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Gamry Instruments PCI4/300 Potentiostat/Galvanostat/ZRA Operator's Manual

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Summary of Contents for Gamry Instruments PCI4/300 Potentiostat/Galvanostat/ZRA

  • Page 1 sales@artisantg.com artisantg.com (217) 352-9330 | Visit our website - Click HERE...
  • Page 2 PCI4 Potentiostat/Galvanostat/ZRA Operator's Manual includes both the PCI4/300 Potentiostat/Galvanostat/ZRA PCI4/750 Potentiostat/Galvanostat/ZRA Copyright 1997-2011 Gamry Instruments, Inc. All rights reserved. Printed in the USA. Revision 5.2 February 28, 2011...
  • Page 4 Limited Warranty Gamry Instruments, Inc., warrants to the original user of this product that it shall be free of defects resulting from faulty manufacture of the product or its components for a period of two years from the date of shipment.
  • Page 5 Disclaimers Gamry Instruments, Inc., cannot guarantee that the PCI4 Potentiostat will work with all computer systems, operating systems, or third party expansion cards and peripherals. The information in this manual has been carefully checked and is believed to be accurate as of the time of printing.
  • Page 6 (215) 682-9331 Email techsupport@gamry.com Mail Gamry Instruments, Inc. 734 Louis Drive Warminster, PA 18974 If you write to us about a problem, provide as much information as possible. If you are having problems with installation or use of your PCI4 Potentiostat, it would be helpful if you called from a phone near to your computer, where you can type and read the screen while talking to us.
  • Page 8 Table of Contents Limited Warranty ........................ii Disclaimers ..........................iii Copyrights and Trademarks ..................... iii If You Have Problems ......................iv Chapter 1 -- Introduction ......................1-1 About This Manual..................... 1-1 CE Compliance Required for Sale in Europe ............... 1-1 About the PCI4 ......................
  • Page 9 Reference Electrode ..................5-6 Instrument Settings..................5-7 EIS Speed ..................... 5-7 Ancillary Apparatus ..................5-7 Floating Operation ..................... 5-7 Appendix A -- PCI4/300 Specifications ................... 6-1 Appendix B -- PCI4/750 Specifications ................... 6-3 Appendix C -- Changing PCI4 Settings ..................6-5 Overview........................
  • Page 10 This manual does not discuss software installation or operation. Software support for the PCI4 is described in the Gamry’s On-line Help system. All the Gamry Instruments' applications which run under the Gamry Framework control the PCI4 via a PSTAT object. See the Framework’s On-line Help for information concerning PSTAT objects and their functions.
  • Page 11 Chapter 1 -- Introduction -- Potentiostat Schematic Diagram The PCI4/300 and PCI4/750 are two members of Gamry Instruments’ PCI4 Potentiostat family. They share a number of characteristics with the other members of this family, especially in the areas of signal generation and signal preconditioning prior to A/D conversion.
  • Page 12 Chapter 1 -- Introduction -- Potentiostat Schematic Diagram Figure 1-1 PCI4 Analog Circuits in Potentiostat Mode...
  • Page 13 Chapter 1 -- Introduction -- Potentiostat Schematic Diagram A few points concerning this schematic: The circuits on the right side of the schematic are on the Potentiostat card and those on the left are on • the Controller Card. The dotted line shows the separation between the two portions of the instrument.
  • Page 14 In order to make this manual more readable we have adopted some notational conventions. These are used throughout this manual and all other Gamry Instruments manuals. Numbered lists. A numbered list is reserved for step by step procedures, with the steps always •...
  • Page 15 Chapter 1 -- Introduction -- Notational Conventions...
  • Page 16 Chapter 2 -- Installation -- Computer Requirements Chapter 2 -- Installation A PCI4 Potentiostat is only useful after it has been installed in a Windows compatible computer. If you purchase a PCI4 in a system that includes both a computer and an applications software package, Gamry Instruments, Inc.
  • Page 17 Chapter 2 -- Installation -- Multiple Potentiostat Systems Multiple Potentiostat Systems Gamry’s current Framework software (Revision 4.2) allows a computer to operate several Gamry Instruments potentiostats simultaneously. These can include both PCI4 and older PC4 family devices in the same computer.
  • Page 18 Save the anti-static bags. You must use them if the cards are shipped while not installed in a • computer. This includes occasions when the cards must be returned to Gamry Instruments, Inc. for repair. Plug & Play System Configuration The PCI4 Controller Card is completely compatible with the Windows Plug &...
  • Page 19 Chapter 2 -- Installation -- Connecting the Internal Cables Again, remove the retaining screw and slot cover, saving the screw for use later. Remove one card from its anti-static bag. Plug this card into one slot. Make sure the card seats securely in the edge card connector on the motherboard.
  • Page 20 Chapter 2 -- Installation -- Cell Cable Installation Cell Cable Installation The Cell Connector is a 9 pin female D connector on the Potentiostat card. The standard cell cable has a 9 pin D connector on one end and a number of leads terminated with banana plugs on the other.
  • Page 21 These messages will also be seen when a PCI4 family instrument is moved to a new PCI slot. In this case, you can select Install the software automatically even if you do not have the Gamry Instruments CD. The driver that was previously installed on your computer’s hard drive will be used...
  • Page 22 PCI4. If you cannot locate your authorization codes, please contact Gamry Instruments or your local Gamry Sales representative for assistance. To enter an authorization code, simply click on the Add button. A dialog box will appear as shown in Figure 2-5.
  • Page 23 Chapter 2 -- Installation -- Multiple Potentiostat Systems Multiple Potentiostat Systems Gamry’s current Framework software (Revision 5.1) allows a computer to operate up to 16 Gamry Instruments potentiostats simultaneously. The 16 potentiostats can include both PCI4 family devices and the newer PC5 family devices.
  • Page 24 Figure 2-6 Device Manager Window You can now right click on any of the Devices listed under Gamry Instruments and select Properties to look at or change its configuration. Authorization Codes and Label...
  • Page 25 When you are finished making changes press OK to store the changes. Application Software Installation and System Checkout Software installation is slightly different for each Gamry Instruments, Inc. application package. Refer to the software installation instructions in the Installation Manual for each application package in your system.
  • Page 26 Chapter 2 -- Installation -- Calibration Calibration After you have run the system checkout procedure(s), you should calibrate each PCI4 Potentiostat installed in your system. A calibration script is provided with the Gamry Framework. The Installation Manual for every major application package contains instructions for calibration using this script. CAUTION: PCI4 calibration calls for an external resistive dummy cell.
  • Page 27 Chapter 3 -- Cell Cable Connections -- Cell Indicator Chapter 3 -- Cell Cable Connections Cell Indicator The PCI4 is equipped with four LED indicators, located on the Potentiostat card mini-panel. The uppermost, yellow, LED functions as a Cell Indication. It lights whenever the PCI4 cell switch is on and goes dark whenever the cell is at open circuit.
  • Page 28 The alligator clip on a cell connection can be removed to access the underlying banana plug or pin jack. If you need to permanently change the terminations on your cell cable, feel free to remove the banana plugs and replace them with your new termination. Gamry Instruments can provide additional standard or special cell cables.
  • Page 29 Chapter 3 -- Cell Cable Connections -- ZRA Mode Cell Connections ZRA Mode Cell Connections The PC4 can function as a precision Zero Resistance Ammeter (ZRA). It maintains two metal samples at the same potential and measures the current flow between the samples. It can also measure the potential of the samples versus a reference electrode.
  • Page 30 Chapter 3 -- Cell Cable Connections -- Membrane Cell Connections Table 3-3 Cell Cable Connections for a Membrane Cell Color Type Name Normal Connection Blue Banana Plug Working Sense Connect to reference electrode #1 Green Banana Plug Working Electrode Connect to counter electrode #1 White Pin Jack Reference...
  • Page 31 Chapter 4 -- Stability in Potentiostat Mode -- Capacitive Cells and Stability Chapter 4 -- Stability in Potentiostat Mode Capacitive Cells and Stability All potentiostats can become unstable when connected to capacitive cells. The capacitive cell adds phase shift to the potentiostat's feedback signal (which is already phase shifted). The additional phase shift can convert the potentiostat's power amplifier into a power oscillator.
  • Page 32 • I/E converter resistors. These capacitors are connected to relays that are under software control. Contact your local Gamry Instruments' representative for more information concerning changes in these settings. Lower the reference electrode impedance. Make sure that you don't have a clogged reference •...
  • Page 33 Chapter 4 -- Stability in Potentiostat Mode -- Improving Potentiostat Stability Provide a high frequency shunt around the cell. A small capacitor between the red and white cell • leads allows high frequency feedback to bypass the cell. See Figure 4-2. The capacitor value is generally determined by trial and error.
  • Page 34 Chapter 4 -- Stability in Potentiostat Mode -- Improving Potentiostat Stability Add resistance to the counter electrode lead. See Figure 4-3. This change lowers the effective gain • bandwidth product of the control amplifier. As a rule of thumb, the resistor should be selected to give one volt of drop at the highest current expected in the test being run.
  • Page 35 Chapter 5 -- Measurement of Small Signals -- Overview Chapter 5 -- Measurement of Small Signals Overview The PCI4 is a sensitive scientific instrument. It can resolve current changes as small as 0.01 picoamps (10 amps). To place this current in perspective, 0.01 pA represents the flow of about 60,000 electrons per second! The small currents measured by the PCI4 place demands on the instrument, the cell, the cables and the experimenter.
  • Page 36 Chapter 5 -- Measurement of Small Signals -- Measurement System Model and Physical Limitations Figure 5-1 Equivalent Measurement Circuit R shunt C shunt R in C in Unfortunately technology limits high impedance measurements because: Current measurement circuits always have non-zero input capacitance, i.e. C >...
  • Page 37 Chapter 5 -- Measurement of Small Signals -- Measurement System Model and Physical Limitations For purposes of approximation, the Noise bandwidth, δF, is equal to the measurement frequency. Assume a ohm resistor as Z . At 300 K and a measurement frequency of 1 Hz this gives a voltage noise of 41 µV cell rms.
  • Page 38 Chapter 5 -- Measurement of Small Signals -- Measurement System Model and Physical Limitations For an R of 10 ohms, an error < 1% demands that R must be > 10 ohms. PC board leakage, relay leakage, and measurement device characteristics lower R below the desired value of infinity.
  • Page 39 Chapter 5 -- Measurement of Small Signals -- Hints for System and Cell Design are common. This shunt capacitance cannot be distinguished from "real" capacitance in the cell. If you are measuring a paint film with a 100 pF capacitance, 5 pF of shunt capacitance is a very significant error. Shunt resistance in the cell arises because of imperfect insulators.
  • Page 40 IR compensation with cell cables longer than 5 meters. We do not recommend that you use the PCI4 with any cables not supplied by Gamry Instruments. The PCI4 cable is not a simple cable like a typical computer cable. The PCI4 cable includes a number of individually shielded wires contained within an overall shield.
  • Page 41 Chapter 5 -- Measurement of Small Signals -- Floating Operation Reference electrodes often develop high impedances as they see use. Anything that can clog the isolation frit can raise the electrode impedance. Avoid using saturated KCL based references in perchlorate ion solutions Instrument Settings There are several things to remember in setting up a very sensitive experiment.
  • Page 42 Chapter 5 -- Measurement of Small Signals -- Floating Operation...
  • Page 43 Appendix A -- PCI4/300 Specifications -- Appendix A -- PCI4/300 Specifications Control Amplifier Compliance Voltage > ± 20 volts @ 150 mA Output Current > ± 300 mA Unity Gain Bandwidth (software selectable) >1 MHz, > 200 kHz, > 90 kHz, > 20 kHz Slew Rate (software selectable) >50 V/µsec, >...
  • Page 44 Appendix A -- PCI4/300 Specifications -- Auxiliary D/A Output Range ± 5 volts or 0 to 10 volts Resolution 2.5 mV Environmental Operating Temperature 0-70 °C (inside computer) Specification Temperature 25 °C Potentiostat Mode Applied E Range ± 11 volts Accuracy ±...
  • Page 45 Appendix B -- PCI4/750 Specifications -- Appendix B -- PCI4/750 Specifications Control Amplifier Compliance Voltage > ± 15V @ 15 mA, > ± 12 volts @ 500 mA Output Current > ± 750 mA Unity Gain Bandwidth (software selectable) >1 MHz, > 200 kHz, > 90 kHz, > 20 kHz Slew Rate (software selectable) >50 V/µsec, >...
  • Page 46 Appendix B -- PCI4/750 Specifications -- Auxiliary D/A Output Range ± 5 volts or 0 to 10 volts Resolution 2.5 mV Environmental Operating Temperature 0-70 °C (inside computer) Specification Temperature 25 °C Potentiostat Mode Applied E Range ± 11 volts Accuracy ±...
  • Page 47 The Gamry Framework requires a "GAMRY5.INI” file. This file is used to name the potentiostats in the system. Turnkey systems are configured appropriately for the items you have purchased with that system. User installed systems should be configured using the Setup programs that come with Gamry Instruments' Windows based application software.
  • Page 48 The copy of "GAMRY5.INI" actually used by the software must be located in the Windows directory (normally C:\WINDOWS). The Setup programs provided with Gamry Instruments' software either install "GAMRY5.INI" in the correct directory or modify an existing file in this location.
  • Page 49 Appendix C -- Changing PCI4 Settings -- Removing a Potentiostat from an Existing System Figure C-1 Portion of a Typical "GAMRY5.INI" File [Framework5] Version=5.0 SystemDir=C:\Program Files\Gamry Instruments\Framework 5\ ScriptDir=C:\Program Files\Gamry Instruments\Framework 5\Scripts\ PACKAGE0=DC105 [PCI4750-12345] CMSDriver=PCI4.DLL LABVIEWDriver=PCI4LV.DLL BaseAddress= PstatClass=PCI4 FraCurveClass=FRACURVE4 BoardNo=1...
  • Page 50 Appendix C -- Changing PCI4 Settings -- Interrupt Level Setting Most peripheral devices in an AT compatible computer coordinate I/O (input/output) operations with the microprocessor by means of hardware interrupts. An interrupt is a request by a device that the computer suspend the program it's currently running, and perform an I/O operation.
  • Page 51 This shield acts as an extension of the computer’s chassis, keeping the RF emission level lower than the limits in the regulations. Note that use of cell cables not designed and sold by Gamry Instruments can result in excessive RF radiation.
  • Page 52 Appendix D -- I/O Connections for the PCI4 -- The Cell Connector We strongly recommend that you use an earth grounded Faraday shield whenever you are measuring small currents. See Chapter 5 for a discussion of Faraday shields. The Cell Connector The Cell Connector is a 9 pin female D shaped connector on the Potentiostat Card.
  • Page 53 Appendix D -- I/O Connections for the PCI4 -- Aux A/D Input Table D-1 Cell Connector Signal Name Working Sense Normally connected to the working electrode. This is the high impedance negative input of the differential electrometer. A 260 Ω series resistor at the cell end of the coax cable on this input is required for system stability.
  • Page 54 Appendix D -- I/O Connections for the PCI4 -- Control Signal Input Control Signal Input The Control Signal Input allows you to inject a signal into the PCI4's potential or current control circuits. One use for this input is modulation of the applied voltage or current. This input is the upper-middle SMC connector on the Controller Card mini-panel.
  • Page 55 Appendix D -- I/O Connections for the PCI4 -- I Channel Output In controlled potential mode (and ZRA mode), the potential applied to the cell is the sum of the applied potential and the control input voltage. For example, if the programmed voltage is +2 volts, and +1 volt is applied to the control input, the cell voltage (E ) will be +3 volt.
  • Page 56 Appendix D -- I/O Connections for the PCI4 -- Miscellaneous I/O Connector Miscellaneous I/O Connector This connector contains a number of chassis ground related signals. It is the miniature 15 pin female D shaped connector on the PCI4 Controller Card. Be careful, the ground on this connector is not the PCI4 floating ground.
  • Page 57 Appendix E – Auxiliary A/D Input Characteristics -- Overview Appendix E – Auxiliary A/D Input Characteristics Overview The Controller Card used in the Gamry Instruments PCI4 Potentiostat has jumpers that configure the input circuitry used for the Aux A/D function. Jumper Identification The three jumpers that configure the Aux A/D input are in a cluster located at the right side of the Controller Card.
  • Page 58 Appendix E – Auxiliary A/D Input Characteristics -- Filter Selection Filter Selection J602 controls filtering of the Aux A/D input. With J602 removed, there is no filtering on this input. With J602 in place (the default setting), a single pole RC filter is used to limit noise into the A/D. The nominal cutoff frequency of this filter is 20 Hz.
  • Page 59 Appendix F – CE Certificate -- Certificate of Conformance Appendix F – CE Certificate Certificate of Conformance 6-17...
  • Page 60 Appendix F – CE Certificate -- Certificate of Conformance 6-18...
  • Page 61 Comprehensive Index -- green cell lead, 3-2 Comprehensive Index grounds, 6-9 high frequency shunt, 4-3 [Framework5] Section in GAMRY5.INI, 6-6 hints, 5-5 alligator clip, 3-2 I Channel Output, 6-13 ancillary apparatus, 5-7 I/O address, 6-8 authorization codes, 2-9 I/O connections, 6-9 autoclave, 6-9 input capacitance, 5-1 Aux A/D Input, 6-11...
  • Page 62 Comprehensive Index -- removing a card set, 6-7 ringing, 4-1 schematic, 1-2 shorter black lead, 3-2 small signals, 5-1 stability, 4-1 static discharges, 2-3 stress apparatus, 6-9 turn-key system, 2-1 V Channel Output, 6-13 voltage noise, 5-4 white cell lead, 3-2 Windows Update, 2-6 working electrode, 3-2 cell connections, 3-3...

This manual is also suitable for:

Pci4/750 potentiostat/galvanostat/zra