Autolab Manual
Autolab Manual
Autolab Manual
User manual
Table of contents
1 Introduction .................................................................................................... 7
1.1 The philosophy of NOVA .......................................................................... 7
1.2 Working with NOVA .............................................................................. 10
1.2.1 The toolbar buttons ......................................................................... 10
1.2.2 The toolbar menus .......................................................................... 12
1.2.3 Views and frames ............................................................................ 13
1.3 NOVA workflow ..................................................................................... 16
1.3.1 The commands ................................................................................ 16
1.3.2 The measurement sequence ............................................................ 17
1.3.3 The Signal sampler .......................................................................... 18
1.3.4 The Options ..................................................................................... 24
1.4 Global and local sampler/options............................................................ 26
1.5 Data management ................................................................................. 28
1.6 Customizing NOVA................................................................................. 31
1.6.1 Profiles ............................................................................................ 31
1.6.1.1 Level based ............................................................................... 32
1.6.1.2 Hardware based ....................................................................... 33
1.6.1.3 Application based ..................................................................... 34
1.6.1.4 Hide/Show option ..................................................................... 35
1.6.1.5 Hidden commands warning ...................................................... 39
1.6.2 Sorting function for the commands browser.................................... 40
1.6.3 Import/Export profiles ...................................................................... 40
1.6.4 Software options ............................................................................. 42
1.6.4.1 Graphics ................................................................................... 43
1.6.4.1.1 Default graphical settings .................................................... 43
1.6.4.1.2 Plot Legend settings ............................................................ 45
1.6.4.1.3 Maximum number of points in real time view ...................... 46
1.6.4.2 Autolab display ......................................................................... 47
1.6.4.3 Advanced settings..................................................................... 48
2 The Setup view ............................................................................................. 51
2.1 The workspace ....................................................................................... 51
2.2 The procedure editor and the structure of procedures ............................ 52
2.3 Simple editing ........................................................................................ 57
2.4 Advanced editing ................................................................................... 60
2.4.1 Adding/Removing commands .......................................................... 60
2.4.2 Removing commands ...................................................................... 62
2.4.3 Adding commands .......................................................................... 64
2.4.4 Cut and Copy Paste commands .................................................... 69
2.4.5 Favorite commands ......................................................................... 72
2.4.6 Enabling/Disabling commands ......................................................... 73
2.4.7 Adding extra commands.................................................................. 76
2.4.8 Linking commands .......................................................................... 79
2.4.8.1 Understanding links .................................................................. 79
2.4.8.2 Removing links.......................................................................... 81
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6|Page
1 Introduction
NOVA is designed to control all the Autolab potentiostat/galvanostat instruments
with a USB connection. It is the successor of the GPES/FRA software and
integrates two decades of user experience and the latest .NET software
technology.
NOVA brings more power and more flexibility to the Autolab instrument, without
any hardware upgrade.
NOVA is designed to answer the demands of both experienced electrochemists
and newcomers alike. Setting up an experiment, measuring data and performing
data analysis to produce publication ready graphs can be done in a few mouse
clicks.
NOVA is different from other electrochemical software packages. As all
electrochemical experiments are different and unique, NOVA provides an
innovative and dynamic working environment, capable of adapting itself to fit
your experimental requirements.
The design of NOVA is based on the latest object-oriented software architecture.
NOVA is designed to give the user total control of the experimental procedure and
a complete flexibility in the setup of the experiment.
This user manual provides in-depth details about the functionality of NOVA. It
explains the most important features of the software, using many practical
examples. The user manual has four chapters:
Chapter 1
Chapter 2
Chapter 3
Chapter 4
Method #2
CV staircase
with pH
Method #3
CV linear
scan
Method #4
LSV staircase
Frequency range
Method #n
Method #5
Impedance
Potentiostat
Set E DC
Amplitude
DC potential
Set cell
ON
Wait
Apply
frequency
Measure Z
Set cell
OFF
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Repeat
Measure Z
Set cell
Wait
Set E
Potentiostat
Frequency range
Automatic current ranging
User defined
Impedance
Amplitude
DC potential
The NOVA approach allows the user to program an electrochemical method in the
same language used by the instrument.
This new object-based design philosophy has led to the current version of NOVA.
As any task can be solved generically, the software is slightly less intuitive than a
method-based application. Depending on the complexity of the experiments, the
learning curve can be more or less long. For this reason, we advise you to study
carefully this User manual as well as the Getting started.
Because of the large number of possibilities provided by this application, it is not
possible to include the information required to solve each individual use case. A
number of typical situations are explained using stand-alone tutorials (refer to the
Help menu Tutorials). These tutorials provide practical examples.
In case of missing information, do not hesitate to contact Metrohm Autolab at the
dedicated [email protected] email address.
9|Page
The toolbar shows a number of buttons, some of which might be grayed out (in
which case the attached instruction cannot be performed) or highlighted (which
indicates a persistent state of NOVA).
This section provides an overview of the toolbar buttons.
New Procedure, clears the procedure editor frame
Save Procedure, saves the currently edited procedure in the database
Print Procedure, prints the currently edited procedure on the default
printer
Setup view, switches to the Setup view (highlighted button, i.e. active
status)
Multi Autolab view, switches to the Multi Autolab view
Measurement view, switches to the Measurement view
Analysis view, switches to the Analysis view
Start measurement 1, starts the measurement by executing the currently
edited procedure
Pause measurement 2, pauses the measurement (click the start button
again to continue)
Skip command 2, interrupts the current command and jumps to the next
command in the procedure
1
2
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The Autolab display can also be shown by pressing the F10 key.
Only active in the Setup view. This button is greyed out in the two other views.
5
The following actions can be undone/redone: delete command, move command, insert
command, link/unlink command parameter.
6
Only active in the Measurement view. This button is grayed out in the two other views.
4
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Setup
Multi Autolab
Manage multiple
Autolab devices
Setup procedures for
multiple instruments
Start experiments on
multiple instruments
Measurement
Analysis
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Analysis results
View data in 2D or 3D
Perform calculations
Build new plots
Export data
Manage the database
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Figure 1.5 Comparison of the Set potential command (left) and the CV staircase command
(right)
Note
The command parameters for the CV staircase command are shown in different
colors. More information on this color scheme is provided in Chapter 2 of this
manual.
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Start
measurement
Procedure
validation
Set Autolab
property
Display data
Sample signals
Options
Stop
measurement
Store data
points
Figure 1.6 The basic steps in a NOVA procedure
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Current
Time
Potential
Sampler
Auxiliary
(QCM, T,
pH, )
Figure 1.7 The sampler is used to measure the electrochemical response of the cell
in the procedure
Figure 1.8 Modifying the signal sampler for the cyclic voltammetry experiment
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The Edit Sampler window will be displayed. In this window, the available
electrochemical signals displayed (see Figure 1.10). A checkbox is provided for
each signal.
optimized signal.
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Time
(1 sample)
40 s
WE(1).Potential
(1 sample)
40 s
WE(1).Current
(Optimized sample)
20 ms
The total time spent sampling Time and WE(1).Potential is roughly 40 s 9 while the
time spent sampling the WE(1).Current signal is about 20 ms or 16.67 ms 10,
depending on the line frequency defined in the Hardware setup (50 or 60 Hz).
If an extra signal has to be sampled, for example the WE(2).Current provided by
the BA module, it must be selected in the sampler window. This extra signal can
then be sampled once just like Time and WE(1).Potential, or for a longer time, in
which case it will be measured several times and averaged. Figure 1.12 shows the
Edit Sampler window corresponding to this situation.
10
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If more than one signal is optimized, the total available time has to be shared.
Figure 1.13 shows a schematic representation of this situation.
Note
The maximum number of signals can be measured optimized is six.
Last segment
Time
(1 sample)
WE(1).Potential
(1 sample)
40 s
40 s
WE(2).Current
(Optimized sample)
WE(1).Current
(Optimized sample)
10 ms
10 ms
Note
The WE(1).Current signal is always sampled in the last sampling step.
Figure 1.14 shows a practical example of sampling an electrochemical signal,
using a single A/D conversion for each data point or the optimized sampling
method. The measured signal is the pH, provided by the pX module for the
Autolab PGSTAT. Using the sample optimization reduces the noise pickup during
the measurement.
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Figure 1.14 A practical example showing the benefits of sampling a signal Optimized
If the WE(2).Current signal must be recorded in the same sampling segment as the
WE(1).current, the Sample alternating option can be used (see Figure 1.15). Using
this option, the WE(1).Current and the WE(2).Current signals will be sampled at
the same time, in an alternating way.
Figure 1.15 The Sample alternating option can be used to sample signals in the same
segment
The equivalent sampling time will still be the same as in the previous case, but
using this option, both signals will be collected at the same time (see Figure 1.16).
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WE(2).Current
(Optimized sample)
Time
(1 sample)
40 s
WE(1).Potential
(1 sample)
40 s
Current
(Optimized sample)
20 ms
Figure 1.16 Sampling an external signal using the sample alternating option
Note
Using the sampler lets the user define exactly which electrochemical signal to
record during a measurement and when these signal have to be recorded.
1.3.4 The Options
The options can be used at the very end of each sampling step to evaluate the
measured data and change the data acquisition settings, test a cutoff condition or
trigger a special action.
The following actions are part of the options:
Automatic current ranging
Cutoff 11
Autolab control 12
Automatic Integration Time 13
The Options can be defined for each measurement command. To edit the options,
click the options button in the procedure editor (see Figure 1.17).
11
For more information on the Cutoff option, please refer to the Cutoff tutorial, available from the
Help menu.
12
For more information on the Autolab control option, please refer to the Autolab control tutorial,
available from the Help menu.
13
For more information on the Automatic Integration Time option, please refer to the FI20 Filter
and Integrator tutorial, available from the Help menu.
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Figure 1.17 Modifying the options for the cyclic voltammetry experiment
The Edit Options window will be displayed (see Figure 1.19). In this window, the
Automatic current ranging settings can be defined, for each working electrode (on
the Automatic current ranging tab). Additionally, the Cutoff tab can be used to
define cutoff conditions for the measured signals and the Autolab control tab can
be used to define special actions for the Autolab instrument 14. If an analog
integrator is available, the Automatic integration time option can be specified in
the final tab.
14
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If the Automatic current ranging option is used, the current range will be adjusted
if necessary, at the end of the sampling step, based on the last recorded value of
the current 15. If the Cutoff option is used for a sampled signal, the last recorded
value of this signal is tested against the threshold value defined in the cutoff.
Specific actions can be triggered by the Cutoff11 (Stop command, Stop complete
procedure, etc.).
1.4 Global and local sampler/options
The signal sampler and options detailed in the previous sections (see Sections
1.3.3 and 1.3.4) can be defined for the complete procedure and for each
measurement command that supports the use of the signal sampler and/or
options in the procedure.
When the sampler or options are defined for the whole procedure, these will be
referred to as global properties. All the measurement commands included in the
procedure will use the global sampler or global options.
When the sampler or options are defined for a single command in the procedure,
these will be referred to as local properties. Only this single command in the
procedure will use these properties and these will overrule the settings specified in
the global sampler and options.
15
The current range is set one range higher when the measured current is > than 3 times the active
current range. The current range is set one range lower when the measured current is < than 0.3
times the active current range.
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Figure 1.20 The Cyclic voltammetry potentiostatic procedure (local sampler defined for the
CV staircase command)
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The database management window will appear, displaying the path for four
different pre-defined databases (see Figure 1.22). Each database is located in a
folder on the computer.
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Figure 1.22 The database management window with the four default databases
16
The Commands database is used to store user defined NOVA commands. Please refer to Chapter
2 of this User manual for more information.
17
The Circuit database is used to store equivalent circuits used in the fitting and simulation of
electrochemical impedance spectroscopy data. Please refer to the impedance spectroscopy tutorial
for more information.
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Figure 1.23 A file browser window is used to change the location of the database folder
The database browser window can be used to create a new database by clicking
the
button. This will create a new folder, which can be renamed and
used as a new database (see Figure 1.24).
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Note
It is possible to rename existing database folder by right-clicking the folder and
selecting the Rename option from the context menu. The same menu can be
used to delete a folder.
1.6 Customizing NOVA
Two different customization options are provided in NOVA:
Profiles: this option is used to filter the contents displayed in NOVA
according to one or more profiles. The software comes with a number of
factory default Profiles, but it is possible to create additional user-defined
profiles. More information is provided in Section 1.6.1.
Software options: this is used to define more advanced software options,
like the default plot options, the Autolab display and the saving mode of
the data files. More information is provided in Section 1.6.4.
1.6.1 Profiles
A profiling scheme is available in NOVA. Using this tool, it is possible to hide some
commands in order to simplify the user interface. Depending on the active profile,
some commands or procedures are hidden from view in order to filter out the
most relevant information. The profiles can be adjusted using the dedicated Profile
menu (see Figure 1.25).
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Figure 1.25 The profile menu can be used to set the user profile
Figure 1.26 The active profile or combination of profiles is indicated in the status bar of
NOVA
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Figure 1.27 Difference between the basic (left) and the advanced (right) profile
Note
The intermediate profile is the default level based profile selected upon
installation of Nova.
Important
The selected level based profile is always on.
1.6.1.2 Hardware based
All the commands and the procedures in NOVA have been tagged with a
hardware requirement marker. When the hardware-based profile is active, only
the procedures and commands that can be executed with the connected
instrument are shown. In Figure 1.28, the Autolab procedures are shown without
and with the hardware-based profile active, for a AutolabIII. Since the AutolabIII
is not fitted with the required hardware, several procedures are hidden.
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Figure 1.28 Overview of the Autolab procedures with a AutolabIII (left, hardware-based
profile not active and right, hardware-based profile active)
Figure 1.29 Difference between the corrosion (left) and the electroanalytical (right) profile
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Note
It is possible to combine all the profile schemes at the same time. For example,
it is possible to set the profile to show hardware-based and intermediate
commands and procedures for the energy application (see Figure 1.30).
Figure 1.30 It is possible to combine several profiles at the same time (intermediate,
hardware-based and energy related)
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Once an item has been hidden from view, it will not be shown until it is unhidden.
To unhide hidden commands, procedures or command parameters, select the
Show all option from the Profiles menu (see Figure 1.32).
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Figure 1.32 Select the Show all option from the Profile menu to display all hidden items
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When a command group is hidden, the whole group will become invisible.
Finally, in the procedure editor, it is possible to hide or unhide command
parameters, using the same method (see Figure 1.35). For example, if the interval
time is not important, it can be hidden from view. This can be used to further
simplify the user interface.
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Figure 1.35 Hiding and unhiding command parameters in the procedure editor
Figure 1.36 A warning is displayed when commands are hidden by the active profile
To reveal the hidden commands, select the Show all option from the Profile menu
or adjust the active profile using the same menu.
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This means that any number of profiles can be created and used at any time using
this method.
It is possible to reset the user-defined profiles to default by using the Reset user
profile option from the Profile menu (see Figure 1.38). A confirm message will be
displayed when the user profile is reset (see Figure 1.39).
Figure 1.39 A confirmation message is displayed with the user settings are reset
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Selecting the Options displays the NOVA options window (see Figure 1.41). Three
different groups are shown in the left-hand side panel of the window:
Graphics
Autolab display
Advanced settings
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Figure 1.43 The default plot options can be defined in the NOVA options
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Figure 1.45 The NOVA options allow the serial number to be activated or deactivated in the
legend
Figure 1.46 shows an example of plot legends with and without the serial number
of the instrument displayed.
Figure 1.46 Plot legend with (left) and without (right) the serial number of the instrument
displayed
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If the total number of points shown in one of the four plot areas in the
measurement view exceeds the value defined for the Maximum number of points
setting, data points from finished commands will be removed in chronological
order.
Important
A smaller number of points will increase the update rate of the plots during a
measurement and reduce the memory usage of the computer. A larger number
of points will decrease the refresh rate and increase memory usage.
This setting is overruled by the Use maximum number of points in real time view
(see Figure 1.48).
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When the Use maximum number of points property is set to No, the software will
try to display all the measured data points in each plot area (up to a limit of 10000
data points for each individual plot).
1.6.4.2 Autolab display
In this category, the colors used in the Autolab display can be defined (see Figure
1.49).
Figure 1.49 The colors used in the Autolab display can be changed
Three different colors are used in the Autolab display. The Active LED color is used
to highlight active settings of the instrument and indicate the noise levels for
potential and current signals in the Autolab display. The Inactive LED is used to
show the inactive settings and the Alarm LED color is used to display warnings
(see Figure 1.50).
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Warning LED
Noise gauge
Active LED
Inactive LED
Figure 1.50 The colors used in the Autolab display are defined in the NOVA options
Note
The settings are grouped into two categories: Basic and Expert. The Expert
settings are used for debugging purposes and these settings should not be
changed. Detailed information on these settings falls outside of the scope of
this manual.
The following Basic settings can be changed:
Auto save measured data (Yes/No): this setting defines if the data is
saved automatically at the end of a measurement (default: yes). When this
option is set to No, the user is prompted to specify the Name and the
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Clear measurement plot before start (Yes/No): this setting defines if the
measurement must be cleared before each measurement (default: yes).
Hidden warning: this option can be used to reset hidden warnings. Click
the
button to reset all hidden warning in the validation dialog (see
Figure 1.53).
Warnings can be hidden in the validation screen by using the right-click menu (see
Figure 1.54).
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Figure 1.55 A time out is used when a Warning is displayed in the Procedure validation
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Figure 2.1 Selecting the Setup view from the toolbar or the View menu
The setup view, which is the default startup view of NOVA, has several important
features shown in Figure 2.2.
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User log
Note
The User log and the Toolbar are elements common to all the views of the
Nova software. The Start button is visible in all the views, except the Multi
Autolab view.
The two most important parts of the Setup view are the procedure editor frame,
which provides a visual workspace for creating/editing procedures and the
procedure and command browser frame, on the left of the screen, which
displays a list of available procedures and commands. The toolbar also features
some procedure editing related buttons that will be described in this chapter.
2.2 The procedure editor and the structure of procedures
The procedure editor provides a framework for editing procedures. An existing
procedure can be loaded into this frame from the procedure browser and can
then be edited to fit your needs.
When NOVA is started for the first time, the procedure editor frame is empty
(Seven lines are displayed: New procedure, Remarks, End status Autolab, Signal
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Figure 2.3 The empty procedure editor frame and the factory standard procedures located
in the Autolab group
An empty procedure editor frame always displays the seven lines shown in Figure
2.3 and these can be edited during the procedure creation process. New
procedure is the default name for all new procedures.
The procedures displayed under the Autolab group in the procedure browser
frame are factory standard procedures. They are always available in NOVA and
cannot be deleted.
To load a procedure into the editor frame, right-click an existing procedure in the
procedure browser frame and select the Open for editing option from the menu
(see Figure 2.4). It is also possible to double click the procedure to load it in the
procedure editor.
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Figure 2.4 Loading the cyclic voltammetry potentiostatic procedure into the procedure
editor frame
Figure 2.5 The procedure editor frame with the loaded cyclic voltammetry potentiostatic
procedure
Figure 2.6 Revealing the parameters of the cyclic voltammetry procedure and the general
structure of a NOVA procedure. The highlighted red lines correspond to the electrochemical
signals sampled during the measurement
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Potential applied
Time
WE(1).Current
Scan
WE(1).Potential
Index
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Figure 2.7 A detailed view of the cyclic voltammetry potentiostatic procedure and its
default parameters (note the detailed tooltip)
Each command shown in the expanded view of the procedure has a number of
parameters that can be edited. These parameters are indicated in black (Start
potential, Scan rate, etc). Some values are indicated in light grey. This means that
they cannot be edited by the user but that they are dependent on the other userdefined parameters. Figure 2.7 shows that the CV staircase command has seven
parameters that can be edited by the user as well as a signal sampler and options.
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Figure 2.8 A detailed view of the CV staircase command in the contracted form
Note
Positioning the mouse pointer on the CV staircase command will display a
tooltip which provides an overview of the parameters (see Figure 2.7 and Figure
2.8).
The five commands preceding the CV staircase command in this procedure
(Autolab control, Set potential, Set cell, Wait time and Optimize current range) are
used as a pre-treatment.
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Note
When the scan rate is changed, the line shown between brackets next to the
CV Staircase command is updated (from [0.000, 1.000, -1.000, 0.000, 2,
0.10000] to [0.000, 1.000, -1.000, 0.000, 2, 0.20000]).
Changing the scan rate of the cyclic voltammetry procedure has an effect on some
of the grey parameters. The interval time originally was 24.4 ms and now is 12.2
ms, because the scan rate has been doubled. If the upper vertex potential is
changed to 0.8 V, the Estimated number of points will also change (see Figure
2.10).
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Figure 2.10 Changing the upper vertex potential has an effect on the Estimated number of
points
The procedure can now be started using the new experimental parameters.
2.4 Advanced editing
The previous section described a very straightforward use of the NOVA procedure
editor: loading a procedure, editing some parameters and running the experiment.
This section will cover a more advanced use of the procedure editor. It is the most
important part of this chapter. Special attention will be given to concepts like
timing and linking.
2.4.1 Adding/Removing commands
Section 2.3 described the use of ready-made Autolab procedures. While these
procedures can be used without modifying their structure, it might be necessary to
change them to fit a specific need. A typical example is the standard Chrono
amperometry procedure.
Load the Chrono amperometry ( t > 1 ms) procedure into the procedure editor.
This procedure has a pre-treatment step just like in the case of the cyclic
voltammetry procedure. During this procedure, the potential of each step is set
using the Set potential command and the response of the cell is measured using
the Record signals (>1 ms) command.
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Figure 2.11 The default Autolab Chrono amperometry ( t > 1 ms) procedure (the Record
signal (> 1 ms) command is expanded to show the details of the command)
The potential used for each step can be edited in the same way as the previous
example. However, editing a chrono amperometry measurement is not only done
by changing the duration of the potential steps and the interval time, but also by
changing the number of potential steps.
Note
Nova has been developed according to the Windows guidelines. This means
that the user interface of the software works as any other Windows
application. Selection of multiple items while holding the CTRL key, drag &
drop, dragging while holding the CTRL key, context-sensitive menus through
the right mouse button and using the mouse wheel are all standard Windows
actions, which are present in Nova.
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Figure 2.12 Removing the third potential step from the procedure (1/2)
Figure 2.13 Removing the third potential step from the procedure (2/2)
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Figure 2.14 The Undo option is also available from the right-click menu
Note
Clicking the redo button,
, button in the toolbar or using the CTRL-Y
keyboard shortcut will redo the last undone action. It is also possible to rightclick the procedure editor and select the redo option from the context menu
(see Figure 2.15).
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Figure 2.15 The Redo option is also available from the right-click menu
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18
Please refer to the Command list description, available from the Help Tutorials menu, for more
information on each command.
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Figure 2.17 The Set potential and Record signals (> 1 ms) commands used in the Chrono
amperometry procedure
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Pay attention to the mouse pointer when the command is dragged on the
procedure editor. Depending on the type of command and the location in the
procedure editor, the mouse pointer can have three different shapes.
Add command: the command can be added at the pointer location.
Insert command: the command can be inserted at the pointer
location. All commands located below this position will be shifted
downwards.
Error: the pointer location is not valid for the selected command.
19
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Figure 2.19 Inserting a Record signals (> 1 ms) command in the procedure
Having added the two commands, their parameters can be edited in order to set
the potential to the required level and sample the current for the required amount
of time, with a convenient sampling rate (see Figure 2.20).
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Figure 2.20 Editing the parameters for the two added commands
Note
In the Record signal (> 1 ms), the duration must be longer than the interval
time.
2.4.4 Cut and Copy Paste commands
It is also possible to use the well known cut/copy and paste options to duplicate a
command or a group of commands already present in the procedure. For example,
to add an additional Set potential command and an additional Record signals (> 1
ms) command to the original Chrono amperometry ( t > 1 ms) procedure, select
the last two Set potential and Record signals (> 1 ms) and right click the selected
commands. Select the Copy option from the context menu (see Figure 2.21).
Note
The CTRL-X (for Cut), CTRL-C (for Copy) and CTRL-V (for Paste) keyboard
shortcuts also work.
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Figure 2.21 Select the copy option from the right-click menu
To paste the copied (or cut) commands, right-click the command below which the
commands need to be pasted and select the Paste option from the context menu
(see Figure 2.22).
Note
Paste commands are always added below the selected command.
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The copied commands will be added to the procedure, below the selected
command (see Figure 2.23).
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Figure 2.24 The Favorite commands group automatically ranks the ten most used
commands
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Figure 2.25 It is possible to manually remove commands from the Favorite group using the
right-click menu
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Figure 2.26 Unchecking the Enabled option will disable the command
A disabled command will be displayed in grey in the procedure editor (see Figure
2.27).
If you start the experiment, you should only see two potential steps, the first step
having a duration of 5 seconds and the second step having a duration of 10
seconds (5 seconds + 5 extra seconds from the third potential step, as Record
signals (> 1 ms) command used to record the third step has not been disabled in
Figure 2.27).
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Figure 2.28 The potential profile used during the measurement on the dummy cell (a) using
the original Chrono amperometry procedure (top) and the modified procedure (bottom)
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Expand the inserted command. A Message box has the following parameters:
Title of box: this is the title of the Message box. By default, the Title of box
is automatically linked to the Serial number of the instrument (Instrument
parameter). This link can be broken if necessary 20. If no instrument is
connected, the Title of box will be unlinked.
Message: this is the message to display in the Message box.
Time limit (s): this defines an optional count down for the Message box.
Use time limit: defines whether the time limit should be used. When this
parameter is set to No, the Message box will be displayed indefinitely.
Type in the following strings for the Message parameter (see Figure 2.31):
Message: Switch off the nitrogen purge!
20
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When the measurement start, before the cell is switched on, NOVA will display a
window displaying the reminder message (see Figure 2.32).
Note
If the Use time limit parameter is set to No, the procedure will not continue
until the OK button is clicked. The Message box command can therefore be
used as an interrupt command. It holds the procedure until the user clicks the
OK button. Messages box commands can be placed anywhere in the
procedure.
Note
As explained in Section 2.4.5, the Message box command will be added to the
Favorite commands group when dragged into the procedure (see Figure 2.33).
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Figure 2.33 The Message box command is added to the Favorite commands group when
dragged into the procedure editor
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Figure 2.34 The links used in the Cyclic voltammetry potentiostatic procedure
Links are shown as grey lines on the right-hand side of the procedure editor
frame, under the Links column. In the example shown in Figure 2.34, a link is used
between Potential parameter of the initial Set potential command and the Start
and Stop potential parameters of the CV staircase command.
Two extra links are used to link the WE(1).Current and the Potential applied signals
to the Y and X axis of the i vs E plot, respectively. The Z axis is linked to the Index
signal.
The three potential values (Set potential, Start potential and Stop potential) are
linked. Editing one of them will immediately change all of them to the new value.
Click the Stop potential value and change it to 0.2 V. Press the enter key to
confirm the change. This will not only change the value of the Stop potential, but
also of the Start potential and the Set potential value (see Figure 2.35).
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Figure 2.35 Changing the value of one parameter changes the values of all the other
parameters it is linked to
Note
The link connecting the three potential parameters changes from grey to black.
This happens whenever one or more parameters or signals that are linked are
selected, making it easy to identify the relationship in the procedure.
Existing links can be removed or modified and new links can be created.
2.4.8.2 Removing links
In the previous example, all three potentials are linked. If the Stop potential should
differ from the Start potential and the Set potential value, then the link to the
other parameters has to be removed. Click the Stop potential parameter to select
it and click the Unlink selected parameter
button in the toolbar to remove the
link (see Figure 2.36).
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If the Start potential is now set back to 0 V, only the value of the Set potential will
be set to the same value. The Stop potential value will remain equal to 0.2 V since
it is no longer linked to the two other parameters (see Figure 2.37).
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Note
Only one parameter can be unlinked at a time.
Links can also be broken using the right-click menu, or using the CTRL-U keyboard
shortcut (see Figure 2.38).
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Figure 2.38 Links can also be broken using the right-click menu or using the CTRL-U
keyboard shortcut
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Note
Removing an existing link requires only one selected parameter. Creating a link,
on the other hand, requires at least two selected parameters.
Links can also be created using the right-click menu, or using the CTRL-L keyboard
shortcut (see Figure 2.40).
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Figure 2.40 It is possible to create links and remove links using the right-click menu
Note
The Undo Unlink option is also provided in the right-click menu (see Figure
2.40). The Undo and Redo options can be used to restore broken links or break
restored links.
2.4.8.4 Links: the programming tools of NOVA
Links can be used to program in NOVA. Using links, procedure parameters can be
linked with one another. Results of data handling steps can be used for plotting or
as new parameters for the rest of the experiments. Using links, it is possible to
program just about any measurement sequence.
Links can be used to create interactive or dynamic procedures, which allows a
change to a procedure parameter while the experiment is running depending on
parameter values provided by the user or calculated by the software, during the
experiment.
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Expand the inserted command. An Input box has the following parameters:
Title of box: this is the title of the Input box. By default, the Title of box is
automatically linked to the Serial number of the instrument (Instrument
parameter). This link can be broken if necessary 21. If no instrument is
connected, the Title of box will be unlinked.
Message: this is the message to display in the Input box.
Value: this is the default value for the input value of the Input box.
Time limit (s): this defines an optional count down for the Input box.
Use time limit: defines whether the time limit should be used. When this
parameter is set to No, the Input box will be displayed indefinitely.
In this example, the Input box command will prompt the user to enter the
requested scan rate for the cyclic voltammogram. The preset value for this
procedure is 100 mV/s but this value will be overruled by the user once the
procedure is started.
Type in the following parameters (see Figure 2.42):
Message: Enter the value of the scan rate, in V/s
Value: 0.050
Time limit (s): 30
Use time limit: no
21
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To instruct the software to use the value typed into an Input box, a link must be
created between the Value parameter of the Input box and the parameter in the
procedure it is supposed to replace, in this case, the scan rate.
Creating this link can be done in the same way as in the previous section. Hold the
CTRL key, select the Value parameter of the Input box and the Scan rate
parameter of the CV Staircase command and press the Link selected parameters
button in the toolbar (see Figure 2.43).
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Figure 2.43 Linking the Input box value to the scan rate
When the link is created, a new black line appears on the right side of the
procedure editor frame, linking the value of the Input box to the scan rate. The
scan rate also changes from 0.1 V/s to 0.050 V/s when the link is created, thus
substituting the preset value with the default value of the Input box.
Note
Using Input box commands and links allows the creation of interactive
procedures. This can simplify research when a procedure has to be repeated a
number of times but with different parameters. It also provides a very useful
educational tool.
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B
C
Figure 2.45 The chrono charge discharge procedure
The first segment (A), the pretreatment, consists of four separate commands:
Autolab control
Set potential (0 V)
Set cell (On)
Wait time (10 s)
All these commands are timed commands and they will be executed without
interruption. To provide a visual indication, a green line is shown on the left-hand
side of the procedure editor (see Figure 2.46).
Figure 2.46 The four commands in section A are all timed commands
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Figure 2.47 The second part of the procedure contains the repeat loop and the
measurement sequence
The Repeat n times command creates a repeat loop. Since this command is not a
timed command, it creates a break in the green timing guide, indicating that there
will be an interruption at each repetition.
Commands that are placed inside the Repeat n times command will be repeated n
times when the procedure is executed. However, this is only true for those
commands that are located on the second level under the Repeat n times
command.
All the commands that are located under the Repeat n times command will be
repeated.
The four commands located inside the Repeat n times command are all timed
commands and they will be executed without interruption. This is again indicated
by the green timing guide located on the left-hand side of the procedure editor
(see Figure 2.47).
During the measurement, the two potential steps (Set potential command) and
the two chrono measurements ( Record signals (>1 ms) command) will be executed
without timing interference from background Windows activity.
The final segment of this procedure consists of a single command that turns the
cell off when the measurement is finished (see Figure 2.48). Since this is again a
timed command, the timing guide will be shown on the left hand side.
Figure 2.48 The final segment of the procedure is used to switch the cell off at the end of
the measurement
The timing of the full procedure is interrupted at two locations, as indicated by the
timing guide on the left-hand side of the procedure editor (see Figure 2.49).
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>
>
Figure 2.49 The timing of the procedure is interrupted at the beginning and at the end of
the Repeat n times command
The interruptions are located before and after the Repeat n times command. Since
the Repeat n times command is not a timed command, it creates a small
interruption in the measurement timing. This interruption will be observed at each
repetition. Depending on the activity of the host computer, the interruption can be
in the range of a few seconds.
Figure 2.50 shows the potential profile used in the standard chrono charge
discharge procedure. A sequence of steps is repeated ten times during the
measurement. The potential changes from 0 V to 1.2 V.
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Figure 2.50 The potential profile used in the standard chrono charge discharge procedure
Detailed inspection of the data shown in Figure 2.50 shows that the time delay
between two recorded steps within the same repeat loop is 0.012 s (30.979 s
30.967 s) whereas the time delay between two consecutive steps located in two
different repetitions is ~ 0.6 s (17.385 s 16.773). This illustrates the timing
difference and the time delay introduced by untimed commands like a Repeat n
times command (see Figure 2.51).
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Note
The time between timed commands will always be very accurately determined
by the internal clock of the Autolab. The time delay introduced by untimed
commands will be affected by the background activity of the host computer
and will therefore be less predictable.
2.5.2 Building advanced procedures
The final section of this chapter describes how to use the procedure editor to
create an advanced procedure from scratch.
Click the
button to clear the procedure editor frame. The editor will display an
almost empty procedure editor frame (see Figure 2.52).
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The seven lines displayed in the procedure editor frame are the default
components of each procedure.
Note
The default Signal sampler includes the Time and WE(1).Current (optimized)
signals. The default Options are set to No Options. Please refer to Sections
1.3.3 and 1.3.4 for more information on the Signal Sampler and the Options,
respectively.
In this section, the step-by-step construction of an advanced procedure will be
illustrated. The intention is to create a procedure that performs a Linear sweep
voltammetry measurement at four different, pre-defined, scan rates. This
procedure will be designed with a preconditioning stage.
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Autolab control
Set potential
Set cell
Wait time
Optimize current range
Select the Autolab control command and drag it into the procedure editor (see
Figure 2.53).
To set the parameters of the Autolab control command, click the button located
on the right-hand side of the procedure editor window (see Figure 2.54).
22
It is a good habit to set the instrument to the correct settings at the beginning of a procedure.
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A new window, called Autolab control, will be displayed (see Figure 2.55). This
window displays the settings currently defined on the connected instrument and
can be used to change any of the instrument settings at any time during a
procedure. In Figure 2.55, the basic settings for the main potentiostat/galvanostat
can be defined 23.
For this procedure, the Autolab control command will be used to set the
instrument to potentiostatic mode and in the 1 mA current range. Using the dropdown menus, set the Mode and the Current range settings to Potentiostatic and
1 mA, respectively (see Figure 2.56).
23
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Figure 2.56 Using the Autolab control command to set the instrument to Potentiostatic
mode and in the 1 mA current range
Click the OK button to close the Autolab control window. The settings specified
Figure 2.56 will now be displayed in the procedure editor, below the Autolab
control command (see Figure 2.57).
Figure 2.57 The Autolab control settings are displayed in the procedure editor
Next, locate the Set potential, Set cell, Wait time and Optimize current range 24
commands and drag them into the procedure editor, under the Autolab control
command (see Figure 2.58).
24
For more information, please refer to the Command list document, available from the Help
menu.
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Figure 2.58 Adding the Set potential, Set Cell, Wait time
and Optimize current range commands
A warning symbol ( ) will be visible in the procedure editor, next to the Optimize
current range command (see Figure 2.58). This warning symbol only appears after
adding the Optimize current range command to the sequence.
A toolip is available for each warning in the procedure editor (see Figure 2.59).
Figure 2.59 A tooltip is available for each warning in the procedure editor
Note
To provide help in the procedure building process, validation of the procedure
is performed in the background, in real time. Whenever a problem is detected,
NOVA will display a warning symbol ( ) next to the command(s) afftected by
this problem. Whenever an error is detected, NOVA will display an error symbol
( ) next to the command(s) affected by this error.
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Note
As soon as the cell is set to On status in the procedure editor, the warning
symbol ( ) next to Optimize current range command is cleared since the
warning is no longer valid (see Figure 2.61).
Figure 2.61 The warning is removed when the Cell status is switched to On in the
procedure editor
The value of the preconditioning potential is not yet defined. It will be linked to
the start potential of the linear sweep voltammetry command which means that
its value is not relevant at this time.
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Figure 2.62 Adding the Repeat for each value command to the procedure
The Repeat for each value command creates a repeat loop, for which the number
of repetitions is equal to the number of pre-defined values of the command.
Add the LSV staircase command, from the Measurement Cyclic and linear
sweep voltammetry group to the Repeat for each value command. Next, add an
additional Set potential command to the sequence, as shown in Figure 2.63.
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Figure 2.63 Adding the LSV staircase , Set potential and Wait time commands to the
procedure
For this example, the Start potential of the LSV staircase command will be -0.06 V
and the Stop potential will be set to 0.55 V. The start potential value will also be
used as the preconditioning potential.
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Figure 2.64 Modifying the LSV staircase parameters and creating the link with the
preconditioning potential
The Repeat for each value command has three default pre-defined values (1, 2 and
3). To change these values, click the
button located on Values parameter line
(see Figure 2.65).
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This will open a Range builder window that can be used to construct a sequence
of values to be linked to the scan rate of the LSV staircase command (see Figure
2.66).
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The Range builder is a useful tool that can be used to edit the sequence of the
Repeat for each value command. There are two ways to add values to the range.
The first option is to type each individual value in the Value field on the top
of the window and click the
button.
The second option is to use the Range generator, which is selected by
pressing the
button. This option is suitable for adding a large
number of values to the range.
Note
The Range builder provides a
button to remove any previously added
values and a sort button which can be used to sort the values of the range.
Click the
button to remove the default values from the range and click the
button to display the Range generator window (see Figure 2.67).
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The Range generator is used to create a list of values using the following
parameters:
Begin value: the first value of the list
End value: the final value of the list
Nr of values: the total number of values in the list
Step type: the distribution of the values in the list (linear, logarithmic or
square root)
Note
If a list of identical values needs to be created, the End value checkbox can be
unchecked. When this is done, only the Begin value will be used to create the
list.
For this example, we are going to use a total of four values, ranging from
0.050 V/s to 0.5 V/s, with a square root distribution. Type these parameters in the
range generator window and press the
button to generate the list of
values, click the
button to close the generator window and return to the
Range builder window. The generated list of values will be displayed in the Values
field of the Range builder window (see Figure 2.68).
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Figure 2.68 Closing the Range generator window will update the contents of the Range
builder window
Note
It is possible to sort the list in ascending or descending order by clicking the
button located in the Range builder window.
Click the OK button to return to the procedure editor. The Repeat for each value
command will be updated (see Figure 2.69). To complete the setup of the repeat
loop, the values of the command have to be linked to the Scan rate parameter of
the LSV staircase command (see Figure 2.69).
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Figure 2.69 The updated Repeat for each value loop: the values are linked to the Scan rate
parameter of the LSV staircase command
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Check the WE(1) checkbox to activate the automatic current ranging option for
the working electrode and set the highest and lowest current ranges to 10 mA
and 1 A respectively (see Figure 2.71).
Click the
button to close the Automatic current ranging window. You will
be prompted to define for which measurement commands in this procedure you
want to use this option, through the Preview changes window. There are two
commands in this procedure that can use the automatic current ranging options
(see Figure 2.72). Since these options are intended to be used in the whole
procedure, click the Select all button to check all the available measurement
command and then press the
button to validate the options for these
commands.
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Figure 2.72 Choosing the measurement commands for which to use the options
Note
It is also possible to open the Options by clicking the
button in the quick
access toolbar which appears when the procedure header is selected (see
Figure 2.73).
Figure 2.73 Opening the Options editor can also be done by clicking the
quick access toolbar
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button in the
Click the
button to close the Sampler editor window. Again, NOVA will
prompt you to choose for which measurement commands you want to use this
sampler, through the Preview changes window (Figure 2.75). Select all the
measurement command and press the
button.
25
Please refer to Chapter 1 of this User Manual for more information on the different sampling
strategies in Nova.
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Figure 2.75 Choosing the measurement commands for which to use the sampler
Note
It is also possible to open the Sampler by clicking the
button in the quick
access toolbar which appears when the procedure header is selected (see
Figure 2.76).
Figure 2.76 Opening the Sampler editor can also be done by clicking the
quick access toolbar
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button in the
Figure 2.77 The i vs E Plot used in combination the LSV staircase command
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LSV staircase command. This triggers the quick access toolbar to appear (see
Figure 2.78).
Figure 2.78 The quick access toolbar can be used to add plots to the measurement
command
Note
The list of plots shown in the quick access toolbar depends on the signals
defined in the signal sampler. If the WE(1).Potential signal is not sampled, the E
vs t and the E vs log(t) plots will not be available (see Figure 2.79).
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Figure 2.79 The list of plots shown in the drop-down list depends on the signal sampler
settings (left: WE(1).Potential sampled; right: WE(1).Potential not sampled)
Click the
button in this toolbar to display a list of available plots in a drop-down
list and select the E vs t plot to add it to the LSV staircase command.
The E vs t will be added to the LSV staircase command and the X and Y inputs of
the plot will linked automatically to the signals provided by the command (see
Figure 2.80).
Figure 2.80 The E vs t plot command is automatically linked to the signals provided by the
LSV staircase command
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Figure 2.82 Changing the remarks for the Cyclic voltammetry potentiostatic procedure
The remarks can be used to add information on the cell setup (electrolyte, working
electrode, reference electrode, etc.). This information will be stored alongside the
measured data.
When the remarks field has been edited, the procedure can be saved into the My
procedures database. To do this, change the name of the procedure from New
procedure to User manual example in the procedure editor and go to the File
menu in the toolbar, and select the Save procedure as new option. This will add
the currently edited procedure to the My procedures database. The procedure is
logged in this database by name, time and date and, if the mouse pointer is
moved over it, it will display a tooltip showing the remarks for this procedure as
well (see Figure 2.83).
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Note
The remarks field can contain several lines of comment. All the added lines will
be displayed in the tooltip which is very convenient for managing several user
defined procedures. The tooltip also displays the location of the procedure file.
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Figure 2.84 The Check procedure tool is available in the Tools menu
Alternatively the keyboard shortcut Alt + F1 can also be used. NOVA will check the
procedure for errors. If no errors are detected, the No problems found Message
will be displayed (see Figure 2.85).
Figure 2.85 The No problems found message is displayed when no errors are detected
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Figure 2.86 The LSV curves obtained using the procedure described in this section
(left plot #1: i vs E, right plot #2: E vs t)
Figure 2.87 Dragging and dropping the Autolab Cyclic voltammetry potentiostatic
procedure into the procedure editor
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Figure 2.88 Choosing the Options and Sampler settings to use for the Cyclic voltammetry
potentiostatic
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Figure 2.89 The Cyclic voltammetry procedure added to the procedure editor
Select the Cyclic voltammetry galvanostatic procedure and drop it into the
procedure editor, after the cyclic voltammetry procedure. When the mouse button
is released, a message will be displayed (see Figure 2.90).
Figure 2.90 Choosing the Options and Sampler settings to use for the Cyclic voltammetry
galvanostatic procedure
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Figure 2.91 The procedure editor with the two complete procedures
Connect dummy cell (c) and press the start button. When the measurement starts,
the procedure will first execute the complete Cyclic voltammetry potentiostatic
procedure, using Automatic current ranging. When the first part of the
measurement is finished, the Cyclic voltammetry galvanostatic procedure starts.
The Autolab control command will switch the potentiostat to galvanostatic mode
and set the current range to 1 mA, before performing the current scan.
Figure 2.92 and Figure 2.93 show the measured data on the dummy cell (c). The
first part of the measurement corresponds to the potentiostatic cyclic
voltammetry. The measurement stops after 47 seconds. The second part of the
measurement corresponds to the galvanostatic cyclic voltammetry, which starts
after 55 seconds. The time difference between the two measurements stems from
the preconditioning stage at the beginning of the cyclic voltammetry galvanostatic
measurement.
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Figure 2.92 The first part of the measurement (Cyclic voltammetry potentiostatic):
measured current vs time
Figure 2.93 The second part of the measurement (Cyclic voltammetry galvanostatic):
measured potential vs time
The Options and Sampler can be modified for the whole procedure or for each
individual procedure in the procedure editor. Click the
button located next the
Sampler in the procedure editor or use the quick access toolbar (see Figure 2.94).
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The sampler editor will be displayed. For illustration purposes, the WE(1).Charge
signal will be added to the sampler (see Figure 2.95).
Click the
button to close the Sampler window. The Preview changes
window will be displayed, allowing you to choose for which measurement
commands in the procedure this sampler should be used (see Figure 2.96).
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2.7 My commands
The final section of this chapter describes the My commands framework. This
feature allows you to create new commands. A specific database is available to
store your own commands. The location of this database can be defined using the
database manager (see Figure 2.97).
Figure 2.97 The database manager can be used to define a Commands database
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Click the
button to close the editor. The specified settings will be
displayed in the procedure editor (see Figure 2.101).
Figure 2.101 Settings defined in the Autolab control command are shown in the procedure
editor
To save the Autolab control command with all the defined settings in the My
commands group, right-click on the Autolab control command and select the Save
in My commands option from the context menu (see Figure 2.102).
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Figure 2.102 Right-click the Autolab control command and select the Save in My
commands option
A window will be displayed. Herein, a name for the My command can be specified
and remarks can be added. This is helpful for bookkeeping purposes, in order to
identify the command more easily. For this example, a name and remarks are
provided as shown in Figure 2.104.
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Click the
button to close the window. This specific version of the Autolab
control command will be added to the list of My commands (see Figure 2.105).
Note
The remarks are shown in the tooltip.
2.7.2 Creating complex My commands
The example shown in the previous section shows how to create a single My
command. It is also possible to group commands together to create a complex set
of commands as a single My command.
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Figure 2.106 The Nested procedure command can be used to group commands
, in the toolbar
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Figure 2.108 The Nested procedure command creates a subsequence in the procedure
editor
From the command browser, add the following commands into the procedure
editor, ensuring that they are added to the Nested procedure sequence (see Figure
2.109):
Autolab control
Set potential: 1.2 V
Set cell On
Wait time (s): 5
Optimize current range
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Note
Make sure that the commands are added to the Nested procedure sequence.
Use the Autolab control command to set the instrument to High stability, select
the 1 mA current range and set the Autolab to potentiostatic mode (see Figure
2.110).
Figure 2.110 Set the initial Autolab conditions using the Autolab control interface
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Figure 2.111 Select the Save in My commands option from the right-click menu
You will be prompted to specify a name and remarks for the command (see Figure
2.112).
In the example shown here, the whole Nested procedure will be saved in the My
commands database, as My Potentiostatic Preconditioning. Once the
button is clicked, the whole Nested procedure will be saved in the My commands
database (see Figure 2.113).
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Figure 2.114 Adding a My command into the procedure editor creates a copy of the
original command
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Real time information on the measured data and the procedure is shown and
updated as the data is collected. Figure 3.2 provides an overview of the
Measurement view.
Note
By default, Nova switches to the Measurement view automatically when the
Start button is pressed. Refer to Section 1.6.4.3 for more information.
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Procedure progress
Parameter editor
User log
Figure 3.3 Up to four different plots can be displayed in the measurement frame
Note
The contents of the plots are defined in the procedure setup (see next Section).
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Figure 3.4 The procedure progress frame during the standard Autolab linear polarization
procedure (the LSV staircase command is highlighted, indicating that NOVA is currently
running that command)
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Figure 3.5 Overview of the command parameters that can be changed during a
measurement (left: Wait time (s) command, right: CV staircase command)
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Figure 3.6 Parameters can be changed by typing the new value and clicking the
button
Note
Not all command parameters can be changed in real time. For more
information on the parameters that can be modified in the measurement view,
please consult the Command list document, available from the Help menu in
Nova.
3.2 Measurement plots
The measurement view is used to display the recorded data points during the
experiment, or the results of calculation or data handling instructions added to the
procedure. Up to four different plots can be used in the measurement view and it
is possible to display one, two or four plots at the same time. The initial contents
of these plots are defined in the procedure setup. Each Plot command added to
the procedure in the Setup view has two parameters that define the plotting
settings in the Measurement view (see Figure 3.7).
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Figure 3.7 - The i vs E plot command used in the Autolab cyclic voltammetry potentiostatic
procedure
The following parameters can be specified in the Setup view for each plot:
Show during measurement (Yes/No): defines if the plot should be
displayed in the measurement view during the experiment. When this
parameter is set to No, then the plot is not shown during the
measurement. The plot is, however, added to the data set and is available
for plotting in the Analysis view.
Measurement plot number (1, 2, 3 or 4): defines the location of the plot
in the Measurement view. Up to four plots can be shown in the
measurement view (see Figure 3.8).
Figure 3.8 The location of the four plots available in the Measurement view
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Figure 3.9 shows an example of four plots displayed in the measurement view
during an impedance spectroscopy measurement. Plot #1 corresponds to the
Nyquist plot, plot #2 is the Bode plot (both modulus and phase), plot #3 is the
Lissajous plot and plot #4 shows the resolution for both channels plotted versus
time.
Figure 3.9 Example of four plots shown in the measurement view during an impedance
spectroscopy measurement
Note
The contents of each plot are removed whenever the type of signal used on the
X-axis changes during a measurement.
3.2.1 Adding and removing plots in real time
While the measurement is running, it is possible to add or remove plots from the
measurement view. To add a plot, right-click a measurement command in the
procedure progress frame and use the context-sensitive menu to add a new plot
to the measurement, as shown in Figure 3.10.
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Figure 3.10 The right-click menu can be used to add a new plot to the measurement
The list of available plots shown in the context menu depends on the signals
sampled during the measurement. In Figure 3.10, the WE(2).Current, recorded
through the Bipotentiostat module, is present in the signal sampler for the CV
staircase command. It is therefore possible to add the i(WE2) vs E plot to the
measurement, on plot #2.
To remove a plot, right-click on the plots shown below the command and select
the Delete option from the context menu (see Figure 3.11).
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Note
The data is saved at the end of the measurement using the plots existing at the
end of the experiment. If plot options are changed during the experiment, the
last used plot options will be saved.
3.3 Clearing the measurement view and zooming
During the measurement, the clear measurement plot
button can be clicked at
any time to clear all the plots in the measurement view. The plotting of the data
points will resume after the plot has been cleared. The measured data points are
however kept in memory.
Note
The clear plot button can be extended by clicking the arrow button located
next to the clear plot button. This will show a context menu with which any
one of the four plots can be cleared (see Figure 3.13).
Figure 3.13 It is possible to clear a specific plot in the measurement view by extending the
Clear plot button
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Figure 3.14 Right click the plot to select the Enable Zooming / Moving option
Note
Additional options are available in the context menus in the measurement view.
More information is provided in Chapter 4 (Section 4.7.3 to 4.7.13).
26
If a wheel mouse is not available, it is possible to use the + and keys on the keyboard to
achieve the same results.
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Figure 3.15 Choose the Autolab display option from the view menu or use the dedicated
button in the toolbar to open the Autolab display window
27
The colors used in the Autolab display can be set using the Tools Options menu.
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Potential
Serial number
Current
Manual settings
Active current range
Experimental control
Experiment data
Measurement progress
Figure 3.16 An overview of the Autolab display during a CV measurement (Autolab III)
The available current ranges are displayed on the right-hand side of the Autolab
display. The highest and lowest possible current range depend on the hardware
settings (in the case of Figure 3.16, the instrument is a Autolab III, therefore the
highest current range is 10 mA). The serial number of the instrument is located in
the header of the Autolab display window 28.
The selected current range is highlighted. The
button located in the
29
Autolab display can be used to reverse the scan direction .
The active settings are highlighted. It the case of Figure 3.16, the settings are:
Potentiostat mode (PSTAT label)
Current range 1 mA (1 mA label)
High stability on (HSTAB label)
Cell on (CELL ON label)
Most of the labels of the manual control are interactive. A setting of the Autolab
potentiostat can be changed by clicking the corresponding label.
Clicking the labels of the manual control will also update the settings displayed on
the front panel of the instrument.
The information displayed at the bottom of the Autolab display window depends
on the experimental method.
28
This is the indentifying serial number of the instrument. When the Autolab is used in
combination with an external USB interface, the serial number of the USB interface is shown.
29
This option is only available for cyclic voltammetry and linear sweep voltammetry staircase.
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Figure 3.17 Adding the FRA manual control to the Autolab display
The FRA manual control panel can be used to control the FRA2 or FRA32M
module and to perform impedance measurements (see Figure 3.18).
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Figure 3.18 The FRA manual control panel can be used to control the FRA2 module through
the Autolab display
This panel also displays measured impedance values during a frequency scan 30.
3.4.3 Collapsible panels
At any time, it is possible to click on the
button located in the top left corner of
an Autolab display panel to collapse the contents of this panel in order to hide the
information (see Figure 3.19).
30
More information can be found in the Impedance spectroscopy tutorial, available from the Help
Tutorials menu.
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Potential
Current
Figure 3.20 The noise gauges are indicating the noise levels qualitatively
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4 Analysis view
Data analysis is performed in the Analysis view. The Analysis view can be accessed
at any time, even during an ongoing measurement, by clicking the corresponding
button
in the toolbar or selecting the Analysis view from the View menu (see
Figure 4.1).
This view, like the other views of the NOVA software, has a specific layout, with
several areas of interest. An overview of the analysis view is given in Figure 4.2.
Note
Like all the frames in Nova, the frames in the data analysis view can be resized.
Moreover, the user log can be toggled off using the view menu. This allows you
to maximize the size of the Data analysis frame for a better overview of the
data.
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Database frame
Quick access toolbar
Plot area
Data explorer frame
Analysis frame
User log
The Start/Stop button, toolbar and the User Log are both common to all views of
NOVA. Other noteworthy areas of the Analysis View are:
Database: displays the list of available data sets that can be used in the
data analysis view. Each entry of the database has a name, a time stamp
and a remarks field.
Data explorer: displays the data set(s) currently selected for data analysis.
Plot area: displays the selected data points in a 2D or 3D plot.
Analysis frame: displays the control parameters and the results of data
analysis tools.
4.1 Introduction
This chapter of the user manual explores the Analysis view and provides in-depth
information about this essential part of the software. Some examples are provided
in this chapter and the corresponding data sets are available in the Demo
database folder, which is created during the installation of NOVA 1.10. This
database contains all the examples used in this chapter.
4.1.1 The database
To use the database, click the
button on the right of the area displaying the
path of the Measured data database. Change the path to the Demo Database
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Figure 4.3 Loading the Demo database by setting as the Data database
The demonstration database has been set as a Data database. Its contents are
displayed in the database frame of the Analysis view (see Figure 4.4).
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Database frame
Figure 4.4 The contents of the database are displayed in the database frame in the analysis
view
31
This is the serial number used by the software to identify the instrument. For measurements
performed on an Autolab with an external USB interface, the serial number of the USB interface
will be used to identify the device.
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The data can be sorted on Procedure name, Time stanp, Remarks, Instrument
serial number and Instrument description.
4.1.1.2 Data filtering
The database also provides a filtering option that can be useful when exploring a
database with a lot of entries. By using the filter option, it is possible, for example,
to select all measurements that have been obtained using a specific instrument.
Click the Demo 01 Copper deposition entry of the database and right-click on
the Instrument header. Select Filter with selected dropped on row, using a Like
option (see Figure 4.7).
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The contents of the database will be updated, displaying only the database entries
obtained with the instrument with serial number AUT83072 (see Figure 4.8).
The eleven data sets displayed in the filtered database have being obtained with
the same instrument as the one used for the Demo 01 Copper deposition entry
of the database (AUT83072)). By using the filtering option described above, only
the data sets for which the serial numbers are the same, are displayed.
To remove the filter, right-click the database header and select the Show all
option from the context menu (see Figure 4.9). This will restore the database to its
original content, displaying all the data sets.
Figure 4.9 Select the Show all option to view the entire contents of the database
Note
Use the Best fit and Best fit all to automatically adjust the width of the columns
in the database.
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Figure 4.10 Select the Store in Repository option to create a backup of the database entry
The store in repository option adds a copy of the original data set in the database
using the backup creation time as the time stamp (see Figure 4.11).
Figure 4.11 The repository backup creates a copy of the original data set
Once a backup has been added to the repository, it is possible to modify the
original data set and restore it at any time by choosing the Restore from
Repository (see Figure 4.12). It is also possible to create more than one backup in
the data repository.
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Figure 4.12 Restoring the original data set from the repository backup
Note
Using the Restore from repository removes any modification of the current data
set and restores the data set to the backed up status.
4.1.1.4 Merging data
The database also allows the merging of two or more files. When database entries
are merged, a new file containing the procedures and the data from the merged
files will be copied to the new file. This can be used to involve the data from two
or more different measurements in a calculation or other data handling steps
described in this chapter.
To merge two or more data files in the database, select the files by clicking them
while holding the CTRL key pressed. The selected files will be highlighted in the
database frame (see Figure 4.13).
Right-click the selected database entries and select the Merge data option from
the context menu (see Figure 4.14).
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Figure 4.14 Right-click the selected entries and select the Merge Data option
Figure 4.15 A popup dialog is displayed when the files are merged
Using the window, a new database filename can be specified and the remarks
field for the merged file can be edited. Pressing the
button and closes the
editor, adding a file to the database (see Figure 4.16).
The new file will contain the data from the source data files.
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A name and a location for the file can be specified (see Figure 4.18).
Figure 4.18 Specifying a name and location for the exported file
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To import a data file, right-click anywhere in the database frame and select the
Import data option from the context menu (see Figure 4.20).
Figure 4.20 The dialog shown during the importing of data files
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Figure 4.21 The Show in Windows explorer option provides a shortcut to the location of a
database entry
A Windows explorer window will open, showing the location of the selected file
(see Figure 4.22).
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Note
It is possible to delete multiple files at the same time. Deleted data files are
automatically moved to the Recycle bin.
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Figure 4.24 Loading a data set from the database into the data explorer
Note
The Demo 01 Copper deposition entry of the demo database contains a cyclic
voltammogram for copper deposition on platinum, recorded in 0.1 M CuSO4 in
0.1 M H2SO4 solution. The reference electrode was a Ag/AgCl (KCl satd) and
the counter electrode was a platinum wire.
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Note
Clicking the i vs E line will change it to bold lettering, and it will be highlighted.
The bold lettering indicates that the data set is currently plotted in the
data analysis frame.
The highlighted status indicates that the data set plotted in the data
analysis frame is currently also the active plot (in the case of an overlay of
several plots, only one can be active).
4.2.2 Changing the data set display settings
The way the data is displayed is controlled by the signals used for the plot. The
data from example #1, shown in Figure 4.25, is displayed using the Potential
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Changing the display settings in order to plot the potential in function of time as
described in the picture above will change the display of the data set and a
familiar saw-tooth potential profile of a cyclic voltammogram will be plotted (see
Figure 4.27).
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Note
Changing the signals used to display the data points from example #1 also
changes the labels displayed on the axes of the plot.
Warning
The time signal is the total elapsed time since the beginning of the
measurement. It includes the preconditioning time used during the experiment.
If required, it is possible to use the calculate signal tool to correct the time scale
(see section 4.10).
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The Plot Options window will be displayed. Through this window, it is possible to
customize every aspect of the selected plot (see Figure 4.29). It is possible to
change the plot color, the plot style, the point markers, axes configuration, etc.
Note
The settings defined in the Plot options window are used for both 2D and 3D
plots. It is possible to define specific settings for both data presentation formats
by clicking the Advanced button in the Plot options window.
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The plot options window has four different tabs, which can be used to define
different aspects of the plot.
4.2.4 Data tab
The items located on this tab are related to the plot appearance. It is possible to
choose from different plot style, to change the plot color and size and define a
point style. It is also possible to change the position of the Y-axis (see Figure 4.29).
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The plot options window provides a convenient interface for changing all the
available plot settings at the same time. It is still possible to change specific plot
options by right-clicking the corresponding items on the plot directly. For example,
right-clicking on a plot axis will display a menu from which some of the options
available in the Axes settings tab can be defined (see Figure 4.33).
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Note
Contrary to the setting defined in the Plot Options window, the settings
defined using the context menu are only valid for the related item in the active
plot. Changing the Y-axis settings in a 2D plot does not affect the appearance
of the corresponding 3D plot.
As an example, select the i vs E plot from Example #1 data set and using the Plot
Options window, change the plot settings to a red Combi plot, using a size 10
pyramid as a symbol, plotting 1 point out of 40 and using a size 2 line (see Figure
4.34).
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Note
The i vs E has changed color and is preceded by a red pyramid symbol (i vs E).
This feature makes it easier to identify a specific plot in an overlay (see Section
4.4).
4.2.8 Creating new plots
It is often convenient to plot experimental data in different ways. NOVA offers this
possibility directly from the analysis view. Using the right-click menu, it is possible
to add any number of new plots to a data set. Two different types of plots can be
created: a command-specific predefined plot or a generic Custom plot. In this
section, both options will be illustrated.
NOVA provides a number of predefined plots for every measurement command.
The experimental data from Example #1 was measured using the CV staircase
command, for which a total of nine predefined plots are available. To add any of
these plots to the data set, right-click the CV staircase line in the data explorer and
select the Add Plot option from the context menu.
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Note
The number of available plots depends on the signals available in the data set.
It is also possible to add a plot to the measurement by using the quick access
toolbar. Clicking the
button displays the list of available plots (see Figure 4.37).
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Figure 4.37 Using the quick access toolbar to add a plot to the data set
Select the Log(i) vs E plot. This will add a predefined plot to the data set,
displaying the WE(1).Current on the Y-axis, in logarithmic scaling and the Potential
applied on the X-axis. The plot will be displayed using the default plot settings (see
Figure 4.38).
It is also possible to add a generic new plot to the data set, simply called Custom,
which does not have any predefined settings. To do this, right-click the CV
Staircase line in the data explorer frame and select the Add Plot option (see
Figure 4.39).
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The newly created Custom plot does not have any signals assigned for X, Y and Z
and therefore does not plot anything until these are defined by the user.
Change the signals in order to plot the measured current relative to the time. (X =
Time, Y = WE(1).Current). Change the plot settings to a red Combi plot, using a
black pyramid upside down as a symbol, size 10, plotting 1 point out of 40 and
using a size 2 line (Figure 4.40).
Figure 4.40 Setting the options for the newly added plot
This new plot should like the one displayed in Figure 4.41.
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Each plot can be renamed. To change the name of a plot from Custom to
something else, right-click the Custom line you want to edit and select the
Properties option. A small window will be displayed which allows you to edit the
name of the plot (see Figure 4.42).
Rename the first plot E vs t and the third plot to i vs t (see Figure 4.43).
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Note
If the ongoing session of Nova is closed or if the data set is removed from the
data explorer frame before the changes have been saved, a warning message
will be displayed prompting the user to choose whether or not to update the
database. Clicking the
button will update the database in the same way
/
as the Save button. Choosing No will discard all the changes. A
button is also available, for all the open data sets (see Figure 4.45).
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Figure 4.46 Using the Save the data in the database option to update
the whole data set
When the 3D button is clicked, NOVA will display the data from example #1 in a
perspective, 3D plot (see Figure 4.49).
Press and hold the right arrow key on your keyboard to rotate the 3D plot around
the Y-axis, slowly bringing the time axis in plane with your computer screen (see
Figure 4.50).
Note
You can use the CTRL key in combination with the arrow key to rotate the plot
faster. Press the Page Up and Page Down keys to spin the plot in the X/Y plane.
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Alternatively, click anywhere on the 3D plot, and move the mouse in any direction,
while holding the mouse button, to spin the plot in the direction of your choice
(see Figure 4.51).
Figure 4.51 Moving the 3D plot with the help of the mouse pointer
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To view the EQCM(1). Frequency signal versus the applied potential, right click
the CV staircase line in the data explorer and choose the Frequency vs E from the
Add Plot context menu (see Figure 4.54).
It is also possible to add the Frequency vs E plot to the CV staircase using the
quick access toolbar (see Figure 4.55).
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Figure 4.55 Adding the Frequency vs E plot using the quick access toolbar
You should have two completely different plots at your disposal, shown in Figure
4.56.
Figure 4.56 The two plots for the data set from example #2: the measured current relative
to the applied potential (top) and the EQCM frequency change relative to the applied
potential (bottom)
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Note
In the data explorer frame, both the Frequency vs E and the i vs E plot lines
are displayed in bold lettering, indicating that both plots are shown in the data
view frame. However, only the latter is highlighted, indicating that the i vs E
plot is currently active. Clicking the Frequency vs E line will highlight it, thus
setting it to active.
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Figure 4.59 Creating an overlay on the Measurement view using data plotted in the
Analysis view
The data shown in the analysis view will be copied as it is displayed to the location
specified in the measurement view. If more than one plot is shown in analysis
view, all the visible plots will be sent to the measurement view.
Note
The overlay is only shown if the plot is visible in the measurement view. Click
the ,
or
button in the toolbar to display more than one plot in the
measurement view.
Warning
Overlays created this way must have the same signal on the X axis.
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This data set was obtained using the Repeat for each value command, with four
values used in procedure for the scan rate of the LSV staircase. The first LSV was
obtained with a scan rate of 0.01 V/s, the next LSV was recorded with a scan rate
of 0.020 V/s, and so on.
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Figure 4.61 The overlay plot of the four linear sweep voltammetry curves
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Figure 4.62 Opening the plot options window for the whole data set
Set the plot style to a size 2, red Line plot. Click the OK button to confirm the
change. The four LSV curves will now be displayed using the new plot options (see
Figure 4.63).
Figure 4.63 The four LSV plots displayed using the new plot options
Changing the plot settings of an individual plot is still possible. Right-click the last
LSV staircase of the data set (0.1 V/s) in the data explorer frame to access the plot
options of that particular plot. Change the settings to a size 2, blue Combi plot,
using a size 10 star marker symbol and plotting 1 point out of 40. The overlaid
plot should now look like the one displayed in Figure 4.64.
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Figure 4.64 Changing the plot options for the linear sweep voltammetry
recorded at 0.1 V/s
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Changing the plot options for the whole data set only modifies the options for the
plots which do not have user-defined local options (in this case, the plot
corresponding to a scan rate of 0.1 V/s is not affected).
To remove the user-defined local options, open the Plot options window for the
0.1 V/s plot (use the right-click procedure), and press the
button (see
Figure 4.66).
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Figure 4.66 Resetting the plot options for the 0.1 V/s plot (1/2)
Pressing the
button will remove the local options of the plot and the
global options will be used instead (see Figure 4.67).
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Figure 4.67 Resetting the plot options for the 0.1 V/s plot (2/2)
If the global options are changed again, all the plots in the overlay will be
displayed using these new options, including the 0.1 V/s plot.
4.6.3 Changing the plot settings in an overlay plot
The curves shown in Figure 4.67 are all displayed as the WE(1).Current vs the
Potential applied. This means that all the curves in the overlay are plotted using
the same electrochemical signals. If it is required to change the electrochemical
signals used to display the curves in the overlay, two options are available.
The first option is to change the electrochemical signals used to display each
curve, one after the other. This is quite time consuming, especially for overlays
with a large number of plots.
The second option is to change the electrochemical signals of all of the plots of
the overlay, by using the Apply to selected option (see Figure 4.68). This option
can be accessed by right-clicking the signal to change and click the small arrow
next of the new electrochemical signal to use.
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Figure 4.68 Using the Apply to selected option to change the plot setting of all the plots in
the overlay
If this option is used to change the electrochemical signal used on the X-axis for
the overlay to the time signal, the resulting plot will look like the one displayed in
Figure 4.69.
Figure 4.69 Changing the plot settings for all the plots in the overlay using the apply to
selected option
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Figure 4.70 The grid settings can be adjusted using the right-click menu
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Figure 4.71 The background style of NOVA can be changed using the dedicated right-click
menu item
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From the Show sub-menu, you can select some additions for the plot:
Show Origin (2D)
Show Legend (2D, 3D)
Show Title (2D, 3D)
Show Global minimum and maximum (2D)
Show Local minimum and maximum (2D)
Show Coordinates (2D)
Show Positioning Lines (2D)
All these additions can be toggled on and off at any time and the changes can be
saved in the database using the save button, .
Show Origin (2D plots only): this option will display the origin of the plot (0, 0)
on the 2D graph (two orange lines are shown). The scaling of the plot is adapted if
required. Figure 4.73 below shows the same cyclic voltammogram plot with its
origin.
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Show Legend (2D & 3D plots): this option will display a legend for the data set(s)
plotted in the 2D graph, using the color and markers, as well as the name of the
plot(s). Figure 4.74 shows a typical example.
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Figure 4.75 The serial number of the instrument is provided in between brackets when no
instrument description is provided
The position, the font and the style of the legend can be edited using a specific
right-click menu. A total of eight positions are available for a 2D plot and four
positions for a 3D plot as well as three different border styles. The legend can also
be hidden from view using this menu (see Figure 4.76). The legend settings are set
independently for each type of plot.
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Figure 4.76 The legend sub-menu for position, border style and font edition
Show Title (2D & 3D plots): this option will display a title for the data set(s)
plotted in the 2D graph. As with the legend, the format of the title and of the
subtitle can be edited using the right-click menu. Their position can be chosen
from three predefined settings, both for the 2D and for the 3D plots, although the
settings are independent for each type of plot. Figure 4.77 shows the default title
for the 2D plot, and the right-click menu used for editing text, font and position of
the title and the subtitle.
Figure 4.77 Displaying the title and the subtitle and using the right-click menu
for editing
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Figure 4.78 Showing the position of the Global minimum and maximum
Note
In the case of an overlay plot using two different Y-axes, the maximum and
minimum for both axes are displayed.
Show Local minimum and maximum (2D plots only): this option displays the
points of the plot corresponding to the relative lowest and the highest value of
the signal shown on the Y-axis. When the automatic scaling option is used for the
Y-axis, the Local minimum and maximum correspond to the Global minimum and
maximum. Figure 4.79 shows the location of the Local minimum and maximum
for a specific portion of the cyclic voltammogram of example #1. The labels can be
removed by selecting this option once again.
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Figure 4.79 Showing the position of the Local minimum and maximum
Note
It is not possible to show the Global and the Local minima and maxima.
Selecting one of the two options automatically deselects the other one.
Show coordinates (2D plots only): this option displays the coordinates of the
mouse cursor in the 2D, as a tooltip. The coordinates shown depend on the
scaling and the types of axes chosen for the plot. The coordinates are refreshed
when the mouse pointer is moved. Figure 4.80 shows the results of this option on
the 2D plot.
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Figure 4.80 Showing the coordinates of the mouse pointer on the plot
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Figure 4.81 Showing the pointer coordinates for a dual Y-axis overlay plot
Show Positioning lines (2D plots only): this option will display the two lines,
following the position of the mouse pointer and helping in locating the position of
the pointer on the screen (Figure 4.82).
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This will change the mouse pointer to a hand. Click anywhere on the displayed
plot. A tooltip label will appear, together with an arrow, locating the point you
just clicked and displaying some information about the point: index of the point in
the data set, X, Y and Z coordinates of the plot (see Figure 4.84).
Note
The information shown in the tooltip depends on the signals used for plotting
the experimental data. In the example shown in Figure 4.84, the X, Y and Z
signals are Potential applied, WE(1).Current and Time, respectively.
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Figure 4.84 Displaying data information using the step through data option
Clicking anywhere else on the plot will display the same information for the new
point. Holding the left and right arrow keys on the keyboard will walk through
the whole data set, in reverse and forward direction, respectively. It is also possible
to scroll the mouse wheel up or down, if available, to walk through the data. At
any time, you can press the insert key on the keyboard to add the label and the
locating arrow to the plot (see Figure 4.85).
Figure 4.85 Walking through the data using the keyboard arrows or the mouse wheel
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Figure 4.87 Accessing the axes options in a 2D plot (top) and a 3D plot (bottom)
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Note
The Tick Angle setting is not available in 3D plots. For 2D plots, the tick angle
can be set to any value between 0 to 90 degrees.
4.7.7 2D Specific options
Axes Coupling: choose from independent, iso-metric, or iso-tropic.
4.7.8 3D Specific options
Origin Axes: overrides any axis position setting by moving the intersection
of the axis at the origin of the plot (point 0, 0, 0).
Location: set the position of the axis relative to the scale of the other axes.
The default setting uses the minimum of each axis to locate the origin of
the 3D plot. Choose maximum to locate the axis at the highest value of the
first available axis. Choose maximum alternate to locate the axis at the
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Figure 4.90 Enabling zooming and zooming back using the right-click menu
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Figure 4.92 Scroll zoom. Scrolling in (left) and scrolling out (right)
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Figure 4.93 Slide zoom: expanding the Y-axis (left) and contracting it (right) using the
sliding zoom function
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If the mouse scroll function is used while the mouse pointer is located on top of
one of the 3 axes of the plot, the axis will expand or contract depending on the
scrolling direction (see Figure 4.96).
Figure 4.96 Expanding the X-axis using the mouse scroll function
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Figure 4.97 X/Y analysis tools can be added directly to a plot in the analysis view
It is also possible to add this type of analysis by clicking the plot directly and
selecting the required analysis tool using the quick access toolbar (see Figure
4.98).
Figure 4.98 X/Y analysis tools can be added directly to a plot using the quick access toolbar
The analysis tools in this group use the X and Y values of the plot they are added
to.
4.8.1.1 SG Smooth
The Savitzky-Golay (SG) smoothing tool can be used to remove noise from
measurements in order to enhance the signal to noise ratio of experimental data.
The SG Smooth method is described in Anal. Chem.,36,1627 (1964). It involves a
polynomial fit through the experimental data. This method is also called weighted
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A new item, called SG Smooth, will be added to the data set in the data explorer
frame, below the i vs E plot (see Figure 4.101).
Click the SG Smooth item. A new area will be displayed on the right-hand side of
the plot. This part of the view allows the definition of settings used in the SG
Smooth tool (see Figure 4.102).
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Note
Changing the settings of the SG Smooth tool automatically updates the
Smoothed plot.
4.8.1.2 FFT Smoothing
The FFT smoothing technique can be used to remove a specific frequency or
frequency range from a data set, in order to attenuate the influence of the
selected frequency or frequency range and improve the signal-to-noise ratio.
In order to identify the different frequency components present in a given data
set, the FFT smooth function first transposes the source data from the time
domain into the frequency domain by Fourier transformation.
The FFT smooth method can be used with four different filtering strategies:
Low pass: all the contributions from frequencies higher than the userselected cutoff frequency are rejected. This method can be used to remove
high frequency noise from a measurement.
High pass: all the contributions from frequencies lower than the userselected cutoff frequency are rejected. This method can be used to remove
low frequency noise from a measurement.
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To use the FFT Smooth tool, right-click the i vs E plot in the data explorer frame
and, from the context menu, select the FFT Smooth tool (see Figure 4.107).
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A new item, called FFT Smooth, will be added to the data set in the data explorer
frame, below the i vs E plot (see Figure 4.108).
Click the FFT Smooth item. A frequency domain plot will be shown. On the X axis,
the frequency contributions are shown, in Hz. On the Y axis, the intensity is
shown, in arbitrary units (see Figure 4.109).
Figure 4.109 The frequency domain plot showing the amplitude vs frequency
A new area will be displayed on the right-hand side of the plot. This part of the
view allows the definition of settings used in the FFT Smooth tool (see Figure
4.110).
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Figure 4.111 Specifying the cutoff frequency for a low-pass or high-pass FFT filter
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Figure 4.112 Two frequencies need to be specified in the FFT Smooth options panel for
band pass or band stop filtering
Note
Frequency 1 must be smaller than Frequency 2.
Alternatively, the mouse pointer can be used to select an area of the plot defining
the frequency band for the band pass or band stop filter. Click the frequency
domain plot at one of the required frequency limits and, while holding the mouse
button, drag an area across the plot. Release the mouse button at the other
frequency limit to define the frequency band to be used in the FFT Smooth filter
(see Figure 4.113).
Figure 4.113 The frequency band can be defined graphically by dragging an area across the
plot
Two lines will be drawn on the plot to indicate the positions of the frequencies in
the plot (see Figure 4.113). These values will also be shown in the FFT Smooth
options.
Tip: use the Show coordinates option to help define the frequency or frequency
range in the FFT Smooth analysis tool (see Figure 4.114).
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Figure 4.114 Use the Show coordinates options to easily define the frequency or frequency
range in the FFT Smooth analysis tool
The smoothed data will be automatically generated using the filtering conditions
specified through the FFT Smooth options panel or graphically (see Figure 4.115).
Figure 4.115 The Smoothed data plot generated by the FFT Smooth tool
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Starting at a potential of -1.2 V, four peaks are visible in the data set. The last
peak, located around 0 V does not have a linear baseline. The baseline fit tool can
therefore be used to correct the data for this non-linearity.
To correct the data using a polynomial baseline fit, right-click the i vs E plot in the
data explorer frame and, from the context menu, select the Add analysis
Baseline correction Polynomial fixed order (see Figure 4.117).
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Figure 4.118 The newly added Polynomial fit fixed order analysis item
Click the Polynomial fixed order analysis item. The mouse pointer will change to a
cross and a new area will be displayed on the right-hand side of the plot (see
Figure 4.119).
The area located on the right of the 2D plot is used to set the parameters of the
baseline fit. Set the Polynomial order to 4 for this example. The point selection
style field should be set to Snap to data.
Note
When the Snap to data option is used, the software automatically positions the
marker on the closets data point on the plot. Use the Free selection option to
define points not on the curve.
Using the left mouse button, click a total of 5 measured data points in the 2D plot
area. These points are used to define the points through which the baseline should
pass. Since a baseline of 4th polynomial order is used, a minimum of 5 points are
required, although more than 5 can be defined.
Figure 4.120 shows an example of marker location used to calculate the
polynomial baseline. When the fifth marker is placed, the baseline will be
calculated and plotted in the 2D plot area (see Figure 4.120).
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Note
The number of markers required to drawn a polynomial baseline is equal to the
polynomial order +1.
The calculated baseline is not yet suitable for this experimental data and it requires
additional fine tuning. This is possible in two different ways:
By adding extra marker points
By moving existing marker points
4.8.1.3.1 Adding extra marker points
The first way to fine tune the baseline calculation is to add new markers to the
plotted data. Figure 4.121 shows the same plot as in Figure 4.120, but with an
extra marker located close to the positive end of the potential scan. When the
new marker is placed, the baseline is recalculated and replotted in the 2D plot
area.
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Figure 4.121 Adding extra markers to the baseline allows to fine tune the calculation
The new marker allows for a better definition of the baseline at the positive end of
the potential scan, compared to Figure 4.120. It is possible to keep adding
markers to the baseline in order to improve the fit, if required.
Adding extra markers to a specific area of the curve increases the relative
importance of that specific area of the plot in the baseline fit.
4.8.1.3.2 Moving marker points
A second option that can be used to fine tune the calculated baseline is to move
markers that are already placed on the plot. In order to do this, right-click on an
existing marker point and select the Move option from the menu (see Figure
4.122).
Note
The same menu can be used to remove an existing marker point from the plot.
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Figure 4.122 Right-clicking an existing marker point allows you to move or remove the
marker
After choosing the move option, a label showing the X and Y coordinates of the
point will be displayed below the selected marker. Using the right and left key on
the keyboard, it is possible to move the selected marker along the plot (see Figure
4.123).
Figure 4.123 Choosing the move option allows you to relocate the marker
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Figure 4.125 Selecting the Residual plot generated by the baseline correction tool
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Figure 4.126 The data point from Demo 10 after baseline correction
Note
The fitted Y values (corresponding to the baseline) and the corrected Y values
(corresponding to the corrected data) are available in the data grid.
4.8.1.4 Peak search
The peak search analysis tool can be used to locate and characterize peaks in an
experimental curve. The peak search tool searches for peaks that fit the userdefined search criteria and displays information about the peaks in the Analysis
view. NOVA offers two types of peak search modes: Automatic or Manual.
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To use the peak search analysis tool, right-click the i vs E plot in the data explorer
frame and, from the context menu, select the Peak search tool (see Figure 4.128).
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Figure 4.128 Adding the peak search analysis tool to the data
A new item, called Peak search, will be added to the data set in the data explorer
frame, below the i vs E plot (see Figure 4.129).
Click the Peak search analysis item. A new area will be displayed on the right-hand
side of the plot. This part of the view allows the definition of the selection criteria
for the peak search tool (see Figure 4.130).
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Figure 4.132 The results of the peak search analysis are displayed in the data grid
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Figure 4.133 Changing the peak search conditions automatically updates the results
Figure 4.134 In Manual search mode, the base line can be defined
In this case, the base line mode selection will become available (see Figure 4.134).
Note
The peak area is calculated only when the Linear Curve Cursor or the
Polynomial methods are used.
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Figure 4.135 Defining an exponential baseline for the peak (left location of the first point,
right location of the second point and drawing of the baseline)
Figure 4.136 Using the zero base method to specify the base line
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Figure 4.137 Using the polynomial baseline mode (left specification of the waypoints for
the polynomial baseline, right pressing Enter validates the polynomial baseline)
Note
The polynomial search method locates the peaks in the curve segment closest
to the first point defining the polynomial baseline.
Linear Curve Cursor: this option uses a linear baseline in the determination
of the peaks. To define the baseline, click on the plot area. The software
automatically connects the initial point to the nearest data point. While
holding the mouse button pressed, drag the mouse across the plot area to
define the baseline. When the mouse button is released, the final X
position of the mouse pointer is used to define the X position of the final
point of the baseline, on the curve (see Figure 4.138).
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Figure 4.138 Using the Linear curve cursor method to specify the baseline (left location of
the first point, right location of the second point and drawing of the baseline)
Linear Free Cursor: this option uses a linear baseline in the determination
of the peaks. To define the baseline, click on the plot area and while
holding the mouse button pressed, drag the mouse across the plot area.
When the mouse button is released, the final X,Y position of the mouse
pointer is used to define the final point of the baseline (see Figure 4.139).
Figure 4.139 - Using the Linear free cursor method to specify the baseline (left location of
the first point, right location of the second point and drawing of the baseline)
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Note
The base points used to specify the tangent baseline are indicated by the small
vertical lines on the plot (see Figure 4.140).
Linear Rear: this option finds peaks by extending the baseline located after
the peak. To define the baseline, click on the plot area. The software
automatically connects the initial point to the nearest data point. While
holding the mouse button pressed, drag the mouse across the plot area to
define the baseline. When the mouse button is released, the final X
position of the mouse pointer is used to define the X position of the final
point of the baseline, on the curve. The tangent is then extended
backwards and the peak is located (see Figure 4.141).
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Note
The base points used to specify the tangent baseline are indicated by the small
vertical lines on the plot (see Figure 4.141).
Linear Front Tangent: this option finds peaks by extending the baseline
located in front of the peak. The baseline is defined by clicking on the plot
area and, while holding the mouse button pressed, dragging the mouse
across the plot area, drawing a straight line. The software automatically
connects the baseline to the curve at the data point for which the first
derivative is the closest to the slope of drawn baseline (see Figure 4.142).
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Figure 4.142 Using the Linear front tangent baseline search method
Note
The base points used to specify the tangent baseline are indicated by the small
vertical lines on the plot (see Figure 4.142).
Linear Rear Tangent: this option finds peaks by extending the baseline
located after the peak. The baseline is defined by clicking on the plot area
and, while holding the mouse button pressed, dragging the mouse across
the plot area, drawing a straight line. The software automatically connects
the baseline to the curve at the data point for which the first derivative is
the closest to the slope of drawn baseline (see Figure 4.143).
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Figure 4.143 - Using the Linear rear tangent baseline search method
Note
The base points used to specify the tangent baseline are indicated by the small
vertical lines on the plot (see Figure 4.143).
Use the manual peak search function in combination with the Show coordinated
option (available from the right-click menu see section 4.7.3). This will display
the X and Y coordinates of the mouse pointer, while the baseline is defined,
making it easier to fine tune the position of the peak (see Figure 4.144).
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Figure 4.144 Fine tuning the markers of the base line using the Show coordinates option in
combination with the manual peak search tool
It is important to be able to fine tune the base line used in the manual peak
search, after the search has been performed. It is possible to redefine the position
of the left and right markers defining the base line. To do this, right-click the peak
label and select either the Move left base point or the Move right base point, to
redefine the left and right markers, respectively (see Figure 4.145).
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Figure 4.145 Choosing the Move left base point option allows you to move the base line
marker
A label will display the coordinates of the base point on the plot (Figure 4.146).
Figure 4.146 The selected base point can be moved using the left and right key
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button
Figure 4.147 Pressing the Reset button removes previous results from the analysis results
frame
Note
The results of the Peak search are stored in the data grid.
4.8.1.5 Regression
The regression analysis tool can be used to perform different regression
calculations on measured data points. A wide range of functions can be used in
this type of calculation:
Linear no offset: performs a linear regression using the =
equation.
Linear: performs a linear regression using the =
+ equation.
Polynomial fixed order: this calculation uses a
order polynomial
function in the regression calculation. The value of is defined by the user.
Polynomial maximum order: this calculation uses all the polynomial
functions up to a maximum of , defined by the user. The regression
providing the smallest 2 (Chi-squared) is automatically selected by the
software.
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Figure 4.148 The regression tool can be added to a plot using the right-click menu
Double click on the demo file Demo 04 - Hydrodynamic LSV with increasing
rotation rate entry of the demo database to load it into the data explorer frame.
This file contains data points recorded at different rotation rates with the Autolab
RDE in a 0.05 M [Fe(CN)6] 4-/3- in 0.2 M NaOH solution.
The data file contains a total of six linear sweep voltammograms (see Figure
4.149).
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This demo file also includes an additional item, located at the end of the file in the
. This analysis item is designed to
data explorer frame, called Hydrodynamic i vs
perform a simple Levich analysis on data recorded using forced-convection. This
item automatically generates a Levich plot and performs two linear regressions on
the plotted data, using the linear and the linear no offset regression methods (see
Figure 4.150).
Figure 4.150 The Hydrodynamic i vs analysis tool automatically adds two regression
lines to the Levich plot
Click the Regression item in the data explorer. The Levich plot will be displayed in
the plot area, along with the linear regression line (see Figure 4.151).
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Figure 4.151 Clicking the Regression item in the explorer view displays the Levich plot and
the regression line
Clicking this regression item also displays the parameters of the regression analysis
tool on the right-hand side of the plot (see Figure 4.152).
Figure 4.152 The parameters of the Regression analysis tool are located on the right-hand
side of the plot
The regression tool has a number of parameters that can be defined in the control
interface:
Search mode: Automatic or Manual. When the Automatic mode is used,
the whole data set is used in the regression. Using the manual search mode
lets the user define a window in which to use the regression calculation.
The window is determined by clicking and holding the left mouse button
while moving the mouse left or right.
Regression type: Defines the type of regression.
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Figure 4.153 The results of the linear regression are displayed in the data explorer
The automatic regression tool does not extend the calculated curve beyond the
experimental data points. For plotting purposes, it might however be useful to
extend the regression line through the origin of the plot. To do this, switch to
Manual search mode (see Figure 4.154).
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Once the search region has been defined, the calculation is performed
automatically using the settings defined in the control interface. Using this
approach, the regression line can be extended through the origin of the plot as
shown in Figure 4.155.
If the shift key is pressed while the search window is defined, it is possible to fine
tune the search window (see Figure 4.156).
Figure 4.156 The shift key allows to fine tune the search window
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Right click the CV staircase item in the data explorer frame, and select the i vs t
plot from the plot context menu (see Figure 4.158).
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A new plot, showing the current vs time recorded during this experiment will be
added to the data set. Click this new plot to display the plot in the analysis view
(see Figure 4.159).
To calculate the derivative of current vs time, right-click the i vs t item in the data
explorer and select the Derivative tool from the Add Analysis menu (see Figure
4.160).
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A new item, called Derivative, will be added to the data set in the data explorer
frame, below the i vs t plot (see Figure 4.161). An additional plot, called Derivative
plot is automatically added to the Derivative analysis item.
Click the Derivative plot to display the first derivative of the current (see Figure
4.162).
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Right click the CV staircase item in the data explorer frame, and select the i vs t
plot from the plot context menu (see Figure 4.164).
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A new plot, showing the current vs time recorded during this experiment will be
added to the data set. Click this new plot to display the plot in the analysis view
(see Figure 4.165).
To calculated the integral of current vs time, right-click the i vs t item in the data
explorer and select the Integrate tool from the Add Analysis menu (see Figure
4.166).
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A new item, called Integrate, will be added to the data set in the data explorer
frame, below the i vs t plot (see Figure 4.161).
An additional plot, called Integrate plot is automatically added to the Integrate
analysis item.
Click the Integrate plot to display the integral of the current vs time (see Figure
4.168).
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Note
The results of the Integral are stored in the data grid.
4.8.1.8 FFT Analysis
The FFT Analysis tool can be used to transform experimental data from the time
domain into the frequency domain, in order to identify the different frequency
components present in a given data set.
The transformation from time domain to frequency domain through the Fast
Fourier Transform algorithm assumes that the data outside of the measured time
segment is either zero or that the data in this segment repeats periodically.
Double click on the demo file Demo 16 FRA impedance entry of the demo
database to load it into the data explorer frame. This file contains impedance
spectroscopy data points recorded on the Autolab dummy cell (c).
Click the Nyquist Z vs Z plot in the data explorer frame to display the data points
from this demo file (see Figure 4.169). The data is presented as a Nyquist plot but
it can also be plotted as a Bode plot (Bode modulus and Bode phase plots are
available).
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Note
Detailed information on impedance spectroscopy measurement can be found in
the Impedance spectroscopy tutorial, available from the Help Tutorials
menu.
Click the
button next to the FRA frequency scan item in the data explorer. This
item will be expanded and the list of the individual frequencies used during the
measurement will be displayed. Expand the #1 FRA frequency scan 10 kHz group
and the FRA single frequency group to reveal three plots: E% (AC) vs t, i% (AC) vs
t and Lissajous (see Figure 4.170).
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Figure 4.170 The raw recorded values are available for each individual frequency
To use the FFT Analysis tool, right-click the E% (AC) vs t plot in the data explorer
frame and, from the context menu, select the FFT Analysis tool (see Figure 4.171).
A new item, called FFT Analysis, will be added to the data set in the data explorer
frame for the 10 kHz frequency (see Figure 4.172).
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Click the FFT plot generated by the FFT Analysis tool to display the transformed
data (see Figure 4.173).
Figure 4.173 The raw impedance data after transformation from the time domain into the
frequency domain
The transformed data shows a single peak at 10 kHz consistent with the applied
frequency. The rest of transformed data shows the contributions from
environmental or instrumental noise.
Note
The transformed data is displayed in logarithmic scale on the Y axis. The data is
shown in arbitrary units.
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To use the corrosion rate analysis tool on this data set, right-click the i vs E item in
the data explorer frame and select the Corrosion Rate from the Add analysis
context menu (see Figure 4.175).
34
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Figure 4.175 The Corrosion Rate analysis tool can be added to the data through the rightclick menu
Two different corrosion rate tools are available from the context menu:
Corrosion rate, Tafel slope: this tool is used to calculate the Tafel slope
and the determination of the exchange current density.
Corrosion rate, fit: this tool can be used to perform a calculation similar to
that of the Tafel slope tool. Additionally, the data is fitted using the ButlerVolmer equation:
=
Where
is the corrosion current,
is the corrosion potential,
the anodic and cathodic Tafel constants, respectively.
and
are
Figure 4.176 The corrosion rate, Tafel slope is added to the data set
Click the corrosion rate data analysis item to display the data from the data set, in
logarithmic scaling (see Figure 4.177).
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Figure 4.177 The Tafel slope analysis tool automatically displays the experimental data in
logarithmic scaling
Additionally, the control parameters of the Tafel slope analysis tool will be
displayed on the right-hand side of the plot. This part of the view allows the
definition of parameter for the Tafel slope analysis (see Figure 4.178).
log| |
log| |
When the Tafel slope analysis tool is selected, the mouse pointer changes to a
cross. Using the mouse pointer, click two points in the plot to specify the linear
part of the anodic branch (see Figure 4.179). Once the second point is clicked, a
line will be drawn on the plot.
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Figure 4.179 The Tafel slope analysis tools requires the specification of the linear segments
of the Tafel plot (1/2)
The same must be repeated for the cathodic branch of the plot. Once both linear
segments have been defined, the intercept is determined and indicated in the plot
(see Figure 4.180).
Figure 4.180 - The Tafel slope analysis tools requires the specification of the linear segments
of the Tafel plot (2/2)
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Figure 4.181 The results of the Tafel slope analysis are shown in the data explorer frame
=
2.303
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2.303
Figure 4.182 Adding the corrosion rate, fit analysis tool to the data set
A new item, called Corrosion rate, fit will be added to the data set in the data
explorer frame (see Figure 4.183).
Figure 4.183 The corrosion rate, fit is added to the data set
Click the corrosion rate data analysis item to display the data from the data set, in
logarithmic scaling (see Figure 4.184).
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Figure 4.184 The corrosion rate, fit analysis tool automatically displays the experimental
data in logarithmic scaling
Additionally, the control parameters of the corrosion rate, fit analysis tool will be
displayed on the right-hand side of the plot. This part of the view allows the
definition of parameter for the corrosion rate analysis, similarly to the Tafel slope
analysis item (see Figure 4.185).
Figure 4.185 The parameters for the corrosion rate, fit analysis tool
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Figure 4.186 The corrosion rate, fit analysis tools requires the specification of the linear
segments of the Tafel plot (1/2)
The same must be repeated for the cathodic branch of the plot. Once both linear
segments have been defined, the intercept is determined and indicated in the plot
(see Figure 4.187).
Figure 4.187 - The corrosion rate, fit analysis tools requires the specification of the linear
segments of the Tafel plot (2/2)
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Figure 4.188 The results of the Tafel slope analysis are shown in the data explorer frame
The reliability of the fitting results greatly depends on the data provided as input
for the fitting algorithm. A number of conditions must be verified for the data
points to be valid 35. Particular care must be taken when defining the linear section
of the Tafel plot at large overpotentials. As a rule of thumb, the linearity of the
Tafel plot should extend over at least one decade of current.
The following information is provided in the data explorer frame:
b a & b c: the anodic and cathodic Tafel coefficient, in V/decade.
Ecorr, Calc: the corrosion potential calculated from the intercept on the
Tafel plot, in Volts.
Ecorr, Obs: the observed experimental corrosion potential, in Volts.
35
See A. J. Bard and L. R. Faulkner, Electrochemical Methods, Fundamentals and Application, 2nd
Edition, Wiley (NY), Chapter 3; R. Baboian, Electrochemical Techniques for Corrosion Engineering,
NACE; C. H. A. Brett and A. M. O. Brett, Electrochemistry, Principles, Methods and Applications,
Oxford Science Publications; D. C. Silverman, Practical Corrosion Prediction Using Electrochemical
Techniques, Uhlig's Corrosion Handbook, 2nd Edition.
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Figure 4.189 Data set analysis tools can be added directly to a plot in the analysis view
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is the specified
Double click on the demo file Demo 19 Cyclic voltammetry Fe2+/Fe3+ entry of the
demo database to load it into the data explorer frame. This file contains data
points of a cyclic voltammetry staircase experiment recorded in a 0.05 M
[Fe(CN)6] 4-/3- in 0.2 M NaOH solution. The number of scans is three.
To add the iR drop correction analysis tool to this data set, right-click the CV
staircase item in the data explorer frame and select the iR drop correction analysis
item from the context menu (see Figure 4.190).
Figure 4.190 Select the iR drop correction analysis tool to add it to the data set
Figure 4.191 The uncompensated resistance value can be specified in a popup window
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Figure 4.193 The uncompensated resistance can be adjusted at any time by clicking the iR
drop correction item in the data explorer
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Figure 4.194 The linear sweep voltammograms recorded at different rotation rates
This data set was recorded using the default Autolab Hydrodynamic linear sweep
procedure. This procedure automatically adds the Hydrodynamic i vs
analysis
tool to the data at the end of the experiment. This tool is therefore already added
to the data (see Figure 4.195).
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Figure 4.196 Right-click the analysis item and select the Delete option from the context
menu to remove the data analysis tool from the data set
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The Hydrodynamic i vs
analysis tool will be added again to the data set,
providing a Levich plot as well as two different linear regression lines (see Figure
4.198).
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Figure 4.199 Select the Calculate charge analysis tool to add it to the data set
A new item, called Calculate charge, will be added to the data set, below the CV
staircase item. Two plots, Q vs E and Q vs t are automatically generated by this
analysis tool (see Figure 4.200).
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Figure 4.200 The Calculate charge analysis item automatically generates the Q vs E and the
Q vs t plots
Click the Q vs t plot to display the plot. The plot should be similar to the plot
obtained with the same data set in combination with the integrate analysis tool
(see Figure 4.201 and Figure 4.168).
Figure 4.201 The Q vs t plot generated by the calculate charge analysis tool
Click the Q vs E plot to display the same information plotted versus the applied
potential. The plot should look like the one shown in Figure 4.202.
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Figure 4.202 The Q vs E plot generated by the calculate charge analysis tool
Note
The data provided by the Calculate charge command is stored in the data grid.
4.9 The data grid
The data grid works as a spreadsheet that can be used to perform calculations on
measured signals, to create new signals, to filter experimental data points or
procedure parameters, and to export the data to Excel or ASCII. New signals
created in the grid can then be used to plot the measured data in a different way.
To access the data grid, click the corresponding button
toolbar (see Figure 4.203).
Figure 4.203 Clicking the Show data grid button in the toolbar will display the data grid
instead of a 2D or 3D plot
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Figure 4.204 Displaying the data grid of the data set from example #1
You can scroll down to inspect every value of these signals. For each value of
WE(1).Potential applied, a corresponding value of WE(1).Current, Time,
WE(1).Potential, index and scan is displayed.
Note
The data grid shows the values for the whole data set which means that the
highlighted plot has no influence on the displayed. Each plot uses the same set
of data points.
Note
The data grid shown in Figure 4.204 displays two columns containing values of
the potential. The first one is labeled Potential applied while the other is
labeled WE(1).Potential. The Potential applied signal contains the values of the
potential set by the software during the measurement, while the
WE(1).Potential signal shows the values of the potential recorded during the
experiment.
Using the data grid, it is possible to export the measured data points to other
software packages for data analysis (Excel, Origin, SigmaPlot, ). This can be
done by right-clicking the data grid and by choosing the Export to ASCII file (see
Figure 4.205).
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Note
It is also possible to open the Calculate signal tool by clicking the CV staircase
item in the data explorer frame and clicking the
button in the quick access
toolbar (see Figure 4.207).
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Figure 4.207 The calculate signal tool is also available from the quick access toolbar
Clicking the
button will display the calculate signal window, which can be used
to define a new signal and the required expression to calculate it (see Figure
4.208).
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293 | P a g e
Figure 4.209 Creating a new signal by adding 197 mV to the applied potential signal
The final step required to calculate a new signal is to select which signals should
be used for each parameter. Click the E parameter from the list and click the
button next to CV staircase group in the Signals list. This will display all the
available electrochemical signals provided by the CV staircase measurement
command. Double click the Potential applied signal to assign the values of this
signal to the parameters E (see Figure 4.210).
Note
Once the values of a signal have been assigned to a parameter of the
expression builder, the name of the parameter will be displayed next to the
signal, in between brackets (see Figure 4.210).
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Figure 4.210 Selecting the values of the Potential applied signal for the parameter E
Figure 4.211 The newly created signal values shown in the data grid. The matching
expression is shown on the right-hand side
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Figure 4.212 Creating a new plot using the modified potential scale
The new 2D plot should now look like the one displayed in Figure 4.213.
Figure 4.213 Plotting the data from example #1 using the corrected potential scale
296 | P a g e
Figure 4.214 Using the Single value check box reduces the result of the calculate signal to a
single value
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Figure 4.215 The four LSV curves of the Demo 05 data set
The Demo 05 data set was obtained using the Repeat for each value command,
with four values used in procedure for the scan rate using in the LSV staircase
measurement. The first LSV was obtained with a scan rate of 0.01 V/s, the next
LSV was recorded with a scan rate of 0.02 V/s, and so on.
The overlay plot of all four LSV curves is provided below (see Figure 4.216).
298 | P a g e
Figure 4.216 The four LSV curves obtained using four different scan rates
As the scan rate increases, the anodic current increases. For a reversible system,
like the [Fe(CN) 6]4- / [Fe(CN) 6]3- system, the peak current,
is proportional to the
square root of the scan rate:
= 2.69 10
where is the area of the electrode, is the number of electrons, is Faradays
constant,
is the bulk concentration of the electroactive species,
is the
diffusion coefficient and is the scan rate.
A plot of the peak current vs the square root of the scan rate should yield a
straight line. The procedure used to measure the data points of the Demo 05
example included an automatic peak search command. Therefore, the peak height
and peak position is available for each individual curve in the data set.
The data grid provides a tool, called the Build signal, which is designed to create
such a plot, by filtering and selecting information coming from the available
signals and the procedure parameters.
299 | P a g e
Figure 4.217 Select the whole data set and click the
the signal builder
This will open the Filter and Select Signals window (see Figure 4.219).
Note
It is also possible to open the Calculate signal tool by clicking the CV staircase
item in the data explorer frame and clicking the
button in the quick access
toolbar (see Figure 4.218).
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Figure 4.218 The build signal tool is also available from the quick access toolbar
Note
Since the new signals use values of all the measurements in the data set,
clicking the header is required.
The Filter and select signals window has two frames. The frame on the left
contains five groups. Each group contains the individual commands used in the
procedure, along with the electrochemical signals and the parameters. The frame
301 | P a g e
Figure 4.220 Detailed view of the Repeat for each value linked to the Control external
device command
Expand the Measurement cyclic and linear sweep voltammetry group in the left
frame, and then expand the LSV staircase item. Eight items will be displayed (see
Figure 4.221):
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Figure 4.221 Adding the value of the scan rate to the filter
Double click the Scan rate (V/s) located under the LSV staircase group to add it to
the list in the frame on the right-hand side (Figure 4.222).
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Figure 4.222 Double click the scan rate item to add it to the filter and select list
Clicking the OK button generates a new signal, called Scan rate (V/s) in the data
grid. This signal contains four values (see Figure 4.223).
The signal obtained using the signal builder contains all the scan rate values used
in the LSV staircase command.
4.11.3 Selecting the values of the peak height
The second signal which is required for the plot is a signal containing the values of
the peak height. For this example, a filter designed to extract the values of the
peak height for curve will be constructed.
Click the Build signal button
to open the Filter and select signals window. In the
Analysis general, locate the Peak height in the Peak search list. Double click the
Peak height item to add it to the filter (see Figure 4.224).
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Figure 4.224 Adding the Peak height from the Peak search group to the filter
Click the OK button to validate the filter. A new signal will be created in the data
grid, containing the values of the peak height for each LSV Staircase curve of the
data set (see Figure 4.225).
Figure 4.225 The data grid and the two filtered signals
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Figure 4.226 Creating the square root of the angular frequency signal
Three signals should now be available in the data grid (see Figure 4.227).
306 | P a g e
A new custom plot will be added to the data explorer frame. Set the X-axis signal
to Square root scan rate and the Y-axis signal to Peak height. Rename the plot to
Reversibility plot.
Note
Only three signals are defined for the whole data set (Scan rate, Square root
scan rate and peak height). Therefore, only these three signals can be used for
the plot (see Figure 4.229).
307 | P a g e
Figure 4.229 Defining the plot settings for the custom plot
Figure 4.230 shows the resulting plot, after changing the plot settings to a Point
plot, using a size 8 diamond as a marker. As expected, the points align on a
straight line.
Note
The show origin option is used in the plot.
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309 | P a g e
A total of three scans were recorded in this experiment. The windower will be
used in this section to extract the data points from the second scan.
4.12.1 Adding a windower
To use the windower, which will be used to extract a cross section from the data
grid, right-click the CV staircase galvanostatic and select the Add Windower
option from the context menu (see Figure 4.232). This will add a new item, called
Windower to the data set.
310 | P a g e
Figure 4.233 The windower tool is also available from the quick access toolbar
Adding the windower tool triggers the Windower editor window to appear (see
Figure 4.234).
The following items need to be specified for the Windower tool to work properly:
Source: this is the source signal used to window the data. The source
signal is one of the available signals available in the data set (Time, Scan
number, WE(1).Potential, ). Only one source signal can be selected.
Simple (checkbox): this specifies if the simple editor is used (selected by
default).
Values: this defines the values of the selected source signal to use in the
windower.
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As soon as the source is defined, the Windower editor displays a list of available
values for the selected signal in the frame in the middle (see Figure 4.236). Since
this data set only contains three scans, three checkboxes are provided, one for
each scan.
312 | P a g e
Figure 4.236 The contents of the Windower editor are updated as soon as the source
signal is defined
Select the checkbox corresponding to the second scan in the editor to select the
second scan for the windower (see Figure 4.237).
Click the
button to close the editor and add the specified windower to the
data set (see Figure 4.238).
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Switch to a 2D plot and select the E vs i plot added to the Windower and change
the plot options to a size 3 red line plot. The data points from scan number two
will be displayed (see Figure 4.240).
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Figure 4.241 The original data set (WE(1).Potential vs time blue curve) and
scan number 2, selected using the windower (red curve)
Click the added windower item in the data explorer to reveal the control
parameters, defined in the editor, on the right-hand side of the 2D plot (see Figure
4.242).
Figure 4.242 The control parameters of the windower are displayed on the right-hand side
of the plot
Figure 4.243 Adding items to the windower will automatically update the
selected data
Note
It is possible to use the right-click menu on the list displayed in the control
interface to quickly select or deselect all the available check boxes. It is also
possible to easily invert the selection (see Figure 4.244).
Figure 4.244 The right-click menu allows you to quickly select or deselect the available
check boxes
316 | P a g e
In Figure 4.245, the selection begins at 2 and ends at 3, which is the same
selection as specified in Figure 4.243. This selection mode is useful when the
number of available values for the selected signal is very high.
Note
When the number of values for the selected source signal exceeds 300, Nova
will automatically switch from simple to advanced.
Switch the source signal from Scan to Time, using the dropdown list (see Figure
4.246).
Using the advanced selection mode and the Time signal as a source, it is possible
to select, for example, all the points measured from 20 s to 40 s (see Figure
4.247).
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36
318 | P a g e
Figure 4.249 Adjusting the X axis scale in order to graphically select the second scan
With the X axis adjusted, right-click the E vs t plot and select the Create
Windower from X axis option from the context menu (see Figure 4.250).
Figure 4.250 Select the Create Windower from X axis to create a windowed set of data
With the X axis adjusted, right-click the E vs t plot and select the Create
Windower from X axis option from the context menu (see Figure 4.250). A
windower will be added to the dataset (see Figure 4.251). This windower
automatically uses the signal plotted on the X axis as the Source and the minimum
and maximum of the X axis scale as the beginning and end of the windower,
respectively.
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3
3D plot, 184, 185
3D plot rotation, 185
A
Abort measurement, 11
Add commands, 76
Add link, 81, 84
Add plot, 179
Adding commands, 64
Advanced procedure editing, 90, 122
Analog to digital conversion, 21
Analysis view, 10, 15, 155
Anodic branch, 273
Anodic charge, 153
Anodic stripping, 234
Apply to selected, 199
Autolab control, 97
Autolab Control, 97
Autolab Control Tabs, 98
Autolab Display, 47, 149
Autolab procedures, 53, 119
Automatic current ranging, 24, 56, 110, 111
Automatic integration time, 24
Automatic peak search, 194, 240, 243, 244
Automatic scaling, 216
Auxiliary signal, 127
Averaging, 19
Axes Coupling, 216
Axis labels, 169, 214
Axis location, 216
Axis scale type, 215
Axis scaling, 177
Axis settings, 172
B
Baseline correction, 233, 239
Baseline mode, 225, 243
Begin value, 107
BMP, 217
Build procedure, 95
Build signal, 298
Bulk concentration, 299
Butler-Volmer equation, 276
C
Calculate charge, 264, 287
Calculate signal, 291, 293, 294, 305
Cathodic branch, 273
Cathodic charge, 153
CELL ON label, 150
D
Data analysis, 155, 222, 225, 242, 273, 277
Data analysis frame, 156
Data analysis toolbar, 183
Data backup, 161
Data conversion, 166
Data database, 29
Data explorer frame, 156
Data format, 215
Data grid, 168, 244, 289
Data information, 211
Data location, 211
Data point marker, 236
Data point selection, 235
Data presentation, 139
Data repository, 161
Data set analysis tools, 222, 280
Database, 28, 156
Database manager, 28
321 | P a g e
E
Edit Axis, 216
Edit Axis Color, 216
Edit Label Color, 216
Edit Label Font, 216
Edit options, 25
Edit procedure, 53
Edit sampler, 20
Edit Tick Text Font, 216
Edit title, 206
Electrochemical methods, 119
Electrochemical signals, 18, 56, 199
Enable commands, 73
Enable zooming option, 217
End key, 213
End status Autolab, 52, 56
End value, 107
EQCM, 188
EQCM(1). frequency, 189
Exchange current, 271
Expand one level, 11
Export data, 164
Export to ASCII, 289, 290
Export to Excel, 289, 290
Expression builder, 291, 293
External signals, 18, 20
F
F10 key, 149
Factory standard procedures, 119
Fast Fourier Transform, 227, 267
FFT, 227, 267
FFT filter type, 229
FFT Smoothing, 227, 267
File menu, 12, 119
Filter and select signals, 298, 300
Filter data, 298
Filter database, 159
Filter scan rate, 303
Find data, 166
First derivative, 262
Fixed minimum size scaling, 216
Fixed scaling, 216
Forward, 259
FRA measurement,, 153
Functions, 293
G
GIF, 217
Global plot options, 196
GPES, 57
Grid, 201
Grid (coarse), 201
Grid (fine), 201
H
Help menu, 13
High resolution plots, 201
High stability, 150
Highest current range, 111, 150
Home key, 213
HSTAB label, 150
I
Import data, 164
Individual plot, 195
Input box, 87
Insert commands, 67, 76
Insert label, 212
Insert procedure, 122
Integrate, 264
Integrate plot, 266
Interrupt, 78
J
JPG, 217
L
Legend, 203
Legend font, 205
Legend position, 205
Legend style, 205
Levich plot, 257, 281, 283
Line frequency, 21
Linear distribution, 107
Linear regression, 255
Linear sweep voltammetry, 96, 102
Link, 56
Link Input box, 87
Link parameters, 11
Linking, 60, 81
Linking commands, 79
Linking parameters, 79
Links, 79
Load data, 168
Load database, 156
Local plot options, 196
Logarithmic distribution, 107
Lowest current range, 111
LSV staircase, 102
M
Major tick, 201
Manual control, 149
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N
New database, 30
New procedure, 10, 52, 53
Noise filtering, 224
Noise reduction, 224
Nova strategy, 7
Nr of values, 107
Number of points in search window, 226, 243,
244
Number of potential steps, 61
Number of scans, 59
Number of significant digits, 243, 244, 259, 273,
277
Number of stop crossings, 59
O
OCP determination, 142, 147
Open circuit potential, 147
Optimize current range, 58, 101
Optimized, 110, 113
Optimized signal, 20, 21, 22
Options, 53, 56, 110, 113
Origin, 203
Origin Axes, 216
Original Dimensions, 218
Orthogonal projection, 187
Overlay, 188, 191, 194
Overlay in measurement view, 192
Overload, 47
Overrule global plot options, 196
P
Paste to powerpoint, 201
Pause measurement, 10
Peak current, 194
Peak height, 304
Peak search, 223, 240
Q
QCM thickness, 188
R
Range builder, 105, 106
Range generator, 106
Real time information, 139, 149
Record signals, 60, 61, 65, 67, 68
Regression, 255
Regression type, 258
Remarks, 52, 56, 118, 119, 120, 158, 183
Remove background, 202
Remove commands, 62
Remove link, 81
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S
Sampler, 19, 20
Sampler editor, 113
Sampling rate, 67
Sampling time, 23
Save Image File, 217
Save in My commands, 136
Save plot settings, 183
Save procedure, 10, 119
Save to database, 183
Save to database button, 183
Scaling mode, 216
Scan rate, 193, 302
Scan selector, 314
Search mode, 258
Second signal, 18, 127, 188
Segments, 19
Sequence of procedures, 123
Set cell, 58
Set potential, 58, 60, 67
Setup view, 10, 15, 51
SG Smooth, 223
SHE, 293
Show all links, 11, 79
Show Coordinates, 208
Show global maximum and minimum, 207
Show Label, 216
Show Legend, 204
Show local maximum and minimum, 207
Show Origin, 203
Show Positioning lines, 210
Show Title, 206
Signal averaging, 19
Signal builder, 300
Signal sampler, 18, 53, 56, 113
Signal to noise ratio, 22, 223
Signals, 293
Smoothing, 223
Sort database, 159
Square root distribution, 107
Standard database, 29
Standard Hydrogen Electrode, 293
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Start button, 52
Start measurement, 10
Start/stop button, 141
Step through data, 213
Step through Data, 211
Step type, 107
T
Tafel slope analysis, 271
Tick Text Angle, 216
TIF, 217
Time, 20
Time stamp, 158, 183
Timed procedure, 54, 60
Title, 56, 203
Toggle Text Location, 217
Toolbar, 10
Tools menu, 13
Tooltip, 58
Trigonometric operators, 293
Tutorials, 9, 13, 222
U
Unlink parameters, 11
Unlinking, 81
Upgrade from previous versions, 166
Use My Commands, 137
Use procedure options, 123
Use procedure sampler, 123
User database, 29
User log, 52, 141
User-defined view, 222
V
View menu, 12
W
Wait time, 58
WE(1).Potential, 113
Windower, 309
Windower source, 310
WMF, 217
X
X/Y analysis tools, 222
Z
Zooming, 148, 217
03/2013
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3526 KM Utrecht
The Netherlands