Multi Autolab Tutorial - Metrohm Autolab · NOVA Multi Autolab tutorial . Figure 7 – Adjusting the hardware setup of the M101 or M204 modules installed in the Multi Autolab cabinet

NOVA Multi Autolab Tutorial

Version 1.11.0

NOVA Multi Autolab tutorial

Table of Contents

1 – Multi Autolab support framework ................................................................... 3 2 – Multi Autolab support ..................................................................................... 3

2.1 – Multi Autolab driver ................................................................................. 6 2.2 – Multi Autolab connection ......................................................................... 7 2.3 – Multi Autolab hardware setup .................................................................. 8 2.4 – USB hub control ....................................................................................... 9

3 – Multiple Autolab support .............................................................................. 11 3.1 – Hardware setup ...................................................................................... 12

4 – Single Autolab use ........................................................................................ 14 4.1 – Switching devices ................................................................................... 15

5 – Multi Autolab use ......................................................................................... 17 5.1 – Adding instruments to the Multi Autolab configuration .......................... 19 5.2 – Fast configuration .................................................................................. 22 5.3 – Type of experiments available in the Multi Autolab configuration ........... 23 5.4 – Same procedure started at the same time .............................................. 23

5.4.1 – Selecting instruments ...................................................................... 23 5.4.2 – Specifying a procedure .................................................................... 24 5.4.3 – Specifying data storage ................................................................... 25 5.4.4 – Defining the plot options ................................................................. 26 5.4.5 – Running the measurement............................................................... 27 5.4.6 – Viewing the data ............................................................................. 33

5.5 – Same procedure started sequentially ...................................................... 34 5.6 – Different procedures started at the same time ........................................ 38 5.7 – Different procedures started sequentially ............................................... 43

5.7.1 – Procedure editing from Multi Autolab view ..................................... 43 6 – Instrument synchronization ........................................................................... 44

6.1 – The Multi Autolab software synchronization command .......................... 46 6.1.1 – Synchronization from the same procedure ....................................... 48 6.1.2 – Synchronization from the different procedures ................................ 52

6.2 – The Multi Autolab hardware synchronization command ......................... 56 6.2.1 – Synchronization from the same procedure ....................................... 58 6.2.2 – Synchronization from the different procedures ................................ 63

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1 – Multi Autolab support framework

This version of NOVA can be used to control the Multi Autolab instrument fitted with the M101 or M204 potentiostat/galvanostat module. Additionally, it can also be used to control more than one Autolab from the same computer, up to a limit of 8 or 16 instruments1.

The instruments can be directly connected to USB ports located on the computer or to a USB hub. The instruments connected to the same computer can be of any type.

Using the Multi Autolab support, it is possible to perform the following experiments on two or more instruments:

• Perform the same measurement on each instrument at the same time or sequentially

• Perform different measurements on each instrument at the same time or sequentially

The following configurations are presently supported by the Multi Autolab framework in NOVA:

1. Multi Autolab instrument fitted with M101 or M204 modules (see Section 2).

2. Multiple Autolab instruments (see Section 3). 3. Combination of both: the Multi Autolab instrument can be combined with

other Autolab instruments up to a cumulated total of 8 or 16 instruments1 (each M101 or M204 module counts as one instrument).

2 – Multi Autolab support

Nova provides support for the Multi Autolab instruments with M101 or M204 modules. There are two different Multi Autolab instruments available, each fitted with twelve module bays (see Figure 1):

• Multi Autolab/M101, which can accommodate up to twelve M101 potentiostat/galvanostat modules. These instruments are identified with a serial number starting with MAC8.

• Multi Autolab/M204, which can accommodate up to twelve M204 potentiostat/galvanostat modules. These instruments are identified with a serial number starting with MAC9.

1 The maximum number of instruments depends on the USB driver used to control the instruments. Please refer to the Getting started manual for more information.

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Figure 1 – Overview of the Multi Autolab with M101 or M204 modules (the module bay labels are indicated by the arrows)

The M101 or M204 modules are identical in specifications to the stand alone PGSTAT101 or PGSTAT204, respectively.

Each module bay of the Multi Autolab cabinet is identified by a label. From left to right, these labels are 1, A, 2 B, … 6, F, as shown in Figure 1. A M101 or M204 potentiostat/galvanostat can be installed in any one of the available module bays. An optional module can be installed in any one of the available bays labeled with a letter (A to F).

When the optional module is present, it will work in combination with the Autolab M101 or M204 module installed in the module on the left.

The following optional modules can be used in the Multi Autolab:

• BA: dual mode Bipotentiostat module. • EQCM: electrochemical quartz crystal microbalance. • pX1000: pH and T measurement module. • MUX: multiplexer module. • FRA32M: impedance analyzer module.

Figure 2 shows an example of a Multi Autolab cabinet fitted with six M101 or M204 modules (positions 1 to 6) and six optional modules (positions A to F).

A B C D E F

1 2 3 4 5 6

Warning

It is not possible to use M101 modules in a Multi Autolab/M204 or to use M204 modules in a Multi Autolab/M101.

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Figure 2 – Example of a Multi Autolab fitted with M101 or M204 module (6) and optional modules (6)

For example, if a BA module is installed in module bay B, it will work in combination with the M101 or M204 module installed in module bay 2.

BA BA EQCM EQCM pX1000 pX1000

M101 M101 M101 M101 M101 M101

BA BA EQCM EQCM pX1000 pX1000

M204 M204 M204 M204 M204 M204

Note

Optional modules must be combined with a M101 or M204 module.

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2.1 – Multi Autolab driver

Two USB drivers are installed alongside NOVA on the computer. One driver is reverse compatible with older versions of NOVA and with the predecessor software (GPES/FRA). Using this driver, only 8 instruments can be controlled from the same computer. The other driver is a NOVA only driver which is supported in NOVA 1.7 or higher. With this driver, a total of 16 instruments can be controlled from the same computer.

For Multi Autolab cabinets with 8 or more M101 or M204 modules, the use of the NOVA only driver is mandatory. For Multi Autolab cabinets with less than 8 M101 or M204 modules, the NOVA only driver is highly recommended.

It is possible to quickly switch from one driver to the other by using the Driver Manager2 application (see Figure 3).

Figure 3 – The Driver Manager application can be used to quickly switch drivers

2 More information about the Driver Manager can be found in the Getting started manual.

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Figure 4 – Error messages are provided when more than 8 instruments are connected to the same computer using the GPES compatible driver

The available M101 or M204 will be selected randomly depending on the initialization speed of each M101 or M204 module. The excess instruments will not be available for measurements.

2.2 – Multi Autolab connection

When a Multi Autolab is connected to the computer through USB, NOVA will setup each M101 or M204 module. The initialization progress can be tracked in the taskbar (see Figure 5).

Note

When a Multi Autolab instrument fitted with more than 8 M101 or M204 modules is connected to the computer through the GPES compatible driver, NOVA will initialize the first 8 M101 or M204 modules and will provide a connection error message in the user log for the other M101 or M204 modules (see Figure 4).

Warning

The GPES compatible driver is not available on a 64 Bit version of Windows.

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Figure 5 – When several instruments are connected to the same computer, the initialization process can be tracked in the taskbar

2.3 – Multi Autolab hardware setup

In order to work with the Multi Autolab instrument, it is necessary to adjust the Hardware setup. After initialization, the M101 or M204 modules installed in the Multi Autolab cabinet are identified in the serial number of the cabinet (MAC8XXXX or MAC9XXXX) and the position of the module in the cabinet according to the numbering scheme explained in the previous section (see Figure 1 and Figure 6).

Figure 6 – Adjusting the hardware setup of the M101 or M204 modules installed in the Multi Autolab cabinet (1/2)

The M101 or M204 should be selected in the Main Module frame of the Hardware setup. Additional modules can be selected, if applicable (see Figure 7).

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Figure 7 – Adjusting the hardware setup of the M101 or M204 modules installed in the Multi Autolab cabinet (2/2)

2.4 – USB hub control

The Multi Autolab cabinet is fitted with an internal USB hub that allows the Multi Autolab to be shared in between a maximum of three computers running the same version of Nova. When the Multi Autolab is connected to the main USB connector, the host computer controls all twelve module bays. If an additional host computer is connected to the either one of the sub USB connectors (sub-1 or sub-2), that PC will take over the control of the module bays indicated in the labels below the sub USB connectors (see Figure 8).

Note

The incompatible modules are greyed out.

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Figure 8 – The USB hub located on the back plane of the Multi Autolab cabinet

Depending on the connection to the USB hub, the host computer can control the following module bays:

• main USB: all the module bays in the Multi Autolab cabinet are controlled. • sub-1 USB: module bays 3, C, 4 and D are controlled. • sub-2 USB: module bays 5, E, 6 and F are controlled.

For example, connecting a computer to the sub-2 USB connector on the back plane will provide control over the modules installed in bays 5, E, 6 and F, exclusively. Connecting an additional computer to the main USB connector will provide control over all the remaining modules (1, A, 2, B, 3, C, 4, D). If a third PC is connected to the sub-1 USB connector, control over the modules in bays 3, C, 4 and D will be transferred from the computer connected to the main USB connector to the computer connected to the sub-1 connector.

Figure 9 shows how the computer transfers control of module bays 3, C, 4 and D to another computer when the second computer is connected to the sub-1 USB connector.

Caution

Never change the USB connections while an experiment is running on any of the Multi Autolab channels since this could lead to a loss of control of an experiment and a loss of data.

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Figure 9 – Connecting another computer to one of the sub USB connectors takes over control of the instruments connected to that sub USB hub

3 – Multiple Autolab support

Nova provides support for the Multiple Autolab instruments connected to the same computer. Compared with the Multi Autolab instrument, this configuration involves physically separated devices, but the software support is the same. In this respect, Multiple Autolab support is virtually identical to the support provided for the Multi Autolab instrument.

Note

For more information on the driver setup for Multiple Autolab instruments, please refer to Section 2.1. For more information on the initialization of the multiple Autolab instruments, please refer to Section 2.2.

Note

When Multi Autolab instruments fitted with M101 or M204 modules are connected to the same computer together with single Autolab instruments (for example, a Multi Autolab with M101 or M204 modules and a PGSTAT302N), each M101 or M204 module counts as an individual instrument with respect to the maximum number of instruments that can be controlled by the computer (8 for the GPES compatible driver and 16 for the NOVA only driver).

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3.1 – Hardware setup

In order to work with more than one Autolab on the same computer, the hardware setup of each instrument must be adjusted, if necessary. When two or more instruments are connected and initialized on the same computer, the Hardware Setup option of the Tools menu will be automatically adjusted in order to allow the user to specify the Hardware Setup for each instrument (see Figure 10).

Figure 10 – When two or more instruments are connected to the same computer, the Hardware Setup of each instrument can be specified from the modified Tools menu

The available instruments are identified by the serial number of the instrument (AUTXXXXX, µ3AUTXXXXX) or by the serial number of the external USB interface (USBXXXXX), if applicable (see Figure 10).

Note

Instruments with serial number beginning with AUT9 or with µ2AUT7, connected through an external USB interface, are identified by the serial number of the interface, USB7XXXX. Instruments with an internal USB interface, or instruments with serial number beginning with AUT7 connected through an external USB interface, are identified by their own serial number.

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Figure 11 – The Hardware Setup can be specified for each connected instrument

Adjust the hardware setup, if needed, and click to close the Hardware Setup window. When prompted, click to save the changes (see Figure 12).

Note

The Hardware Setup only needs to be specified once for each instrument. Each Hardware Setup is stored on the computer with the indentifying serial number of the instrument. If a Hardware Setup already exists on the computer for a connected instrument, it is not required to specify it again.

Note

If applicable, a FRA2 Calibration file can be imported for every connected instrument (Please refer to the Getting started manual for more information).

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Figure 12 – Saving the changes to the hardware setup

4 – Single Autolab use

When two or more instruments are connected to the same computer, an additional Select instrument toolbar will be displayed (see Figure 13). Using the drop-down list provided in this toolbar, any one of the available instruments can be selected.

Figure 13 – The Select instrument toolbar is automatically displayed when two or more instruments are connected to the same computer

The selected instrument will be set as the active instrument on which any compatible procedure can be started, in the same way as in a single Autolab configuration. The Autolab display is automatically adjusted and will display the available settings, as well as the serial number identifying the selected device (see Figure 14).

Figure 14 – The Autolab display is automatically adjusted for the specified instrument

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The serial number of the selected instrument is also indicated in the procedure editor (see Figure 15).

Figure 15 – The identifying serial number of the selected instrument is indicated in the procedure editor

When a measurement is running on the selected instrument, the Select instrument toolbar on the right-hand side will be grayed out (see Figure 16).

Figure 16 – The Select instrument toolbar is not available when the selected instrument is measuring

When the measurement is completed, the Select instrument toolbar will become available again.

4.1 – Switching devices

If no measurement is running, it is possible to switch from one device to another by selecting the identifying serial number in the Select instrument toolbar, as shown in Figure 13. The procedure editor as well as the Autolab display will be automatically adjusted (see Figure 17).

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Figure 17 – When another instrument is selected using the Select instrument toolbar, the procedure editor and the Autolab display are automatically adjusted

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5 – Multi Autolab use

When two or more instruments are connected to the same computer, it is possible to perform the same or different experiments on the connected instruments, at the same time. It is also possible to start several measurements on each instrument, sequentially. This differs from the options described in the previous section, since it is possible to start a measurement on one or more devices while other devices connected to the same computer are still measuring.

To control more than one instrument at a time, it is necessary to switch to the dedicated Multi Autolab view. This can be done by clicking the button in the toolbar or by selecting the Multi Autolab view from the view menu (see Figure 18).

Figure 18 – Selecting the Multi Autolab view from the toolbar or the View menu

The Multi Autolab view, shown in Figure 19 is a dedicated interface in which one or more connected Autolab devices can be added to a Multi Autolab configuration

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Figure 19 – The dedicated Multi Autolab view

Note

When the Multi Autolab view is selected, the Start button is not available anymore. Normal measurements cannot be started from this view.

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5.1 – Adding instruments to the Multi Autolab configuration

In order to perform measurements on more than one instrument at the same time, or sequentially, from the Multi Autolab view, the involved instruments need to be added to the Multi Autolab configuration. This is achieved by clicking the button in the lower right-hand corner of the Multi Autolab view. When this button is clicked, an Instrument configuration panel will be added to the Multi Autolab view (see Figure 20).

Figure 20 – Clicking the button will add an Instrument configuration panel to the Multi Autolab view

Each panel can be used to define a number of instrument related properties. The most important property is the identifying serial number of the instrument, which can be selected from the Instrument dropdown list (see Figure 21).

Figure 21 – The instrument dropdown list can be used to add one of the available instruments to the Multi Autolab configuration

Using the button, it is possible to add more instrument configuration panels to the Multi Autolab view. For each panel, a serial number of one of the available devices must be defined (see Figure 22).

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Figure 22 – Multi Autolab view with three instruments panels

For each instrument added to the Multi Autolab configuration, it is possible to define a Description. This is a small string that can be used in Multi Autolab measurements in order to easily recognize from which instrument the data originated. In the example shown in Figure 23, the model of the instrument has been used in the three description field, respectively.

Note

Each available instrument can be selected once. Only the instruments added to the Multi Autolab configuration can be involved in a Multi Autolab experiment.

Warning

The maximum number of instruments is 8 when GPES compatible drivers are used. When the NOVA only drivers are used, the maximum number of instruments is 16. Please refer to the Getting Started manual for more information.

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Figure 23 – A description can be added to each instrument panel

Once all the instruments have been added to the Multi Autolab configuration, a name can be given to this configuration and some remarks can provided in the dedicated frame (see Figure 24).

Figure 24 – Configuration name and remarks can be specified in the dedicated frames

The specified Multi Autolab configuration can then be saved by selecting the Save Multi Autolab Configuration option from the File menu (see Figure 25).

Figure 25 – Saving the Multi Autolab configuration (1/2)

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A location and name for the file needs to be specified (see Figure 26). Saved Multi Autolab configurations can be loaded at any time by selecting the Open Multi Autolab Configuration from the File menu (see Figure 25).

Figure 26 - Saving the Multi Autolab configuration (2/2)

5.2 – Fast configuration

It is possible to create a Multi Autolab configuration quickly, in which all the connected Autolab devices are added automatically. To do this, click the Generate default configuration button located on the right-hand side of the Multi Autolab view (see Figure 27).

Figure 27 – Click the Generate default configuration button to automatically create a Multi Autolab configuration involving all the connected instruments

Using this option, the Multi Autolab configuration is pre-configured in order to perform the same measurement on all the connected instruments. All the

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instruments in the configuration are selected and a unique color is pre-defined for each device3.

5.3 – Type of experiments available in the Multi Autolab configuration

Four different experimental configurations can be encountered when working with the Multi Autolab view:

1. Same procedure on all the selected instruments at the same time: in this mode, one or more instruments are selected by the user and the same procedure is started on all the selected instruments at the same time.

2. Same procedure on one or more of the available instruments, sequentially: in this mode, one or more of the available instruments are used to perform the same procedure, but the measurements are started sequentially.

3. Different procedures on all the selected instruments at the same time: this mode is similar to the first mode, with the only difference that different procedures are used.

4. Different procedure on one or more of the available instruments, sequentially: this mode is similar to the second mode, with the only different that different procedures are used.

The different modes will be described in detail in the next sections of this tutorial.

5.4 – Same procedure started at the same time

In this mode, all the selected instruments will be used to perform the same measurement at the same time. The measurements will start at the same time. However, depending on the events on each instrument, the measurements can stop at the same or at different times. It is possible to introduce a synchronization command in the procedures. This advanced feature will be explained at the end of this tutorial.

5.4.1 – Selecting instruments

For this mode, one or more of the available instruments can be selected by clicking the checkbox next to each individual instrument in the Multi Autolab view. In the example shown in Figure 28, Instruments 1 and 2 have been selected, Instrument 3 is not selected.

3 Please refer to the next section for more information.

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Figure 28 – It is possible to select any available instrument by clicking the checkbox in each individual instrument panel

Since Instrument 3 is not selected, it will not be involved in the measurement.

5.4.2 – Specifying a procedure

In the Multi Autolab view, it is possible to define the procedure to be executed by the selected devices in two different ways:

1. By using the active procedure: in this case, the procedure that is currently open in the Setup view, will be used.

2. By specifying a specific procedure file: in this case, a specific Nova procedure (.nox) file, already stored on the computer, will be used4.

To use the active procedure, simply click the checkbox next to the Use active procedure property in the individual instrument panels (see Figure 29).

4 This option will be illustrated in the next section.

Note

It is possible to use a combination of both modes.

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Figure 29 – Using the active procedure for the Multi Autolab measurement

As example, we will use the Autolab Cyclic voltammetry potentiostatic procedure. Switch the Setup view and load this standard procedure in the procedure editor frame (see Figure 30).

Figure 30 – Setting the Autolab Cyclic voltammetry potentiostatic as the active procedure

5.4.3 – Specifying data storage

In the Multi Autolab view, it is possible to define two different locations for data storage:

1. By using the database: in this case, the result from the measurement performed on each instrument will be automatically stored in the user defined database.

2. By specifying a specific file: in this case, a specific Nova data (.nox) file and location is specified by the user before the measurement starts5.

5 This option will be illustrated in the next section.

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To automatically store the data in the user-defined database, simply click the checkbox next to the Store in database property in the individual instrument panels (see Figure 31).

Figure 31 – Using the database to store the data for the Multi Autolab measurement

5.4.4 – Defining the plot options

It is convenient to define specific plot options for each instrument involved in the Multi Autolab measurement in order to recognize the data plotted in the Measurement view. The button can be used to specify the plot settings for each device. Clicking this button displays the plot options window in which the settings, to be used during the measurement by a specific instrument, can be defined (see Figure 32).

Note

It is possible to use a combination of both modes.

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Figure 32 – The plot options can be defined for each instrument independently

5.4.5 – Running the measurement

To start the measurement on the selected instruments, click the Start Selected button located at the bottom of the Multi Autolab view (see Figure 33). The active procedure will be checked for each instrument. If no problems are encountered, the measurements will start.

Note

The plot options defined in the Multi Autolab view will override the options defined in the procedure.

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Figure 33 – Click the Start Selected button to start the measurement on the selected instruments

During the measurements, the Status of the each instrument will be updated in the Multi Autolab view. The status of instruments that are involved in a measurement will be greyed out (see Figure 34).

Figure 34 – The status of each instrument is updated in the Multi Autolab view

In the example shown in Figure 34, instruments 1 and 2 are Measuring.

To see the experimental data during the measurement, it is necessary to switch to the Measurement view, by clicking the button or by selecting the Measurement view option from the View menu.

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The measured data points obtained from the selected instruments will be displayed in the Measurement view, using the plot settings defined in the procedure and the plot options defined in the Multi Autolab view. In the example shown in Figure 35, the data from the Autolab Cyclic voltammetry potentiostatic procedure is plotted on plot #1 and plot #2 in the measurement view.

Figure 35 – A Multi Autolab measurement example (plot#1 i vs E: red line plot, Channel 1; blue line plot, Channel 2 / plot #2 i vs t: red line plot, Channel 1; blue line plot, Channel 2)

Plot #1 and plot #2 show the i vs E and i vs t, respectively, for both instruments. The Y axis locations, labels and plot options have been defined in the Multi Autolab

Note

The measurement view is not automatically selected when a Multi Autolab measurement starts.

Note

The i vs t plot has been added to the CV staircase command in the procedure used in this example.

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view, through the Plot Options. The signals to plot and the plot locations have been defined in the Autolab Cyclic voltammetry potentiostatic procedure, which was modified for this example. Instrument 1, MAC80007#1 (Channel 1) is connected to the Autolab dummy cell (c) while Instrument 2, MAC80007#2 (Channel 2) is connected to dummy cell (e).

During the measurement, it is also possible to show the Autolab display window, by pressing the F10 shortcut key or by selecting the Autolab display option from the View menu. This window can be used to track the status of all the instruments involved in the measurement. Figure 36 shows the details of Instrument 2 (MAC80007#2) in the main Autolab Manual Control frame, as well as a summary of the status of all the instruments involved in the measurement at the bottom of the frame.

Figure 36 – The Autolab display shows the detailed status of all the instruments involved in the Multi Autolab measurement

The two collapsible panels located at the bottom of the Autolab display window provide a general overview of all the instruments currently involved in the multi Autolab measurement. The WE(1).Potential and WE(1).Current values are shown6, as well as the active current range. A voltage and current overload warning is also available for each device (see Figure 36).

6 The availability of the values shown in the Autolab display window depends on the plot settings used in the Measurement view. In order to show the values of E and i during the measurements, the WE(1).Potential and WE(1).Current must be sampled (using the signal sampler).

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Furthermore, it is possible to Pause (and Resume) or Stop the procedure on any instrument involved in the multi Autolab measurement, by clicking the Pause , Resume and Stop buttons located in the small panels in the Autolab display (see Figure 37).

Figure 37 – Using the buttons located in the Autolab display to Pause, Resume and Stop measurements (MAC80007#1 is paused, MAC80007#2 is measuring)

In Figure 37, the measurement on Instrument 1 - MAC80007#1 (Channel 1) is paused. It can be resumed by the user by clicking the Resume button. Pressing the button will stop the measurement for this device.

The details of Instrument 2 – MAC80007#2 (Channel 2) are shown because the Select instrument toolbar, shown in Figure 35, is set to MAC80007#2.

When the procedure running on one of the instruments stops (or is stopped by the user or by a cutoff condition), the Autolab display panels will be adjusted.

In the example shown in Figure 38, the measurement on MAC80007#2 (Channel 2) is finished while MAC80007#1 (Channel 1) is still measuring. The small panel for Channel 2 is removed from the Autolab display at the end of the experiment.

Note

This toolbar cannot be adjusted during a measurement.

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Figure 38 – When the procedure stops on one of the instruments, its panel is removed from the Autolab display

Likewise, the status of MAC80007#2 (Channel 2) is also updated in the Multi Autolab view, indicating that it is currently available for another measurement (see Figure 39).

Figure 39 – When the procedure stops on one of the instruments, its status is automatically updated in the Multi Autolab view

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5.4.6 – Viewing the data

In this example, the data storage options defined in the Multi Autolab view, specify that the measured data points should be automatically stored in the user-defined Database (see Figure 31).

In the database frame, available in the Analysis view, individual entries will be created for each instrument at the end of the experiment (see Figure 40).

Figure 40 – Measurements are automatically stored in the database if the Store in database option is used in the Multi Autolab view

In the database, two extra columns are shown: Instrument and Instrument description. These two columns are used to show the identifying serial number of the instrument used in the experiment and the Instrument description, provided in the Multi Autolab view, respectively.

In the example shown in Figure 40, a third entry is shown in the database. This entry does not have an Instrument description because it contains the data obtained with MAC80007#1, used in single Autolab mode.

Using the database it is possible to filter the contents, as explained in the Nova user manual. For example, selecting one of the measurements obtained with MAC80007#1 and then right-clicking on the Instrument column and selecting the Filter selected dropped on row – Like option from the context menu, will update the contents of the database frame, showing only the measurements obtained with this instrument (see Figure 41).

Note

If no description is provided in the Multi Autolab view for a specific instrument, the Instrument description field will also be empty when a Multi Autolab measurement is finished on that instrument.

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Figure 41 – Filtering the database using the right-click menu

Select the Show all option from the same menu to show all the measurements in the database again (see Figure 42).

Figure 42 – Use the Show all option to show all the measurements in the database

5.5 – Same procedure started sequentially

In this mode, all the selected instruments will be used to perform the same measurement. However, the measurement will be started sequentially.

The setup for this mode is identical to the one shown in the previous section. First of all, two or more instruments are added to a Multi Autolab configuration (see Figure 21). An instrument description is provided, if necessary, for each instrument (see Figure 23). A procedure is defined, and in this section the procedure currently available in the Setup view will be used (see Figure 29). Finally, data storage options are defined. In this example, these settings will be identical to those used in the previous section (see Figure 31). In this example, instrument 3 will be used in the same way as instruments 1 and 2 (see Figure 43).

Figure 43 – The multi Autolab configuration used in this example

The difference with respect to the previous section is that in this mode, identical measurements will be started on several Autolab instrument, sequentially. To illustrate this, the procedure defined in the Setup view, which is a modified Autolab

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Cyclic voltammetry procedure already used in the previous example, will be started on instruments 1 and 2 (MAC80007#1 and MAC80007#2). Once the measurements are running on these two instruments, the same procedure will be started on instrument 3 (MAC80007#3).

Select Instrument 1 and 2 in the multi Autolab view by clicking the checkbox next to these two instruments and press the Start selected button to start the measurement on these devices (see Figure 44).

Figure 44 – Starting the measurement on the first two instruments

The measurements will start as shown in the previous section, and the status of instruments 1 and 2 will be updated to Measuring (see Figure 44). While these instruments are measuring, deselect them by removing the checkbox and click the checkbox for instrument 3 (MAC80007#3). Press the Start selected button again to start the measurement on this instrument (see Figure 45).

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Figure 45 – Starting the measurement on instrument 3 while instruments 1 and 2 are still measuring

The same measurement will now start on instrument 3 (MAC80007#3). The multi Autolab view will be updated, indicating that all three devices are currently measuring. When the measurement finishes on Instrument 1 and 2, the multi Autolab view will be updated, indicating that these two instruments are Ready (see Figure 46).

Note

The and buttons can be used to quickly select or deselect all instruments available in the multi Autolab view.

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Figure 46 – When the measurement finishes on instruments 1 and 2, they will become available for a new experiment

When the measurement starts on instrument 3, an additional summary panel will be added to the Autolab display (see Figure 47).

Figure 47 – An additional panel for instrument 3 is added to the Autolab display during the measurement

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5.6 – Different procedures started at the same time

In this mode, all the selected instruments will be used to perform a different measurement, at the same time.

For this experimental setup, it is necessary to prepare a valid procedure for each experiment. Each procedure must then be saved in a specific location by the user.

To illustrate this measurement option in the Multi Autolab view, two default Autolab procedures will be used:

• Cyclic voltammetry potentiostatic • Linear polarization

Switch to the Setup view and load the Linear polarization procedure in the procedure editor. This procedure will be used without any modification (see Figure 48).

Figure 48 – The Autolab Linear polarization procedure

Select the Export procedure option from the File menu and specify a location in which the procedure file for the Linear polarization experiment will be saved (see Figure 49).

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Figure 49 – Export the procedure to a convenient location

Once the first procedure is saved, a second procedure can be loaded in the procedure editor, modified according to the experimental requirements and exported to a convenient location on the computer. This can be repeated for every experimental procedure.

Load the Autolab cyclic voltammetry procedure in the procedure editor (see Figure 50). This procedure needs to be modified because the plot location defined in the two procedures is set to plot #1 by default. If both procedures are started at the same time, the measurement view will be forced to display data from two completely different experiments on the same plot.

Figure 50 – The Autolab Cyclic voltammetry potentiostatic procedure

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Expand the CV staircase command in the procedure editor and change the plot location of the i vs E plot to plot #2 using the dropdown list (see Figure 51).

Figure 51 – Adjusting the plot location for the Cyclic voltammetry potentiostatic procedure

Switch to the Multi Autolab view and select instruments 1 and 2 by clicking the checkbox for these two instruments. Uncheck the Use active procedure checkbox for Instrument 1 (MAC80007#1), as shown in Figure 52.

Figure 52 – Uncheck the Use active procedure for Instrument 1 in the Multi Autolab view

Next, click the button located in the instrument panel to specify the location for the .nox file that was exported in the initial part of this section (see Figure 49), as shown in Figure 53.

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Figure 53 – Click the button to specify the location of the procedure to be used with Instrument 1 (MAC80007#1)

For Instrument 2 (MAC80007#2), the procedure currently loaded in the procedure editor will be used, so the Use active procedure checkbox can stay active. However, for every instrument involved in the measurement, a specific .nox file location can be defined. The same location can be specified for more than one instrument, in which case a situation similar to the first experimental condition will be obtained.

The Multi Autolab view should now look as shown in Figure 54.

Figure 54 – The Multi Autolab configuration used in this example: Instrument 1 (MAC80007#1) will perform the Linear polarization experiment and Instrument 2

(MAC80007#2) will perform the Cyclic voltammetry potentiostatic experiment

Click the Start selected button to start the measurements on both instruments (see Figure 54). The OCP determination command included in the Linear polarization procedure triggers the appearance of the OCP determination window, specifically for Instrument 1 (see Figure 55).

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Figure 55 – The OCP determination window is shown at the beginning of the measurement on Instrument 1 (MAC80007#1) while Instrument 2 (MAC80007#2) is running the Cyclic

voltammetry procedure

While Instrument 1 (MAC80007#1) is performing the determination of the OCP value, Instrument 2 (MAC80007#2) starts plotting values on plot #2. When the OCP determination is finished, the data recorded during the linear polarization experiment is plotted on plot #1 (see Figure 56). The data from Instrument 1 is obtained with dummy cell (c) and the data from Instrument 2 is obtained with dummy cell (e).

Note

The identifying serial number of the instrument involved in the OCP determination is shown in the header of the window.

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Figure 56 – A Multi Autolab measurement example (plot#1 log(i) vs E: blue line plot, Linear polarization experiment on Instrument 1 (MAC80007#1) / plot #2 i vs E: red line plot, Cyclic

voltammetry on Instrument 2 (MAC80007#2)

5.7 – Different procedures started sequentially

In this mode, a different experiment will be performed on all the selected instruments, but the measurements will start sequentially.

The setup for this mode is identical to the one shown in the previous section. First of all, two or more instruments are added to a Multi Autolab configuration (see Figure 21). An instrument description is provided, if necessary, for each instrument (see Figure 23). Two different procedures are specified (see Figure 54) and data storage options are defined. In this example, these settings will be identical to those used in the previous sections (see Figure 31).

5.7.1 – Procedure editing from Multi Autolab view

When different procedures are used at the same time, or sequentially, one or more of the procedures used are pre-defined and stored as .nox files on the computer.

It is possible to edit the procedures saved as .nox files used in the Multi Autolab view, directly from this view. When a procedure path is specified in the Procedure field in the Multi Autolab view (as explained in Section 5.6), the button

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located next to the procedure path can be clicked to open a dedicated procedure editor (see Figure 57).

Figure 57 – Editing a procedure from the Multi Autolab view

A new window will be displayed, showing condensed procedure editor (see Figure 58).

Figure 58 – The condensed procedure editor

This editor displays the contents of the saved procedure, as well as all the individual commands. New commands can be dragged into the procedure editor, if required. It is also possible to modify command parameters and links in the procedure. The edited procedure can be saved by clicking the button in the toolbar (see Figure 58).

6 – Instrument synchronization

Regardless of the measurement strategy used in the Multi Autolab view, the measurements running on different instruments will never be synchronized with one another. By default, each instrument will perform the commands located in the specified procedure without interacting with the other devices connected to the same computer.

Note

The modifications to the procedure are not stored unless the procedure is saved by clicking the button in the toolbar.

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Synchronization between instruments can however be desirable in some experimental conditions. For example, in the case of the experiment illustrated in Figure 54 Figure 56, the OCP determination performed on Instrument 1 (MAC80007#1) introduces a significant delay with respect to the cyclic voltammetry measurement running on Instrument 2 (MAC80007#2). The OCP determination takes an unspecified amount of time, up to a maximum of 120 s (the time limit value of the command).

Two synchronization commands are available in Nova:

• Multi Autolab software synchronization: this command can be used with any type of Autolab and allows synchronization between the involved instruments. The timing is controlled by the software.

• Multi Autolab hardware synchronization: this command can only be used to synchronize M101 or M204 modules located inside the same Multi Autolab device. The timing is controlled by the hardware and it is more accurate than the software synchronization.

Figure 59 – Switching the Profile to Advanced

Note

Both commands are Advanced commands and the NOVA profile must be set to Advanced for these commands to be displayed in the commands browser (see Figure 59).

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6.1 – The Multi Autolab software synchronization command

Using the Multi Autolab software synchronization command located in the Measurement – general group of commands, one or more synchronization points can be added to any procedure in order to force two or more Autolab instruments to synchronize (see Figure 60).

Figure 60 – The Multi Autolab software synchronization command is available in the Measurement – general group

The Multi Autolab software synchronization command (MASS), can be added anywhere in a procedure to introduce a synchronization point for Multi Autolab measurements. Figure 61 shows an example of the use of the MASS command in the Cyclic voltammetry potentiostatic procedure. In this example, the synchronization command has been inserted between the Optimize current range command and the CV staircase command.

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Figure 61 – Adding the Multi Autolab software synchronization command to the Cyclic voltammetry potentiostatic procedure

The MASS command has the following parameters:

• Number of participating Autolab instruments: specifies the number Autolab instruments to synchronize. The synchronization is triggered as soon as this number is reached or when the optional time limit has been reached.

• Group name: defines a unique name for the synchronization point. • Time limit (s): defines a time limit for the synchronization command. • Use time limit (Yes/No): toggles the time limit check on or off. • Abort procedure after time limit (Yes/No): forces the procedure to stop

when the Time limit is reached and the Use time limit check is on.

Warning

The timing accuracy of the Multi Autolab software synchronization command is ± 100 ms.

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The MASS command can be used in two different situations:

• In the same procedure: this applies to the Multi Autolab use explained in the Section 5.4 and 5.5. In this case, the instruments involved in the measurement are running the same procedure, in which case the MASS command is automatically included in each procedure.

• In different procedures: this applies to the Multi Autolab use explained in the Section 5.6 and 5.7. In this case, the instruments involved in the measurement are running different procedures, in which case the MASS command must be added to all the procedures used in the experiment.

6.1.1 – Synchronization from the same procedure

When the Multi Autolab view is used to perform the same procedure on more than one instrument, the MASS command can be used to force the instruments to synchronize at a given point in the procedure.

To illustrate this, the examples shown in Section 5.4 and 5.5 will be used. Load the Cyclic voltammetry procedure in the Setup view and add the MASS command to the procedure, between the Optimize current range command and the CV staircase command, as shown in Figure 61.

Note

It is only possible to synchronize measurements that are started at the same time from the Multi Autolab view.

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Adjust the parameters of the synchronization command as shown in Figure 62.

Figure 62 – Setting up the synchronization command

Switch to the Multi Autolab view and setup the experimental conditions as shown in Figure 63.

Figure 63 – The settings used in the Multi Autolab view

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This example can be performed in two different ways:

• Select Instrument 1 and Instrument 2 and press the Start Selected button. This corresponds to the measurement strategy detailed in Section 5.4.

• Select Instrument 1 and press the Start Selected button, then repeat the same steps for Instrument 2. This corresponds to the measurement strategy detailed in Section 5.5.

Both methods will yield exactly the same result. The first instrument to reach the Multi Autolab software synchronization command will hold until the other instrument reaches this command. This will force the CV staircase command to be executed on both instruments at the same time.

The experimental data obtained using this example is shown in Figure 64.

Note

While holding at the synchronization point, no hardware settings are modified on instruments. In this example, the synchronization point is defined before the CV staircase command, which means that the instruments reaching the synchronization point will hold with the cell ON and 0 V applied on the working electrode, until all the required instruments reach this point or until the Time limit is reached, if applicable.

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Figure 64 – A Multi Autolab measurement example using the Multi Autolab software synchronization command (plot#1 i vs E: red line plot, MAC80007#1 (Channel 1); blue line

plot, MAC80007#2 (Channel 2) / plot #2 i vs t: red line plot, MAC80007#1 (Channel 1); blue line plot, MAC80007#2 (Channel 2)

Plot #1 and plot #2 show the i vs E and i vs t, respectively, for both instruments. The Y axis locations, labels and plot options have been defined in the Multi Autolab view, through the Plot Options. The signals to plot and the plot locations have been defined in the Autolab Cyclic voltammetry potentiostatic procedure, which was modified for this example. Instrument 1, MAC80007#1 is connected to the Autolab dummy cell (c) while Instrument 2, MAC80007#2 is connected to dummy cell (e).

The measurements are now synchronized.

Note

The i vs t plot has been added to the CV staircase command in the procedure used in this example.

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It is possible to add more than one Multi Autolab software synchronization command to a procedure. However, the Group name must be unique.

6.1.2 – Synchronization from the different procedures

When the Multi Autolab view is used to perform the different procedures on two or more instruments, the Multi Autolab software synchronization command can be used to force the instruments to synchronize at matching points in the procedures.

To illustrate this, the examples shown in Section 5.6 and 5.7 will be used. Load the Linear polarization procedure in the Setup view and add the MASS command to the procedure, between the Optimize current range command and the LSV staircase command. Adjust the parameters of the synchronization command as shown in Figure 65.


Export this modified procedure to a convenient location, using the Export procedure option in the File menu (see Figure 66).

Note

If the number of instruments involved in the Multi Autolab measurement is larger than the number of instruments specified in the Multi Autolab software synchronization command, the synchronization will be triggered as soon as the number of instruments specified in the command is reached.

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Figure 66 – Export the modified Linear polarization procedure

Load the Autolab cyclic voltammetry potentiostatic procedure in the procedure editor. Change the i vs E plot location from plot #1 to plot #2, as shown in Figure 51, to avoid plotting data from different experiments on the same plot.

Add the Multi Autolab software synchronization command to the procedure, between the Optimize current range command and the CV staircase command. Adjust the parameters of the command as shown in Figure 67.

Figure 67 – Adding the synchronization command to the Cyclic voltammetry potentiostatic procedure


Note

The Multi Autolab software synchronization command parameters are identical in the two procedures (see Figure 65 and Figure 67).

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Both methods will yield exactly the same result. The first instrument to reach the Multi Autolab software synchronization command will hold until the other instrument reaches this command. This will force the Cyclic voltammetry procedure to hold until the OCP determination running on Instrument 1 is finished. In the example shown Figure 56, the Cyclic voltammetry measurement started while the OCP measurement was still running on Instrument 1. This does not happen in this example because both instruments are synchronized before the CV staircase command (for Instrument 2) and the LSV staircase command (for Instrument 1).

Note

Make sure that the location of the procedure used for Instrument 1 corresponds to the location of the modified Linear polarization procedure specified in Figure 66.

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Figure 69 – A Multi Autolab measurement example (plot#1 log(i) vs E: red line plot, Linear polarization experiment on Instrument 1 (MAC80007#1) / plot #2 i vs E: blue line plot, Cyclic


Note

While holding at the synchronization point, no hardware settings are modified on instruments. In this example, the OCP determination command included in the Linear polarization procedure will delay Instrument 1 with respect to Instrument 2. Since the synchronization point is defined before the CV staircase command, the second instrument will wait with the cell ON and 0 V applied on the working electrode, until the first instrument reaches the synchronization point.

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6.2 – The Multi Autolab hardware synchronization command

Using the Multi Autolab hardware synchronization command located in the Measurement – general group of commands, one or more synchronization points can be added to any procedure in order to force two or more M101 or M204 modules located inside the same Multi Autolab instrument to synchronize (see Figure 70).

Figure 70 – The Multi Autolab software synchronization command is available in the Measurement – general group

The Multi Autolab hardware synchronization command (MAHS), can be added anywhere in a procedure to introduce a synchronization point for Multi Autolab measurements. Figure 71 shows an example of the use of the MAHS command in the Cyclic voltammetry potentiostatic procedure. In this example, the synchronization command has been inserted between the Optimize current range command and the CV staircase command.

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Figure 71 – Adding the Multi Autolab hardware synchronization command to the Cyclic voltammetry potentiostatic procedure

The MAHS command has the following parameters:

• React on Stop or Skip (Yes/No): specifies if the synchronization can be stopped by the user during a Multi Autolab measurement.

• Time limit (s): defines a time limit for the synchronization command. • Abort procedure after time limit (Yes/No): forces the procedure to stop

when the Time limit is reached and the Use time limit check is on.

The MAHS command can be used in two different situations:

• In the same procedure: this applies to the Multi Autolab use explained in the Section 5.4 and 5.5. In this case, the instruments involved in the measurement are running the same procedure, in which case the MAHS command is automatically included in each procedure.

• In different procedures: this applies to the Multi Autolab use explained in the Section 5.6 and 5.7. In this case, the instruments involved in the measurement are running different procedures, in which case the MAHS command must be added to all the procedures used in the experiment.

Warning

The timing accuracy of the Multi Autolab hardware synchronization command depends on the setting defined for the React on Stop or Skip parameter.

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6.2.1 – Synchronization from the same procedure

When the Multi Autolab view is used to perform the same procedure on more than one instrument, the MAHS command can be used to force the instruments to synchronize at a given point in the procedure.

To illustrate this, the examples shown in Section 5.4 and 5.5 will be used. Load the Cyclic voltammetry procedure in the Setup view and add the MAHS command to the procedure, between the Optimize current range command and the CV staircase command and adjust the parameters of the synchronization command as shown in Figure 72.


To allow the M101 or M204 modules to synchronize, one additional parameter must be set in the Autolab control command. Click the button located next to this command in the procedure editor, as shown in Figure 73.

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Figure 73 – Adjusting the Autolab control command

In the Autolab control window, locate the Synchronization line property in the advanced options and set it to On status using the switch, as shown in Figure 74.

Figure 74 – Setting the Synchronization line for the M101 or M204 module

Note

The hardware synchronization resets the synchronization bit to the Off status after synchronization has occurred. If several synchronization are included in the procedure, the Synchronization bit status must be set to On status before each MAHS command.

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Expand the CV staircase command in the procedure editor and add a ivs t plot command to it. Change the plot location of the i vs t plot to plot #2 using the dropdown list (see Figure 75).

Figure 75 – Adding a i vs t plot to the procedure


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Both methods will yield exactly the same result. The first instrument to reach the Multi Autolab hardware synchronization command will hold until the other instrument reaches this command or until the time limit is reached. This will force the CV staircase command to be executed on both instruments at the same time, unless the time limit is reached.


Note

While holding at the synchronization point, no hardware settings are modified on instruments. In this example, the synchronization point is defined before the CV staircase command, which means that the instruments reaching the synchronization point will hold with the cell ON and 0 V applied on the working electrode, until all the required instruments reach this point or until the Time limit is reached, if applicable.

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Figure 77 – A Multi Autolab measurement example using the Multi Autolab hardware synchronization command (plot#1 i vs E: red line plot, MAC80007#1 (Channel 1); blue line

plot, MAC80007#2 (Channel 2) / plot #2 i vs t: red line plot, MAC80007#1 (Channel 1); blue line plot, MAC80007#2 (Channel 2)

Plot #1 and plot #2 show the i vs E and i vs t, respectively, for both instruments. The Y axis locations, labels and plot options have been defined in the Multi Autolab view, through the Plot Options. The signals to plot and the plot locations have been defined in the Autolab Cyclic voltammetry potentiostatic procedure, which was modified for this example. Instrument 1, MAC80007#1 is connected to the Autolab dummy cell (c) while Instrument 2, MAC80007#2 is connected to dummy cell (e).

The measurements are now synchronized.

It is possible to add more than one Multi Autolab hardware synchronization command to a procedure. However, the synchronization bit must be reset to On using the Autolab control command before each MAHS command.

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6.2.2 – Synchronization from the different procedures

When the Multi Autolab view is used to perform the different procedures on two or more instruments, the Multi Autolab hardware synchronization command can be used to force the instruments to synchronize at matching points in the procedures.

To illustrate this, the examples shown in Section 5.6 and 5.7 will be used. Load the Linear polarization procedure in the Setup view and add the MAHS command to the procedure, between the Optimize current range command and the LSV staircase command. Adjust the parameters of the synchronization command as shown in Figure 78.


Export this modified procedure to a convenient location, using the Export procedure option in the File menu (see Figure 79).

Figure 79 – Export the modified Linear polarization procedure

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Load the Autolab cyclic voltammetry potentiostatic procedure in the procedure editor. Change the i vs E plot location from plot #1 to plot #2, as shown in Figure 80, to avoid plotting data from different experiments on the same plot.

Figure 80 – Adjusting the plot settings for Cyclic voltammetry potentiostatic procedure

Add the Multi Autolab hardware synchronization command to the procedure, between the Optimize current range command and the CV staircase command. Adjust the parameters of the command as shown in Figure 81.

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Figure 81 – Adding the synchronization command to the Cyclic voltammetry potentiostatic procedure



Note

The Multi Autolab hardware synchronization command parameters are identical in the two procedures (see Figure 78 and Figure 81).

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Both methods will yield exactly the same result. The first instrument to reach the Multi Autolab hardware synchronization command will hold until the other instrument reaches this command or until the time limit is reached. This will force the Cyclic voltammetry procedure to hold until the OCP determination running on Instrument 1 is finished. In the example shown Figure 56, the Cyclic voltammetry measurement started while the OCP measurement was still running on Instrument 1. This does not happen in this example because both instruments are synchronized before the CV staircase command (for Instrument 2) and the LSV staircase command (for Instrument 1).


Note

Make sure that the location of the procedure used for Instrument 1 corresponds to the location of the modified Linear polarization procedure specified in Figure 79.

Note

While holding at the synchronization point, no hardware settings are modified on instruments. In this example, the OCP determination command included in the Linear polarization procedure will delay Instrument 1 with respect to Instrument 2. Since the synchronization point is defined before the CV staircase command, the second instrument will wait with the cell ON and 0 V applied on the working electrode, until the first instrument reaches the synchronization point or until the time limit is reached.

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Figure 83 – A Multi Autolab measurement example (plot#1 log(i) vs E: red line plot, Linear polarization experiment on Instrument 1 (MAC80007#1) / plot #2 i vs E: blue line plot, Cyclic


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Documents

Multi Autolab Tutorial - Metrohm Autolab · NOVA Multi Autolab tutorial . Figure 7 – Adjusting the hardware setup of the M101 or M204 modules installed in the Multi Autolab cabinet