Gamry Reference 600+ Operator's Manual
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Gamry Reference 600+ Operator's Manual

Potentiostat/galvanostat/zra
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Reference 600+
Potentiostat/Galvanostat/ZRA
Operator's Manual
Copyright  2018 Gamry Instruments, Inc.
Revision 6.2
January 9, 2018
988-00006

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  • Page 1 Reference 600+ Potentiostat/Galvanostat/ZRA Operator’s Manual Copyright  2018 Gamry Instruments, Inc. Revision 6.2 January 9, 2018 988-00006...
  • Page 3 If You Have Problems Please visit our service and support page at www.gamry.com/service-support/. This page contains information on installation, software updates, and training. It also contains links to the latest available documentation. If you are unable to locate the information you need from our website, contact us via email using the link provided on our website.

  • Page 4: Limited Warranty

    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 original shipment date of your purchase.
  • Page 5 The information in this manual has been carefully checked and is believed to be accurate as of the time of printing. However, Gamry Instruments, Inc. assumes no responsibility for errors that might appear. Copyrights ...

  • Page 7: Table Of Contents

    ................ 25 ® Running the Framework ....................25 Framework Device Status Bar ................... 25 Gamry Instrument Manager ....................26 Blink Button ........................29 Changing the Label ......................29 The Reference 600+ Customization Label ................ 30 Chapter 4: Calibration ........................33 Introduction ........................
  • Page 8 Membrane Cell Connections .................... 41 Chapter 6: Panel Indicators and Connectors .................. 43 Front Panel........................43 Rear Panel ........................46 Chapter 7: Stability in Potentiostat Mode ..................53 Capacitive Cells and Stability .................... 53 Improving Potentiostat Stability ..................53 Chapter 8: Measurement of Small Signals ..................57 Overview .........................

  • Page 9: Chapter 1: Safety Considerations

    Inspection When you receive your Reference 600+ Potentiostat/Galvanostat/ZRA, inspect it for evidence of shipping damage. If you find any damage, please notify Gamry Instruments Inc. and the shipping carrier immediately. Save the shipping container for possible inspection by the carrier.

  • Page 10: Grounding In The Reference 600

    AC mains to the AC power adapter. If your Reference 600+ has been provided without an AC line cord, or a cord that is not compatible with your local AC mains socket, obtain a line cord certified for use in your country. Contact your local Gamry Representative or email to techsupport@gamry.com if you are uncertain what AC line cord to use.

  • Page 11: Operation With Earth-Grounded Cells And Auxiliary Apparatus

    Operation with Earth-Grounded Cells and Auxiliary Apparatus As described above, the Reference 600+ circuitry is isolated from earth ground, allowing it to make measurements on cells that include an earth ground. This ground isolation is often called floating operation. Cells with earth ground include many autoclaves, pipelines and storage tanks, and many fuel cell systems.

  • Page 12: Defects And Abnormal Stresses

    Caution: Do not block the airflow into or out of the Reference 600+ chassis. While the circuitry should suffer no damage caused by excessive heat, the Reference 600+ enclosure may become uncomfortably hot to the touch if insufficient air flows through the chassis. Running the Reference 600+ without adequate cooling could shorten the time to failure of some of the circuitry.

  • Page 13: Service

    Try plugging your Reference 600+ into a different AC power branch circuit. • Plug your Reference into a power-line surge-suppressor. Inexpensive surge-suppressors are now generally available because of their use with computer equipment. Contact Gamry Instruments, Inc. if these measures do not solve the problem.

  • Page 14: Ce Compliance

    The European Community has instituted standards limiting radio frequency interference emitted by electronic devices, setting limits for susceptibility of apparatus to RF energy and transient events, and mandating safety requirements. Gamry Instruments, Inc. has designed and tested the Reference 600+ to comply with these standards.

  • Page 15: Chapter 2: Introduction

    This manual covers the installation, safety, and use of the Gamry Instruments Reference 600+ Potentiostat/Galvanostat/ZRA. This manual describes use of a Reference 600+ with Revision 7.0 (and later revisions) of the Gamry Framework software. It is equally useful when setting up a newly-purchased potentiostat or modifying the setup of an older potentiostat for use with new software.

  • Page 16: Notational Conventions

    The Reference 600+, like all Gamry potentiostats, requires a computer for its use. Unlike our older potentiostats, the Reference 600+ connects to the computer through a USB connection. The USB connection has become truly universal, with USB ports found on all modern computers. Gamry’s software currently supports up to 16 Reference 600+ Potentiostats connected to one computer.

  • Page 17: Chapter 3: Instrument Circuitry

    Chapter 3: Instrument Circuitry Reference 600+ Schematics and Block Diagrams If you are not familiar with electronic schematics or potentiostats, you probably want to skip this chapter. This information is for expert use only and is not required for routine use of the Reference 600+. The following figures are partly schematic diagrams and partly block diagrams.
  • Page 18 Figure 3-1 Reference 600+ Potentiostat Board in Potentiostat Mode Simplified Schematic/Block Diagram...
  • Page 19 • Calibration components are not shown. • Gamry’s software can disconnect the signal generator from the Potentiostat. Once disconnected it can be used for other experimental control tasks. • Overload protection and overload detection are not shown. Good engineering practice demands that any possible misconnection of the cell leads will not damage the instrument.
  • Page 20 • The DDS can generate fixed-amplitude sine waves with frequencies between 5 MHz and 1 mHz. In practice, Gamry’s EIS software uses the Scan DAC to generate sine signals if frequency is below 1 Hz. The low-pass filter removes high-frequency distortion in the “raw” DDS output.
  • Page 21 Figure 3-3 One A/D Signal Chain in the Reference 600+ Notes for Figure 3-3: • This diagram shows one of three identical ADC channels. One channel is dedicated to measurement of the potentiostat’s current signal, another is used to measure the voltage, and the third is switched between a wide selection of possible signals.
  • Page 22 Note that this circuit must be calibrated to obtain reasonable accuracy. A section of the Reference 600+ calibration procedure allows users to calibrate this input. • The other two inputs to the Aux channel are reserved for use in future Gamry Instruments’ systems.
  • Page 23 This reduces noise pick-up. • Unlike previous Gamry Instruments’ Potentiostats, the Reference 600+ calibration data are stored in the instrument, not in a data file. When a Reference 600+ is moved from one computer to...
  • Page 24 Figure 3-6 DC-DC Power Conversion Notes for Figure 3-6: • Note the ground isolation between the input power and the Reference 600+ circuitry. The Reference 600+ chassis is connected to the Floating Instrument Ground. Transformers and digital isolators are the only components connected between the grounds. •...

  • Page 25: Chapter 4: Installation

    Chapter 4: Installation This chapter of the Gamry Instruments Inc. Reference 600+ Operator’s Manual covers normal installation of the Reference 600+. We assume the Reference 600+ is installed as part of a Gamry Framework-based electrochemical measurement system containing a Microsoft Windows ®...

  • Page 26: Physical Location

    • Microsoft ® Windows ® 7 or newer is required with Gamry Framework™ software version 7. Framework version 6 is compatible with Windows XP and newer. Both 32-bit and 64-bit versions of these ® operating systems are supported. •...

  • Page 27: Quick-Start Guide For System Installation

    An Internet download of Gamry’s software downloads a self-extracting .EXE file. Running this file extracts the software and begins the same installation process as you get with a physical medium. If you have inserted the Gamry DVD or flash drive into your computer and the Gamry Setup program does not start automatically:...

  • Page 28: Power Cord And Power Connection

    Figure 4-2 Rear Panel of the Reference 600+ Power Cord and Power Connection The Reference 600+ does not plug directly in the AC mains supply. Instead, the mains are connected to an external power supply, which supplies a regulated 24 V DC output. This regulated DC is then connected to the Power In jack on the rear of the Reference 600+.

  • Page 29: Power-Up Test

    Caution: If the Power LED goes on, then turns off and stays off, the Reference 600+ is not working properly! Contact Gamry Instruments or your local Gamry Instruments representative as soon as possible if this power-up test fails.

  • Page 30: Front Panel Usb Led

    The Cell Cable connector is a 25-pin female D-type connector on the front of the Reference 600+. All of Gamry’s standard cell cables have a 25-pin D-type connector on one end and a number of leads terminated with banana plugs on the other. The D-type connector end of the cable is connected to the Cell Cable connector on the front of the Reference 600+.

  • Page 31: Multiple Potentiostat Systems

    Framework Device Status Bar By default, the Gamry Framework shows a Device Status Bar under its main menu (Figure 4-3). If you don’t see the Device Status Bar when you run the Gamry Framework, it has been disabled in the Framework Options menu.

  • Page 32: Gamry Instrument Manager

    This is an indication of a version mismatch between firmware and instrument. Gamry Instrument Manager You can use Gamry’s Instrument Manager (GIM) application to make changes to the configuration of your Reference 600+ system. Find the application through the Options menu in the Gamry Framework. Use the Instrument Manager to: •...

  • Page 33: Firmware Update

    Authorization Code field. 3) Choose the package to which you will be upgrading in the Package menu, and then enter the corresponding ten-digit Authorization Code. Gamry Instruments gives you the Authorization Code. Click the OK button. A status box opens and the instrument restarts. When this is complete the instrument is at the new tier.
  • Page 34 If the firmware is compatible with software version, the Device Info area appears as: Reference Family instruments only use instrument and communication (comm) firmwares, and do not use a PLD firmware. Interface Family instruments use all three firmwares. Gamry does not recommend altering the firmware versions unless necessary.

  • Page 35: Blink Button

    Click the OK button. The instrument is now ready to be used. Select And Update The Select And Update button is available at all times, even if an update is not required. Gamry recommends not altering the firmware if it is not necessary. This tool allows you to change individual firmwares (instrument, PLD, Comm).

  • Page 36: The Reference 600+ Customization Label

    4. Click the label itself, and then enter a new, unique name. The Reference 600+ Customization Label Introduction to the Reference 600+ Customization Label Battery tests are a good example of when multiple tests of a particular battery composition and/or construction are generally required.
  • Page 37 If ® you are using the Gamry-supplied label sheet, identify the location on the sheet where the new label is found. 1) If you are writing by hand on a blank label, do it now.
  • Page 38 8) Replace the black bezel. Reattach the four screws to fix the bezel in place. 9) Rename the Reference 600+ in the Gamry Framework software to match the new label. Use the Framework Options, Instrument... dialog box. In the resulting dialog box, select the device you...

  • Page 39: Chapter 4: Calibration

    The Reference 600+ recognizes the type of cable connected to its cell connector. It maintains a separate AC calibration table for each type of cable. The Gamry Framework will not let you use AC calibration data recorded using a 60 cm shielded cable for experiments run using a Twisted Pair cable optimized for low- impedance EIS measurements.
  • Page 40 Caution: The standard Reference 600+ calibration calls for an external resistive dummy cell. Your Reference 600+ was shipped with a 200 Ω Calibration Cell, which includes a 200 Ω, 0.05% accurate resistor. After calibration, please place this Calibration Cell in a safe place where you can find it if your unit requires recalibration.

  • Page 41: Cable Calibration

    Cable Calibration This procedure uses an external resistive Calibration Cell. Caution: The Reference 600+ cable calibration calls for an external resistive dummy cell. Your Reference 600+ was shipped with a 20 kΩ Calibration Cell including a 20 kΩ, 0.05% accurate resistor. After calibration, please place this Calibration Cell in a safe place where you can find it if your unit requires recalibration.
  • Page 42 Shield’s grounding post. (Note that the photograph below left is of a 200 Ω cell, so is only a general representation of the procedure.) 4) Open Gamry Framework™ software. Select Experiment > Named Script... The Select a script to run window appears.

  • Page 43: Low I Range Dc Calibration

    6) In the Cable Tag field, enter a unique name for the cable you are calibrating. Choose the desired Action radio button: • To calibrate the cable, choose Cal Cable. • To reset the vales to zero (if, say, the calibration doesn’t work), choose Zero Values.
  • Page 44 Most corrosion experiments or macro-electrode measurements involve currents much too large to be affected by this difference. The Gamry Framework includes a special “Low I DC Current” calibration procedure that corrects the Reference 600+ offsets to minimize this problem. The procedure uses a script that:...

  • Page 45: Chapter 5: Cell Connections

    Chapter 5: Cell Connections Normal Cell Connections Each Reference 600+ in your system was shipped with a standard, shielded cell cable (part number 985- 00071). It is a 60 cm complex cable with a 25-pin D-type connector on one end and four banana plugs and two pin jacks on the other end.

  • Page 46: Zra Mode Cell Connections

    If your cell is a typical glass laboratory cell, all of the electrodes are isolated from earth ground. In this case, you may be able to reduce noise in your data by connecting the Reference 600+’s Floating Ground to an earth ground.

  • Page 47: Membrane Cell Connections

    Table 5-2 Cell Cable Connections for ZRA Mode Color Type Name Normal Connection Blue Banana Plug Working Sense Connect to metal sample #1 Green Banana Plug Working Electrode Connect to metal sample #1 White Pin Jack Reference Connect to a reference electrode Banana Plug Counter Electrode Connect to metal sample #2...
  • Page 48 Reference electrode #1 and counter electrode #1 must be on one side of the membrane, and reference electrode #2 and counter electrode #2 must be on the other side.

  • Page 49: Chapter 6: Panel Indicators And Connectors

    Gamry Instruments-supplied cell cable. In addition to the pins used for cell connections, the Reference 600+ Cell Connector also uses five pins to read a cell cable ID. Gamry’s software compensates for the cell-cable characteristics for optimal system performance, especially in EIS (Electrochemical Impedance Spectroscopy).
  • Page 50 Do not interrupt a firmware update that is in progress. An incomplete update can render a Reference 600+ inoperable until it is returned to Gamry for reprogramming. Should the firmware update be interrupted, contact Gamry before starting the return process.
  • Page 51 Cell On LED The Cell On LED glows yellow whenever the Reference 600+ is actively applying voltage or current to the electrochemical cell attached to the Cell Cable. Avoid touching the cell cable leads whenever the Cell On LED is lit, because the quality of the data being collected in your experiment may be compromised.

  • Page 52: Rear Panel

    Overload indications when the cell is being connected or disconnected are common and usually do not indicate a problem. Overloads can also be seen when one of the cell leads is disconnected from the other cell leads, even though the cell is off. Again, this does not indicate a problem. A steadily glowing Overload LED during an experiment most likely indicates a problem is occurring.
  • Page 53 switches the power from this jack to the input of the Reference 600+’s DC-DC converter. All protection circuitry, including the in-rush current limiter, are located after this switch. Normally, the DC power is connected before the Power switch is turned ON. However, no damage occurs if this switch is already in the ON position when the Power In cable is connected, or the AC power input is connected to the external power supply.
  • Page 54 Measuring temperature in a cell before making a CV measurement that will be used to calculate reaction kinetics. Gamry Instruments chose not to provide a thermocouple with the Reference 600+. There is simply too much variety in the mechanical design of thermocouple probes.
  • Page 55 Four digital outputs can be used to turn on external devices under control of an Explain experimental control script. • Some of Gamry applications assign three of the digital outputs to control stirring, flow of de- aeration gas, and formation of mercury drops on a mercury-drop electrode.
  • Page 56 current ranges. The effective bandwidth of the current signal falls as you reach the nA and pA current ranges. IE Stability capacitors further slow the response. The outer shell of this BNC connector is connected to the Reference 600+’s floating ground. Caution: The shell of the I Monitor BNC is connected to the Reference 600+’s Floating Ground.
  • Page 57 if a coaxial cable is connected to the BNC. Its output impedance is approximately 200 Ω in parallel with 220 pF. Ext. Sig.In BNC The Ext. Sig.In BNC connector allows you to add a voltage to the Reverence 600’s Signal Generator. This signal is summed with the other signal-generator sources, including the IR DAC, the Scan DAC, and the DDS output.
  • Page 58 Caution: The shell of the Sig. Gen.Out BNC is connected to the Reference 600+’s Floating Ground. Connection of this BNC to a piece of earth-ground-referenced equipment can compromise the Reference 600+’s ability to float, and invalidate data collected on earth-grounded cells.

  • Page 59: Chapter 7: Stability In Potentiostat Mode

    Increase the Reference 600+’s I/E stability setting. The Reference 600+ includes three capacitors that can be connected in parallel with its I/E converter resistors. These capacitors are connected to relays that are controlled by software. Contact your local Gamry Instruments’ representative for more information concerning changes in these settings.
  • Page 60 Figure 7-1 Fast Combination Reference Electrode White Cell Lead 100 pF to 10 nF Platinum Electrolyte...
  • Page 61 • 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 7-2. The capacitor value is generally determined by trial and error. One nF (1000 pF) is a good starting point. In a sense, this is another form of an AC-coupled low-impedance reference electrode.
  • Page 62 • Add resistance to the counter electrode lead. See Figure 7-3. This change lowers the effective bandwidth of the control amplifier. As a rule of thumb, select the resistor to give 1 V of drop at the highest current expected in the test being run. For example, if you expect your highest current to be around 1 mA, you can add a 1 kΩ...

  • Page 63: Chapter 8: Measurement Of Small Signals

    Chapter 8: Measurement of Small Signals Overview The Reference 600+ is a very sensitive scientific instrument. It can theoretically resolve current changes as small as 1 femtoampere (1 × 10 A). To place this current in perspective, 1 fA represents the flow of –15 about 6000 electrons per second! The small currents measured by the Reference 600+ place demands on the instrument, the cell, the cables...
  • Page 64 Figure 8-1 Equivalent Measurement Circuit R shunt C shunt Icell R in C in Unfortunately technology limits high-impedance measurements because: • Current measurement circuits always have non-zero input capacitance, i.e., C > 0. • Infinite R cannot be achieved with real circuits and materials. •...
  • Page 65 measurement can reduce the bandwidth by integrating the measured value at the expense of additional measurement time. With a noise bandwidth of 1 mHz, the voltage noise falls to about 1.3 V rms. Current noise on the same resistor under the same conditions is 0.41 fA. To place this number in perspective, a 10 mV signal across this same resistor will generate a current of 100 fA, or again an error of up to ...
  • Page 66 current are DC and can be tuned out in impedance measurements. As a general rule, the DC leakage should not exceed the measured AC signal by more than a factor of 10. The Reference 600+ uses an input amplifier with an input current of around 1 pA. Other circuit components may also contribute leakage currents.

  • Page 67: Hints For System And Cell Design

    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. No material is a perfect insulator (infinite resistance).
  • Page 68 5 m. We do not recommend that you use the Reference 600+ with any cables not supplied by Gamry Instruments. The Reference 600+ cable is not a simple cable like a typical computer cable. The Reference 600+ cable includes a number of individually shielded wires contained within an overall shield.

  • Page 69: Floating Operation

    Try to avoid: • Narrow-bore or glass-frit-tipped Luggin capillaries. • Poorly conductive solutions, especially in Luggin capillaries. • Asbestos-thread and double-junction reference electrodes. Reference electrodes often develop high impedances as they are used. Anything that can clog the isolation frit can raise the electrode impedance. Avoid using saturated KCl-based references in perchlorate-ion solutions.

  • Page 71: Appendix A: Reference 600+ Specifications

    Appendix A: Reference 600+ Specifications All specifications are at an ambient temperature of 25°C, with the Reference 600+ powered using the external power supply shipped with the unit, a standard shielded 60 cm cell cable, and the cell enclosed in a Faraday shield.

  • Page 72: Current Measurement

    Reference 600+ Specifications Current to Voltage Converter Maximum Full Scale Range Note 11 Minimum Full Scale Range Note 11 600 (after ×100 gain) Voltage across Rm mV at Note 12 full scale Output Voltage (at BNC and ADC in) full scale Input Offset Current Note 13 Range Zero Offset...
  • Page 73 Reference 600+ Specifications Galvanostatic Mode 600 Maximum Full Scale Current Note 11 60 Minimum Full Scale Current Note 11 Accuracy Dominated by current-to-voltage converter accuracy shown above 3.0 Sig Gen Voltage for Full Scale Current Auxiliary A/D Input (see Appendix D) 3 Range (differential) 3.6...
  • Page 74 Reference 600+ Specifications General Power Input Voltage Range 22 to 26 volts Power 1 nA Leakage Current Note 20 (floating, earthed Working Electrode) Dimensions 10 × 20 × 30 Note 21 Weight Note 21 Dimensions of External Power Adapter 7.5 × 3.5 × 15 Note 22 Weight of External Power Adapter Note 22...
  • Page 75 20. See Appendix D. 21. Isolation quality has both DC factors and AC factors (predominately at the 300 kHz power-supply frequency). Only the DC leakage current is shown here. Consult Gamry’s technical support for additional information. 22. Excluding external power adapter and any cables supplied with unit.
  • Page 76 Reference 600+ Specifications...

  • Page 77: Appendix B: Reference 600+ Cell Cable Connector

    Reference 600+ Cell Cable Connector Appendix B: Reference 600+ Cell Cable Connector Chapter 5Error! Reference source not found. describes the connections between a cell cable and an electrochemical cell. This appendix describes the other end of the cell cable. Multiple pins assigned to the same signal are connected together on the Reference 600+’s Potentiostat board.
  • Page 78 Reference 600+ Cell Cable Connector Designing cell cabling for a 5 MHz potentiostat is not a trivial task. Gamry Instruments does not recommend user-designed cables (except as a last resort). In many cases we can build a custom cable to meet your specific needs. We’ll also be happy to discuss your cabling requirements and give you...

  • Page 79: Appendix C: Misc. I/O Connector

    Misc. I/O Connector Appendix C: Misc. I/O Connector The Misc. I/O connector contains a number of signals used to connect the Reference 600+ to external apparatus. It is the miniature 15-pin female D-shaped connector on the rear panel of the Reference 600+. Be careful: the ground pins on this connector are isolated from both the Reference 600+ floating ground and earth ground.
  • Page 80 Misc. I/O Connector...

  • Page 81: Appendix D: Auxiliary A/D Input Characteristics

    Appendix D: Auxiliary A/D Input Characteristics Appendix D: Auxiliary A/D Input Characteristics The controller board used in the Gamry Instruments Reference 600+ Potentiostat has software switches that configure the input circuitry used for the Aux A/D function. The CMOS switches are set using a function call in an Explain script. Once the CMOS switches are set, they remain in the selected position until another script resets them.
  • Page 82 Appendix D: Auxiliary A/D Input Characteristics ...

  • Page 83: Appendix E: Ce Certificate

    Declaration of Conformity According to ISO/IEC Guide 22 and CEN/CENELEC EN 45014 Manufacturer's Name and Location: This declaration is for the Gamry Instruments product models: Reference 600+ Potentiostat/Galvanostat/ZRA. The declaration is based upon compliance with the following directives: EMC Directive 89/336/EEC as amended by 92/31/EEC and 93/68/EEC...
  • Page 84 Appendix E: CE Certificate...

  • Page 85: Certificate Of Conformance

    Appendix E: CE Certificate Certificate of Conformance...

  • Page 86: Comprehensive Index

    Comprehensive Index Comprehensive Index 25 pin D ............24 environmental stress ......... 6 AC adapter ............3 Ext. Sig. In BNC ..........51 ADC channels ..........15 External Signal..........51 air-cooling ............5 fans ..............5 ancillary apparatus.......... 63 Faraday shield .......... 40, 61 Aux A/D ............
  • Page 87 Power LED ............. 43 state-machine ..........15 Power PC ............17 static electricity..........7 Power PC firmware ........17 storage ............. 6 power-line transient ......... 7 support ............1 Power switch ..........23, 46 telephone assistance ......... 1 power-up self-test ........... 23 temperature .............

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