MicroVacuum QCM-I Mini User Manual

Quartz crystal microbalance with impedance analysis

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Volume 1.

QCM-I Mini and eQCM-I Mini

QUARTZ CRYSTAL MICROBALANCE WITH

QCM-I Mini and eQCM-I Mini Operator's Manual

IMPEDANCE ANALYSIS

User Manual

MicroVacuum Ltd.

 1993-2018

Kerékgyártó u. 10, Budapest, H-1147, Hungary

Phone +36 1 252 1991 • Fax +36 1 221 7996

E-mail:

info@microvacuum.com

Web:

http://www.microvacuum.com/

QCM-I Mini and eQCM-I Mini User Manual Rev3

Volume

Edition: 2018/12

Revision: 3

Table of Contents

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Page 1 Volume 1. QCM-I Mini and eQCM-I Mini User Manual Rev3 Volume QCM-I Mini and eQCM-I Mini QUARTZ CRYSTAL MICROBALANCE WITH IMPEDANCE ANALYSIS User Manual MicroVacuum Ltd.  1993-2018 Kerékgyártó u. 10, Budapest, H-1147, Hungary Phone +36 1 252 1991 • Fax +36 1 221 7996 E-mail: info@microvacuum.com...
Page 2: Table Of Contents
T A B L E O F C O N T E N T S SAFETY ................................5 General Safety ....................................5 Measuring Head, Sensor Holder and Flow Cell ..........................6 INTRODUCTION ..............................7 QCM-I MINI PRINCIPLE OF OPERATION ......................8 QCM-I M ..........................8 EASUREMENT RINCIPLE ..............................
Page 3 Microscopy ....................................40 Low Profile Holder ..................................41 Channel A: External Sensor-Holder Adaptor ..........................41 Calibration Kit ..................................... 42 Custom External Sensor-Holder ..............................42 BIOSENSE 3 SOFTWARE FOR QCM-I MINI ......................43 10.1 ............................... 43 OGIN Evaluation Mode ..................................43 TROUBLESHOOTING ............................
Page 4 Excel® are registered trademarks of the Microsoft Corporation Windows® and QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum Revision: 3...
Page 5: Safety
Safety Safety In no event shall MicroVacuum ever be held responsible or liable for any direct, indirect, incidental, special or consequential damages or costs whatsoever resulting from or related to the use or misuse of the QCM-I Mini instrument or components thereof, even if MicroVacuum has been advised, knows of, or should be aware of the possibility of such damages.
Page 6: Measuring Head, Sensor Holder And Flow Cell
Safety Turn the QCM-I Mini or eQCM-I Mini off when not in use. An appropriate risk assessment should be undertaken before the instrument is left operating unattended. Measuring Head, Sensor Holder and Flow Cell WARNING! RISK OF FIRE HAZARD. Use only sample liquids with a self-ignition point higher than 85°C in the sample volume of the flow modules.
Page 7: Introduction
Introduction Introduction The QCM-I Mini is a precision instrument for the determination of the mass and viscoelastic properties of thin films attached to the surface of a quartz crystal sensor. These films, which may be a wide range of molecular or atomic layers from metals to physisorbed polymers, surfactants or immobilized biological samples, are monitored in real time either in liquid or in the vapor phase.
Page 8: Qcm-I Mini Principle Of Operation
(D, determined by QCM-D using the “ring-down” technique) and is inversely proportional to the Quality factor (Q) of the crystal: Sauerbrey, G. Z. Phys. 1955, 155, 206 QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum Revision: 3...
Page 9: Limits Of Operation
D. Johannsmann, Viscoelastic, mechanical and dielectric measurements on complex samples with the quartz crystal microbalance. Phys. Chem. Chem. Phys. 10, 4516–4534 (2008) K. Kanazawa, J. G. Gordon, Anal. Chim. Acta 1985, 175, 99–105 QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum...
Page 10: Maximum Loads
, shown in Figure 3. The resonant frequency and FWHM D. Johannsmann, The Quartz Crystal Microbalance in Soft Matter Research: Fundamentals and Modeling, Springer International Publishing, Switzerland, 2015. QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum Revision: 3...
Page 11 Other experimental data is also recorded from the experiment, depending on modules installed, such  Temperature (measured on channel A,)  Flow (where fluidic pump control option is enabled,) QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum Revision: 3...
Page 12: Qcm-I Mini Instrument Description
Figure 5: QCM-I Mini measurement unit rear view (left) and underside showing EC working electrode connector (right). The signals are generated and data is collected in the QCM-I Mini measuring unit before being sent to the computer. The PC communicates with the QCM-I Mini unit via Manufacturer supplied USB cable. Microsoft Windows™...
Page 13: Temperature Measurement And Temperature Control Module
External Sensor Holder There is a sensor connector (Channel B) on the front face of the QCM-I Mini for connecting to external sensor holders, see Figure 4. A range of holders and custom holders are available for different applications, detailed in chapter 9 of this manual.
Page 14: Potentiostat
An external potentiostat is used to control the electrochemical measurement. An electrochemistry module is available for the BioSense 3 software to integrate measurements using Gamry and MicroVacuum supplied potentiostats. QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum...
Page 15: Qcm-I Mini Specification
Power Supply ( 100V-240V AC / 50-60 Hz ) Table 1: QCM-I Technical Specification * Based on BioSense analysis using Sauerbrey equation and with data smoothing option enabled. QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum Revision: 3...
Page 16: Getting The Equipment Ready For Use
If any of the components are damaged, please contact the vendor immediately. Install the QCM-I Mini on a solid, clean, stable, laboratory bench away from direct sources of heat or draft. Do not block the ventilation openings on the bottom and side of the equipment. Ensure that the laboratory power supply is suitable for the power adapters provided.
Page 17: Qcm-I Mini Installation With Microsoft Surface Pro
Pro; it should start up immediately. Wait for Windows® to load fully before turning-on the QCM-I Mini. Turn on the QCM-I Mini by pressing the on/off button shown in Figure 7 for 2 s, or off for 4 s. The button lights up blue when on.
Page 18 Getting the Equipment Ready for Use Figure 9: QCM-I Mini with Surface Pro schematic layout Figure 10: QCM-I Mini, Surface Pro and USB Hub Accessory schematic layout QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum Revision: 3...
Page 19: Installation Using Desktop Pc Or Nuc Computer
Wait for Windows® to load fully before turning-on the QCM-I Mini. Turn on the QCM-I Mini by pressing the on/off button shown in Figure 12 for 2 s, or off for 4 s. The button lights up blue when on.
Page 20 Getting the Equipment Ready for Use Figure 13: QCM-I Mini with NUC PC schematic layout QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum Revision: 3...
Page 21: Instrument Testing
Instrument Administrator using TeamViewer. Please see the QCM-I Software Manual for information about TeamViewer. First install the QCM-I or QCM-I Mini (detailed above). Next unpack and install the potentiostat, according to the manufacturers instructions. Connect it to the power supply and via USB to a USB port on the QCM-I computer or USB Hub provided.
Page 22 Getting the Equipment Ready for Use Figure 15: Gamry Potentiostat and QCM-I Mini schematic diagram, showing the Reference, counter and working electrode connections. Figure 16: Electrochemical Flow-cell Sensor Holder, QSHE-014 (left) and underside of QCM-I Mini thermal chamber showing the working electrode 2mm banana connector from the potentiostat (right).
Page 23: Temperature Control
The measuring head (Channel A) of the QCM-I Mini unit is heated/cooled by a Peltier device with a stability of +/- 0.02°C. The heating/cooling operation of the Peltier device is controlled by a Watlow temperature controller built-into the QCM-I Mini instrument.
Page 24: Sensors
5MHz sensors as standard, however the modular sensor-holders allow either 14 mm diameter or 1” diameter quartz crystals to be used with the QCM-I Mini. The table below shows the geometry and electrode configuration of the 1” and 14 mm QCM sensors.
Page 25: Electrode Materials
Notice that there is no outward evidence of mode QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum...
Page 26: Temperature Effects
Keep the crystals in a clean and dry place. When not in use store them in their original box and wrapper.  Avoid touching the metal electrodes of the crystal.  Rinse only with deionized water, or another appropriate residue-free solvent, before drying the crystal. QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum Revision: 3...
Page 27: Sensor Cleaning
For sensors which are going to be re-used, some cleaning steps can be started with the sensor still in the QCM-I Mini to monitor removal of material deposited during the previous experiment. The cleaning steps required will also depend on whether the sensors are nominally clean or have been previously used and have been coated or contaminated by the experiment.
Page 28: Uv-Ozone Cleaning
The process leaves the sensor surface hydrophilic, typically with a low water contact angle. Commercial UVO cleaners are available; please contact MicroVacuum Ltd. for more information. This is not suitable for removing large amounts of contamination, for which a solution based clean or O plasma cleaning is more appropriate.
Page 29: Detergent
Some materials that are bound to the sensor surface with electrostatic interactions can be very effectively removed with rinsing in alternate HCl (1M) and NaOH (1M) solutions, however extended immersion in NaOH will damage the quartz crystal surface. QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum...
Page 30: Flow Cell Assembly
Place the PEEK flow-cell lid onto the holder base. Tighten the screws alternately, to ensure that the O-rings are uniformly compressed onto the crystal. Figure 20: Mounting a sensor in the flow cell QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum Revision: 3...
Page 31 The flow-cell in Channel A needs 5 to 10 minutes to reach the set temperature in the thermal sensor chamber. Start the QCM measurement after the temperature has stabilized. QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum...
Page 32: Electrochemical Flow Cell Assembly
When filling the flow cell, take care to flush the cell completely to ensure that there are no bubbles trapped in the outlet, so that there is a good electrical contact to the reference electrode. QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum...
Page 33: Flow-Cell Fluidic Configurations
8.2 MANUAL STATIC CELL The standard basic configuration of the QCM-I Mini leaves the fluidic system to be provided by the customer. However it is supplied with a luer fitting for a syringe and an on/off valve. The syringe can be used to manually suck or push sample through the flow cell.
Page 34: Peristaltic Pump
(not generally an issue with a good quality pump) and means that the peristaltic tubing can be unclamped when not in use which will extend its operational lifetime. Figure 25: Schematic Diagram for sample introduction controlled by peristaltic pump. QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum...
Page 35: Peristaltic Pump And Selector Valve
This maximizes the sharpness of the buffer to sample transition during sample introduction and wash out. Figure 27: Schematic Diagram for fixed volume sample injection under continuous flow. QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum...
Page 36 After sample injection, when the valve is returned to the Load position, the sample loop must be thoroughly washed/ rinsed so that all the previous sample is removed and cannot contaminate the next sample injection. QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum...
Page 37: Sensor Holders, Adaptors And Modules
A to produce a dummy signal for instrument test or training purposes. Only the fundamental, 3 and 5 overtone frequencies are available with this module. QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum Revision: 3...
Page 38: Immersion And Open Sensor Holder
~0.5M KCl solution. Seal the inlet and outlet tubing to prevent the solution from evaporating. If the electrode has been left dry it can recover after immersion in water. Other metals are available for the counter electrode, such as Cu or stainless steel. QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum...
Page 39: High Pressure Sensor Holder
Both sides of the sensor crystal are exposed so the response is double that obtained from a conventional single sided sensor and there is no net pressure difference across the sensor surface. QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 ©...
Page 40: Vacuum Sensor Holder
Figure 35: QCM sensor holder for vacuum application with CF feedthrough and temperature measurement. Microscopy Part. No.QSH-mic. Figure 36: QCM sensor holder for microscopy with a transparent ITO coated sensor crystal for inverse microscopy QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum Revision: 3...
Page 41: Low Profile Holder
Figure 37: Low profile sensor-holder. 3 mm thick. The low profile sensor-holder allows a sensor to be mounted away from the QCM-I Mini instrument in a constrained location, primarily for the measurement of deposition from the vapor or gas phase, such as on the bed of a printer or spray coater or in a vacuum system.
Page 42: Calibration Kit
Calibration Kit Part No.: MV-cal Figure 39: RF Calibration Kit for QCM-I Instruments. The calibration kit is used to calibrate the line impedance of the QCM-I Mini channels and is available for use by the system Administrator. Custom External Sensor-Holder The QCM-I Mini instrument is designed to allow a wide range of external sensor heads to be connected to it.
Page 43: Biosense 3 Software For Qcm-I Mini
Username: “user” and Password: “user”. Evaluation Mode The software can be started without QCM-I Mini instrument connected, in which case it will run only in evaluation mode, but the “Data evaluation only” box has to be selected. Figure 40: User Login Window Troubleshooting 11.1 ERROR MESSAGES...
Page 44: Support
Support Support MicroVacuum offers remote customer support via preinstalled TeamViewer software. This support requires that the computer of QCM system is connected to the internet, and the QCM measurement system is switched on. 12.1 HOW TO ESTABLISH REMOTE CONTACT? The date and time of the remote contact should be decided via e-mail. At the prefixed time please follow the steps bellow: 1.
Page 45: Warranty
MicroVacuum will, at its option, either repair or replace any product that proves to be defective. To exercise this warranty, contact MicroVacuum for RMA # at the address below. Returns will not be accepted without RMA #. The owner will send the product, transportation prepaid, to MicroVacuum Ltd.
Page 46: Appendix 1: Sensor Data Sheets
APPENDIX 1: Sensor Data Sheets APPENDIX 1: Sensor Data Sheets QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum Revision: 3...
Page 47: Appendix 2: Sensor-Holder Module Data Sheets
APPENDIX 2: Sensor-Holder Module Data Sheets APPENDIX 2: Sensor-Holder Module Data Sheets QCM-I Mini and eQCM-I Mini User Manual Edition: 2018/12 © MicroVacuum Revision: 3...

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