Please have your instrument model and serial numbers available, as well as any applicable software and firmware revisions. If you have problems in installation or use of a system containing a Reference 3000, please call from a phone next to your computer, where you can type and read the screen while talking to us.
Disclaimers Disclaimers Gamry Instruments, Inc. cannot guarantee that the Reference 3000 Potentiostat/Galvanostat/ZRA will work with all computer systems, operating systems, or third-party software applications hardware/software. The information in this manual has been carefully checked and is believed to be accurate as of the time of printing.
Inspection ............................... 9 Product Safety ............................9 AC Mains Connection to the Power Brick ....................9 Grounding in the Reference 3000 ......................10 Operation with Earth-Grounded Cells and Auxiliary Apparatus .............. 11 Temperature and Ventilation ......................... 12 Defects and Abnormal Stresses ......................12 Environmental Limits ..........................
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Table of Contents Low I Range DC Calibration ........................38 Cable Calibration ..........................39 Procedure to calibrate the cable ....................40 Chapter 6: Cell Connections ......................... 43 Cell Cable Overview ..........................43 Ancillary Apparatus ........................43 AE Connections ..........................43 Fuses in the Cell Cable ..........................
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Table of Contents Other AC Specifications ........................ 97 Appendix F: Power LED Blink Codes ......................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 .........................
AC Mains Connection to the Power Brick The Reference 3000 does not connect directly to an AC Mains supply. Instead, the mains are connected to the desktop AC adapter (power brick), which outputs 24 V DC, which in turn powers the Reference 3000.
The Reference 3000 is normally provided with an AC line cord suitable for your location. This AC line cord connects the AC mains to the AC power adapter. If your Reference 3000 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.
An earth ground connection can cause problems when testing batteries, fuel cells, or capacitors. Many of these devices can source huge currents, often tens or hundreds of amperes. If the Reference 3000 chassis is earth grounded, and another location in the stack is accidentally (or intentionally) connected to earth ground, a portion of the stack is shorted through the Reference 3000’s cell cable.
It has been subjected to environmental stress (corrosive atmosphere, fire, etc.). Do not use your Reference 3000 or any other apparatus if you think it could be hazardous. Have it checked by qualified service personnel. Environmental Limits There are environmental limit conditions on the storage, shipping and operation of this equipment. The Reference 3000 is not designed for outdoor use.
Use a cloth lightly dampened with either clean water or water containing a mild detergent to clean the outside of the Reference 3000 enclosure. Alternatively, you can use isopropyl alcohol. Do not use a wet rag or allow fluid to enter the Reference 3000 enclosure. Do not immerse the Reference 3000 in any type of cleaning fluid (including water).
Gamry Instruments, Inc. has designed and tested the Reference 3000 to comply with these standards. The relevant CE regulations include EN 61010 and EN 61326. RoHS Compliance The Reference 3000 has been built using lead-free components and lead-free solder. It is in compliance with the European RoHS initiative.
The Reference 3000 offers two different compliance-voltage and compliance-current settings. You can choose to operate the Reference 3000 set for compliance of 1.5 A and voltages up to 30 V, or you can chose to operate at 3 A and voltages up to 15 V. This choice cannot be changed in the middle of an experimental run.
16 Reference 3000 Potentiostats connected to one computer. The Reference 3000 is isolated from earth ground. It can therefore be used to make measurements on cells that contain an earth-grounded metal. A few of examples of such systems include are autoclaves, large metal storage tanks, stress apparatus, and capillary electrophoresis detectors.
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 3000. The following figures are partly schematic diagrams and partly block diagrams. They are intended to show the basic principles of the Reference 3000 circuitry without the confusion of the full circuitry details.
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The programmable attenuator on Esig prior to the ADC channel scales the Esig voltage to make it compatible with the A/D channel’s 3 V input range. The 0.25 gain setting allows the Reference 3000 to measure potential signals slightly in excess of 10 volts (on a 12-volt full-scale range). Isig is gained to be 3 V full-scale so it does not require a similar attenuation function.
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Instrument Circuitry – Reference 3000 Schematic/Block Diagrams Figure 3-2 Reference 3000 Signal-Generation Circuitry Notes for Figure 3-2: All the resistors summing voltages into the Summing Amplifier input do not have values shown on the diagram. Their values depend on scaling factors too complex for this simplified diagram.
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Instrument Circuitry – Reference 3000 Schematic/Block Diagrams Figure 3-3 One A/D Signal Chain in the Reference 3000 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 cell or stack voltage, and the third is switched between a wide selection of possible signals.
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The Aux ADC BNC input is a differential input. Some of this input’s characteristics can be changed by either jumpers or CMOS switches. Early Reference 3000’s use jumpers to change the characteristics, while later units (shipped after the middle of 2009) use CMOS switches under software control to change the characteristics.
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data and board-revision information. Unlike previous Gamry Instruments potentiostats, the Reference 3000 calibration data is stored in the instrument, not in a data file. When a Reference 3000 is moved from one computer to another, its calibration remains valid.
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Do not use a DC power source other than the AC-adapter model provided with your Reference 3000. Other replacements may void the performance and/or safety characteristics of the Reference 3000. Power input voltages less than 20 V or greater than 26 V can damage the Reference 3000’s power supply.
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Notes for Figure 3-7: One of eight identical channels is shown. The input buffers work over the entire Reference 3000 compliance voltage range. The maximum useable differential voltage between the two inputs on a channel is 5 V.
Front View of a Reference 3000 without AE Option Initial Visual Inspection After you remove your Reference 3000 from its shipping carton, check it for any signs of shipping damage. If you find any damage, please notify Gamry Instruments, Inc., and the shipping carrier immediately. Save the...
Tag a damaged Reference 3000 to indicate that it could be a safety hazard. If the Reference 3000 is taken from a cold location (for example outdoors in winter conditions) to a warm, humid location, water vapor may condense on the cold surfaces inside the Reference 3000, possibly creating a hazardous condition.
The Reference 3000 is compatible with the Windows Plug & Play configuration system. Like most Plug & Play hardware, it is best if you install the software for the Reference 3000 before you install the potentiostat hardware. Gamry Software Setup program normally starts automatically when you place the Gamry Instruments Software disk (or Gamry Instrument Software flash drive) into your computer.
DC Power In jack on the rear of the Reference 3000 (see Figure 4-2). The external power supply provided with the Reference 3000 is rated for operation from 100 to 240 V AC, at frequencies from 47 to 63 Hz. It should be usable worldwide.
One quick test is to power up the Reference 3000 and watch the blue Power LED indicator on the front panel of the Reference 3000 (see Figure Error! Reference source not found.). After connecting DC power to the Reference 3000, turn on its rear panel Power switch (see Figure 4-2).
Installation – First-time Device Installation in Windows® First-time Device Installation in Windows® These instructions presume you have already installed Gamry software Revision 7.0 or higher. Running the Framework Regardless of your electrochemical application, Gamry recommends running the Gamry Framework after you install new Framework software or add a potentiostat to your system.
The Reference 600 labeled Jims Ref600 has a white indicator, showing it is plugged in but cannot be used. This is an indication of obsolete firmware. Though no Reference 3000 was used in this example, its status indicator behaves in the same manner described above.
Instrument Manager Dialog Box Each Gamry potentiostat in the system appears in the list on the left. All Gamry Instruments potentiostats that are known to the system are displayed in the Instrument Manger. Select an instrument by clicking on its name.
Firmware Update Your Reference 3000 was shipped with the latest version of all its firmware. From time to time, Gamry makes changes to the instrument’s firmware code, and a firmware update is required to make use of the new or improved code.
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You are then 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 progress of the update. The USB LED on the Reference 3000 should also turn red during the procedure.
Framework’s Experiment drop-down menu. The Reference 3000 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.
Low I Range DC Calibration The standard Reference 3000 calibration is performed with the cell leads connected to a 2 k resistor. During the calibration procedure, DC current-range offsets are recorded with the cell switch turned off. A DC current measurement is made on each of the eleven current ranges in the Reference 3000.
The Low I DC Calibration is not a full calibration. You must run a full DC Calibration on your Reference 3000 before you run the Low I DC calibration. Remember that the Reference 3000 must have a full DC calibration on the same type of cable you use for the Low I DC Calibration.
Calibration – Cable Calibration Procedure to calibrate the cable 1) Connect the Chassis Ground on the back of your potentiostat to a known, good earth ground. 2) Connect the cell cable to the correct color-coded receptacles on the 2 kΩ Calibration Cell. 3) Place the Calibration Cell inside the Calibration Shield, close the lid, and connect the black floating- ground lead of your cell cable to the Shield’s grounding post.
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Calibration – Cable Calibration 4) Open Gamry Framework™ software. Select Experiment > Named Script... The Select a script to run window appears. From the list of scripts, choose calcable.exp, then click the Open button. 5) The Cable Capacitance Calibration window appears. In the Cable Tag field, enter a unique name for the cable you are calibrating.
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Calibration – Cable Calibration 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 acknowledge completion.
Fuses in the Cell Cable The Reference 3000 could be damaged if currents much larger than 3 A were to flow into or out of the Counter electrode or Working electrode leads. Improper connection to a battery, fuel cell, or super-capacitor could cause this type of damaging current to flow.
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Counter electrode. The black pin jack is connected on the Reference 3000 end to Floating Ground. This is the circuitry ground for the analog circuits in the Reference 3000. In most cases, leave this terminal disconnected at the cell end. When you do, take care that its metal contact does not touch any of the other cell connections.
Make sure that your earth-ground connection is made to a legitimate source of earth ground. Consult a qualified electrician if you are uncertain how to obtain an earth ground. Connecting the Reference 3000 to an incorrect and unsafe voltage can create a safety hazard (see Chapter 1 for details).
This type of connection is a stack connection. Special experiment scripts allow the Reference 3000 to control and measure stack voltages as large as its compliance voltage (15 V or 30 V). These scripts refer to Stack Mode cell connections. The cell connections in Stack Mode differ from those in Potentiostatic and Galvanostatic modes.
#2 and counter electrode #2 must be on the other side. Fuses in the Cell Cable All standard Reference 3000 Counter/Working cell cables include fuses in the current-carrying leads. These fuses protect the instrument from the extremely large currents that can flow through an improperly connected electrochemical-energy generation or storage device (including batteries, fuel cells, and capacitors).
Cell Connections – Fuses in the Cell Cable Always turn off the Reference 3000 and disconnect both ends of the Counter/Working cable before checking or replacing the fuses in the cable. In this fuse arrangement, you can remove the fuse from the cable by unscrewing the brass knurled nut on the fuse holder, just below the banana plug.
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Cell Connections – Fuses in the Cell Cable Always turn off the Reference 3000 and disconnect both ends of the Counter/Working cable before checking or replacing the fuses in the cable. Access to the fuses requires removal of two screws located on opposite sides of the hood covering the D-connector end of the Counter/Working cable.
Cell Connections – Fuses in the Cell Cable Testing For Open Fuses A Gamry Framework test checks for blown fuses without having you remove the fuses. A simple Potentiostatic test is run on the Calibration Cell with the Gamry UDC4 Dummy Cell. The test is run using the “Set a Voltage.exp”...
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Both fuses can blow at the same time. If the fuse test indicates an open fuse, and the fuses both check out good with an ohmmeter, some other problem has occurred in the cables or the instrument. Contact Technical Support at Gamry Instruments at your earliest convenience.
In addition to the pins used for cell connections, the Reference 3000 Counter/Working Connector also uses five pins to read a cell cable ID. Gamry’s software can compensate for the cell-cable characteristics for optimal...
EIS (Electrochemical Impedance Spectroscopy). Power LED The Power LED is located on the lower left of the Reference 3000 front panel. It normally glows a steady blue, when the Reference 3000 is turned on and has passed some simple self-tests.
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USB LED When the Reference 3000 is first turned on, the Power LED glows steadily for a second or two, blink three times, and then go to its normal steady blue output. Each blink in this sequence indicates successful completion of a portion of the Power PC’s power-up self-test routine.
Interrupting a firmware update can cause a catastrophic failure of your system. Do not turn off the Reference 3000, do not unplug the USB cable, and do not stop the operation of the host computer when the USB LED is a continuous red color.
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The control amplifier has lost control of the cell. Remember that the Reference 3000 can be operating with compliance limits of 1.5 A at 30 V or with compliance limits of 3.0 A at 15 V. The absolute value of the cell current may be trying to exceed the compliance current, or the absolute value of the counter electrode voltage may be trying to exceed the compliance voltage setting.
The rear panel contains one switch and a large number of connectors. See photograph below. Power In Jack The Reference 3000 derives all its power from a +24 V DC supply connected to the Power In jack on the lower right side of the rear panel. The input current is less than 5 A.
If your facility owns both Reference 600’s and Reference 3000’s, you must insure that the smaller power adapter from the Reference 600 is not used to power a Reference 3000. The Reference 3000 will not power up with the smaller adapter. Fortunately, neither the Reference 3000 nor the small power adapter will be damaged if connected in error.
USB Port The USB port on the rear panel of the Reference 3000 is a Type B connector as defined in Revision 1.1 and 2.0 of the USB Specification. Use a standard, shielded, Type A/B cable to connect this port to a computer’s USB port or a USB hub (preferably an externally powered hub).
Reference 3000 are fully powered. Thermocouple Input The Reference 3000 has a T/C Type K jack for a type K thermocouple. The ISO standard calls for color-coded mini-thermocouple connections. Yellow is the color assigned to type K thermocouples. The mating connector on your thermocouple should therefore be yellow.
Custom cables with the shield connected to pin 6 of the D-connector are preferred. I Monitor BNC The I Monitor BNC connector represents the output of the 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.
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 IR DAC, the Scan DAC, and the DDS output.
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 counts. This is a resolution of 100 µV per bit.
The AE is a factory-installed option for the Reference 3000. The AE acronym stands for Auxiliary Electrometer. The AE allows eight independent, high-voltage differential electrometer channels available to be read by the Reference 3000’s A/D converter. Difference voltages (between the two inputs of each channel) of up to 5 V can be measured.
Auxiliary Electrometer Option – Experiments CMR is especially important when the AE is used to measure the voltage of individual cells in a battery or fuel- cell stack. Cells near the Working Electrode have relatively low DC voltages, because the working electrode voltage is near ground.
Auxiliary Electrometer Option – Connections Using Custom Cables High side of even channel Analog Input Even Ch + Purple working side Ground Floating Ground Digital input !Cable Ground if cable present Digital In !Power On Ground if AE powered Ground Floating Ground Note that pins 8 and 9 must be grounded on any cable that is used to take voltage readings.
Whenever you see sharp breaks in the current recorded on the system, you should suspect oscillation. The Reference 3000 has been tested for stability with cell capacitors between 10 pF and 0.1 F. In all but its fastest control amp speed setting, it is stable on any capacitor in this range—as long as the impedance in the reference-electrode lead does not exceed 20 k.
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Stability in Potentiostat Mode – Improving Potentiostat Stability Figure 9-1 Fast Combination Reference Electrode White Cell Lead 100 pF to 10 nF Platinum Electrolyte 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 9-2.
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Stability in Potentiostat Mode – Improving Potentiostat Stability Figure 9-3 Resistor Added for Stability Resistor White Reference Counter Green Working...
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 Reference 3000 place demands on the instrument, the cell, the cables, and the experimenter. Many of the techniques used in higher-current electrochemistry must be modified when used to measure pA currents.
Measurement of Small-current Signals – Measurement System Model and Physical Limitations unwanted capacitance across the cell shunt current-measurement circuit’s stray input capacitance current-measurement circuit’s stray input resistance measurement circuit’s input current In the ideal current-measurement circuit, R is infinite while C and I are zero.
Measurement of Small-current Signals – Measurement System Model and Physical Limitations where: k = Boltzmann’s constant 1.38 × 10 –23 T = temperature in K F = noise bandwidth in Hz R = resistance in Ω. For purposes of approximation, the noise bandwidth, F, is equal to the measurement frequency. Assume a Ω...
AC signal by more than a factor of 10. The Reference 3000 uses an input amplifier with an input current of around 5 pA. Other circuit components may also contribute leakage currents. You therefore cannot make absolute current measurements of very low pA currents with the Reference 3000.
Try to avoid AC powered or computerized apparatus within your Faraday shield. Cell Cable Length and Construction The Reference 3000 is shipped with a 60 cm shielded cell cable. We also offer extended length cables and unshielded cables as options at extra cost.
Many experiments with the Reference 3000 involve cells with small capacitances, the value of which may be important. In these cases, the capacitance between the Reference 3000’s cell leads can result in an error. The Reference 3000 alligator clips can have 10 pF or more of mutual capacitance if they are run alongside each other.
Reference 3000 cell leads. Floating Operation The Reference 3000 is capable of operation with cells where one of the electrodes or a cell surface is at earth ground. Examples of earth-grounded cells include: autoclaves, stress apparatus, pipelines, storage tanks and battleships.
Chapter 11: EIS Measurement of Small Impedances Overview The Gamry Instruments Reference 3000 is a high-performance measurement instrument used for all types of electrochemical testing. Unlike many other electrochemical instruments, it offers outstanding performance for tests with signals consisting of small currents and high impedances, and for tests involving large currents and very small impedances.
EIS Measurement of Small Impedances – What is Mutual Inductance? An illustration of two-terminal measurements versus four-terminal measurements is provided in Figure 11-1. Both schematic diagrams show a resistance measurement made by passing a known current through an unknown resistance, R .
Fortunately, passing the same current in opposite directions through adjacent wires tends to cancel the external field. This also minimizes the net inductance in the wires. In all Gamry Instruments Reference 3000 Counter/Working cables, the current-carrying leads are bound together.
EIS Measurement of Small Impedances – How Should You Hook Up Your Cell? The Reference 3000 has two cell cables, so that we can separate the current-carrying wires from the sense wires. The current-carrying pair is in the Counter/Working Cable and the sense pair is in the Sense Cable.
Appendix A: Reference 3000 Specifications All specifications are at an ambient temperature of 25C, with the Reference 3000 powered using the power adapter shipped with the unit, standard shielded 60 cm cell cables, and the cell enclosed in a Faraday shield.
7) The bandwidth is for a sine-wave source with a 50 output impedance driving either input. The bandwidth is well in excess of this specification, which is limited by the measurement equipment used in testing the Reference 3000. 8) CMRR is common-mode rejection ratio. It specifies the ability of the differential electrometer to reject...
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Reference 3000 Specifications with a 50 output impedance and measuring the error as a function of frequency. Resistance in either input causes a loss of CMRR. 9) Voltage measurement is actually performed with a 3 V signal input to the ADC signal chain. A 4 attenuator divides down higher-voltage electrometer outputs, so they fit into a 3 V input, thus making...
Multiple pins assigned to the same signal are connected together on the Reference 3000’s Potentiostat board. If you need to connect this signal outside the Reference 3000, you need a wire connected to any one of the D-connector pins.
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Reference 3000 Cell Connectors Table B-2 Sense Inputs Connector Pin(s) Signal Name CBL_ID2 One of 4 cable ID bits. Used to identify the type of cell cable attached to the unit. Pull to a logic High through a resistor. Ground to set the bit low.
Misc. I/O Connector Appendix C: Misc. I/O Connector This connector contains a number of signals; it connects the Reference 3000 to external apparatus. It is the miniature 15-pin female D-shaped connector on the rear panel of the Reference 3000. Caution: The ground pins on this connector are not the Reference 3000 floating ground.
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Power: 50 mA maximum current Caution: Floating operation of the Reference 3000 can be compromised by improper connection of cables to the Misc. I/O Connector. Do not use standard 15-pin shielded cables with this connector. Custom cables with the shield connected to pin 6 of the D-connector are required.
CMOS switches set using software. The changeover occurred in 2009. We usually ask that you return your Reference 3000 to Gamry Instruments if you need to change the hardware jumpers. This information is provided so a qualified service technician can change the Aux A/D input jumpers in the field.
Auxiliary A/D Input Characteristics Input Impedance Selection Two jumpers are associated with the input impedance, J902 and J903. With J902 and J903 installed, the Aux A/D input has a 100 k input impedance. This is the default setting. With the jumpers installed, the potentiostat can be calibrated without a cable on the input BNC connector.
Auxiliary Electrometer Specifications Appendix E: Auxiliary Electrometer Specifications Unless otherwise mentioned, all specifications apply at 22C, zero common-mode voltage versus Ground FA, input voltages with Z < 10 Ω, and all channel inputs (other than those of the channel under test) at zero volts versus Ground FA.
If there are multiple problems, the communications board takes code priority over the memory module. Severe problem The red LED, which normally switches off after a rapid boot-up, remains illuminated. If you receive one of the above codes, please call Gamry Instruments Service Department for assistance.
Gamry Instruments 734 Louis Drive Warminster, PA 18974 This declaration is for the Gamry Instruments product model: Reference 3000 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 ...
Manufacturer's Name and Location: Gamry Instruments 734 Louis Drive Warminster, PA 18974 This declaration is for the Gamry Instruments product model: Reference 3000 Potentiostat/Galvanostat/ZRA The declaration is based upon compliance with the following directives: Electromagnetic Compatibility Regulations 2016 Electrical Equipment (Safety) Regulations 2016 ...
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