Advanced Measurement Technology 273A Manuel utilisateur

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a/k/a Princeton Applied Research, a subsidiary of AMETEK , Inc.

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Princeton Applied Research* warrants each instrument of its own manufacture to be free of defects in materialand workmanship.

Obligations under this Warrantyshall be limited to replacing, repairing or giving credit for the purchase price, at our option, of any

instrument returned, shipment prepaid, to our Service Department for that purpose within ONE year of delivery to the original

purchaser, provided prior authorization for such return has been given byan authorized representative of Princeton Applied

Research.

This Warranty shallnot applyto any instrument, which our inspection shall disclose to our satisfaction, to have become defective

or unworkable due to abuse, mishandling, misuse, accident, alteration, negligence, improper installation, or other causes beyond

our control. This Warrantyshall not apply to anyinstrument or component not manufactured by Princeton Applied Research.

When products manufactured by others are included in Princeton Applied Research equipment, the original manufacturer's

warrantyis extended to Princeton Applied Research customers.

Princeton Applied Research reserves the right to make changes in design at any time without incurring any obligation to install

same on units previously purchased.

THERE ARE NO WARRANTIES THAT EXTEND BEYOND THE DESCRIPTION ON THE FACE HEREOF. THIS WARRANTY

IS IN LIEU OF, AND EXCLUDES ANYAND ALL OTHER WARRANTIES OR REPRESENTATIONS, EXPRESSED, IMPLIED

OR STATUTORY, INCLUDING MERCHANTABILITYAND FITNESS, AS WELL AS ANYAND ALL OTHER OBLIGATIONS OR

LIABILITIES OF PRINCETON APPLIED RESEARCH, INCLUDING, BUT NOT LIMITED TO, SPECIAL OR CONSEQUENTIAL

DAMAGES. NO PERSON, FIRM OR CORPORATION IS AUTHORIZED TO ASSUME FOR PRINCETON APPLIED

RESEARCH ANY ADDITIONAL OBLIGATION OR LIABILITY NOT EXPRESSLY PROVIDED FOR HEREIN EXCEPT IN

WRITING DULY EXECUTED BY AN OFFICER OF PRINCETON APPLIED RESEARCH.

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A. Contact the Customer Service Department (865-482-4411) or your localrepresentative to discuss the problem. In manycases

it will be possible to expedite servicing by localizing the problem.

B. If it is necessary to send any equipment back for service, we need the following information.

1. Model number and serialnumber. 5. Your telephone number and extension.

2. Your name (instrument user). 6. Symptoms (in detail, including controlsettings).

3. Your address. 7. Your purchase order number for repair charges (does not apply to

repairs in warranty).

4. Address to which the instrument

should be returned. 8. Shipping instructions (if you wish to authorize shipment by any

method other than normal surface transportation).

C. U.S. CUSTOMERS —Ship the equipment being returned to:

Advanced Measurement Technology, Inc. PHONE: 865-482-4411

801 S. Illinois Avenue FAX: 865-483-2133

Oak Ridge, TN 37831

ATTN: Customer Service

D. CUSTOMERS OUTSIDE OF U.S.A. —To avoid delay in customs clearance of equipment being returned, please contact the

factoryor the nearest factory distributor for complete shipping information.

*Princeton Applied Research is a registered trademark of Advanced Measurement Technology, Inc. All other trademarks used herein are the

property of their respective owners.

iii

TABLE OF CONTENTS

Safety Instructions and Symbols ............................................................vi

Cleaning Instructions .....................................................................vi

1. INTRODUCTION .....................................................................ix

1.1. Overview ....................................................................... 1

1.2. About this Manual ................................................................. 1

1.3. Controlling the Model 273A .......................................................... 2

1.4. PolarityConvention ............................................................... 3

1.5. InspectionofNewInstrument ........................................................ 3

1.6. Maintenance and Service ........................................................... 3

2. SAFETYCONSIDERATIONS ........................................................... 5

2.1. Introduction ...................................................................... 5

2.2. Safety Mechanism ................................................................ 5

2.3. Power Voltage Selection and Line Fuses ............................................... 5

2.4. CellCable....................................................................... 7

2.5. Defects and Abnormal Stresses ...................................................... 8

2.6. Ventilation....................................................................... 8

2.7. This Apparatus as a Source of Radio Frequency Interference ................................ 8

2.8. TransientSensitivity ............................................................... 9

3. CHARACTERISTICS ................................................................. 11

3.1. Specifications ................................................................... 11

3.1.1. PowerAmplifier ............................................................ 11

3.1.2. DifferentialElectrometer ..................................................... 11

3.1.3. CurrentMeasurement........................................................ 11

3.1.4. Potential/CurrentControl ..................................................... 11

3.1.5. IR Compensation ........................................................... 12

3.1.6. System................................................................... 12

3.1.7. ComputerInterfaces......................................................... 12

3.1.8. Weight ................................................................... 12

3.1.9. Size ..................................................................... 12

3.1.10. Power Requirements ....................................................... 12

3.1.11. Rack Mounting ............................................................ 12

3.1.12. BatteryBackup............................................................ 12

3.1.13. Front-Panel Connectors ..................................................... 12

3.1.14. Rear-Panel Connectors ..................................................... 13

3.1.15. 273A/92 Electrochemical Impedance Interface Option .............................. 14

3.1.16. Accessories .............................................................. 14

3.1.17. PolarityConvention ........................................................ 14

3.1.18. MetricHardware........................................................... 14

3.2. Internal Organization ............................................................. 15

3.2.1. Introduction ............................................................... 15

3.2.2. Bus ..................................................................... 15

3.2.3. Applied Potentials and Currents ................................................ 15

3.2.4. AnalogCircuits............................................................. 15

3.2.5. Cell Switch and Relay ....................................................... 16

3.2.6. IR Compensation ........................................................... 18

3.2.7. Integration ................................................................ 18

3.2.8. AnalogtoDigital............................................................ 18

3.2.9. OUTPUT and AUX DIGITAL Connector .......................................... 18

iv Model 273A Potentiostat/Galvanostat User’s Manual

3.2.10. 273A/92 Electrochemical Impedance Interface Option .............................. 19

4. INITIALCHECKS.................................................................... 21

4.1. Introduction ..................................................................... 21

4.2. Required Equipment .............................................................. 21

4.3. Setup ......................................................................... 21

4.4. Procedure ...................................................................... 22

5. OPERATING INSTRUCTIONS .......................................................... 25

5.1. Introduction ..................................................................... 25

5.2. Front Panel ..................................................................... 25

5.2.1. Alphanumeric Display ........................................................ 25

5.2.2. I Overload and E Overload .................................................... 27

5.2.3. ScanStatusDisplay......................................................... 27

5.2.4. SCANSETUPGroup ........................................................ 28

5.2.5. INTERFACEGroup ......................................................... 35

5.2.6. CONTROLGroup........................................................... 36

5.2.7. MODEGroup.............................................................. 38

5.2.8. CELLGroup............................................................... 38

5.2.9. INPUTGroup.............................................................. 39

5.2.10. FILTERGroup ............................................................ 40

5.2.11. IRCOMPENSATIONGroup.................................................. 40

5.2.12. EMonitor ................................................................ 46

5.2.13. CURRENT RANGE Group ................................................... 46

5.2.14. OUTPUTGroup ........................................................... 47

5.3. Rear Panel ..................................................................... 48

5.3.1. CellInterface .............................................................. 49

5.3.2. RecorderInterface .......................................................... 49

5.3.3. Auxiliary Interface .......................................................... 50

5.3.4. PowerAmpMonitor ......................................................... 50

5.3.5. Aux A/D Input .............................................................. 50

5.3.6. ElectrometerMonitor ........................................................ 50

5.3.7. ACIOutput ............................................................... 50

5.3.8. ACEOutput............................................................... 50

5.3.9. MultiplexedOutput.......................................................... 51

5.3.10. AC Input ................................................................. 51

5.3.11. 273A/92 Electrochemical Impedance Interface Option .............................. 51

5.3.12. RS-232C Interface ......................................................... 51

5.3.13. IEEE-488/GPIB Interface .................................................... 51

5.4. DifferentialElectrometer........................................................... 51

5.5. Model 273A Standard Environmental Conditions ........................................ 53

5.5.1. Operating Conditions ........................................................ 53

5.5.2. Non-Operating Conditions .................................................... 54

5.5.3. International Standards ...................................................... 54

APPENDIX A. PINOUTS ................................................................ 55

A.1. CellInterface(36pins) ............................................................ 55

A.2. Recorder Interface (mating connector DP15P) .......................................... 55

A.3. Auxiliary Interface (mating connector DB9S) ........................................... 56

A.4. IEEE-488 GPIB Interface .......................................................... 57

A.5. RS 232C Interface ............................................................... 58

APPENDIX B. RACK MOUNTING ......................................................... 59

INDEX............................................................................... 61

WARNING Using this instrument in a manner not specified by the manufacturer may impair the protection

provided by the instrument.

CAUTION To prevent moisture inside of the instrument during external cleaning, use only enough

liquid to dampen the cloth or applicator.

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This manual contains up to three levels of safety instructions that must be observed in order to avoid personal

injury and/or damage to equipment or other property. These are:

DANGER Indicates a hazard that could result in death or serious bodily harm if the safety instruction is not

observed.

WARNING Indicates a hazard that could result in bodily harm if the safety instruction is not observed.

CAUTION Indicates a hazard that could result in property damage if the safety instruction is not observed.

Please read all safety instructions carefully and make sure you understand them fully before attempting to use

this product.

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To clean the instrument exterior:



Unplug the instrument from all voltage sources.



Remove loose dust on the outside of the instrument with a lint-free cloth.



Remove remaining dirt with a lint-free cloth dampened in a general-purpose detergent and water solution.

Do not use abrasive cleaners.



Allow the instrument to dry before reconnecting the power cord.

vi Model 273A Potentiostat/Galvanostat User’s Manual

1. INTRODUCTION

1.1. Overview

The Model 273A Potentiostat/Galvanostat features both front-panel and computer control for

virtually unlimited flexibility and utility. It uses the latest analog and microcomputer design

advances to provide high performance, ease of use, and greater versatility in electrochemical

measurements.

The instruments 100 V compliance and 1 A output capability allows rapid and accurate potential

or current control in virtually any electrochemical cell. The high compliance voltage is particularly

important in maintaining potential control when working with high-resistance, dilute electrolytes

or non-aqueous solvents. Moreover, it enables faster charging of the cell capacitance, allowing

the potentiostat to rapidly respond to step transitions in the control potential.

Component selection, shielding, grounding, and circuit design are all carefully optimized for

minimum internal electronic noise, giving high sensitivity and a quiet output signal. A low pass

filter facilitates dealing with noise arising in the cell itself.

The Model 273A uniquely addresses the critical question of stability versus speed. The user can

select a HIGH SPEED mode to take advantage of the potentiostat's extraordinarily fast rise time.

Alternatively, the user can select the HIGH STABILITY mode for oscillation-free operation with

almost any cell.

A high-performance, four-terminal current-to-voltage converter circuit is inducted for accurate,

rapid, low-drift current measurements, free of degradation from cell-cable resistance,

capacitance, and inductance.

The Model 273A uses an external differential electrometer. Not only does this approach further

assure freedom from cell-cable effects, but it allows the use of two reference electrodes to

control the potential across an interface, such as a membrane. In addition, the electrometer can

be configured to provide a remote sensing contact to the working electrode and so eliminate any

potential error resulting from high current in the contact resistance.

1.2. About this Manual

The Model 273A Potentiostat/Galvanostat can be operated either directly with its front-panel

controls or remotely from a personal computer or workstation. This Instruction Manual provides

details of the physical and electrical characteristics of the Model 273A, and describes how to

operate it as a stand-alone instrument controlled from its front panel.

Instructions for operating the unit remotely via either the RS-232C or GPIB (IEEE-488) interface

port are given in the separately bound Model 273A Remote-Programming Command Handbook.

In addition to the command descriptions, the Command Handbook gives detailed explanations of

GPIB (IEEE-488) and RS-232C communications, including rear-panel switch settings,

communications protocols, and some useful communications routines. Also included in the

Command Handbook is an application note on waveform programming„one of the most useful

functions of the Model 273A.

This Instruction Manual is organized into five chapters and three appendices. Chapter 1 provides

a general description of the Model 273A. Be sure you understand the information in Section 1.4

about the polarity convention used in this instrument.

The 100 V output and high current capability of the Model 273A make it potentially lethal if not

used with care and respect. Chapter 2 describes recommended safety precautions for operating

it. Chapter 2 also explains how to set the instrument for operation with different input power

voltages, replace the power line fuse, and determine whether power is applied to the counter

electrode connector.

2Model 273A Potentiostat/Galvanostat User’s Manual

Chapter 3 describes the physical and electrical characteristics of the instrument. It includes a

description of the electrical circuitry and internal organization of the instrument, and the functions

of the front- and rear-panel connectors. Pinouts of the connectors are given in Appendix A, and

schematic diagrams and component layouts are shown in Appendix C. After you inspect the

Model 273A for shipping damage, but before you begin to use it, run the initial performance

checks given in Chapter 4 to ensure that the instrument operates correctly. Then, using the

operating instructions given in Chapter 5, you may begin operation of your unit.

The Model 273A may be mounted in a standard 19-in. (475 cm) rack assembly. Appendix B

provides mounting instructions.

1.3. Controlling the Model 273A

Front-Panel Controls

The front panel is configured for maximum versatility in experiment definition. An optimally

human-engineered Scan Setup section is provided to allow cyclic staircase. voltammetry,

corrosion experiments, and other pulse and staircase waveforms to be easily performed. The

alphanumeric liquid crystal display assists in setting up an experiment and in presenting

real-time data. A Scan Status Display additionally provides continuously updated status

information as the experiment advances. A simple touch of a button implements such advanced

features as automatic current ranging and current-interrupt IR compensation. BNC connectors on

the front and rear panels make all pertinent signals available for analog recording.

Remote Computer Control

By interfacing the Model 273A to an external computer via the GPIB or RS-232C Interface,

complete remote control of the instrument is readily accomplished using the Electrochemical

Command Set, a group of over 100 mnemonic software instructions specifically developed for

electrochemical measurements. These commands place unprecedented flexibility in the hands

of the electrochemist. They provide:



Access to all front-panel functions.



Control of all timing functions.



Application of pulse and staircase waveforms



Automatic acquisition of data with or without current auto-ranging-



Data averaging in real-time.



Internal storage and arithmetic data manipulation.

These commands and all necessary instructions for operating the Model 273A via an external

computer are described in the separately bound Model 273A Remote-Programming Command

Handbook.

The Model 273A is fully equipped with the necessary hardware to implement experiments from

your computer, including:



Two 14-bit digital-to-analog converters for versatile waveform generation.



A 12-bit analog-to-digital converter to measure current and potential.



An on-board microprocessor to perform the experiment defined by the Command Set.



On-board memory to store the programmed parameters and data point values.

When the programmed experiment is finished, the data can be transferred to the computer for

plotting or further processing.

Chapter 1—Introduction 3

Warning! The protective grounding could be rendered ineffective in damaged apparatus.

Damaged apparatus should not be operated until its safety has been verified by

qualified service personnel. Damaged apparatus should be tagged to indicated to a

potential user that it may be unsafe and that it should not be operated.

1.4. Polarity Convention

The Model 273A follows the American polarity convention and the display indications are

consistent with that convention. Positive current is catholic, that is, a current is defined as

positive if reduction is taking place. Negative current is anodic, that is, a current is defined as

negative if oxidation is taking place.

In potentiostatic operation, making the applied potential more positive will make the current tend

to be more anodic. Conversely, making the applied potential more negative will make the current

tend to be more catholic. This is true for all potential sources, including EXTERNAL INPUT.

In galvanostatic operation, making the applied current more positive by any means except

applying a potential to the EXTERNAL INPUT will tend to make the current more catholic.

Making the applied current more negative will tend to make the current more anodic. This sense

is reversed at the front panel external input. Them making the input more positive will make the

cell current more anodic. Making the input more negative will make the cell current more

cathodic.

Bear in mind that the EXTERNAL INPUT is a high-impedance (100 k



) input in both

potentiostatic and galvanostatic operation. (In galvanostatic operation, 1 V applied results in a

full-scale current.)

1.5. Inspection of New Instrument

Newly received apparatus should be inspected for shipping damage. If any is noted, immediately

notify Princeton Applied Research and file a claim with the carrier. Save the shipping container

for possible inspection by the carrier.

1.6. Maintenance and Service

The Model 273A Potentiostat/Galvanostat has been designed for optimum reliability, and

requires no periodic maintenance.

This manual contains no service information. The Model 273A is very difficult to service in the

field; special fixtures and services are required that are not readily obtainable except at the

factory or at certain affiliate facilities. Contact the factory service department or the affiliate in

your area if service is required.

There are no operator serviceable parts inside. Refer servicing to qualified personnel.

4Model 273A Potentiostat/Galvanostat User’s Manual

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