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Biolin Scientific QSense Operator's Manual

High temperature chamber
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QSense High Temperature Chamber
Operator Manual
Compatible with the QSense Analyzer and Explorer Systems
© 2021 Biolin Scientific AB

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  • Page 1 QSense High Temperature Chamber Operator Manual Compatible with the QSense Analyzer and Explorer Systems © 2021 Biolin Scientific AB...
  • Page 2 The only warranties for the products and services are the ones stated in the associated purchase agreements. Nothing in this manual should be interpreted as a further warranty. © 2021 Biolin Scientific AB Publisher Biolin Scientific AB, Sw eden Jennie Ringberg Editor...

  • Page 3: Table Of Contents

    Running a Mesurement ........................ 21 After Measurement ........................ 24 Flammable Sample Liquids ........................ 24 Optional Modules QSense Window Module (QWM) (Optional) ................................25 Assembling the Window Module ................................. 26 Cleaning the Window Module ................................. 27 QSense Ellipsometry Module (QELM) (Optional) ................................
  • Page 4 Contents Operator Manual QSense PTFE Module (QTM) (Optional) ................................37 Chapter 5 Temperature Settings in QSoft 401 ........................ 38 Main Window ........................ 39 Temperature Programming Chapter 6 QSoft401 Acquisition software ........................ 41 Installing software Installing driver ................................41 ........................ 44 Automatic software update ........................

  • Page 5: Chapter 1 Introduction

    Introduction Introduction This manual describes how to install and use your QSense High Temperature Chamber, QHTC 101, to make QCM-D measurements for real-time studies of surfaces or surface-bound processes such as adsorption, interactions and changes of mass and mechanical properties in ultra-thin films.

  • Page 6: General Comments On High Temperature Measurements

    Meaning QCM-D Quartz Crystal Microbalance with Dissipation Monitoring Frequency Dissipation sensor The QSense sensor flow module The removable sensor housing on the chamber platform Warnings, Cautions and Notes WARNING! The exclamation mark inside a triangle means that the manual needs to be consulted for operating, cautionary, or safety information before using the device.
  • Page 7 Operator Manual Introduction RISK OF BURNS! Statements identify conditions or practices that could result in personal injury or loss of life. CAUTION! Statements identify conditions or practices that could result in damage to equipment or other property. Note! Notes emphasize important points. ©...

  • Page 8: Chapter 2 Safety

    QSense Analyzer or Explorer instrument or components thereof, even if Biolin Scientific has been advised, knows of, or should be aware of the possibility of such damages. Biolin Scientific emphasizes the importance of consulting experienced and qualified professionals to assure the best results when using the QSense Analyzer or Explorer instrument.

  • Page 9: Measurement Chambers And Modules

    Measurement Chambers and Modules This refers to all measurement chambers provided by QSense and described in this manual, e.g. the QSense Chamber Platforms (QCP 401, QCP 101 and QHTC 101), the QSense Flow Module (QFM 401), and all accessory modules.

  • Page 10: Peripheral Equipment

    Safety Operator Manual Never heat up any medium with a boiling point lower than the maximum temperature that any part of the chamber may reach. Do not expose any parts other than the sample volume to water and other liquids. If liquid is spilled inside the electronics part of the Chamber Platform, disconnect it from the electronics unit and have it checked by an authorized person.

  • Page 11: Chapter 3 Installation

    Installation Unpacking and Inspection The QSense QHTC 101 chamber is a high precision piece of equipment and should be handled with care. Upon delivery, check immediately for damage to the product or packaging material. In case of damage, contact Biolin Scientific or your local provider before further installation (see Chapter "Support and Service").
  • Page 12 Installation Operator Manual Connect the two cables of the chamber platform to the sockets on the front of the electronics unit. Note that one of the three sockets is not used for the QHTC 101 chamber platform (it is only used for the Analyzer model): The six-pin cable has two tabs on the casing - fits only to left- hand socket on the electronics...

  • Page 13: Verification Of Installation

    Operator Manual Installation Verification of Installation When the software has been installed, and the instrument has been connected via the USB cable, turn on the electronics unit by pressing the power button. If successful, the green lamp around the power button will be illuminated. As a final test, correct installation of the instrument and software will allow the temperature controller, which is found at the lower left corner of the main window, to be turned on: Turn on the temperature...

  • Page 14: Automatic Software Update

    QSoft401 starts it will check for an internet connection and if found it will contact QSense update server to see if a new version is available. If it finds one it will ask you if you want to update at this point. If your computer is not connected to the internet you will have to check from another computer that is.

  • Page 15: Chapter 4 Operation

    This chapter highlights aspects important for high temperature measurements and the usage of the QHTC 101 chamber. For a more thorough description of the operation procedures, please refer to the QSense Analyzer or Explorer Operator's manuals. To minimize distortion of measurements in the liquid phase, the sample liquid should be prepared carefully.

  • Page 16: The Qhtc 101 Chamber Set-Up

    Operation Operator Manual Note! Please observe the following points before preparing the chamber and flow module(s) for measurements: Always rinse with purified water or another appropriate pure liquid (e.g., alcohol) before drying the parts of the chamber/flow module. Always use nitrogen or another non-reactive gas when blow-drying any part of the chamber/ flow module.

  • Page 17: Working With The Flow Module

    Operator Manual Operation the chamber. Reserve at least 50 cm above the hot plate and chamber. The temperature of the hot plate should be adjusted to maximum 120 °C. Working with the Flow Module CAUTION! Older versions of the Flow module do not withstand temperatures higher than 120 °C.
  • Page 18 Operation Operator Manual 4. Put the lid on. Between measurements, rotate the flow module upside down on the chamber platform (with thumb screws pointing up) for stable handling during sensor loading, etc. © 2021 Biolin Sc ientific AB...

  • Page 19: Running A Mesurement

    Operator Manual Operation Running a Mesurement CAUTION! Before starting an experiment, ensure that the sample fluid is chemically compatible with the measurement chamber and the sensor. The standard parts of the chamber exposed to the sample consist of the following materials: Chamber walls: Titanium, grade 2 Temperature stabilizing loop: A-type Viton®...
  • Page 20 Operation Operator Manual adjusted to 20 ºC below the working temperature. (III) If the desired working temperature is 140 ºC - 150 ºC, the temperature of the hot plate should be set to 120 ºC. Step 6. Activate the temperature control (see Chapter: "QSoft 401"). Adjust the temperature set point to desired value and wait 5-10 minutes for equilibration (longer time may be needed if the set temperature differs greatly from room temperature).

  • Page 21: After Measurement

    Usually, extensive cleaning is only needed between different experiment setups. For further cleaning protocols, please refer to the "Instrument care and sensor pre-cleaning" document at www.biolinscientific.com/qsense. RISK OF BURNS! Make sure that the module is at safe handling temperature before touching.
  • Page 22 The metal parts can be immersed into a sonicator bath for thorough cleaning. For cleaning protocol suggestions, please refer to the QSense document "Instrument care and sensor pre-cleaning". © 2021 Biolin Sc ientific AB...
  • Page 23 8. Rinse all parts thoroughly in pure water, and blow dry with nitrogen or another inert gas. Rubber Viton parts will need to be replaced from time to time. For more information, refer to QSense price list. © 2021 Biolin Sc ientific AB...

  • Page 24: Flammable Sample Liquids

    Below is a description of these modules. Please note that the QSense Electrochemistry Module (QEM) and QSense Window Electrochemistry Module (QWEM) are not compatible with the QSense High Temperature Chamber (QHTC) and QSense High Pressure Temperature Chamber (QHPTC).

  • Page 25: Qsense Window Module (Qwm) (Optional)

    The window inside the module itself is made of sapphire glass. Specifications QWM 401 Sensors Compatible with all QSense 14 mm sensors Internal volume ~100 µl (above the sensor) Type of measurements...

  • Page 26: Assembling The Window Module

    Take extra care when screwing the middle plate (2) to the upper plate (5). Overtightening the screws can crack the glass slide. Side view of the Explorer chamber with QSense Window Module mounted (dimensions in mm). © 2021 Biolin Sc ientific AB...

  • Page 27: Cleaning The Window Module

    The flow part is made of titanium (as for the standard QFM 401 Flow Module), and standard o- rings are made of Viton®; hence, they should be cleaned according to QSense standard cleaning recommendations (see www.biolinscientific.com/qsense). Windows can be cleaned with Hellmanex II cleaning solution for optical components or similar (see www.hellma-...

  • Page 28: Qsense Ellipsometry Module (Qelm) (Optional)

    Scientific. The angle of incidence is 65º, and equals the angle of reflection. The Ellipsometry Module can only be used with QSense Explorer or QHTC chamber platform, as you need optical access from both ends of the module and the design of the Analyzer chamber platform does not allow for this.

  • Page 29: Using The Ellipsometry Module

    Using the Ellipsometry Module As for the standard flow module QFM 401, preparing a measurement includes: cleaning of the flow paths and sensor (see QSense cleaning recommendations at www.biolinscientific.com/qsense) making sure that the 12x1 mm O-ring lies flat under the sensor...

  • Page 30: Assembling The Ellipsometry Module

    Operation Operator Manual 4.6.2.2 Assembling the Ellipsometry Module For thorough cleaning between experiments, and maintenance, the module can be disassembled completely: - Module base with electrode connections - Insulator lid - Viton® sealing gasket - Optical glass window with holder and O-ring (x2) - Titanium flow part - Distance plate...
  • Page 31 Operator Manual Operation There is 1 inlet port and 3 outlet ports on the titanium flow part. The corresponding inlet port on the PTFE tubing connector is marked with a notch. The four small O-rings sealing between the titanium flow part and the PTFE tubing connector can be removed for cleaning if necessary.
  • Page 32 When you feel the resistance in the screw, tighten it about 1/4 turn. Front view of the Explorer chamber with QSense Ellipsometry Module mounted (dimensions in mm). Indicated angle is for the laser beam. Top view of the Explorer chamber with QSense Ellipsometry Module mounted (dimensions in mm).

  • Page 33: Cleaning The Ellipsometry Module

    Operator Manual Operation Side view of the Explorer chamber with QSense Ellipsometry Module mounted (dimensions in mm). 4.6.2.3 Cleaning the Ellipsometry Module Please refer to the standard cleaning recommendations by QSense (see www.biolinscientific.com/qsense "Instrument care and sensor pre-cleaning") as the ellipsometry module is made of our standard materials (titanium and PTFE flow part, Viton®...

  • Page 34: Qsense Humidity Module (Qhm) (Optional)

    The liquid is in contact with titanium, GORE® membrane and Viton in the standard setup. Specifications QHM 401 Sensors Compatible with all QSense 14 mm sensors Internal volume 100 µl between the sensor and the membrane, 120 µl from inlet to outlet (above membrane)

  • Page 35: Tabled Relative Humidity For Salts

    Operator Manual Operation 4.6.3.1 Tabled Relative Humidity for Salts Below is a list of relative humidity values (RH) for some standard salt solutions at temperature 25 °C. By using these saturated solutions, a series of humidity values can be created and used with the Humidity Module.

  • Page 36: Qsense Open Module (Qom) (Optional)

    180º wrong. Specifications QOM 401 Sensors Compatible with all QSense 14 mm sensors Sample volume Application dependent due to wetting of the surface, typical range is 10-300 µl...

  • Page 37: Qsense Ptfe Module (Qtm) (Optional)

    Avoid any changes during an experiment, e.g. different flow rates and temperature. Specifications QTM 401 Sensors Compatible with all QSense 14 mm sensors Internal volume 100 µl (above the sensor) Type of measurements Flow or stagnant liquid measurements*...

  • Page 38: Chapter 5 Temperature Settings In Qsoft 401

    QHTC 101 chamber. For a more thorough description of the settings and the usage of the software, please refer to the QSense Analyzer or Explorer Operator's manuals Open QSoft 401 via the Start Menu, or via the path C:/Program Files(x86)/QSense/QSoft401 (if you used the default installation path).

  • Page 39: Temperature Programming

    Operator Manual Temperature Settings in QSoft 401 C lick on the Temperature control panel on the main window to open the temperature settings window. Insert the desired value and click "OK". WARNING! RISK OF FIRE HAZARD. Never heat up any medium with ignition point lower than the maximum temperature that any part of the chamber may reach.
  • Page 40 Temperature Settings in QSoft 401 Operator Manual A temperature program consists of a number of steps (at least two). For each step there is a starting temperature and a time. The time denotes how long it should take before reaching the temperature of the next step.

  • Page 41: Qsoft401 Acquisition Software

    QSoft401 requires that the PC has a USB 2.0 or higher compatible port in order to acquire data. The latest software can be found on Biolin Scientific's website, in the Support Portal. To install the software, just double-click the "QSoft401_Installer.exe" file you either downloaded or have on your installation USB memory stick.
  • Page 42 QSoft401 Acquisition software Operator Manual 3. Click “Install” for the dialog “Would you like to install this device software” in 64 bit operating system. In 32 bit operating system, the dialog “Windows can’t verify the publisher of this driver software” will appear. Select “Install this driver software anyway”.
  • Page 43 Operator Manual QSoft401 Acquisition software 64 bit Windows 7 4. Click “Finish” at Completing the Device Driver Installation Wizard. 5. Switch on the Device and plug it in USB2.0, or higher, port. There will be an information message showing “Installing device driver software”. ©...

  • Page 44: Automatic Software Update

    QSoft401 starts it will check for an internet connection and if found it will contact Biolin Scientific update server to see if a new version is available. If it finds one it will ask you if you want to update at this point. If your computer is not connected to the internet you will have to check from another computer that is.

  • Page 45: Main Window

    Operator Manual QSoft401 Acquisition software Main window When the electronics unit is turned on, the Temperature Controller can be accessed. It is recommended to turn this on first, so that the Chamber platform and flow modules can stabilize while continuing with other settings. If the temperature controller was turned on before the instrument was shut down last time, it will turn on automatically.

  • Page 46: Find Resonances

    QSoft401 Acquisition software Operator Manual 6.3.2.1 Find resonances Note: this window is not available for Initiator. The crystals to be included in the measurement are chosen in the Included crystals panel. For the Explorer (E1), and Extreme Temperature chambers, there will be only one possible sensor to "choose"...
  • Page 47 Operator Manual QSoft401 Acquisition software latest sweep for each resonance (if any) will be saved. The Notes section of the data file contain the found resonance frequencies and dissipation factors. Different types of measurements demand different time resolution. If very fast processes needs to be recorded, higher amount of data points per minute are sampled by moving the pin below towards High speed.

  • Page 48: Advanced Find Resonance Settings

    QSoft401 Acquisition software Operator Manual Decay amplification Sets the amplification level of the signal from the sensor before it reaches the analog-to-digital converter. Decay length Sets how many data points should be collected for the numerical fit. Decay average Sets how many decay curve fittings should be calculated before presenting an averaged value on the screen.

  • Page 49: Temperature Programming

    Operator Manual QSoft401 Acquisition software large value will increase the sweep speed but will also increase the risk of missing resonance peaks. Average The number of amplitude measurements averaged for each frequency step. Initial resonance estimate Determines which resonance peak QSoft401 should use as the initial resonance estimate. For normal AT-cut sensors, the first peak around the nominal resonance frequency is the desired peak.

  • Page 50: Measurement Windows

    QSoft401 Acquisition software Operator Manual A temperature program consists of a number of steps (at least two). For each step there is a starting temperature and a time. The time denotes how long it should take before reaching reaching the temperature of the next step. The temperature slope is automatically calculated based on the temperature difference between current row temperature and the next and how long time is specified.
  • Page 51 Operator Manual QSoft401 Acquisition software You can restart a measurement if an acquisition is already ongoing. The ongoing measurement will be terminated and a new will start promptly. You will not be asked to save the terminated measurement until you try to close the measurement window. However, if you want to save it, just will When starting the acquisition, one f and D vs Time chart for each included sensor crystal will appear.
  • Page 52 QSoft401 Acquisition software Operator Manual notes document. F and D chart panels Acquired frequency values are plotted in various hues of blue and presented on the left hand axis, while dissipation values are plotted in red to yellow hues and presented on the right hand axis: Note that the f and D values are automatically offset so they all start at zero.

  • Page 53: Curve Tools

    Operator Manual QSoft401 Acquisition software The offset function allows you to choose a different time than time zero for which all the curves are offset to zero. Curve tools are explained here. Zooming To zoom in on a specific area of a chart, hold the left mouse button and drag the mouse down and to the right.

  • Page 54: Terminating A Measurement

    QSoft401 Acquisition software Operator Manual When the Curve tool dialog is shown, there are two green sliding bars on the chart. The calculated f and D shifts and slopes between these two bars are automatically updated in the Curve tool window as you move them. Slopes are calculated as the slope of a straight line fitted to the data between the bars.

  • Page 55: Temporary (Backup) Measurement File

    Operator Manual QSoft401 Acquisition software A Save file dialogue will appear. Enter a file name and click Save to save your data. If for some reason the measurement was terminated by a computer, power or program failure, data is saved in a temporary file that can be retrieved next time QSoft401 is launched. See here for details.

  • Page 56: Condense A Measurement

    QSoft401 Acquisition software Operator Manual Include column names If checked, the first row in the exported data file will contain the exported data series names. If not check, a data row will be the first row in the new file. Opens a Save dialog that lets you enter the name of the file to which you will export data.

  • Page 57: Tools

    Operator Manual QSoft401 Acquisition software menu. You can either manually set how large time gap it should be in the new data file between the two measurements or let QSoft use the actual time difference. If the first data file was recorded after the data that is to be appended, you have to set a new time difference.

  • Page 58: About

    This is for debugging purpose and only relevant in communication with Support in case of a malfunctioning instrument. About QSoft401 Copyright © 1998-2021 Biolin Scientific AB All Rights Reserved QSoft401 Help v.1.0 © 2021 Biolin Sc ientific AB...

  • Page 59: Materials Guide

    Operator Manual Materials Guide Materials Guide All metal parts contacting sample fluids are made of titanium, grade 2 Tubing to/from modules is made of PTFE Pump tubing is made of Tygon, R-3607 Standard O-rings are made of A-type Viton® Standard flow module sealing gaskets are made of A-Type Viton® Highly resistant O-rings are made of Kalrez®...
  • Page 60 Materials Guide Operator Manual such as swelling, embrittlement, cracking, softness, or change of size or weight. If there is no sign of deterioration, test the sample in the instrument setup under the conditions of your application. © 2021 Biolin Sc ientific AB...

  • Page 61: Support And Service

    When it is time for service of your QSense product, please use the same contact information as above. Service of malfunctioning instruments during the limited warranty period is free of charge.

  • Page 62: Technical Specifications Qhtc 101

    Excel, BMP, JPG, WMF, etc. Sensors and sample handling system Number of sensors Volume above the sensor ~40 µl using QSense Flow Module for 5 MHz sensors Minimum sample volume, flow mode Recommended from 300 µl but possible to make adaptations to get down to 200 µl.
  • Page 63 Operator Manual Technical Specifications QHTC 101 Dimensions Height (cm) Width (cm)Depth Weight (cm) (kg) Electronics unit Measurement chamber The temperature stability depends on variations in how the ambient affects the warming or cooling of the chamber. The specified temperature stability may not be reached if the room temperature changes ±...

  • Page 64: Index

    Operator Manual Index Index - I - Initialize - A - - K - Abbreviations acquisition software 11, 41 Kalrez Acronyms - M - - C - Materials Cautions Measurement set-up Chamber Platform typical Cleaning Microscopy cover ellipsometry module - N - window module Cleaning procedures Notes...
  • Page 65 Index Operator Manual - S - Safety precautions Salt solution RH values Sample liquid degassing of Sample liquids preparation of Service Setpoint temperature Solvent properties Storage Support - T - Telephone numbers Temperature 8, 15 stabilization of samples working Titanium Transport Tubing - U -...

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