NOVA MUX Tutorial Version 1.11.0 NOVA MUX tutorial 1 – The MUX module The MUX is an optional module for the Autolab PGSTAT and the Multi Autolab. With the MUX module, it is possible to multiplex the PGSTAT electrode connections 1. Depending on the type of MUX used, measurements on several electrochemical cells or working electrodes can be done sequentially. The MUX module is available in three standard configurations: • MUX-MULTI4: in this configuration, the WE, S, RE and CE leads from the PGSTAT are multiplexed to 4 (or more) sets of connections (see Figure 1). This means that sequential measurements can be performed on multiple independent electrochemical cells. It is possible to add up to 16 MUXMULTI4 boxes in series in order to multiplex up to 64 independent electrochemical cells. WE1 WE2 WE3 WE4 S1 S2 S3 S4 CE1 CE2 CE3 CE4 RE1 RE2 RE3 RE4 MULTI4 Figure 1 – The MUX-MULTI4 box Note The MUX-MULTI4 is typically used for sequential measurements on individual electrochemical cells or for measurements requiring different electrode arrangements in the same cell (like Van der Pauw measurements). • MUX-SCNR8: in this configuration, the RE and S leads from the PGSTAT are multiplexed to 8 (or more) sets of connections (see Figure 2). This means that the differential amplifier of the PGSTAT can be multiplexed across as many While the MUX module has been designed to multiplex the connections provided by the Autolab PGSTAT, it can be used to multiplex other connections (like the pX module input for example). 1 2|Page NOVA MUX tutorial individual cells. It is possible to add up to 16 MUX-SCNR8 boxes in series in order to multiplex up to 128 sets of RE and S electrodes. RE1 RE2 RE3 RE4 S1 S2 S3 S4 RE5 RE6 RE7 RE8 S5 S6 S7 S8 SCNR8 Figure 2 – The MUX-SCNR8 box Note The MUX-SCNR8 is intended to be used for measurements on individual cells in a series of cells. The most common example is the measurement of cell voltages of individual cells or sections of cells in a fuel cell stack. • MUX-SCNR16: in this configuration, the WE lead from the PGSTAT is multiplexed to 16 (or more) WE connections (see Figure 3). This means that sequential measurements can be performed on multiple working electrodes sharing a common reference electrode and counter electrode. It is possible to add up to 16 MUX-SCNR16 boxes in series in order to multiplex up to 255 working electrodes. 3|Page NOVA MUX tutorial WE1 WE2 WE3 WE4 WE5 WE6 WE7 WE8 WE9 WE10 WE11 WE12 WE13 WE14 WE15 WE16 SCNR16 Figure 3 – The MUX-SCNR16 box Note The MUX-SCNR16 is intended to be used for measurements on individual working electrodes contained in a single electrochemical cell. Corrosion and sensor measurements usually benefit from this hardware extension. The MUX boxes can be connected in series up to a maximum of 16 boxes, as shown in Figure 4. To MUX module in PGSTAT WE1 WE2 WE3 WE4 WE1 WE2 WE3 WE4 WE1 WE2 WE3 S1 S2 S3 S4 S1 S2 S3 S4 S1 S2 S3 S4 CE1 CE2 CE3 CE4 CE1 CE2 CE3 CE4 CE1 CE2 CE3 CE4 RE1 RE2 RE3 RE4 RE1 RE2 RE3 RE4 RE1 RE2 RE3 RE4 MULTI4 MULTI4 Channels 1-4 (MULTI4) Channels 1-8 (SCNR8) Channels 1-16 (SCNR16) MULTI4 Channels 5-8 (MULTI4) Channels 9-16 (SCNR8) Channels 17-32 (SCNR16) To Cell cables PGSTAT (RE, S, WE and CE for MULTI4) (WE/S for SCNR16, RE/S for SCNR8) Figure 4 – Up to 16 MUX boxes can be connected in series Note The MUX boxes must all be of the same type. 4|Page Additional channels WE4 NOVA MUX tutorial Scope of the tutorial The aim of this tutorial is to explain how to use the MUX module to multiplex the connections provided by the Autolab. The use of the manual control and automatic control of the MUX is illustrated using the dummy cell. At any time, one of the available MUX channels can be activated manually or automatically in the software. The MUX can be used for all electrochemical techniques. Caution The MUX modules cannot be used in combination with the Autolab PGSTAT100N or PGSTAT100 and the PGSTAT302F. It is also not possible to use the MUX modules in combination with the Booster10A or the Booster20A. 2 – Hardware setup In order to use the MUX module, the hardware setup in NOVA must be configured accordingly (see Figure 5). Figure 5 – Selecting the MUX module 5|Page NOVA MUX tutorial The number of available channels can be defined in the frame on the right-hand side of the hardware setup window (see Figure 5). This value corresponds to the maximum number of channels available for instrument. 3 – Manual control of the MUX module The MUX module can be controlled manually at any time, using a dedicated panel of the Autolab display. To add the MUX manual control panel to the Autolab display, select the MUX manual control option from the View menu (see Figure 6). Figure 6 – Select the MUX manual control option from the View menu to add the MUX control panel to the Autolab display The MUX manual control panel will be shown whenever the Autolab display is displayed (see Figure 7). Select the Autolab display option from the View menu or press the F10 shortcut key to show the Autolab display. 6|Page NOVA MUX tutorial Figure 7 – The MUX manual control panel The MUX manual control can be used to set the active channel of the MUX. It also displays the currently active channel. In Figure 7, the active channel is 1 and a total of 4 channels are available. The number of available channels depends on the hardware setup. Figure 7 corresponds to the hardware setup shown in Figure 5. Note When the active channel is set to 0, none of the MUX channels are used. Using the manual control, it is possible to switch to any of the available channels by typing the corresponding value in the Select [0..X] field 2 and pressing the button (see Figure 8). Alternatively, the buttons can be used to increase or decrease the channel number. 2 X is the number of available channels – see hardware setup. 7|Page NOVA MUX tutorial Figure 8 – Switching MUX channels Note The new channel is activated as soon as the button is clicked. 4 – Automatic control of the MUX module Control of the MUX module during a measurement is also possible using the Autolab control command. The channel number control of the MUX module is available in the Autolab control window, on the MUX section (see Figure 9). 8|Page NOVA MUX tutorial Figure 9 – The Autolab control window can be used to control the MUX channel The Autolab control can be used at any time during a measurement to change the MUX channel automatically. The selected MUX channel is shown in the procedure editor, below the Autolab control command used to define its value (see Figure 10). Figure 10 – The selected MUX channel is displayed below the Autolab control The MUX(1).Channel parameter shown below the Autolab control command in the procedure editor can also be linked to other parameters, like an input box command or a repeat for each value loop. 9|Page NOVA MUX tutorial 5 – Measurements with the MUX module on the dummy cell A MUX tutorial folder is located in the Program Files\Metrohm Autolab\Nova 1.11\Shared Databases\Tutorials folder (see Figure 11). Using the database manager, set this folder as the Standard database. Figure 11 – Loading the MUX tutorial database The MUX tutorial contains three procedures (see Figure 12). Both procedures illustrate the use of the Autolab control command to switch MUX channels during a measurement. These procedures are to be used on the Autolab dummy cell. Figure 12 – The two MUX tutorial procedures Depending on the hardware configuration, the connection between the MUX and the dummy cell should be as displayed in Figure 13 for the MUX-MULTI4 configuration, in Figure 14 for the MUX-SCRN8 or as in Figure 15 for the MUXSCNR16. 10 | P a g e NOVA MUX tutorial C1 1µF R2 CE WE(+S) (a) R4 100Ω 1MΩ CE1 CE2 C2 1µF R1 RE R3 100Ω S1 WE2 S2 1MΩ R7 10kΩ RE1 RE2 WE1 WE(+S) (b) 1µF C3 WE(+S) (e) R5 WE(+S) (c) 1kΩ C4 R6 1µF 5kΩ WE(+S) (d) DUMMY CELL2 Figure 13 – Overview of the connections to the dummy cell when using the MUX-MULTI4 C1 1µF R2 CE 100Ω WE(+S) (a) R4 1MΩ CE C2 RE 100Ω RE2 R7 10kΩ RE1 S1 S2 WE(+S) (b) R3 1MΩ C3 WE(+S) (e) WE 1µF R1 R5 1µF WE(+S) (c) 1kΩ C4 R6 1µF 5kΩ WE(+S) (d) DUMMY CELL2 Figure 14 – Overview of the connections to the dummy cell when using the MUX-SCNR8 11 | P a g e NOVA MUX tutorial C1 1µF R2 CE 100Ω WE(+S) (a) R4 1MΩ CE C2 100Ω R7 10kΩ RE WE(+S) (b) R3 1MΩ C3 WE(+S) (e) WE1 1µF R1 RE R5 1µF WE(+S) (c) 1kΩ WE2 C4 R6 1µF 5kΩ WE(+S) (d) DUMMY CELL2 Figure 15 – Overview of the connections to the dummy cell when using the MUX-SCNR16 Note In the SCNR16 connect both the WE and the S from the PGSTAT to the WE input of the SCNR16. 5.1 – MUX tutorial 1 – Control of the MUX through an Input box Load the MUX tutorial 1 procedure. Figure 16 shows an overview of the procedure. An Input box is located in between the two Timed procedure commands. The value of the input is linked to the MUX(1).Channel parameter located in the Autolab control command. 12 | P a g e NOVA MUX tutorial Figure 16 – The MUX tutorial 1 procedure Connect the MUX to the dummy cell according to one of the schemes shown in Figure 13 or Figure 15 and press the Start button. A message box will be displayed at the beginning of the experiment (see Figure 17). Figure 17 – A message box is displayed at the beginning of the measurement Click the OK button to continue. A cyclic voltammetry measurement will be performed on the channel 1 of the MUX. During this experiment, the data is displayed on plot number 1 in the measurement view (see Figure 18). 13 | P a g e NOVA MUX tutorial Figure 18 – MUX tutorial measured data part 1 – MUX Channel 1 data on plot #1 At the end of the first measurement, an input box will be displayed (see Figure 19). This input box can be used to set the next value of the MUX channel. For this tutorial procedure, the value should be 2. Figure 19 – An input box is displayed at the end of the first measurement Click OK to continue. The MUX will be switched to channel 2 and the same measurement will be repeated. The data is plotted on plot number 2 in the measurement view (see Figure 20). Note Switch the measurement view to Two plots vertically tiled mode by pressing the button in the toolbar. Note The data shown in Figure 20 corresponds to the data obtained with the MUXMULTI4 or the MUX-SCNR16. 14 | P a g e NOVA MUX tutorial Figure 20 – MUX tutorial measured data part 2 – MUX Channel 1 data on plot #1 (blue curve) and MUX Channel 2 data on plot #2 (red curve) The measured data depends on the hardware configuration. • • MUX-MULTI4 or MUX-SCNR16: Since MUX Channel 1 is connected to dummy cell (a) and MUX Channel 2 is connected to dummy cell (c), the WE(1).Current values vary between ± 1 µA and ± 0.9 mA, respectively. MUX-SCNR8: Since MUX Channel 1 and 2 are connected to dummy cell (a) the WE(1).Current values vary between ± 1 µA on both plots. 5.2 – MUX tutorial 2 – Control of the MUX through the Autolab control command Load the MUX tutorial 2 procedure. Figure 21 shows an overview of the procedure. At the beginning of the experiment, an Autolab control command is used to set the MUX channel to 1. An additional Autolab control is used to switch from channel 1 to channel 2 after the first measurement. Figure 21 – The MUX tutorial 2 procedure 15 | P a g e NOVA MUX tutorial Connect the MUX to the dummy cell according to one of the schemes shown in Figure 13 or Figure 15 and press the Start button. A message box will be displayed at the beginning of the experiment (see Figure 22). Figure 22 – A message box is displayed at the beginning of the measurement Click the OK button to continue. A cyclic voltammetry measurement will be performed on the channel 1 of the MUX. During this experiment, the data is displayed on plot number 1 in the measurement view (see Figure 23). Figure 23 – MUX tutorial measured data part 1 – MUX Channel 1 data on plot #1 At the end of the first measurement, the MUX will switch the active channel to channel 2 automatically. The same measurement will be repeated and the data is plotted on plot number 2 in the measurement view (see Figure 24). Note The data shown in Figure 24 corresponds to the data obtained with the MUXMULTI4 or the MUX-SCNR16. 16 | P a g e NOVA MUX tutorial Figure 24 – MUX tutorial measured data part 2 – MUX Channel 1 data on plot #1 (blue curve) and MUX Channel 2 data on plot #2 (red curve) The measured data depends on the hardware configuration. • • MUX-MULTI4 or MUX-SCNR16: Since MUX Channel 1 is connected to dummy cell (a) and MUX Channel 2 is connected to dummy cell (c), the WE(1).Current values vary between ± 1 µA and ± 0.9 mA, respectively. MUX-SCNR8: Since MUX Channel 1 and 2 are connected to dummy cell (a) the WE(1).Current values vary between ± 1 µA on both plots. 5.3 – MUX tutorial 3 – Control of the MUX through the Repeat for each value command Load the MUX tutorial 3 procedure. Figure 25 shows an overview of the procedure. The measurement is now located inside a Repeat for each value command. The values defined in the repeat loop are linked to the MUX channel in the Autolab control command. The measurement is first performed on channel 1 and then on channel 2. Figure 25 – The MUX tutorial 3 procedure 17 | P a g e NOVA MUX tutorial Connect the MUX to the dummy cell according to one of the schemes shown in Figure 13 or Figure 15 and press the Start button. A message box will be displayed at the beginning of the experiment (see Figure 26). Figure 26 – A message box is displayed at the beginning of the measurement Click the OK button to continue. A cyclic voltammetry measurement will be performed on the channel 1 of the MUX. When the measurement is finished, the cell is switched off, and channel 2 is selected. The same experiment is repeated. The data is plotted on plot number 1 in the measurement view (see Figure 27). Note The data shown in Figure 27 corresponds to the data obtained with the MUXMULTI4 or the MUX-SCNR16. Figure 27 – MUX tutorial measured data 18 | P a g e NOVA MUX tutorial The measured data depends on the hardware configuration. • • MUX-MULTI4 or MUX-SCNR16: Since MUX Channel 1 is connected to dummy cell (a) and MUX Channel 2 is connected to dummy cell (c), the WE(1).Current values vary between ± 1 µA and ± 0.9 mA, respectively. MUX-SCNR8: Since MUX Channel 1 and 2 are connected to dummy cell (a) the WE(1).Current values vary between ± 1 µA on both plots. Both cyclic voltammograms are shown on the same plot. 19 | P a g e NOVA MUX tutorial Hardware specifications The MUX module is available in three versions: • • • MUX-MULTI4: can be used to multiplex all four electrodes provided by the Autolab: CE, RE, S and WE. Using this module, it is possible to work on different electrochemical cells, sequentially. MUX-SCNR8: can be used to multiplex two independent electrodes provided by the Autolab. The most common use of this special module is to multiplex the S and RE connection from the differential amplifier in order to measure the potential difference across several electrochemical interfaces, sequentially. MUX-SCNR16: can be used to multiplex a single electrode provided by the Autolab. The most common use of this module is to multiplex the S+WE in order to perform electrochemical measurements on different working electrodes located in the same cell, sharing the counter and reference electrode. The measurements are performed sequentially. Table 1 provides an overview of some of the MUX module specifications. Module Number of channels Increment per extension Switching time Maximum current MULTI4 4-64 4 5 ms 2A SCNR16 16-255 16 5 ms 2A SCNR8 8-128 8 5 ms 2A Table 1 – Overview of the specifications of the MUX modules Note Inactive MUX channels are kept at open circuit potential at all times. Caution The MUX modules cannot be used in combination with the Autolab PGSTAT100N or PGSTAT100 and the PGSTAT302F. It is also not possible to use the MUX modules in combination with the Booster10A or the Booster20A. 20 | P a g e