External Potentiostats Installation & Operation Manual PP201/211/241 XPOT 07/2013 External Potentiostats -1- CAUTION Prevent the inputs of the device from electrostatic discharge ! This may damage the device. Do not connect active objects such as batteries or fuel cells to the power outputs of the device when the device is off ! This may damage the device. External Potentiostats -2- Unpacking Zahner products are produced carefully, calibrated and tested to achieve a high quality standard. Also the assembling of the accessories and packing is done with great care. Therefore please check the shipment directly after receipt whether the device and all accessories are undamaged. The shipment must contain the following parts: XPOT • • • • • • • XPOT cable for connection of the EPC40/41/42 (Lemosa - Lemosa) cable for connection of a PC USB port (USB-A – D-Sub9) with build-in USB-serial converter 3 cables (red, black, blue) BNC – banana sense cable BNC (green marked) – banana (shielded) power cord this manual PP201/211/241 • • • • • • • PP201/211/241 cable for connection of the EPC40/41/42 (D-Sub9 - Lemosa) cable for connection of a PC USB port (USB-A – D-Sub9) with build-in USB-serial converter 2 cables (red and black) with banana plugs (∅ 4mm) and alligator clips twisted sense cable (Lemosa plug, blue & green cables) power cord this manual -3- External Potentiostats Basics Today, dynamic measurements on electrochemical objects are of great interest. Modern instruments for impedance measurements, cyclic voltammograms and pulse response experiments provide a broad frequency range from µHz to MHz. At the same time, they provide a huge impedance range from µΩ to GΩ. Anyway: for most instruments there is one restriction left, they have a limited current range in the magnitude of some Amperes maximum. In the field of electrochemical power generation for example this is only sufficient for 'small' systems. The electrochemical workstations of the IM6 family provide a current range of ±2,5A (Zennium) and ±3A (IM6) and measure impedances down to some µΩ. Therefore we provide external potentiostats (EL, PP-Series and XPOT) which can extend the application field of the IM system. The four quadrant power potentiostats PP201/211/241 provides up to ±40A (PP241) or up to ±20V (PP211). These devices are designed to do charging/discharging experiments. The XPOT is an external potentiostat for up to ±500mA and ±10V (±25V compliance voltage) used e.g. for disk/ring electrode experiments, multi-cell experiments and light source supply for CIMPS. The external potentiostats are easily integrated in the IM6/Zennium system using EPC40/41/42 controller cards. All functions are controlled directly from the Thales software. Up to 16 external potentiostats may be controlled by one IM6/Zennium system using up to 4 EPC40/41/42 cards. With the MultiCell functionality of the IM systems the connected external potentiostats can be used in parallel. Up to 16 cells may be investigated at the same time. EPC4 / EPC40 / EPC41 / EPC42 The EPC40/41/42 is able to control up to 4 external potentiostats like the EL101/EL300/EL1000, the XPOT and the PP201/211/241. Up to four EPC40/41/42 for a total of 16 external devices can be installed in an IM6 and the Zennium systems. Each port provides analogue and digital interfaces for the communication of the external device with the IM system. The analogue part of the port feeds the device with the DC potential and the AC amplitude at a resolution of 16 bit. Measured current and potential are sent from the external device to the IM to be treated there in the same way as signals from the internal IM cards. The EPC40/41/42 has a bandwidth of 250 kHz. A bi-directional serial communication line allows to digitally control the external potentiostat functions and measuring ranges. ® The XPOT and PP-Series potentiostats can be controlled by a Windows -PC. In this case they provide ® the methods Test Sampling as well as U- and I-curves vs. time. They also work as a LabView Virtual ® Instrument under the LabView software. Furthermore, you can control the XPOT and PP-Series potentiostats in a mixed mode with an IM6/Zennium and a PC in parallel. Both devices can be connected and disconnected in operation. ! Plug or unplug external devices only when both, IM6/Zennium AND the external device, are switched off. Otherwise the devices may be damaged. Selecting an external device All external IM devices are directly controlled by the Thales software. Each device has a unique device number which is identical with the EPC40/41/42 port number. So, if a device is connected to EPC port 3, you address it with the device number 3. Device number '0' is reserved for the internal potentiostats of the IM system. External Potentiostats -4- If an RMUX (relay multiplexer) card is installed, the device numbers of the XPOTs start with 17, not with 1, because the device numbers 1 to 16 are reserved for the 16 RMUX channels then. To select a device, call the Test Sampling page and click one the # symbol next to the Device Identity box. Device Main # An input box will appear where you can input the device number. Potentiostat Number: 1 Now the selected device type is shown in the Device Identity box, for example: Device EL300#1 • • • # If no device has been connected to the addressed EPC40/41/42 port an error message is displayed and the software automatically selects the internal potentiostat. If the selected device is present but has not been activated yet the software starts to calibrate it automatically. If an external device is changed the new device has to be calibrated before use. The calibration is carried out only for the selected device. All other calibration data keep unchanged. If a device number other than 0 is selected, the parameters of the Test Sampling page now are valid for this device. The following methods are available for external devices: EIS impedance measurement C/E parameter impedance measurement I/E current potential curve recording MIE Multiple parallel current potential curve recording POL polarisation measurements C/V cyclic voltammetry AS series measurements Specific parameters for these methods are to be edited in the pages related to the method. Changing devices When changing the device number, the now inactive device will hold its DC conditions such as DC potential and on/off status as long as it is selected anew or the system is shut off. On the other hand only the selected device is internally connected to the FRA. Therefore only this device is able to output an AC signal superimposed to the DC potential. External Potentiostats -5- PP201 / PP211 / PP241 The PP201/211/241 are external Four-Quadrant-Potentiostats. This means that they are able to sink and source current up to 20/10/40 A continuously, both positive and negative. Typical applications are charging/discharging experiments at batteries, accumulators and fuel cells. The PP201/211/241 potentiostats can be operated in both potentiostatic and galvanostatic modes, controlled by the Thales software. The output as well as the input are electrically isolated up to a maximum difference potential against ground of ±12V. Measuring floating objects On the rear of the PP201/211/241 you will find two connectors with a jumper. If the jumper is set, the signal ground is connected to ground via a 100 Ω protective resistor. In contrary to the IM potentiostat (single output stage) the PP (bridge output stage) working electrode is NOT connected to signal ground. This is necessary, if the test object is floating (no metallic or electrolytic contact to ground). If any part of the cell is grounded, the jumper must be removed. silver banana jack (protective ground) ⇔ black banana jack (system ground) ! When investigating floating objects the jumper must be set. Stand-alone mode Besides the usage of the PP201/211/241 as an external potentiostat for an IM6/Zennium system, they also may be used in a stand-alone mode. The setup is done through an IM system or a PC. Cell Connections As its functionality is identical with the main potentiostat, the meaning of the cell connections colours are the same at both devices. In order to minimize stray- and mutual inductance the power lines should be twisted. Normally the PP201/211/241 should only be connected or disconnected to the IM system if both, the IM6/Zennium and the PP201/211/241 are switched off. If you want to use the PP201/211/241 as a stand-alone device, unselect it in the Test Sampling page of the Thales software (you may e.g. change the device number to the main potentiostat). Now you may unplug the PP201/211/241 at the EPC40/41/42 connector. For regaining access to the PP201/211/241, connect it to the EPC40/41/42 and select it in the Test Sampling page of the Thales software. ! Never plug or unplug a PP201/211/241 at the D-Sub9 connector at the backside of the device with the IM switched on. This may damage the system. It is recommended to fix the D-Sub9 connector with the screws to prevent accidental unplugging. External Potentiostats -6- If the PP201/211/241 are unplugged while being selected in the Test Sampling page of the Thales software, it will shut off the current. This is a precaution to prevent undefined situations. The PP201/211/241 need a warm-up time of about 15 minutes after power on. A calibration procedure is initiated automatically with the first access by the IM system. If you access a PP201/211/241 during the warm-up time, please do a forced calibration (EIS menu -> Calibrate) after about 15 minutes. As the PP201/211/241 are optimised for high current (some 100 mA to 20 A) an erroneous current display of some µA is acceptable. Never have a battery connected to the PP when the PP is switched off. This may damage the PP. ! 1. Full Cell Configuration (Standard Kelvin Scheme) PP200 PP200 PP200 PP200 PP200 PP200 pot on power RE sense counter electrode test electrode power TE PP201 PP200 ZAHNER elektrik This configuration is used if complete cell is to be investigated. a Temp (H 2 O) H2 H2 O2 2.a. Half Cell Configuration – Anode PP200 PP200 PP200 PP200 PP200 PP200 pot on power RE sense counter electrode test electrode power TE PP201 PP200 ZAHNER elektrik This configuration is used if the anodic part of the cell is to be investigated. (H 2 O) H Ref2 H2 O2 2 External Potentiostats -7- 2.b. Half Cell Configuration – Cathode PP200 PP200 PP200 PP200 PP200 PP200 pot on power RE sense counter electrode test electrode power TE PP201 PP200 ZAHNER elektrik This configuration is used if the cathodic part of the cell is to be investigated. (H 2 O) H Ref1 2 H2 O2 3. Partial Cell Configuration PP200 PP200 PP200 PP200 PP200 PP200 pot on power RE sense counter electrode test electrode power TE PP201 PP200 ZAHNER elektrik This configuration may be used, if a certain part of a battery or fuel cell stack has to be investigated. (H 2 O) H2 Ref1 Ref2 H2 O2 External Potentiostats -8- XPOT XPOT is a low power 4-quadrant potentiostat which may be used in connection with the impedance spectrometer IM6/Zennium. Using the XPOT allows parallel investigation of different objects. In such multi-cell arrangements, potentiostats which are not addressed, will hold their DC-conditions. XPOT provides a maximum current of ±500mA and a maximum potential of ±10V at a maximum frequency bandwidth of 100kHz. The compliance voltage is ±25 V. Connectors & LEDs Active LED green = XPOT connected to IM system orange = potentiostat on Probe I & E connectors BNC Cell Connectors BNC plugs for connecting the cell: Red = counter electrode Green = reference electrode Black = test (working) electrode Blue = test (working) sense electrode The shields of the BNC connectors are connected to the test electrode (virtual ground) via a 2.2kΩ Ω resistor. ! The Probe I connector of the XPot is different from the Probe I connector of the IM6/Zennium. It is used for special XPot extensions such as CIMPS. Do not connect a UBuffer or a HiZ probe here. Use of the built-in buffer The built-in buffer amplifier may be used to increase the dynamic range of the XPOT up to +/-10V. To select the buffer amplifier mode, call the Check Cell Connections page of the Thales software, select any connection scheme with buffer and set the corresponding gain factor: gain factor output potential range 1 -4V M +4V 0.4 -10 M +10V Measuring floating objects Floating and ground referenced objects demand different connections to the potentiostat. Usually, the ground of the XPOT will be connected to the system ground at its rear panel: silver banana jack (protective ground) ⇔ black banana jack (system ground) ! When investigating floating objects the jumper must be set. -9- External Potentiostats Specifications PP201 PP211 PP241 XPOT pot/gal pot/gal pot/gal pot/gal ±4V / ±10V ±4V / ±20V ±4V / ±5V ±4V / ±10V Pot. accuracy ±0.1% / ±1mV ±0.1% / ±1mV ±0.1% / ±1mV ±0.1% / ±1mV Current range 0A M ±20A 0A M ±10A 0A M ±40A ±10nA - ±500mA Current accuracy 0.25% / ±1mA 0.25% / ±2mA 0.25% / ±1mA 0.2% / ±100pA Power dissipation 250W @ Ta 250W @ Ta 250W @ Ta 30W @ Ta Output power 200W @ Ta 200W @ Ta 200W @ Ta 12W @ Ta Frequency range 10µHz - 200kHz 10µHz – 200kHz 10µHz – 200kHz 10µHz – 200kHz Impedance range 1µΩ - 1kΩ Amb. temperature 0 C M 30 C IM6/Zennium + EPC42 or PC Operating modes Potential range * System requirements o ** o ** 0.1Ω - 1GΩ 0 C M 30 C 0 C M 30 C 0 C M 25 C IM6/Zennium + EPC42 or PC IM6/Zennium + EPC42 or PC IM6/Zennium + EPC42 or PC 1µΩ - 1kΩ o * ** o 1µΩ - 1kΩ o o o o Please note that the maximum frequency range only can be achieved with an IM6 or an Zennium equipped with EPC41 or EPC42. With an IM5d the maximum frequency range of external devices is 30kHz. ** Impedances below 1mΩ must be measured galvanostatically.
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