Gamry Instruments Reference 3000, Operator'S Manual

Page 1: ...Reference 3000 Potentiostat Galvanostat ZRA Operator s Manual Copyright 2012 2021 Gamry Instruments Inc Revision 6 4 August 18 2021 988 00014...

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Page 3: ...ering time on our part can be performed on a contract basis Contact us with your requirements Limited Warranty Gamry Instruments Inc warrants to the original user of this product that it shall be free...

Page 4: ...that might appear Copyrights Reference 3000 Potentiostat Galvanostat ZRA Operator s Manual copyright 2008 2021 Gamry Instruments Inc all rights reserved Gamry Framework copyright 1989 2021 Gamry Instr...

Page 5: ...on 15 About this Manual 15 About the Reference 3000 15 About the Auxiliary Electrometer Option 16 Notational Conventions 16 Chapter 3 Instrument Circuitry 17 Reference 3000 Schematic Block Diagrams 17...

Page 6: ...nnector 54 Power LED 54 USB LED 56 Cell On LED 56 Overload LED 56 Rear Panel 58 Power In Jack 58 Power Switch 59 Chassis Ground 60 USB Port 60 Thermocouple Input 61 Misc I O Connector 61 I Monitor BNC...

Page 7: ...tic Field 83 Separate the pairs 83 Twist the Sense Wires 84 How Should You Hook Up Your Cell 84 Appendix A Reference 3000 Specifications 85 Control Amplifier 85 Differential Electrometer 85 Voltage Me...

Page 8: ...99 Normal Start up 99 Failure in an electronics module 99 Severe problem 99 Appendix G Certifications 101 Declaration of Conformity No DOC 2009 CE REF3000 101 Certificate of Conformance 102 Declaratio...

Page 9: ...zardous live voltages as defined in EN 61010 the standard mentioned above Reinforced insulation again defined in EN 61010 is used to reduce the risk of electrical shock because of this hazardous live...

Page 10: ...lectrochemical tests A Chassis Ground binding post on the rear panel of the Reference 3000 makes for easy implementation of this connection Simply run a wire from this binding post to a suitable sourc...

Page 11: ...ple where the instrument is earthed The User I O connector can be connected to earth grounded apparatus without earth grounding the Reference 3000 if the cable connections are done carefully The metal...

Page 12: ...s visible damage It does not operate properly It has been stored for a long period of time under unfavorable conditions It has been dropped or subjected to severe transport stress It has been subjecte...

Page 13: ...nity from electrical transients including transients on the incoming AC Mains supply and Electrostatic Discharge It has been tested for compliance with EN 61326 1998 Electrical equipment for measureme...

Page 14: ...r branch circuit Plug your Reference into a power line surge suppressor Inexpensive surge suppressors designed for use with computer equipment are now generally available Contact Gamry Instruments Inc...

Page 15: ...involving electrochemical synthesis electroplating and corrosion While it can apply and measure ampere level currents it is also an excellent small signal potentiostat that can work with picoampere an...

Page 16: ...of individual cells in a multi cell fuel cell or battery stack Up to eight completely independent voltages can be measured using this option The measurements are fully differential so cell voltages a...

Page 17: ...asic principles of the Reference 3000 circuitry without the confusion of the full circuitry details The complexity of the Reference 3000 can be quite daunting the Reference 3000 circuit boards contain...

Page 18: ...Instrument Circuitry Reference 3000 Schematic Block Diagrams 18 Figure 3 1 Reference 3000 Potentiostat Board in Potentiostat Mode Simplified Schematic Block Diagram...

Page 19: ...able IEStab capacitor and CASpeed capacitor are actually several fixed value components switched into the circuit and not continuously variable The monitor BNC connectors for Isig and Esig are lightly...

Page 20: ...range Calibration components are not shown The DDS can generate fixed amplitude sine waves with frequencies between 1 MHz and 1 mHz In practice Gamry s electrochemical impedance spectroscopy software...

Page 21: ...n DAC voltage are under the control of a hardware state machine This insures that all waveform and data acquisition timing is tightly controlled and reproducible point to point By default the data acq...

Page 22: ...switches under software control to change the characteristics Contact Technical Support at Gamry com if you are uncertain which type of unit you have Jumper configured Reference 3000s are shipped con...

Page 23: ...Time critical sections of the Power PC code are kept in the processor s fast cache memory The term UART refers to a Universal Asynchronous Receiver Transmitter It converts parallel data to a self cloc...

Page 24: ...effect of power supply noise on the data Additional circuitry that is not shown protects the Reference 3000 against ESD electrostatic discharge and electrical surges Note that the Reference 3000 is a...

Page 25: ...s its own filtering The Aux A D Channel filter is not useful for switched inputs The 10 and 100 gains in the Aux A D channel can be used to improve A D resolution The inputs have an input impedance of...

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Page 27: ...ystem containing a Microsoft Windows compatible computer These instructions assume use with Gamry s Framework Software Revision 7 0 or higher Figure 4 1 Front View of a Reference 3000 without AE Optio...

Page 28: ...ompatible with Revision 1 1 or Revision 2 0 of the USB specification Gamry s Windows based application software packages may impose additional more stringent requirements See the software documentatio...

Page 29: ...e into your computer If you have inserted the Gamry CD or Flash Drive into your computer and the Gamry Setup program does not start automatically 1 Navigate to the root folder of the device containing...

Page 30: ...is delivered with a line cord suitable for use in the United States In other countries you may have to replace the line cord with one suitable for your type of electrical outlet You must always use a...

Page 31: ...0 High Speed USB operation An A B USB cable has different connectors on each end The end with a wider rectangular connector plugs into a USB port on your computer or a similar port on a USB hub The e...

Page 32: ...tatus Bar By default the Gamry Framework shows a Device Status Bar under its main menu see Figure 4 3 If you don t see the Device Status Bar when you run the Gamry Framework it has been disabled in th...

Page 33: ...s indicator behaves in the same manner described above Gamry Instrument Manager Use Gamry s Instrument Manager dialog box to make changes to the configuration of your Reference 3000 system Get access...

Page 34: ...s name Selecting an instrument that is connected and idle blinks its Power LED After a moment your potentiostat should appear next to Devices Present along with a green virtual LED Repeat for addition...

Page 35: ...strument Firmware Handles most of the functions of the Reference 3000 Communications Firmware Handles the USB communications between your Reference 3000 and the host computer Appropriate update files...

Page 36: ...prompted for a file Navigate to the file s location on the Gamry software disk or on your computer s hard drive and then click the Open button The update procedure begins A status bar shows the progre...

Page 37: ...y Support button in GIM One of our support engineers will review the results and provide appropriate advice You run the Instrument Manger by selecting Options Instrument Manager on the Framework Menu...

Page 38: ...input current of the Working sense input amplifier The input current of the Reference input amplifier The input current of a Counter Sense input amplifier Current leakage in the cell switch In most r...

Page 39: ...t that 1 Asks you to disconnect the reference counter and counter sense leads from the calibration cell 2 Measures the I E input and Working sense amp input currents on the 300 pA range 3 Replaces the...

Page 40: ...of your potentiostat to a known good earth ground 2 Connect the cell cable to the correct color coded receptacles on the 2 k Calibration Cell 3 Place the Calibration Cell inside the Calibration Shield...

Page 41: ...The Cable Capacitance Calibration window appears 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...

Page 42: ...ibration 42 7 The Cell Required window appears Make sure that the correct Calibration Cell is attached then click the OK button The calibration runs 8 The Done window appears Click the OK button to ac...

Page 43: ...eference 3000 with ancillary apparatus connected directly to any of the cell leads Examples of ancillary apparatus include DVMs oscilloscopes chart records and data loggers Ammeters and voltmeters reg...

Page 44: ...ide of the device and the blue and green cell leads to the other side Try to connect the white and blue leads as close to the device as possible Connect the red banana plug to the counter or auxiliary...

Page 45: ...and the Orange Counter Sense lead must be connected Table 6 2 Cell Cable Connections for ZRA Mode Color Type Name Normal Connection Blue Banana plug Working Sense Connect to metal sample 1 Green Banan...

Page 46: ...ond end of a stack Black Pin jack Floating Ground Leave open or connect to a Faraday shield The Counter Sense and the Counter leads are connected to one end of a stack The Working and the Working Sens...

Page 47: ...rous because they can result in the battery being shorted through the instrument During the development of the Reference 3000 several prototype instruments without fuses were damaged when connected to...

Page 48: ...cal fuses from the Bussman Corporation The Bussman Part Number is BK GMA 3 15 R Fuses with similar ratings from other manufacturers have not been tested so we cannot recommend their use Fuses Located...

Page 49: ...ws when you reassemble the hood Figure 6 2 Drawing of Fuse holder in the D Connector Hood Four replacement fuses should accompany every Counter Working cell cable shipped by Gamry Instruments The Gamr...

Page 50: ...ace the UDC4 within a Faraday cage Select the command Experiment Utilities Set a Voltage on the Framework s menu bar A dialog box similar to this appears Figure 6 3 Setup Dialog Box for the Set a Volt...

Page 51: ...If this test indicates an open fuse use the procedures described above to check both fuses This test cannot tell which fuse is blown Both fuses can blow at the same time If the fuse test indicates an...

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Page 53: ...high current connections between a Reference 3000 and an electrochemical test cell The Counter Working connector is normally connected to a Gamry Instruments supplied cell cable Gamry s Counter Worki...

Page 54: ...cable In addition to the pins used for cell connections the Reference 3000 Sense Inputs connector also uses five pins to read a cell cable ID Gamry s software can compensate for the cell cable charact...

Page 55: ...tEchem system without looking at the instrument Serial Label on the bottom of the instrument chassis When the Power LED is off one of the following is true The rear panel power switch is off There is...

Page 56: ...ed to the Cell Cable Avoid touching the cell cable leads whenever the Cell On LED is lighted because the quality of the data collected in your experiment may be compromised If you need to make changes...

Page 57: ...voltage step into a perfect capacitor In theory charging the capacitor requires an infinite current The current spike seen at each step in a stepped voltage waveform can easily light the Overload LED...

Page 58: ...ed to the Power In jack on the lower right side of the rear panel The input current is less than 5 A We recommend that you always use the power adapter power brick supplied with your Reference 3000 to...

Page 59: ...or more than 5 A of output current Power Switch The Power switch is located just below the Power In jack It switches the power from this jack to the input of the Reference 3000 s DC DC converter Cauti...

Page 60: ...ug to banana plug lead is provided with your Reference 3000 You may find it useful when making this earth ground connection USB Port The USB port on the rear panel of the Reference 3000 is a Type B co...

Page 61: ...ed for an accuracy of 3 C Even this accuracy is only achieved when the Reference 3000 is calibrated The scaling at the A D converter is 3 V full scale or 300 C full scale The Reference 3000 calibratio...

Page 62: ...Reference 3000 s current measurement circuit With the exception of the filtering described below it is the raw signal It is high bandwidth on the less sensitive current ranges The effective bandwidth...

Page 63: ...ith 220 pF Ext Sig In BNC The Ext Sig In BNC connector allows you to add a voltage to the Reference 3000 s signal generator This signal is summed with the other signal generator sources including the...

Page 64: ...arallel with 220 pF Aux In BNC The Aux In BNC connector allows you to measure a voltage from outside the Reference 3000 using the Reference 3000 s internal A D The scaling is 3 V in equals 30 000 A D...

Page 65: ...can also use the AE to use to measure non electrochemical signals The voltage input to an AE channel can be the output from a temperature pressure or other transducer AC Performance and CMRR Each AE c...

Page 66: ...on mode voltage Maximum DC Error Vcm CMRR 31 V 94 dB 31 V 50 000 620 V This is quite small compared to the 1 5 V cell voltage so we can ignore it At 100 kHz the CMRR is specified to be at least 74 dB...

Page 67: ...voltage readings The analog inputs are both labeled with labels on the wires and color coded The wires are black for odd numbered channels Channel 1 3 5 and 7 and red for the even numbered channels C...

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Page 69: ...is stable not oscillating it may exhibit ringing whenever there is a voltage step applied to the cell The Reference 3000 s D A converters routinely apply steps even when making a pseudo linear ramp W...

Page 70: ...The counter electrode is the low impedance electrode eliminating the need for an additional electrode in the solution Figure 9 2 High Frequency Shunt Red White Green 100 pF to 10 nF Counter Reference...

Page 71: ...Stability in Potentiostat Mode Improving Potentiostat Stability 71 Figure 9 3 Resistor Added for Stability Red White Green Counter Reference Working Resistor...

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Page 73: ...ve current changes as small as 100 femtoamperes 1 10 13 A To place this current in perspective 100 fA represents the flow of only about 600 000 electrons per second The small currents measured by the...

Page 74: ...bove use Kirchhoff s and Ohm s laws to calculate Zcell Zcell ES Rm Vm Figure 10 1 Equivalent Measurement Circuit Icell C shunt R shunt C in R in Rm Unfortunately technology limits high impedance measu...

Page 75: ...a problem averaging reduces the noise bandwidth thereby reducing the noise at a cost of lengthening the experiment Finite Input Capacitance Cin in Figure 10 1 represents unavoidable capacitances that...

Page 76: ...the surface which is larger than the macroscopic geometric area because even a polished surface is rough The impedance of this 40 F electrode assuming ideal capacitive behavior is given by Z 1 j C At...

Page 77: ...e enough to allow a cell cable to enter the shield The shield must be electrically connected to the Reference 3000 s floating ground terminal An additional connection of both the shield and the Refere...

Page 78: ...lts when the cell cables are moved Cell Construction If you need to measure small currents or high impedances make sure that your cell construction does not limit your response A cell where the resist...

Page 79: ...unded cells include autoclaves stress apparatus pipelines storage tanks and battleships The Reference 3000 s internal ground is allowed to float with respect to earth ground when it works with these c...

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Page 81: ...imize errors Why Galvanostatic Mode Even though potentiostatic EIS is the most commonly used EIS technique it is poorly suited to impedance measurements of low impedance batteries fuel cells and super...

Page 82: ...error caused by the resistance of the wires Figure 11 1 Two and Four Terminal Measurements Four terminal measurements are also useful in AC measurements although there is a factor called mutual induc...

Page 83: ...eates a magnetic field The field strength is proportional to the current Fortunately passing the same current in opposite directions through adjacent wires tends to cancel the external field This also...

Page 84: ...ed to lie close to each other minimizing the loop areas Adjacent loops pickup voltages of opposite polarity resulting in cancellation How Should You Hook Up Your Cell Always use four terminal connecti...

Page 85: ...change without notice Control Amplifier High Voltage Low Current Mode Compliance Voltage Min Typ 30 31 5 V Note 1a Output Current Min 1500 mA Note 2 Low Voltage High Current Mode Compliance Voltage M...

Page 86: ...tage across Rm Typ 150 mV at full scale Note 13 Output Voltage at BNC and ADC in Typ 3 0 V at full scale Input Offset Current Max Typ 5 2 pA Note 14 Range Zero Offset Max 0 05 of range Note 14 Gain To...

Page 87: ...300 pA Note 12 Accuracy Dominated by current to voltage converter accuracy shown above Sig Gen Voltage for Full Scale Current 3 0 V Auxiliary A D Input see Appendix D Range differential Typ 3 volts I...

Page 88: ...ference and the working and working sense leads 3 Measured with an external function generator connected to the Ext Sig In BNC 4 The Differential Electrometer Amps are Analog Devices AD8065 Op amps sp...

Page 89: ...erm is usually dominant For large currents A the first term can usually be ignored The units for the error are amperes 14 Drift can be approximated by simple drift in the Range Zero Error In reality a...

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Page 91: ...at the cell end of the cell cable 3 No connect 4 6 11 13 Ground The potentiostat s floating ground Can be used to shield the cell if very low currents need to be measured Also used as a shield for th...

Page 92: ...ntial as Pin 8 Left open at the end of the cell cable 8 Work Sense Connected to the working electrode in most cases see Chapter 5 This lead has a 261 resistor in the cell end of the cable Custom cell...

Page 93: ...m a D A converter is on this connector The scaling is normally 1 mV per bit for a range of 0 to 4 096 V full scale The pin out table for this connector is shown in Table C 1 Caution The ground pins on...

Page 94: ...ce 9 Digital Out 2 A TTL compatible digital output 330 output impedance 10 Digital Out 3 A TTL compatible digital output 330 output impedance 11 Digital In 0 A TTL compatible digital input 2 2 k input...

Page 95: ...x A D input jumpers in the field The CMOS switches are set using a function call in an Explain script After the CMOS switches are set they remain in the selected position until another script resets t...

Page 96: ...r J901 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 Note that source impedances greater than 1 k apprec...

Page 97: ...ential Input Voltage Resolution 1 666 V 16 66 V 166 6 V per bit on all ranges Gain Error 0 3 on all ranges Offset Range 5 12 V offset of differential signal Offset Resolution 166 6 V bit Input Current...

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Page 99: ...DRAM unidentified problem Twice then twice Post SDRAM size error Twice then three times Post ROM checksum error Three times then four times Post Serial init RX buffer Three times then five times Post...

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Page 101: ...following standards as defined in report number R0295 000 from Ergonomics Inc for safety analysis and report number RSI 2772L from Radiation Sciences Inc for EMC test and analysis EMC Standards Title...

Page 102: ...Certifications 102 Certificate of Conformance...

Page 103: ...s based upon compliance with the following directives Electromagnetic Compatibility Regulations 2016 Electrical Equipment Safety Regulations 2016 EMC Regulations Title Class Criteria EN 61326 1 2013 E...

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Page 105: ...0 77 EasyUSB 23 EIS speed 79 electrical noise 77 electrical transients 13 electrons per second 73 enclosed space 12 environmental limits 12 environmental stress 12 External Signal 63 fans 12 Faraday s...

Page 106: ...reference electrode impedance 78 reference electrodes 78 RFI 13 ringing 69 safety 9 schematic 17 service 13 service contract 3 shielding against noise 10 shorting bar 46 Sign Gen Out 64 small signals...