parts and a fan, but in order to make

use of these a separate Temperature Control Unit is required.

The Peltier element enables heating or cooling of the thermostation block (#9in figure 1.8) and hence adjusting the temperature of the measuring chamber.The temperature can be either set manually from the Temperature ControlUnit (figure 1.10) or with the computer by using the KSV QCM ImpedanceAnalyzer software. The useful temperature range is between +10 and +50 oCwith a resolution of 0.1oC.

Figure 1.10:Front panel of the optional Temperature Control Unit.

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2. Brief Instructions

This section describes briefly the steps necessary to install the KSV QCM-

Z500, calibrate it and perform a basic measurement. However, it is stronglyrecommended that this manual is read completely and thoroughly as itcontains valuable information on the required procedures and the working ofthe instrument. Use this section as a checklist and a reference once the actualprocedures are familiar.

2.1 Installation Procedure

Lift the KSV QCM-Z500 microbalance instrument onto a steady table. Install the network card delivered with the instrument onto the

computer. Connect the power cord and the network cross-cable to the instrument.

Plug the power cord into a grounded wall socket and connect thenetwork cross-cable to the installed network card. Connect the signalcable between the main electronics unit and the measuring chamber. Ifa Temperature Control Unit (TCU) is used connect it to the fan,measurement chamber, power supply and computer (note that theTCU connects directly to the computer, and notto the main electronicsunit).

Turn on the power of the main electronics unit and wait for at least 1

minute or until the light on the front panel stops blinking.

Define the IP address of the installed network card as 192.168.168.1and the Subnet mask as 255.255.255.0 in the Windows NetworkConnections screen.

Install the KSV QCM Impedance Analyzer software from the softwareinstallation CD by running setup.exe from the root of the CD.

Start the KSV QCM Impedance Analyzer software by choosingPrograms > QCM > QCM from the Windows Start menu. Check thatthe Status: bar in the software says Program ready formeasurements. If this is not the case check the IP address of thenetwork card, the address of the QCM-Z500 microbalance (should be192.168.168.168) from Edit > Device Parameters in the KSV QCMImpedance Analyzer software and that the internal program is loadedfrom File > Load Program. Also try rebooting.

2.2 Calibration

From the menu bar of the KSV QCM Impedance Analyzer softwareopen Controls > Calibrate.

Insert the appropriate information and press Calibrate.

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Remove the upper module of the axial flow measurement chamber andinsert the calibration tool so that the short circuit part is in line with theelectrodes and the guidance pole goes through the appropriate hole.Press down gently and press OK.

Wait. When instructed to do so remove the calibration tool and pressOK.

Wait. When instructed to do so replace the calibration tool, this timewith the known resistance in line with the electrodes and press OK.

2.3 Cleaning

Remove the upper module, unscrew the nut and take away the teflonchamber construction and the crystal.

Let the cleaning and the rinsing liquids (often pure ethanol and ion-exchanged water are acceptable) flow through the Bypass and theChamber loops.

Wash the interior of the upper module with the cleaning and the rinsingliquids.

Wash the crystal with either chromic acid or a Piranha solution, andrinse with ethanol and ion-exchanged water.

Wash the teflon chamber pieces with the cleaning and the rinsing

liquid.

Replace the chamber pieces and the crystal into the upper module andscrew on the nut. Replace the upper module on top of the lowermodule.

2.4 Measurement Procedure

Check that the valve is set on Stop and fill the reservoir with thebackground liquid (often water). Turn the valve to the Bypass settingand after a few drops have come out return the valve to the Stop

position.

Turn the valve to the Chamber setting and after a few drops have comeout turn the valve to Stop.

If a Temperature Control Unit is used, set the target temperature fromeither the unit itself or the QCM-Z500 Impedance Analyzer program atControls > Temperature Controls. Wait 30 minutes for the instrumentto reach thermal equilibrium.

Click the New Experiment icon. Fill in the relevant information in the

Experimental Setup screen. Use Edit Database to add new items onthe drop-down menus, press Start when finished.

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Select Automatic as the measurement Method and select all of theharmonics. Press Start. Wait for the frequencies of the resonances tosettle.

Empty the reservoir and open the Bypass. Let the background liquiddrain and then pour the sample to the reservoir. When a few milliliters

of the sample have come out from the bypass switch to Stop to wait forthermal equilibrium. Then turn the valve to Chamber.

Allow a few milliliters to pass through the chamber to flush it. Close thevalve and wait for the frequencies to stabilise. Flush with thebackground liquid again or introduce the next sample according to whatis being measured. Press Stop when finished.

2.5 Data Analysis and Reduction

Data analysis is carried out by another program called BrowseExperiments. Open it from either the desktop (QcmBrowse) or fromStart > Programs > QCM > QcmBrowse.

Set the search parameters for the experiment wanted if necessary andselect it from the Experimentsbox. Right-click on it and select Graph toview the graph of the specified harmonic. Change the variable of the x-axis or the y-axis, or add another y-axis from the top right corner of theBrowse Experiments window. Export a graph from Graph > ShowMenu > Export.

Export data either by pressing the Copy to Clipboard icon and pastingin another program (e.g. Notepad in order to save the data in ASCIIformat) or by selecting File > Export/Delete Data. Send theexperiments to be exported to the Destination List and press Export.The file created is only useable by a KSV QCM-Z500 ImpedanceAnalyzer program, use this feature to make backups or to transfer thedata to another computer with the software. Import an experiment filefrom File > Import Data.

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3. Installation

3.1 Mechanical Installation

The KSV QCM-Z500 instrument is delivered in one crate. The crate should beopened carefully and checked to see that it contains the following items:

Main electronics unit

Standard axial flow measuring chamber

Calibration tool

5 gold coated quartz crystals

Network card

Power cord

Network cross-cable

Signal cable between the main electronics unit and the axial-flowmeasuring chamber

Software and manual on CD

Unwrap the plastics around the unit and place the QCM-Z500 on a steadytable, preferably with running clean (ion-exchanged) water nearby.

The KSV QCM-Z500 microbalance has an internal computer running a Linuxoperating system for taking care or the basic calculations duringmeasurements and communications between the instrument and computer.The communication between the computer and the QCM-Z500 microbalanceis carried out by a local network connection. This means that the computerused with the instrument needs to have a network card installed solely for theQCM-Z500 microbalance, and if the network card was already in use (forexample to connect to the internet or an intranet) another one needs to beadded. One is provided with the instrument.

The QCM-Z500 microbalance has been fitted with an IP address which is192.168.168.168 . It can be changed but to do so please contact KSVInstruments directly.

3.1.1 Installing the Network Card

Shut down the computer and open the cover of the computer's central unit.Find a free PCI slot and put the network card delivered with the instrument inthis slot. Remember to attach the network card properly so that it cannotmove in its slot. Start the computer, preferably with Windows 2000 or XP.

Windows will automatically install the network card and no drivers are needed.However, if it cannot be automatically installed (especially common with older

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versions of Windows) Windows will ask for drivers for the network card.Please insert the diskette or CD-ROM from the network card box and directWindows to this media if that should happen.

3.1.2 Connecting Cables

The cables used with the KSV QCM-Z500 microbalance have been chosen sothat no incorrect connections can be made. Before plugging in the powersupply check whether the fuse (number 1 on Figure 2 of 1.3 PhysicalDescription) is in the correct setting. Two different voltage ranges areavailable, 100-120VAC and 220-240VAC. Look at the text at the bottom of thefuse next to the arrow pointing down, this indicates which voltage setting iscurrently in use. To change to the other setting remove the fuse, turn it so thatthe supplied voltage is indicated on the bottom and reattach it.

Figure 3.1:Removing the fuse.

A) Power Supply

Plug in the power cord to the backside of the main electronics unit (#2 infigure 2 in section 1.3 Physical Description). For safety reasons always usegrounded wall sockets for the power supply. If the Temperature Control Unit isavailable then also connect a power cord to the backside of the unit (seeFigure 8 in section 1.3 Physical Description).

B) Measurement Chamber Communication

Connect the 3-pin signal cable between the 3-pin D-connector on the frontside of the main electronics unit (#3 in Figure 2 in section 1.3 Physical

Description) and the 3-pin D-connector on the front side of the standard axialflow measuring chamber (#9 in Figure 4 in section 1.3 Physical Description).

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The 3-pin D-connectors can only be connected one way, though if enoughforce is applied it is possible to attach them in the wrong way. Please avoiddoing so. Remember to tighten the screws on the plugs to avoid accidentallyremoving the cable.

Figure 3.2:The connector cable between the main electronics unit and themeasurement chamber.

C) Network Cable

As this is a connection between two computers a cross network cable isrequired. Attach it to the RJ-42 connector (#4 in Figure 2 in section 1.3Physical Description) on the backside of the main electronics unit and thento the network card on the computer.

Figure 3.3:The back of the main electronics unit.

D) Optional Temperature Control Cable

If the optional Temperature Control Unit (TCU) is available then two cablesneed to be connected from the TCU to the measurement chamber. These

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cables are ready connected to the TCU at the factory, the red cable connectsto the lower module of the chamber (#7 Figure 4 in section 1.3 PhysicalDescription for the standard axial flow measurement chamber) and the blackcable connects to the fan. The red cable receives the temperature readingfrom the thermometer in the module and controls the Peltier element while the

black cable controls the fan.

Figure 3.4: Connecting the Temperature Control Unit to the measurementchamber.

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3.2 Software Installation

3.2.1 Setting Up a Local Area Network Connection

The QCM-Z500 microbalance is directly connected to the PC through a localarea network connection. In order for the communication to work properly thelocal area network parameters for the installed network card should be set inWindows according to the instructions below.

Make sure that the network card is installed in the computer and connected tothe QCM with the cross network cable as explained in section 3.1MechanicalInstallation. Turn on the power of the main electronics unit and wait for about1 minute for the internal Linux operating system to load. The green light onthe top of the front panel stops blinking once the main electronics unit is

ready.

Open Network Connections from the Control Panel. The exact locationdepends on the version of Windows used, the Control Panel can usually befound from the Start menu. In the Control Panel the icon NetworkConnections exists either separately or under Network and InternetConnections >Network Connections.

Figure 3.5: The Network Connections window.

Double-click on Local Area Connection.

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Figure 3.6: The Local Area Connection Status window.

Press Properties.

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Figure 3.7: The Local Area Connection Properties window.

Select Internet Protocol (TCP/IP) and press Properties.

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Figure 3.8: The Internet Protocol Properties window.

Select Use the following IP address option and fill in the IP address192.168.168.1 and Subnet mask 255.255.255.0 as shown above. Press OK.

The communication path between the QCM-Z500 instrument and PC has nowbeen defined. Sometimes it is necessary to restart the computer and theQCM-Z500 microbalance before the connection is activated.

NB! It is also possible to connect the QCM-Z500 microbalance directly to alarger internal local area network (intranet). In such cases the QCM shouldhave an individual IP address reserved for it so that it can be connected to thelarger network in the same way as any other computer. This IP address isthen programmed into the QCM-Z500 microbalance by KSV Instruments incooperation with a local computer support person either before shipping oron-site during installation and training. However, the procedure for setting upthis kind of connection is not described here.

3.2.2 Installing KSV QCM Impedance Analyzer Software

The KSV QCM Impedance Analyzer software is available on the CD-ROMdelivered with the instrument. Insert the CD and open My Computer. Find theCD drive (D:\ on most computers) and open it. Double click on the file

setup.exe.

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The installation program begins with this window. Press Next to continue.

Fill in the Name and Company fields, and press Next.

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To change the installation directory press Browse, otherwise press Next tocontinue.

To change the folder name in the Start menu type it into the ProgramFolders field, otherwise press Next to continue.

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Press Next to continue.

Wait for the installation to complete itself.

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Press Finish to complete the software installation process. To create ashortcut to the QCM program open My Computer and select the folder towhich the QCM software was installed (by default C:\ProgramFiles\KSV\QCM). Right-click on the file QCM.exe and select Send To >

Desktop (create shortcut) from the drop-down menu.

To start the program either double-click on the shortcut on the desktop or fromthe Start menu at Start > Programs > QCM > QCM. This opens the mainmenu of the KSV QCM Impedance Analyzer software.

3.2.3 Checking Software Installation and Communication

First turn on the power of the main electronics unit and let it load its internalprograms for ca. 1 minute (once loaded the blinking green light changes to asteady green light). Start the software by double-clicking on the QCM shortcuton the desktop or choose Start > Program > QCM > QCM from the Startmenu. If the connection between the main electronics unit and the computer isworking the Status: field in the lower right corner will state that the instrumentis Ready for a new Experiment.

Figure 3.9: The QCM Impedance Analyzer main window.

If this is the case then the instrument needs to be calibrated beforemeasurements can be performed. The calibration procedure is described insection 3.3 Calibration below. However, if the main electronics unit is notturned on, the IP address in the KSV QCM Impedance Analyzer software forthe QCM-Z500 microbalance is not correctly defined or there is a problemwith the cables connecting the main electronics unit to the computer thefollowing window will appear:

Figure 3.10: The Error! message.

If this window appears check that the power is turned on and then press OKto continue. In the main menu if the Status: field says Program not loadedfor QCM unit then first try to close and restart the program. If the problempersists then try the following, though do not hesitate to contact your local

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distributor or KSV directly. Often with Windows based programs a problemcan be fixed by restarting the computer so that should be attempted as well.

Check that the green light on the top of the front panel of the mainelectronics unit is on and that it is not blinking. If it is not on check the

power cable for the unit and check that the switch in the back of theunit is in the "on" position, that is with the I pushed towards the unit andO sticking out. If the light is blinking the processor inside the unit is stillstarting up (like turning on the computer it takes time) and wait for it tostop blinking. This should take about a minute.

Check the IP address in the local area network connection by repeatingthe steps described in section 3.2.1 Setting Up a Local Area NetworkConnection. Make sure that the IP address is defined as192.168.168.1 and that the Subnet mask is 255.255.255.0.

Check the cable connecting the main electronics unit to the computer.Do this for example by removing the network cable from anothercomputer connected to the internet or an intranet and replacing it withthe one connecting the unit and the computer. If the connection worksthen reconnect the cable and try restarting the software.

Check the IP address in the KSV QCM Impedance Analyzer software.Do this by selecting Edit > Device Parameters from the main menu.

Check that the IP address is 192.168.168.168. If necessary the lastthree digits can be altered as long as they do not match the IP addressof the local area network connection. Press OK and restart the

software.

Figure 3.11: Device Parameters. Indicate which measurement chamber isconnected and whether a Temperature Control Unit is available.

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Check if the internal program for the QCM is loaded. Select File >Load Program from the main menu. If the text field says Done thatmeans that the internal QCM software has been successfully loaded. Ifthe field is empty press Load Code to attempt to load the program

manually. This will only work if the connection between the mainelectronics unit and the computer is working.

Figure 3.12: Load. If the field is empty pressLoad Codeand wait for the textDoneto appear.

Check if the connection between the main electronics unit and thecomputer is working. After loading the code successfully select File >Connect from the main menu.Press Connect Qcm if no text is visible.If the connection is working the following text will appear Looking upqcm host, Connecting, Connected, Hello from QCM. Ready torockn roll will appear.

Figure 3.13: FormIPClient. Check the connection to the QCM, receiving theabove message indicates that the connection is fine.

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3.3 Calibration

After installing the software and checking that the KSV QCM ImpedanceAnalyzer software and the QCM-Z500 microbalance instrument arecommunicating with the computer the instrument has to be calibrated. Eachmeasurement chamber type has to be individually calibrated, and thefollowing procedure applies to all chambers. The calibration is done in 3steps, with a short circuit, an open circuit and a known resistance. SelectControls > Calibrate from the main menu window to open the Calibrationcontrols window.

Figure 3.14: Calibration controls. Select the measurement chamber availableand pressCalibrate.

If an alternative measurement chamber is in use indicate so in theMeasurement chamberbox. With a new chamber remember to add it to thedatabase first, select Edit > Database or see section 6. The Database fordetails. In the Calibration Parametersbox fill in the values for the fundamentalfrequency F0 (usually 5 MHz), the bandwidth BW (usually 2 MHz) and theknown resistance R (usually 100 Ohm).

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In most circumstances the harmonics are very useful so it is advisable that the11th harmonic is chosen in the Last harmonic includedbox. Press Calibrateto begin the calibration.

Figure 3.15: Calibration instructions, phase 1.

Lift the upper module away from the standard axial measurement chamber toexpose the electrodes. Insert the calibration tool so that the short circuit partof it is in line with the electrodes and the guidance pole goes through thedesignated hole on the tool. Press the calibration tool down gently and press

OK.

Figure 3.16: The calibration tool.

The mouse cursor changes to show an hourglass. After a while (even up to 1minute) the following window will appear.


Remove the calibration tool from the measuring chamber and press OK.

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Wait until this window opens. Replace the calibration tool into themeasurement chamber, this time with the known resistance part in line withthe electrodes. Press the calibration tool down gently and press OK

Figure 3.19: Calibration complete.

Calibration has been completed, press OK to start making measurementswith this chamber.

Calibration of the QCM-Z500 microbalance should only be necessary the firsttime the instrument is installed. However it is recommended that theinstrument is recalibrated every 6 months and each time the instrument ismoved, even from table to table.

The calibration of the instrument can easily be checked by selecting Controls> Test from the main menu.

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Figure 3.20: Test Controls. Select the test conditions and pressStart.

Press Start to see the impedance and phase curve as a function offrequency. By placing the calibration tool in the shortcut orientationimpedance should show a value close to zero, while changing to theresistance orientation of the calibration tool should show an impedance valueof the known resistance (usually 100 Ohm). If this is the case the instrument

calibration is fine, if not then it is recommended to recalibrate the instrument.

For more information on the Test Controls screen please see section 7.Testing and Troubleshooting.

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4. Making a Measurement

4.1 Overview

Once the QCM-Z500 microbalance instrument has been installed and thecommunication between the instrument and the computer is established theinstrument is ready to make measurements. Using the QCM-Z500microbalance is straight forward, but there are certain steps that have to bedone in order to obtain good and reproducible results and those are: cleaningthe measuring chamber, cleaning the quartz crystal, assembling themeasurement chamber, preparing the samples, filling the flow system andmeasuring chamber with a background liquid, starting the software andcollecting the datapoints.

Each step is described in detail below in order to guide the user throughmaking a complete measurement. It is advisable to make the firstmeasurements with either pure liquids or a series of glycerol solutions in orderto get a feeling for the instrument before starting with the actualmeasurements.

The KSV QCM Impedance Analyzer software is an easy to use Windowsbased program capable of being used for various types of experiments, to logdata with real-time graphing and to review results from previous experiments.

The software should be used with Windows 2000 or XP operating systems.Experimental data is stored directly to the hard drive in a single databaselibrary during an experiment. To access previous measurements an additionalprogram, the Browse Experiments, is available. Through it specificmeasurements can be found by searching with the user name, file name,substance used or date of the experiment. Data can be exported as an imageof the graph, as comma or tab delimited lists for use with a spreadsheetprogram or in ASCII format.

4.2 Preliminaries

4.2.1 Starting up the QCM-Z500

When the power of the main electronics unit is turned on, the QCM-Z500microbalance starts to boot up the internal Linux computer. A flashing greenlight on the front panel of the unit indicates that the computer is still loading,much like starting up a computer takes a few minutes. The booting processtakes about 1 minute. Do not open the KSV QCM Impedance Analyzersoftware before booting has finished and the green light has stopped flashingor the connection cannot be made and the software must be restarted.

4.2.2 Cleaning the Axial Flow Measuring Chamber

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In order to have stable and reproducible measurements it is necessary to usea good cleaning procedure for the measuring chamber, i.e. its flow systemand the parts in contact with the sample fluids. The cleaning of the flowsystem and the measuring chamber parts is therefore recommended beforeand immediately after each measurement.

The standard axial flow measurement chamber usually requires a rinse of theflow system and the measuring chamber parts with extensive amount ofethanol followed by ion-exchanged water to be sufficiently clean. However itmight be necessary to use other liquids for cleaning, and finding theappropriate way of cleaning depends largely on the type of experiments soproper cleaning procedures develop by experience.

Here is the recommended method for cleaning the axial flow measuringchamber:

1. Lift the upper module separate from the lower module and take it to asink. Set it down upside-down, unscrew the crystal support nut andremove all of the teflon chamber parts and the guidance pole.

Figure 4.1: Separating the upper module of the axial flow measurementchamber.

2. Set the upper module upright again, turn the valve to the Chamberposition, fill the reservoir with an appropriate cleaning solution and letthe liquid pass through the flow system. Repeat this for each cleaningand rinsing solution (often pure ethanol and ion exchanged water areenough) at least 3 times.

3. Turn the valve to the Stop position and turn the upper module of theaxial flow measuring chamber upside down so that the crystal chamberbody is upwards. Rinse the inner compartment of the crystal chamberbody first with the cleaning solution and then with the rinsing solution.

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4. Dry the flow system and the inner compartment of the crystal chamberbody either by using an aspirator or by blowing nitrogen through thesystem.

5. Clean the 2 Viton o-rings and the teflon crystal holder with appropriatecleaning and rinsing solutions.

Figure 4.2:The crystal support nut, o-rings, teflon chamber, crystal andguidance pole.

6. Dry the o-rings and teflon crystal holder by either using an aspirator orblow them dry with nitrogen.

NB! Check to be sure that the cleaning agent is chemically compatible withthe measurement chamber (see the Chemical Compatibility of Vitonsection at the end of this manual).

4.2.3 Cleaning the Quartz Crystal

Much of the stability and reproducibility of measurements made with the QCMdepend on how well the crystal has been cleaned before use. There areseveral well-known cleaning procedures for quartz crystals and these can

easily be found in literature. Here are 2 ways of cleaning the crystal:

Place the crystal in chromic acid solution for about 1 minute and rinsethe crystal afterwards thoroughly with ion exchanged water. Dry thecrystal by blowing with nitrogen or use an aspirator to suck it dry.

Place the crystal in a Piranha solution (1:3 H2O2:H2SO4) for a couple ofminutes and rinse the crystal afterwards thoroughly with ion exchangedwater. Dry the crystal by blowing with nitrogen or use an aspirator tosuck it dry. Warning! Piranha solution is very corrosive and utmostcare should be taken and proper protective clothing should be used

when handling it.

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Figure 4.3:Sucking the crystal dry.

After either of these cleaning procedures the crystal can be used formeasurements immediately.

4.2.4 Reassembling the Axial Flow Chamber

After all parts of the measuring chamber and the crystal have been cleanedthe standard axial flow measuring chamber is reassembled. Please rememberthat cleanliness is very important during the assembly process as the slightest

contaminations can spoil a measurement. Therefore it is strongly suggestedto use clean tweezers and laboratory gloves when handling the o-rings,crystal holder and the crystal itself as these parts will be in direct contact withthe sample. The crystal support nut, the crystal support body and theguidance pole are not in direct contact with the sample so cleanliness is notas critical.

Figure 4.4:The components of the crystal support chamber of the axial flowmeasurement chamber.

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Start the assembly process by placing the larger o-ring into the crystal holder.

Figures 4.5 and 4.6:Placing the larger o-ring in the crystal holder.

Turn the crystal holder around and place the smaller o-ring in the center of thecrystal holder. Take the crystal and place it on top of this o-ring so that thelarger gold electrode faces downward and that the anchor shaped electrodepoints towards the centering hole.

Figures 4.7, 4.8 and 4.9: Placing the crystal on the smaller o-ring in thecrystal holder.

NB! It is very important that the crystal is loaded into the crystal holder asdescribed because the larger plated electrode of the quartz crystal has to begrounded when it is in contact with the sample fluid. No successfulmeasurements can be performed with the crystal facing the wrong way.

Be careful when handling the crystal, use only tweezers and gently hold the

crystal from its edges. Do not touch the crystal or the plated electrodesdirectly as this will easily contaminate the crystal which will lead to unstableand irreproducible results. If it is necessary to touch the crystal then plasticgloves should always be worn.

The next step in the assembling process is to place the guidance pole in itsposition on the upper module and then load the crystal holder with the o-ringsand the quartz crystal into its position.

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Figures 4.10 and 4.11:Placing the guidance pole and the crystal holder backinto the upper module.

Fit the crystal support body with the spring-loaded pins on the crystal so thatthe pins press the crystal against the o-ring and the guidance pole goes

through the crystal support body. Place the crystal support nut on top of thecrystal support body and screw it tightly to make the o-ring seal hold.

Figures 4.12 and 4.13:Placing the crystal support body.

Figures 4.14 and 4.15:Placing the crystal support nut.

Take the upper module of the standard axial flow measuring chamber andplace it on top of the lower module. The guidance pole which sticks up fromthe lower module prevents any false assembly of these two modules, i.e. theupper module only fits into the lower module one way. On the bottom of the

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lower module there are 2 spring-loaded pins which will be in contact with theelectrodes of the quartz crystal through holes in the crystal support body.

Figure 4.16:Placing the upper module back on the lower module.

4.2.5 Pre-filling the Temperature Loop

It is advisable to start the temperature control of the instrument 20 to 30

minutes before the actual measurement to improve its stability andreproducibility. This can be done with the Temperature Control Unit ifavailable, but even if not it is important to fill the temperature loop and theactual chamber with the background liquid, follow this procedure to do so.

1. Check that the valve is set to Stop and fill the reservoir with thebackground liquid (often water).

2. Turn the valve to the Bypass setting, wait for a few drops to come outand return the valve to the Stop position. Fill the reservoir asnecessary, no air bubbles should be let into the chamber and thus intothe tubing.

3. Turn the valve to the Chamber setting and after a few drops have comeout turn the valve to Stop.

4. If a Temperature Control Unit is available set the target temperaturefrom the QCM-Z500 Impedance Analyzer program by openingControls > Temperature Controls and selecting the appropriatetemperature.

Wait 30 minutes before starting the experiment, use this time to fill in theExperimental Setup and otherwise ready the software side of theexperiment.

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4.2.6 Finalizing the Mechanical Setup

When all of the parts have been cleaned and the axial flow measurementchamber has been assembled check that

All of the cables are connected, especially the one connecting themeasuring chamber to the electronics unit, and that the electronics unitis on.

If a temperature control unit is present make sure that it is connected tothe measuring chamber and the computer directly (and not to the mainelectronics unit).

The outlet tubes have a waste beaker under them so that the wasteliquid is collected and disposed of appropriately.

The temperature loop is filled with the background liquid, and if a

Temperature Control Unit is available then it is set to the targettemperature.

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4.3 The Measurement Process

4.3.1 Software Overview

The KSV QCM Impedance Analyzer software has an easy and user-friendlyinterface. Experiments and any other communication between the computerand the main electronics unit are conducted from the program labeled QCM,and the data from previous measurements can be viewed and analysed fromthe program labeled Browse QCM. This section of the manual is onlyconcerned with taking a measurement, analysing the data is explained in thefollowing chapter of this manual, 5. Data Analysis. Once these proceduresare familiar use the checklist in section 2. Brief Instructions to ensure theproper use of the instrument when running experiments.

To start the QCM program double-click the QCM icon on the desktop orchoose Start > Programs > QCM > QCM. This will open the main menu ofthe program.

Figure 4.16: The QCM Impedance Analyzer main window.

Start a New Experiment

Experimental Setup

Show Sweep GraphShow Graph

Show Measurement Controls

Show Temperature Controls

A new experiment is begun from the Start a New Experiment button. Thisopens the Experimental Setup screen which contains the basic identifyingdata of the measurement, like user, resonator type, etc. After that theMeasurement Controls window along with a Sweep Graph opens.

The Sweep Graph shows impedance and phase against frequency, thenormally used Graph shows frequency change against time. A graph of the

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Calculated Results will open on top of the Sweep Graph once anexperiment is underway with separate Graphs for each harmonic.

Temperature Controls is only available when a Temperature Control Unit isattached, use this to control the temperature of the measuring chamber with

the computer. Alternatively it can be controlled directly from the TemperatureControl Unit itself.

To start a new experiment choose File > New Experiment from the mainmenu window.

4.3.2 Experimental Setup

Fill in the information in the Experimental Setup window to comply with themeasurement. Double-check the Resonator Chamber choice as theautomatic choice might not always apply, and remember that a calibration

must be run with each Resonator Chamber separately. For details oncalibration, please see section 3.3 Calibration. Several fields (like User,Resonator Chamber, etc) have a drop-down menu available. To add itemsonto the menu open the Edit Data Base and select the appropriate tab, formore details please see the 5.2 Edit Database section of this manual.

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Figure 4.17: The Experimental Setup screen. Fill in identifying information onthe experiment.

Name is the identifying name of the measurement, used to help locate thespecific experiment later.

User is the person conducting the measurement.Date records the time and date for future reference. It cannot be altered.

By selecting a Resonator (a quartz crystal) all of the required fields areautomatically filled. If a new Resonator is added fill in the relevant data aboutit into the Database so as to avoid having to fill them in manually each timean experiment is run. Information in the Liquid/Gas and the Addition fieldsare for use when analysing the data as well as for reference.

Once all of therequired information is filled out press Start to continue.

4.3.3 Software Control of the Measurement

When the Experimental Setup has been completed, two windows will open,the Measurement Controls window and the Sweep Graph window. TheSweep Graph plots impedance and phase against frequency, and once theexperiment is begun a Graph of frequency change against time will open ontop of it. If harmonics are selected they will all be shown on separate graphs.The Measurement Controls window controls the measurement chamber,how it resonates and what data is sent back to the computer. In most casesvery little needs to be done in this screen except choosing all of the harmonics

and pressing Start.

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Figure 4.18: The Measurement Controls screen. Select measurement setupand pressStart to begin an experiment.

There is only one measuring Method to choose from by default. This method,Automatic, sets the parameters for the measurements (that is, the Resonator,Search and Sweep Parameters) to fixed values that have been found towork in most cases for measurements involving a gas, a liquid of either highor low density or soft films.

The Resonator, Search and Sweep Parameters cannot be changed whenusing the Automatic method. To change the parameters of the experimentcreate a new Method and fill in the parameters as wanted in the Database.From the Edit menu select Database to access it, please see section 5.2 EditDatabase for details.

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What must be determined before the measurement are the RecordingOptions and the Included harmonics (overtones). The harmonics areselected by checking the respective box, the measurement data will be morecomplete and easier to analyse with more harmonics so it is advisable thatthey are all chosen.

The Measurement Time should be longer than the experiment is expected tolast so that all of the interesting phenomenon will be recorded. WithAutoSave checked the data will automatically be recorded, if uncheckedbegin and end recording with the Rec On and Rec Off butons. The Recbuttons will only be active if AutoSave is not selected.

The software side of beginning the experiment is complete, it is now time toready the chamber for the experiment if this has not yet been finished.

4.3.4 The Measurement Process

Check now that all of the steps in 4.2 Preliminaries have been completed.This means checking that

All of the cables are connected and the electronics unit is on.

If a temperature control unit is present make sure that it is connected tothe measuring chamber and to the computer directly (and not to themain electronics unit).

The outlet tubes have a waste beaker under them so that the waste

liquid is collected and can be disposed of appropriately.

The temperature loop is filled with the background liquid, and if aTemperature Control Unit is available then it is set to the targettemperature.

When ready begin the experiment by pressing Start. The Sweep Graphshould now activate and scan for the capacitance of each harmonicseparately. Once that is finished the Sweep Graph is replaced by the normalGraph which by default shows change in frequency against time.

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Figure 4.19: Graph of change in frequency against time for all harmonics.

Once the frequencies have stabilised it is time to introduce the actual sampleinto the chamber. Follow these steps to do so

Empty the reservoir and open the Bypass. Let the bypass drain thebackground liquid.

Pour the sample liquid into the reservoir. When a few milliliters of thesample have come out from the bypass outlet switch the valve to Stopand wait a few minutes to ensure thermal equilibrium.

Turn the valve to Chamber. Allow a few milliliters to pass through the

chamber to flush it and then put the valve on Stop.

Again wait for the frequencies to stabilise. Flush with the backgroundliquid another time or introduce the next sample according to what isbeing measured. Press Stop when finished, obtaining data for themeasurement is now complete.

The measurement can be stopped at any time before the chosenMeasurement Time has been reached by pressing Stop. This action willbring up a query of whether to keep the experiment data or not. If themeasurement data collected so far should be stored in the database for

further analysis press Yes, but if the measurement data is not useful (for

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example if waiting for frequencies to stabilse before the actual experiment)then press No.

4.3.5 Useful Tips

Whenever operating the valve the some key points about the working of thetubing should be kept in mind. When the sample is a liquid, it is important thatno air bubbles reach the chamber. Thus whenever something is to beintroduced to the chamber it must run through the bypass loop first. Alsowhenever anything is flowing out of the reservoir to either the chamber or thebypass checks should be kept on the level of the liquid. It should always havea few milliliters in reserve.

When changing liquids first empty the reservoir, set the valve to Bypass andallow it to empty. Then flush the bypass loop with the new liquid by filling thereservoir and allowing the liquid to flow down the bypass for several milliliters.It might be necessary to allow more liquid to flow down to clean the tubing.

Whenever changing from the Bypass to the Chamber position or visa versaalways go by Stop.

The volume of liquid in the bypass loop is slightly above 2 ml, so by carefulliquid handling it is possible to exchange the liquid in the actual measuringchamber with 2 ml of the sample liquid. This can be done by letting a smallamount of air into the bypass loop and replacing the actual sample liquid witha less expensive liquid like water, and then with the help of measuring the

amount of this substitute water make sure that the air bubble between theactual sample liquid and the substitute water never reaches the actualmeasuring chamber. This method however requires careful measuring andconcentration to be successful.

The Sample Interval in the Recording options box can be reduced to 0.2seconds i.e. 5 data points can be collected per second. However, this willincrease the noise level of the measured signal and should not be used ifthere is not a real need for fast measurements.

To check that everything is working correctly before starting an actual

measurement it is possible to check the status of the QCM. Start a newexperiment but do not let any liquid into the chamber, and check whatresistance is measured across the crystal. The standard 5 MHz gold platedquartz crystal when clean and dry has a resistance of about 20 Ohm. Letwater into the chamber and check the change in frequency. The change fromair to water should be about -700 Hz. If either of these figures are off thenthere might be a problem with the cleanliness of the crystal, the water or somepart of the QCM.

To view other graphs during the measurement choose different parametersfor the x- and y-axis from the drop-down menu at the top of the Graph

window. An additional curve can be plotted on the same graph by choosing ay2-axis parameter, click on the respective button to change the scale.

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4.4. Window Measurement Chamber - Overview

The window measurement chamber is an alternative to the axial flowmeasurement chamber. The principal concept of the window measurementchamber is the same as that of the axial flow one, that is the sample flowsthrough a chamber where the crystal is housed. However, the liquid flow inthe window measurement chamber is parallel flow, while the standardmeasuring chamber has a axial flow with a stagnant point. The advantages ofthe window measurement chamber are the smaller size, which means thatsmaller sample volumes are required, and a window directly to the chamberwhich allows the user to view what is actually happening in the measuringchamber. It is also possible to use a microscope to observe the microscopicchanges as a sample is introduced.

Image 1:The window measurement chamber.

4.5. Window Chamber - Physical Description

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The window measurement chamber has two modules. The upper modulecontains the main body of the measurement chamber, the chamber itself, andthe valve for controlling the flow direction of the sample whilst the lowermodule consists of the support platform for the measurement chamber, thetemperature control assembly with peltier, heat sink and fan, and the

electronics with connecting electrodes.

Image 2:The upper module of the window measurement chamber.

1) Chamber outlet 5) Finger screw for coverattachment

2) Temperature loop outlet 6) Crystal holder / Measuringchamber

3) 3-way valve for liquid flowdirection control

7) Upper module cover

4) Sample inlet

The quartz crystal is placed in the measuring chamber by turning the uppermodule up-side-down having the 3-way valve in the lower right hand corner,then placing a small O-ring in the crystal holder/measuring chamber, whereafter the crystal is placed in the crystal holder/measuring chamber so that thelarger electrode is downwards while the smaller keyhole electrode is upwards

and points in the opposite direction than the chamber outlet tubing i.e. so thatthe straight cut of the crystal is oriented against the front edge of the upper

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module. This is of utmost importance as the larger electrode which is incontact with the sample liquid phase has to be grounded and only thisorientation of the crystal will ensure this, otherwise the measurementcan not be performed. Hereafter, the measuring chamber is sealed from thecrystal side by using a spring loaded bajonett locking piece so that the two

holes for the lower module contacting pins is aligned horizontally.

Image 3: Placing the quartz crystal into the upper module of the windowmeasurement chamber.

1) Small O-ring 2) Quartz crystal

3) Spring loaded bajonett lockingpiece

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Image 4:The lower module of the window measurement chamber.

1) Connection to main electronics

unit (3-pin D-connector)

6) Fan with heat sink

2) Contacting pins for crystalelectrodes

7) Peltier element for temperaturecontrol

3) Grounding connection forelectrochemical measurements

8) Guiding positioning poles forupper module

4) Socket for temperature control 9) Metal body for heat transfer andelectronics

5) Socket for fan connection fromtemperature control unit

The upper and lower modules of the window measuring chamber is attachedto each other with a finger screw in order to ensure a tight connectionbetween the modules for optimum temperature control of the whole windowchamber measuring module. The measuring chamber is sealed to form anenclosed measuring chamber by placing a large O-ring in the groove of thecrystal holder/measuring chamber, placing the window to seal the chamber,and tightening the fastening nut to keep the quartz/plastic window in place.

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Image 5:The assembled window measuring chamber.

1) O-ring 2) Quartz/plastic window

3) Fastening nut to keep window inplace

4) Finger screw for attachingmodules

The upper module and its components can easily be disassembled for

example for more through cleaning (e.g. sterilization or ultrasound bath) of theviton tubings and the titanium crystal holder/measuring chamber. The mainbody of the upper module is made of aluminum to maximize heat transfer, andthis is attached to the cover with 4 finger screws. By removing these 4 fingerscrews the main body of the upper module can be removed from the cover inorder to access and release the viton tubings and crystal holder/measuringchamber. While cleaning please check that any sample or cleaning solutiondoes not react with Viton from section 9. Appendix A - ChemicalCompatibility of Viton, if necessary alternative substances are available.

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Image 6:The upper module with the cover plate removed exposing the vitontubings and titanium crystal holder/measuring chamber.

1) Finger screws for coverattachment

2) Viton tubings

3) Titanium crystalholder/measuring chamber

4) 3-position valve

4.5.1 The Valve

The sample fluid flows through the 3-position valve into the measurementchamber via a viton tube. The viton tube loops around in the aluminium mainbody of the upper module to ensure that the liquid is appropriatelythermostated before entering above the crystal in the measuring chamber. Byusing the Bypass loop there is also a possibility to exchange sample liquidand pre-temperaturize this without interfering or mixing with the sample liquid

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in the measuring chamber before introducing a new sample liquid into themeasuring chamber. The flow direction of the sample liquid from the samplereservoir is controlled by the 3-position valve, connecting the samplereservoir, the bypass loop and the measuring chamber. Which parts areconnected are defined by the position of the valve marker, and are detailed

below.

BP Sample liquid flow through the Bypass (Temperature) loop fromthe sample reservoir

CH Sample liquid flow into the Measuring chamber from the Bypass(Temperature) loop

STOP No flow of sample liquid

The recommended procedure in operating the valve either for filling thechamber with a sample is to have the valve in the STOP position before fillingthe reservoir. Fill the reservoir and then turn the marker to the BP position.Allow a few drops to come out of the outlet of the Bypass, then turn the valveanti-clockwise through the STOP position to the CH position. Again allow afew drops to come out from the outlet of the measuring chamber and turn thevalve to the STOP position again.

To clean the tubing, set the 3-position valve to BP or CH position and pour thecleaning solution into the sample reservoir. The cleaning solution will thenflow either through the Bypass or the Measuring chamber, be sure to do soabove a sink or so that the chamber and the bypass outlets are above abeaker.

4.5.2 Temperature Control

A Peltier element connects the main aluminum body of the lower module tothe heat sink, and it can be used to control the temperature of themeasurement chamber if an optional Temperature Control Unit is available.Plug the power cable of the TCU to a mains supply and connect the red cablefrom the TCU to the side of the lower module in order to measure and controlthe temperature, and the black cable from the TCU to the back of the lowermodule in order to activate the fan for the heat sink for optimum performance

of the whole temperature control assembly.

Whenever using temperature control in an experiment allow enough time forthe measurement chamber to reach an equilibrium temperature beforestarting a new measurement. About 30 minutes should be sufficient in mostcases.

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4.6 Cleaning the Window MeasurementChamber

4.6.1 Disassembly

The first step in cleaning the window measurement chamber is to separatethe upper module from the lower module by removing the finger screw holdingthe modules together (see Image 5, Section 9.2.). Remove the crystal andsmall O-ring by releasing the spring loaded bajonett locking piece (See Image3, Section 9.2.) and pick out the quartz crystal and small O-ring with tweezers.Then, remove the quartz/plastic window and large O-ring by removing thefastening nut on the upper module (see Image 5, Section 9.2.) and turn theupper module up-side-down so that the quartz/plastic window falls out. If thequartz/plastic window does not fall out, then use the tweezers to gently pressthe window from the quartz crystal side (be careful not to scratch the window).

The disassembly is now complete, the following parts should have been takenaway from the upper module for cleaning:

1) Small O-ring2) Quartz crystal3) Large O-ring4) Quartz/plastic window

4.6.2 Cleaning

Clean the removed parts from the upper module with a cleaning and then arinsing solution. Often by flushing thoroughly with pure ethanol and thencopious amount of ion-exchanged water is sufficient. Be especially attentivewith parts that will be in direct contact with the sample and the crystal, e.g. theo-rings and the glass plate. Dry the parts by blowing with Nitrogen or leavethem drying by their own in the ambient air protected by a clean glassware fordust. Depending on the application where the crystal has been used it mightnot be possible to clean it and a new crystal is needed. The new crystal

should be cleaned as described in Section 4; Measurement Preliminaries.

Clean the Viton tubings and crystal holder/measurement chamber of theupper module by first filling the sample reservoir with cleaning solution andflush thoroughly through both the BP and CH liquid flow directions. Hereafter,flush the crystal holder/measurement chamber with the same cleaningsolution. Repeat this cleaning procedure by using a rinsing solution. Repeatthe whole flushing procedure with a cleaning and rinsing solution asappropriate. Often it is sufficient to use pure ethanol and ion-exchanged wateras the cleaning and rinsing solutions, respectively. Dry the Viton tubings andthe crystal holder/measuring chamber by blowing with Nitrogen or use an

aspirator to remove excess liquid from the tubings and the crystalholder/measuring chamber.

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4.6.3 Assembly

Assemble the window measuring chamber as is described in Section 9.2.

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4.7 Measurement Procedure

4.7.1 Overview

The software procedure with the window measurement chamber is exactly thesame as with the axial flow measurement chamber. Follow the steps insection 3. Installation for details on setting up the computer and theconnection between the computer and the QCM. Add the windowmeasurement chamber to the database by selecting Edit > Database andfrom there open the tab Measurement Chambers and click on the Addicon.Type the name of the chamber, "Window," and the name of the file that will becreated to store the calibration information, for example WindowCal.txt. Seesection 6. The Database for details.

4.7.2 Calibration

During the calibration of the window chamber the calibration tool is placed onthe lower module in a short circuit position, with no calibration tool and in theknown resistance position. The calibration software of the QCM-Z500 willguide the user through these steps.

Open the Calibration Controls window and select Window as themeasurement chamber, see section 3.3 Calibration for details. ClickCalibrate. When instructed to do so place the calibration tool on the lowermodule so that the short circuit position is in line with the electrodes. Push the

tool down gently to set it in place. Remove the tool when instructed to do so.When instructed to do so place the calibration tool back on the lower module,this time with the known resistance in line with the electrodes, and push downgently.

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1) Short circuit position ofcalibration tool

2) Known resistance position ofcalibration tool

3) Spring loaded bajonett lockingpiece

4.7.3 Measurement

Follow the instructions in section 4.3 Measurement Process on making ameasurement. Be sure to select the appropriate chamber in the ExperimentalSetup screen i.e. Window in order to use the correct calibration file for thewindow chamber.

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5. Data Analysis and Reduction

5.1 Overview

Handling the data obtained by QCM-Z500 microbalance measurements is alldone with the separate Browse Experiments program. Use it to review data,print reports, view and manipulate graphs or to export data to anotherapplication. A separate Analysis program exists within the BrowseExperiments screen, the use of which is described in section 5.5 Analysis.

Figure 5.1: Use the Browse Experiments screen to locate and analyseexperiments.

5.2 Browse QCM Measurements

Open the QCM Brows Experiments by clicking on the icon on the desktop orselecting Start > All Programs > QCM > QCMBrowse from the Start menu.

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It can also be found from the installation folder, open My Computer andselect C:\Program Files\KSV\QcmBrowse.exe

The main window is split into four boxes. The Experimentsbox lists all of theexperiments that are on the database and fit the search criteria inserted in the

Find Experimentbox. The data sent by the QCM of the selected experiment isshown in the Original Databox, and if an analysis is run of the experimentthen the results will be shown in the Sampled Databox.

The menu bar includes these options.

File Delete Experiment: deletes highlighted experiment in the Experiments

box. Delete Record: deletes highlighted data point in the Original Data or

Sampled Databox. Copy Data to Clipboard: copies the data of the highlighted experiment to

the clipboard for pasting in another program. Print: Opens a Print Preview screen of a report of the experiment

containing all of the vital information. Export/Delete data: exports or deletes selected data into a format only

recognised by QCM software. Used mainly for backup or transferringdata.

Import data: Imports the exported data. Exit: Closes the Browse Experiments window

View Experimental Setup: Opens the Experimental Setup window of the

highlighted experiment for viewing and editing purposes. Graph: Opens the latest graph viewed, will be blank until some data

has been graphed.

The icons have the most commonly used functions readily available.

Print a report of the highlighted experiment.

Copy the Data of the highlighted experiment to the clipboard forpasting in another program.

View Experimental Setup window of the highlighted experiment forviewing and editing purposes.

View the latest Graph opened.

The axis of the graph can be chosen directly from the top of the BrowseExperiments screen using the x- and y-axis selectors. Next item down is theFind Experimentbox with search parameters that can be filled as far asnecessary. The search fields limit the experiments visible in the Experimentsbox, select an experiment either by clicking on it or by scrolling with thearrows. Once an experiment is selected the Original Databox will show the

following information about the measurement.

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Time [s]: Time at which the data point was taken.Harmonic: The overtone number of the frequency at which the data point was

taken. 1 signifies the fundamental frequency; 3, 5 etc the 3rd, 5th etcharmonic frequency.

Frequency: The measured frequency at the time the data point was taken.

Q: The measured Q-value at the time the data point was taken.D: The measured dissipation value at the time the data point was taken.R: The measured resistance value at the time the data point was taken.Cnd: The measured conductivity value at the time the data point was taken.X: The measuredL: The measured induction value at the time the data point was taken.C: The measured capacitance value at the time the data point was taken.Cp:The measured parasitic capacitance value at the time the data point was

taken.T: The measured temperature at the time the data point was taken.

5.3 Data Graphing

The graphs of the Browse Experiments program are very versatile. Thesame graph can show simultaneously two separate variables plotted against athird variable for any number of experiments. To view the basic graph, right-click on an experiment in the Experiments box and select Graph >Fundamental or Graph > Nth harmonic where N is replaced by the numberof the harmonic.

Figure 5.2: Graph of change of frequency against time for the third harmonic.

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This is the same graph as is open during an experiment, plotting the changein frequency against time. To view the frequency change of anotherexperiment on the same graph right-click on the experiment and select Addto Graph > Fundamental. To view the frequency changes of all of theharmonics of an experiment at the same time select Graph > All. To change

the variable of an axis select a new one from the top of the BrowseExperiments screen, right-click on an experiment and select Graph. Below isan example of all of the harmonics for an experiment.

Figure 5.3: Graph of change of frequency against time for the all harmonics.

To alter the data visible the Data Manipulation menu gives the possibility toignore selected data points. The options are to hide data before a selectedpoint, after a selected point or between two selected points. Hidden data isnot considered when running an Analysis. The Data Manipulation menu is

also used to select sampled data, this is explained below. To select a pointdouble-click on it.

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Figure 5.4: Removing data spikes from view to simplify analysis.

After hiding all of the irrelevant spikes (caused by operating the valve) thegraph looks like this.

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Figure 5.5: Graph of change of frequency against time for the third harmonic,data spikes hidden.

From the Data Manipulation menu this action can be cancelled by clickingUndo Hide, or made permanent by clicking Delete Hidden Data Points

Permanently.

Once a graph is closed it can still be retrieved using the Graph icon on the topof the Browse Experiments screen, this brings up the last graph that wasopened. To alter the display appearance of the graph or to export it selectfrom the Graph menu Show Menu.

Figure 5.6:The graph Menu can be used to alter the appearance of the graphas well as to export the data.

This section features seven tabs: General, Plot, Subsets, Axis, Fonts,Color and Style. The tabs have settings ranging from visual aspects of the

graph to varying the values on the axis, and as most adjustments are familiarfrom other applications they shall not be explained in this manual. There ishowever a help file which can be accessed by clicking Help.

There are two extra buttons on the menu window. Maximize displays a fullscreen version of the graph and Export is used to export data to otherapplications.

An Analysis window can be accessed from the menu which opens whenright-clicking on an experiment in the Experiments box. This can use thenormal continuous data or Sampled data, where specific data is selected from

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the graph of the experiment. This uses the Add Sample and the Add Refbuttons on the bottom of the graph, and is explained in section 5.5 Analysis.

Below the Experimentsbox in the Browse Experiments window is the optionto Normalize graph data. The purpose of normalising is to make the

harmonics comparable to one another by either multiplying or dividing with thechosen variable, either N (number of harmonic) or the square root of N as thenormalising term. Use N when dealing with a rigid film and square root Nwhen dealing with changes in viscocity. Below is a demonstration of hownormalisation works.

Standardgraph

Graphnormalised by

N

The normalised graph clearly demonstrates that the fundamental frequencyexhibits curious differences to the other harmonics. It is often recommendable

to ignore the fundamental in the analysis of QCM measurements.

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5.4 Exporting Data

Data can be exported either as numbers in a data file or as a graph. Theeasiest way is to click on the Copy Data to Clipboard icon, open aspreadsheet program and then paste the data (often from Edit > Paste or bypressing Ctrl + V). To export the data in ASCII format click on Copy Data toClipboard, open Notepad (located by default in Start > Programs >Accessories > Notepad), paste the data by pressing Ctrl + V in Notepad andsave. The lists of experimental data is in the same order as the data in theOriginal Databox in the Browse Experiments screen.

Figure 5.7: Pasting data ontoNotepadto save it in ASCII format.

The data is tab delimited, for a comma delimited list open the Export menu ofthe graph of the required data. Do so by selecting Graph > Show Menu andclicking on Export.

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Figure 5.8: Export data as an image or text file from the graph Menu'sExportscreen.

Choose Text / Data Only from the top and select whether to place the dataon the clipboard (for pasting in another program) or to make a .dat file of it.Press Export to continue.

Figure 5.9: Exporting data as a text file, indicate format styles and pressExport.

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This menu has more specified information on what to export and in whatformat. When finished selecting press Export to continue, either bymanipulating the .dat file created or pasting the data to another program.

To export the graph as an image use the same screen as shown above. First

open the desired graph and from the Graph menu select Show Menu andthen click on Export. The Exporting [Name of Graph] window opens andseveral options as to the image file type are given. Most often JPG will befine. If the image is to be used within a document simply select Clipboard inthe Export Destinationbox and Paste the image onto the document. If savingthe image for later use select File and indicate the folder wanted by clickingBrowse.

When an image file type is selected the Object Size box is visible, givingvarious options on size restriction methods. The default values should be finein most cases and need not be adjusted.

Figure 5.10: Exporting a graph as an image file. Select type, location, sizeand pressExport.

Another way to export data is by selecting Export / Delete Experiments fromthe File menu. From this window multiple experiments can be chosen foreither exporting or deleting. Select the experiments wanted and move themfrom the Source List to the Destination List by clicking the single arrowpointing to the right. To remove experiments from the Destination List selectthem and click the single arrow pointing to the left. The double arrows moveall of the experiments from one list to the other. If just deleting experimentsthen uncheck the Export Experiments box and select Delete All Data.

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Figure 5.11: Exporting data via the Export/Delete Experiments screen.Transfer all files to be exported to the list on the right, indicate whether todelete data or not and clickOK.

If the Use Compression box is checked these files will be stored in acompressed format which requires less disk space. To delete experimentsselect the appropriate box. Click OK to execute the requested function. Note

that to delete experiments without exporting them uncheck the ExportExperiments box.

If exporting experiments the program will prompt for the destination and filename. These files can then be transferred to another computer runninganother KSV QCM Impedance Analyzer. To import an experiment that hasbeen exported to the Experiments list select Import Experiments from theFile menu and locate the file.

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5.5 Analysis

The Analysis window provides useful tools to investigate QCM-Z500microbalance measurements. It can be used to calculate for example thethickness of the film on top of the crystal and the viscoelastic properties of thesample. Additionally the measured frequency change and resistance can becompared to the theoretical values of each harmonic separately, calculatedfrom the given experimental data.

Access the Analysis window by right-clicking on an experiment in theExperimentsbox and selecting Analyze.

5.5.1 Description

Figure 5.12: The Analysis window. Select modelling method, fill in theparameters and pressAnalyze.

The Include harmonics box in the top left corner of the window selects theharmonics to be used in the analysis. Often the fundamental includes peculiarphenomena that is not visible in the other harmonics and thus it might

improve results to leave it out.

Two modeling methods are available, one in which the crystal is covered by arigid film (RF) and a liquid (L) and one in which there is also a viscoelastic film(VF) between the two. The Resonator properties box is filled automaticallyfrom the Database and thus cannot be altered from this screen.

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Use RF+VF+L to observe the rigid and viscoelastic films of liquids.Use RF+L to study viscosity changes in liquids or the rigid films in liquids.

The different tabs present different options and properties used in the

analysis. For more detailed explanation on the differences and the equationsused please see section 8.3 Theory of Impedance Analysis. Most of thefields are filled from the Experimental Setup, others are to be filled withknown or estimated data.

In each Properties box there are several fields, some which have a faintyellow background and can be altered from this screen, some which have awhite background and need to altered from the database if necessary. To addor change a value in these fields access the Database by closing theAnalysis window, opening the Experimental Setup screen and pressing EditDatabase. Due to the equations used (see section 8.3 Theory of Impedance

Analysis for details) some variables can not be fitted simultaneously so achoice between two has to be made. Some variables present a choice ofwhether to fit it or not, those not selected for fitting will be considered constantand those selected will use the given value as the first term in the modeling.

A) RF + VF + L

In the RF+VF+L tab are three boxes, one for the properties of each layer.

The Initial Liquid/Gas Properties box has two fields, Density and Viscosity,

which are filled automatically from the data in the Database.

The Liquid Propertiesbox has several fields that can be adjusted from thisscreen. These are the Density, Thickness, G' and either Viscosity or G'' of thefilm. Each variable presents a choice of whether to Fit it or not. Selectwhether to use viscocity or G'' in the model from the top of the box.

The Rigid Film Propertiesboxhastwo fields that can be adjusted. Those arethe Density and the Thickness of the film. There is also a choice of whether touse that information when modelling or not.

B) RF + L

The RF+L tab is almost the same as the RF+VF+L tab, the main differencebeing the absence of the Viscoelastic Film Properties box. The LiquidProperties box has three adjustable fields which are Density, Viscosity andTau. There is also a choice of whether the liquid is Newtonian or Maxwellian.

The Rigid Film Propertiesbox has two fields that can be adjusted, the Densityand the Thickness of the rigid film of which only one can actually be used inthe fitting.

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The View Fit button opens a new window displaying graphs of the harmonicsindividually. The graph displays both the resistance R and the reactance Xagainst time, and for both variables a measured value and a calculated valueare shown. This can be useful to compare the accuracy of the model againstthe experimental data.

Figure 5.13: The View Fit screen compares the calculated and measuredvalues for each harmonic separately.

The Analyze button runs the modeling program, and the results are displayedon the two graphs on the right side of the screen. The Film thickness graphsimply plots the thickness, in micrometers, of the film on top of the crystal as afunction of time. The Elastic shear modulus and shear viscosity graph hastwo values, the elasticity in mega Pascals and the viscosity in Pascal seconds

against time.

5.5.2 Sampling Data

Experimental data is imperfect, in the above example changing the position ofthe valve caused spikes in the readings. The way to remove these knownerrors from analysis was to hide them from the graph. Another method whichimproves the quality of readings and is to be recommended in most caseswhen running an analysis is to sample the data. Note that in experiments witha large number of data points (e.g. overnight experiment with a reading takenevery second) data sampling significantly reduces the time taken to calculate

an analysis.

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Data sampling works by selecting data sets from the graph of a measurementof the change in frequency of a harmonic against time. Successive samplesare taken from an experiment and compared against a reference reading.Two alternate methods are available, depending on whether the referencevalue is taken from this experiment or another. If the reference reading can be

taken from this experiment then first select the reference value (usually fromthe beginning of the experiment) and check that it is designated SampleNumber 0. Then select successive samples with sequential numb

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