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Model 600C Series
Electrochemical Analyzer/Workstation
User's Manual
CH Instruments
Table of Contents
Chapter 1. General Information
Introduction .......................................................................................................
Electrochemical Techniques ................................................................................
Software Features ..............................................................................................
System Requirements .........................................................................................
Hardware Specifications .....................................................................................
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1-3
1-5
1-9
1-10
Chapter 2. Getting Started
Installation .........................................................................................................
Testing ...............................................................................................................
Some Useful Tips ..............................................................................................
Installing USB Driver Under Windows ….…………………………………..
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2-3
2-4
2-5
Chapter 3. File Menu
Open Command .................................................................................................
Save As Command ............................................................................................
Delete Command ...............................................................................................
Retrieve Command ............................................................................................
Update Instrument Software Command ………………………………………
List Data File Command ...................................................................................
Convert to Text Command ................................................................................
Text File Format Command ...............................................................................
Import Text File Command ...............................................................................
Print Command ..................................................................................................
Print Multiple Files Command ...........................................................................
Print Setup Command ........................................................................................
Exit Command ...................................................................................................
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Chapter 4. Setup Menu
Technique Command ..........................................................................................
Parameters Command .........................................................................................
Parameters for Cyclic Voltammetry ...........................................................
Parameters for Linear Sweep Voltammetry ...............................................
Parameters for Staircase Voltammetry ........................................………..
Parameters for Tafel Plot ...........................................................................
Parameters for Chronoamperometry ..........................................................
Parameters for Chronocoulometry .............................................................
Parameters for Differential Pulse Voltammetry ........................................
Parameters for Normal Pulse Voltammetry ...............................................
Parameters for Differential Normal Pulse Voltammetry ............................
Parameters for Square Wave Voltammetry ................................................
Parameters for A.C. Voltammetry ..............................................................
Parameters for 2nd Harmonic A.C. Voltammetry ......................................
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Parameters for Amperometric i-t Curve ...................................................... 4-23
Parameters for Differential Pulse Amperometry ......................................... 4-25
Parameters for Double Differential Pulse Amperometry ............................. 4-27
Parameters for Triple Pulse Amperometry .................................…..…...... 4-29
Parameters for Integrated Pulse Amperometric Detection ..........…..…...... 4-31
Parameters for Bulk Electrolysis with Coulomtery .................................... 4-33
Parameters for Hydrodynamic Modulation Voltammetry .......................... 4-35
Parameters for Sweep-Step Functions …………………............................ 4-37
Parameters for Multi-Potential Steps ........................................................... 4-39
Parameters for A.C. Impedance .................................................….............. 4-40
Parameters for Impedance - Time ............................................................... 4-42
Parameters for Impedance - Potential ........................................................... 4-44
Parameters for Chronopotentiometry ......................................................... 4-46
Parameters for Chronopotentiometry with Current Ramp .......................... 4-48
Parameters for Mulit-Current Steps ............................………………........ 4-50
Parameters for Potentiometric Stripping Analysis ..................................... 4-51
Parameters for Electrochemical Noise Measurement .................................. 4-53
Parameters for Open Circuit Potential - Time ……..................................... 4-54
System Command ............................................................................................... 4-55
Hardware Test Command ................................................................................... 4-58
Chapter 5. Control Menu
Run Command ...................................................................................................
Pause/Resume Command ...................................................................................
Stop Run Command ...........................................................................................
Reverse Scan Command ...........…......................................................................
Run Status Command .........................................................................................
Repetitive Runs Command .................................................................................
Multiplexer Command .............................................................................……...
Macro Command ................................................................................................
Open Circuit Potential Command .......................................................................
iR Compensation Command ...............................................................................
Filter Setting Command ......................................................................................
Cell Command ....................................................................................................
Step Functions Command ...................................................................................
Preconditioning Command ..................................................................................
Rotating Disk Electrode Command .....................................................................
Stripping Mode Command ..................................................................................
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Chapter 6. Graphics Menu
Present Data Plot Command ...............................................................................
Overlay Plots Command .....................................................................................
Add Data to Overlay Command ..........................................................................
Parallel Plots Command ......................................................................................
Add Data to Parallel Command ..........................................................................
Zoom In Command ............................................................................................
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Manual Result Command ....................................................................................
Peak Definition Command ..................................................................................
X-Y Plot Command ............................................................................................
Peak Parameter Plot Command ..........................................................................
Semilog Plot Command ......................................................................................
Special Plot Command ......................................................................................
Graph Option Command .....................................................................................
Color and Legend Command ..............................................................................
Font Command ...................................................................................................
Copy to Clipboard Command .............................................................................
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Chapter 7. Data Processing Menu
Smoothing Command..........................................................................................
Derivatives Command ........................................................................................
Integration Command .........................................................................................
Semiinteg and Semideriv Command ....................................................................
Interpolation Command ......................................................................................
Baseline Fitting & Subtraction Command ...........................................................
Linear Baseline Correction Command ................................................................
Data Point Removing Command .........................................................................
Data Point Modifying Command ........................................................................
Bkgnd Subtraction Command .............................................................................
Signal Averaging Command ...............................................................................
Mathematical Operation Command .....................................................................
Fourier Spectrum Command ...............................................................................
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Chapter 8. Analysis Menu
Calibration Curve Command ................................................................................
Standard Addition Command ...............................................................................
Data File Report Command ............................…..................................................
Time Dependence Command ...............................................................................
Special Analysis Command ....................….........................................................
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8-7
8-9
Chapter 9. Simulation Menu
Mechanism Command ........................................................................................
Potentials and Rate Constants dialog box ..................................................
Concentration and Diffusion Coefficients dialog box ...............................
Surface Concentration dialog box .............................................................
Concentration at Equilibrium dialog box ..................................................
Simulation Variables dialog box ...............................................................
Simulate Command ............................................................................................
AC Impedance Simulator .....................................................................................
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Chapter 10. View Menu
Data Information Command ............................................................................... 10-1
Data Listing Command ....................................................................................... 10-3
Equation Command ............................................................................................
Clock Command .................................................................................................
Toolbar Command ..............................................................................................
Status Bar Command ..........................................................................................
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10-6
10-6
Chapter 11. Help Menu
Help Topics Command ....................................................................................... 11-1
About Command ................................................................................................ 11-2
Appendix
Cables and Connections .......................................................................…..........
Instructions of Software Update ………..............................................................
Trouble Shooting ...............................................................................................
Maintenance and Service ....................................................................................
Limited Warranty ..............................................................................................
Safety ............................................................................................…………….
Abbreviation of Electrochemical Techniques ......................................…..........
The Model 400 Series Electrochemical Quartz Crystal Microbalance ………..
Techniques for Model 600C Series Electrochemical Analyzer ................…......
Techniques for Model 700C Series Bipotentiostat .............................................
Techniques for Model 800B Series Electrochemical Detector ...……................
CHI900B Scanning Electrochemical Microscope ………………..……………
Model 1000A Series Multi-Potentiostat ……………………………..……..…
Model 1100A Series Power Potentiostat / Galvanostat ……………..……..….
Model 1200A Series Hand-held Potentiostat / Bipotentiostat ………………..…
CHI1550 Pico-Liter Solution Dispenser ……………………………..……..…
CHI200(B) Picoamp Booster and Faraday Cage ................................................
CHI684 Multiplexer ....................................……………………………...........
CHI680 Amp Booster ................................................................………………
CHI682 Liquid/Liquid Interface Adapter ...................................………………
Accessories ……………....................................................................….............
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Chapter 1. General Information
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Introduction
CHI6××C series are computerized electrochemical instruments. The Figure below
shows the block diagram of the instrument. The system contains a fast digital function
generator, a high speed data acquisition circuitry, a potentiostat and a galvanostat (not
available to certain models). The potential control range is ±10V and the current range is
±250mA. The instrument is capable of measuring current down to picoamperes. The
steady state current of a 10µm disk electrode can be readily measured. The instrument
provide very wide dynamic range in experimental time scales. For instance, the scan rate
in cyclic voltammetry can be up to 500V/s with a 0.1mV potential increment or 5000V/s
with a 1mV potential increment. The potentiostat/galvanostat uses 4-electrode
configuration, so that it can be used for liquid/liquid interface measurements, and to
eliminate the effect of contacting resistance of connectors and relays for high current
measurements. Multiplexed data acquisition systems allow an external input signal (such
as spectroscopy signals to be recorded simultaneously with electrochemical data. The
instrument will also automatically re-zero both potential and current, so that periodic recalibration of the instrument can be avoided.
The instrument is controlled by an external PC under Windows environment. It is
easy to install and use. The user interface follows Windows application design guide. If
you are familiar with Windows application, you can use the software even without
operation manual or on-line help. The commands, parameters, and options are in
terminology that most chemists are familiar with. The toolbar allows quick access to the
most commonly used commands. The help system provides context sensitive help. It is
systematic and complete.
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Chapter 1. General Information
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The instrument provides many powerful functions, such as file handling,
experimental control, graphics, data analyses, and digital simulation. Some of the unique
features include macro command, working electrode conditioning, color, legend and font
selection, data interpolation, visual baseline correction, data point removing, visual data
point modification, signal averaging, Fourier spectrum, and equations relating to
electrochemical techniques.
The 600C series is the upgrade from our very popular 600B series. Most
specifications are the same, but the analog-to-digital converter is changed from 12-bit to
16-bit. The maximum sampling rate is 1 M Hz. The software is stored in the FLASH
memory so that we can update software in the instrument by e-mail, instead of mailing
EPROM chips.
The 600C series has a serial port (default) and a USB for data communication
with the PC. You can select either serial port or USB by changing the jumper setting on
the board. However, you can use only one of them.
The 600C series also has a true integrator for chronocoulometry.
A 16-bit highly stable bias circuitry is used for current or potential bias. This
allows wider dynamic range is ac measurements. It can also be used for re-zero the dc
current output.
The model 600C series can be upgraded to be a bipotentiostat. The model 700C
series will be an add-on board to the 600C series. It will therefore be identical to the
600C series when used as single channel. When it is used as bipotentiostat, the 2nd
channel can be controlled at a independent constant potential, to scan or step at the same
potential as the first channel, and to scan with a constant potential difference with the
first channel. We will also try to make more voltammetric and amperometric techniques
work for 2nd channel.
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Chapter 1. General Information
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Electrochemical Techniques
Sweep Techniques
• Cyclic Voltammetry
• Linear Sweep Voltammetry
• Rotating Disk Electrode Voltammetry
• Tafel Plot
• Step-Sweep Functions
Step Techniques
• Chronoamperometry
• Chronocoulometry
• Staircase Voltammetry
• Tast Polarography
• Differential Pulse Voltammetry and Polarography
• Normal Pulse Voltammetry and Polarography
• Differential Normal Pulse Voltammetry and Polarography
• Square Wave Voltammetry
• Step-Sweep Functions
• Multi-Potential Steps
A.C. Techniques
• A.C. Voltammetry and Polarography
• Phase Selective A.C. Voltammetry and Polarography
• Second Harmonic A.C. Voltammetry and Polarography
• A.C. Impedance Spectroscopy
• A.C. Impedance versus Time
• A.C. Impedance versus Potential
Stripping Techniques
• Linear Sweep Stripping Voltammetry
• Differential Pulse Stripping Voltammetry
• Normal Pulse Stripping Voltammetry
• Square Wave Stripping Voltammetry
• A.C. Stripping Voltammetry
• Phase Selective A.C. Stripping Voltammetry
• Second Harmonic A.C. Stripping Voltammetry
Controlled-Current Techniques
• Chronopotentiometry
• Chronopotentiometry with Current Ramp
• Multi-Current Steps
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Chapter 1. General Information
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• Potentiometric Stripping Analysis
Amperometric Detection Techniques
• Amperometric i-t Curve
• Differential Pulse Amperometry
• Double Differential Pulse Amperometry
• Triple Pulse Amperometry
• Integrated Pulse Amperometric Detection
Other Techniques
• Bulk Electrolysis with Coulometry
• Hydrodynamic Modulation Voltammetry
• Open Circuit Potential - Time
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Chapter 1. General Information
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Software Features
User Interface
• 32-bit Windows application with multi-document interface
• toolbar: quick access to the most commonly used commands
• status bar: technique, file status, and command prompt
• pull-down menus
• dialog boxes
• full mouse support
• WYSIWYG graphics
• comprehensive and context sensitive help
File Management
• open data files
• save data file
• delete files
• list data file
• convert to text files: for exporting data to other software, such as spreadsheet
• text file format
• print present data
• print multiple data files
• print setup
Setup
• technique: full repertoire of electrochemical techniques
• experimental parameters: extremely wide dynamic range
• system setup: communication port, polarity of potential and current axis
• hardware test: digital and analog circuitry diagnostic test
Instrument Control
• run experiment: real time data display in most cases
• pause/resume during run
• stop running experiment
• reverse scan direction during run: for cyclic voltammetry
• repetitive runs: automatic data save, signal averaging, delay or prompt
• run status: stir, purge, iR compensation, smooth after run, RDE and SMDE control
status
• macro commands: edit, save, read, and execute a series of commands
• open circuit potential
• iR compensation: automatic and manual compensation, solution resistance, double
layer capacitance and stability test
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Chapter 1. General Information
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• analog filter setting: automatic or manual setting of potential, i/V converter, and
signal filters
• cell control: purge, stir, cell on, SMDE drop collection, pre-run drop knock, and
stabilizing capacitor
• step functions: multiple cycles of step function generator, for electrode cleaning or
other purposes
• working electrode conditioning before running experiment
• rotating disk electrode: (Model 630/650/660) rotation speed, on/off control during
deposition, quiescent time, run, and between runs
• stripping mode: enable/disable, deposition potential and time, stir and purge
conditions
Graphic Display
• present data plot: data plot together with header, filename, parameters, and results
• re-scaling and labeling: axis expression, re-scale and text insertion
• overlay plots: several sets of data overlaid for comparison
• parallel plots: several sets of data plotted side by side
• zoom in: visually selected zoom area
• manual results: visually selected baseline
• peak definition: shape, width, and report options
• X-Y Plot: for your own data points
• peak parameter plot: ip~v, ip~v1/2, Ep~log(v) plots
• semilog plot: current-potential semilog plot
• graph options: video or printer options, axis, parameters, baseline, results, grids,
axis inversion, axis freeze, axis titles, data sets, XY scales, reference electrode,
header, and notes
• color and legend: background, axis, grid, curves, legend size, thickness, and display
intervals
• font: font, style, size and color for axis labels, axis titles, header, parameters, and
results
• copy to clipboard: for pasting the data plot to word processors
Data Processing
• smoothing: 5-49 point least square and Fourier transform
• derivatives: 1st - 5th order, 5-49 point least square
• integration
• convolution: semi-derivative and semi-integral
• interpolation: 2× - 64× data interpolation
• baseline fitting and subtraction: selectable fitting function, polynomial order and
potential range for best fitting and baseline subtraction; particularly useful for trace
analysis
• linear baseline correction: visually selected baseline, slope and dc level
compensation
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Chapter 1. General Information
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•
•
•
•
•
•
data point removing
data point modifying: visual data point modification
background subtraction: difference of two sets of data
signal averaging: averaging multiple sets of data
mathematical operations: both X and Y data array
Fourier spectrum
Analysis
• calibration curves: calculate the unknown concentration and the slope, intercept, and
correlation of the curve; plot the calibration curve; save and read the calibration data
• standard addition: calculate the unknown concentration and the slope and
correlation of the standard addition curve; plot the standard addition curve; save and
read the standard addition data
• data file report: calculate the unknown concentration from the saved data files based
on user defined peak potential range, species, and calibration information. An
analytical report in text format will be generated.; maximum four species of interest
can be defined
• time dependence: calculate the unknown concentration as the function of time from
the saved data files based on user defined peak potential range, and calibration
information; the concentration as function of time will be reported or plotted
Digital CV Simulation
• fast implicit finite difference algorithm
• reaction mechanisms: 10 predefined mechanisms (Model 620C and below); any
combination involving electron transfer, first- and second-order chemical reactions
(Model 630C/650C/660C)
• system: diffusive or adsorptive
• maximum equations: 12
• maximum species: 9
• simulation parameters: standard redox potential, rate of electron transfer, transfer
coefficient, concentration, diffusion coefficient, forward and reverse chemical
reaction rate constants, temperature, electrode area, and experimental parameters
• save simulation parameters
• read simulation parameters
• real time data display
• real time display of concentration profiles
• dimensionless current
• equilibrium data
• automatic search and determine over-determined equilibrium constants
Ac Impedance Simulation and fitting program
• visually equivalent circuit input
• automatic equivalent circuit parameters fitting
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Chapter 1. General Information
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View
• data information: date, time, filename, data source, instrument model, data
processing performed, header and notes
• data listing: data information and numerical data array
• equations: general equations and equations relating to various electrochemical
techniques
• clock
• toolbar
• status bar
Help
• context sensitive help
• index
• using help
• about the application
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System requirements
Operating System: PC with Microsoft Windows 95 / 98 / NT / Me / 2000 / XP
Communication between PC and instrument: RS-232 serial port or USB port
Output device: any printer or plotter supported by Windows
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Hardware Specifications
Potentiostat
Galvanostat (Model 606C, 608C, 660C only)
Potential: ±10 V
Current: ±250 mA
Compliance Voltage: ±12 V
Potentiostat rise time: < 1 µs
Four-Electrode Configuration
Input Impedance of Reference Electrode: 1012 Ω
Minimum Potential Increment in Sweep Techniques: 100 µV
Potential Update Rate: 5 MHz
Potential Scan Rate: 20,000 V/s
Maximum Sampling Rate: 1 M Hz (16-bit)
Current Measurement Range: 1×10-12 - 0.1 A/V in 12 ranges
True integrator for chronocoulometry
Input Bias Current: below 50 pA
Low Current Measurability: below 1 pA
Automatic Re-zeroing: both potential and current against drift
Cell Control: purge, stir, and knock
RDE Rotation Rate Control: 0-10V voltage output for 0 - 10000 rpm
Instrument Dimension: 12.5” (width) × 11” (depth) × 4.75” (height)
Weight: ~12 lb.
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Chapter 2. Getting Started
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Installation
Important Note:
After you unpack the instrument, please check the content carefully. You should find the
instrument, the USB cable, the electrode leads, the software CD-ROM and the User’s Manual. If
you see anything missing, please search carefully inside the box, since the missing items may be
mixed with the packing material. Please do not dump the packing material and box and report
any missing and damage immediately. You should not report missing and damage days later after
you open the packing box.
The instrument does not come with electrodes and other accessories. You need to order
them separately. If you ordered electrodes and accessories, please check carefully and compare
with the packing list. If you see anything missing, please search carefully inside the box, since
the missing items may be mixed with the packing material. Please do not dump the packing
material and box and report any missing and damage immediately. You should not report missing
and damage days later after you open the packing box.
Software:
The instrument will be controlled by an IBM PC with Windows 95/98/NT/Me/2000/XP
operating system. A free serial port or a USB port is required for communication between the
instrument and the computer.
Windows Vista can control the instrument properly, but it has two known problems. It
sometime can not display correctly. The program may not paint single pixel dots correctly and
leave blanks on some area of screen. It was not a problem for all previous versions of Windows,
not for Windows 7 either. You have to choose other legends (such as circle, square, triangle or
line) in the software for data plot to be shown completely. It also does not support all previous
Windows' help files, even the help file was developed using Microsoft development tools. This
problem can be solved by downloading KB917607 service pack from Microsoft website.
The current software is a 32-bit Windows application. It will not work under 64-bit
Windows
Windows 7 32-bit will not control the instrument properly. We are studying this issue.
Refer to your Windows User Manual to be familiar with Windows operation.
To install the software, insert the software CD-ROM. You can run "SET####.EXE" on
the CD-ROM directly to extract the files and the files will be automatically copied to the hard
drive. The default directory is C:\CHI. It is very important to use it for the program and
configuration files. The C:\CHI directory is used for the automatically generated configuration
file (*.cfg). When the program starts, it will always look for the existing configuration file in
C:\CHI directory. When the program ends, it will save the configuration file to the C:\CHI
directory. If the program can not find C:\CHI directory, the configuration files will be spread
everywhere. Next time the program starts, it will not be able to use the configuration file for
customized setting by the user. Once the files have been copied, you can use Windows Explorer
or File Manager to find the executable file "CHI####.EXE" in the C:\CHI subdirectory (or
folder). Double click the filename to start the program.
The installation just copies all the files to the C:\CHI directory. After installation, you
should find CHI####.EXE (executable program), CHI####.HLP (help file) and some test data
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files (*.BIN) in the C:\CHI directory. It is safe to delete any files in the C:\CHI directory later.
In the CD-ROM, you can also find the electronic version of the User’s Manual and the
USB Driver.
Hardware:
The system hardware installation is also easy and simple. After unpacking the
instrument, you should check the power lines. The A.C. voltage was preset in the factory and
is indicated in the serial number label on the back panel. If the A.C. voltage is correct, connect
the instrument to the power through the power cord.
Communication between the instrument and PC is through RS-232 serial port or USB
port. However, you can only use one of them. The default is the serial port. If your computer has
a free serial port (9-pin male connector), it can directly communicate with the instrument. You do
not need to install extra software. If your computer does not have a serial port, you can use USB
port for communication. However, you need to change the jumper position inside the instrument
and install software.
If you use serial port for communication, connect the Com Port 25-pin connector at the
rear panel to the serial port of your PC. The cable is a 9F-25M serial cable (comes with the
instrument). You may need to set the software to a proper port. The default is COM 1. This
setting can be altered through the System command under the Setup menu. You don’t have to
worry about the baud rate. After you alter the setting, please exit the program and restart the
program.
It is important to have a computer with a free serial port. Most computers specify one or
two serial ports. However, they might be used by mouse and fax/modem. Usually COM 2 is not
free. It is recommended to use computers with PS/2 mouse. Since PS/2 mouse does not use com
port, you will have COM 1 as a free com port, and you can still have the fax/modem card
installed. PS/2 mouse is very popular nowadays.
If you have the serial port, we suggest you not to worry about the USB. The USB is really
a USB-Serial adapter. It is a true USB, but it converts the USB to serial port by using the
software provided by the USB chip vendor. It is therefore provide no specific advantages over
the serial port. The reason we put it there is because some computers (such as notebook
computers) may not have the serial port.
If you can not locate a free serial port on your computer, you can try to use USB port to
communication. In order to do so, you need to change the switch setting inside the instrument
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and install the driver software. Figure 2.1 shows the switch position and how to set the selection.
Figure 2.1 Serial port or USB port switch selection. A littler above the 100-pin processor chip, as
pointed by the arrow, there are 6-pin holes (two rows and three columns) for contact block. Wirejumpers are used for setting. The default switch setting is at the left position for RS-232 serial
port selection. If you change the setting by switching to the right position, the selection is the
USB port.
detail.
In the later portion of this chapter, the USB driver software installation is described in
If you consistently get "Link Failed" message, try other computers. The instrument we
delivered was turned on for a week and tested. Nearly in all the cases, the "Link Failed" message
is caused by the computer serial port problem.
The unreliable data communication could be due to some background tasks that generate
interrupt. The serial port data communication is based on interrupt. For some reason Microsoft
Windows makes the priority of interrupt for serial port lower and lower. Other devices, such as
disk access, screen saver, virus scan, internet connection, etc, will all generate interrupt that
could interfere with the serial port data communication. Please turn off the screen saver,
disconnect internet connection, disable virus scan program, and try again.
You should also not use network card. Network will generate background interrupt that
interfere with the data transfer between the PC and the instrument. You should disconnect the
connector to the network card.
If you consistently get Link Failed message after all the efforts, please try USB as the
communication port.
Once the instrument and PC can communicate, you can connect the electrode leads to the
rear panel. The clip with green cover is for the working electrode, the white one is for the
reference electrode, and the red one is for the counter electrode. The black one is a sensing
electrode. Please check the Appendix of this User’s Manual for description of 4-electrode
configuration and the sensing electrode usage.
The Cell Control on the rear panel can be used to control purge, stir, and mercury drop
dislodge. It is also used to control external adapters, such as CHI200B Picoamp Booster, CHI680
Amp Booster, CHI684 Multiplexer, etc. Please see the Appendix for more information.
If you have a Pine Instrument AFMSRX Rotator for RDE, it is possible for the instrument
to control the RDE with the instrument (Model 630C/650C/660C only). Two banana jacks on the
rear panel will provide a voltage of 0 - 10 V, corresponding to a rotation rate of 0 - 10,000 rpm.
You are now ready to use the instrument.
Testing
The instrument was tested before it was shipped. The “*.bin” files that come with the disk
are the data actually acquired with the particular instrument you received .
To test the communication between the computer and the instrument, start the software
and turn the instrument power on. Use the Hardware Test command under the Setup menu. If a
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“Link Failed” message appears, you should check the connection and the port setting. You can
use System command under the Setup menu to see if the port setting matches the port in use.
If the hardware test results appear on the screen, the communication is working. You may
watch the hardware test results and see if everything is okay.
If you want to see if the system will run experiment properly, you can use a 100K ohm
resistor as a dummy cell. Short the reference (white) and counter (red) electrode leads, and
connect the 100K ohm resistor between the red/white clips and working (green) electrode clip.
Select the potential range between 0.5V to -0.5V through the Parameters command under Setup
menu. The sensitivity can be set at 1e-6A/V. Run the experiment through the Run command
under the Control menu. You should see a straight line with current from –5e-6A to +5e-6A.
To test the software performance, you can open a data file through the Open command
under the File menu. There are test data that come with the software. These are the actual test
results of this particular instrument. To open the file, select the file and click OK button, or you
may double click the filename. After you read the data, you can display or process the data. Try
all the commands under the Graphics and DataProc menus. If you don’t feel comfortable about
the changed data, you can reload the data through the Open command again.
Some Useful Tips
If you are familiar with Windows applications, you may not have any problem to use the
instrument. Most of the following tips are for users who do not have much experience with
Windows. However, some of the tips could be helpful to every one.
1.
You should get familiar with the toolbar (a bar with many buttons under the main
menu bar). The toolbar provides quick access to the most commonly used commands. To know
the meaning of the command buttons, click the button and read the comments at the left-lower
corner of the screen.
2.
To select multiple filenames for multiple file printing, overlay or parallel plots,
click the first file name you want to select, drag the mouse down while holding the left button,
you will select successive files. If the files are scattered in the directory, you can select them by
holding the Ctrl key while click each filename.
3.
If you see that the Y axis title is in wrong direction, you can use the Font
command under the Graphics menu to change the rotation angle of Y axis for printing.
4.
To select a file or a technique, you can double click the item. It is equivalent to
click the item and then click OK.
5.
To change the parameters, you can use the TAB key to go through each items. The
text in the edit box will be highlighted. You can directly type the new text. Sometimes, it is
much more convenient and faster than using mouse click and drag.
6.
The internal noise of the instrument is quite low. The most common and most
serious noise source is the line frequency (60 Hz or 50 Hz). There are analog low-pass filters to
reduce noises. At a scan rate of 0.1 V/s, the automatic filter cutoff setting is at 150 or 320 Hz.
The line frequency will pass and noise appears. At a scan rate of 0.05 V/s, the cutoff frequency of
the filter is 15 or 32 Hz. The line frequency noise can be effectively reduced. The line frequency
noise can be reduced if the sample interval is set at multiples of the period of power lines. For
small signals and relatively fast experiments, faraday cage is strongly recommended.
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7.
To display data in different ways, use the Graph Options command under the
Graphics menu. Check Page 6-1 of this manual for available data display formats.
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Installing USB driver under Windows
If you have the serial port, we suggest you not to worry about the USB. The USB is really
a USB-Serial adapter. It is a true USB, but it converts the USB to serial port by using the USB
driver software provided by the USB chip vendor. It is therefore provide no specific advantages
over the serial port. The reason we put it there is because some computers (such as notebook
computers) may not have the serial port.
On the other hand, the USB-serial port driver software may not be perfect. We tried all the
computers that has USB port in our office, they all seem to work, but when it is not working,
besides the installation instructions, we really do not know how to further diagnose and support it,
since the software is not provided by us, we have no control on it.
If you still want to go for it, please set the USB/Serial selection switch inside the
instrument (please see Figure 2.1) and following the following instructions to install the USB
driver software.
(1) Find the CP2101 USB driver software on the software CD-ROM.
(2) Double click the file CP2101.EXE, the following dialog box will appear:
Click “Unzip” button to unzip the files to c:\CP2101 (by default) or other folder.
(3) Go to c:\CP2101 (or other folder), you will find a “SETUP.EXE” file. Double click this filename, a following
dialog box will occur.
Click “Install” button will start installation process. Wait long enough time until the installation is completed.
(4) Connect USB cable (type A-B) from your computer to the instrument. The first time you make the connection,
the computer will prompt new USB device found and will automatically look for the driver and further install it.
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Please wait until this process is completed.
(5) This USB device is really a USB-Serial Port Converter. Under the instrument software, it treats this device as a
serial port. You need to find what port number is assigned to this device. Please select Control Panel (from your
computer Start menu at the lower-left corner) -> Performance and Maintenance -> System -> Hardware ->
Device Manager-> Ports (COM & LPT). You will see the following information:
In this example, USB is assigned to COM5. This number may vary with different computers. It may varies even
with the same computer sometimes (quite rarely). You need to use the System command under the Setup menu to set
the com port number.
In the future, if you see “Can not open comport” error when you start the program, please check Device Manager
again and see what com port number is assigned. If the com port number assignment is changed, you need to set the
com port number in the program accordingly. If you do not see CP2101 icon under the Ports (COM & LPT), please
make sure if your instrument is turned on and the USB cable is connected properly.
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Open Command
Use this command to read an existing data file.
You can only open one data file at a time. This will be the active data. When the
file is read, it places data in the memory and the graphics are updated. The technique and
experimental parameters are also updated. You can only open files generated by this or
an older version of the software.
Since the software uses a multi-document interface, you can open multiple files
by repeating this command.
This command presents an Open dialog box:
The following options allow you to specify the file to select:
File Name
Type or select the filename. This box lists files with the extension you select in
the List Files of Type box.
You don't have to type the extension, the system will automatically attach a “.bin”
extension to the filename.
List Files of Type
Select the type of files you want to open. Only “.bin” (binary data file) is
available.
Drives
Select the drive in which the file is stored.
Directories
Select the directory in which the file is stored.
This command has a toolbar button:
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Save As Command
Use this command to save and name a file.
This command presents a Save As dialog box:
The following options allow you to specify the name and location of the file
you're about to save:
File Name
Type a new filename to save the current data and many variables. A filename can
contain up to eight characters. If an existing filename is used, the system will display
a warning and then proceed.
You don't have to type the extension, the system will automatically attach an
extension to the filename. For a data file, the extension is ".bin" (binary file). For a
macro file, the extension is ".mcr". For a simulation file, the extension is ".sim".
Other extension is not allowed.
List Files of Type
Select the type of file you want to open. Only “.bin” (binary data file) is available.
Drives
Select the drive in which you want to store the file.
Directories
Select the directory in which you want to store the file.
This command has a toolbar button:
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Delete Command
Use this command to delete files.
This command presents a File Deletion dialog box:
The following options allow you to specify the name and location of the file
you're about to delete:
File Name
Type or select the filename(s) you want to delete. This box lists files with the
extension you select in the List Files of Type box. To delete multiple files, point the
mouse cursor to the filename(s) you want to select and click the left mouse button,
while holding the Ctrl key.
The system adds the extension you specify in the Delete Type box.
List Files of Type
Select the type of file you want to delete.
Drives
Select the drive that contains the file(s) you want to delete.
Directories
Select the directory that contains the file(s) you want to delete.
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Retrieve Command
Use this command to retrieve data saved on the hard drive during run. In case an
experiment does not complete due to external interference, interruption, or miss
communication, the data can be partially recovered. This is useful for very slow
experiments. Hours of experimental data can be recovered with this command.
This command is not active by default. If you do not run very slow experiments,
you can re-run the experiment if it is accidentally interrupted. In order to activate this
command, use System under the Setup menu. Check the "Save retrieve data during run"
option.
If you want to retrieve the last run data, do it before you start a new run otherwise
the data will be lost.
Update Instrument Software Command
Use this command to update the software on the instrument side. Only certain
instrument models have this command. If your instrument has this command, please
check the “Instructions of Software Update” Appendix of this User’s Manual,
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List Data File Command
Use this command to list a data file in a text mode. The text format can be altered
with the Text File Format command.
The current data remains unchanged. To view the numerical list of the current
data, execute the Data Listing command under the View menu.
This command presents a List Data File dialog box:
The following options allow you to specify the name and location of the file
you're about to list in a text mode:
File Name
Type or select the filename you want to list. This box lists files with the
extension you select in the List Files of Type box.
You don't have to type the extension. The system will automatically attach an
extension of ".bin" to the filename. Other extensions are not allowed.
List Files of Type
Select the type of file you want to list. Only ".bin" (binary data file) is available.
Drives
Select the drive in which you want to list the file(s).
Directories
Select the directory in which you want to list the file(s).
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Convert to Text Command
Use this command to convert a binary data file to a text file. The text format can
be altered with the Text File Format command.
Multiple files can be selected for conversion. To select multiple files, point the
mouse cursor to the filenames you want to select and click the left mouse button, while
holding the Ctrl key.
The text file can be read by other commercial softwares, such as spread sheet and
data-base handlers.
This command presents a File Conversion dialog box:
The following options allow you to specify the name and location of the binary
file(s) you're about to convert to a text file:
File Name
Type or select the filename(s) you want to list. This box lists files with the
extension you select in the List Files of Type box.
Multiple files can be selected for conversion.
You don't have to type the extension. The system will automatically attach an
extension of ".bin" to the filename. Other extensions are not allowed.
List Files of Type
Select the type of file you want to convert. Only ".bin" (binary data file) is
available.
Drives
Select the drive in which you want to convert the file(s).
Directories
Select the directory in which you want to convert the file(s).
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Text File Format Command
Use this command to select the data format in the text mode.
This command presents a Text File Format dialog box:
The following options allow you to specify the text file format:
Memo
Check this check box if you want the date, time, technique name, labels, and notes
to be included in the output text file.
Parameters
Check this box if you want experimental parameters to be added to the output file.
Results
Check this box if you want experimental results such as peak or wave potential,
current and electrode area to be listed. To select the item to be displayed on screen
when an experiment is complete, execute the Peak Definition command under the
Graphics menu.
Numeric Data
Check this box if you want the numeric data points to be listed.
Separator
Select the separator (comma, TAB, space, or linefeed) to be used between X and
Y data colummns. The data columns will have one of the following format:
X, Y
(comma)
X
Y
(TAB)
X Y
(space)
X
Y
(linefeed)
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This allows you to make the data format compatible with other commercial
software, such as spread-sheet and data base handlers.
Number of Significant Figures
It allows you to control the data precision of the text file. The default is 4
significant digits. This is sufficient for most applications. You can change the setting
to a maximum 10 significant digits. However, more significant digits result larger
data files.
Data Point Interval
This allows you to store or display only a part of the data points. It is helpful
when examining data or to reduce file size. However, some details might be lost.
DigiSim Format for CV and LSV Data
This is only for CV and LSV data. When this box is checked, the text data file
will be readable directly by DigiSim ( Bioanalytical Systems, West Lafayette, IN).
Excel 3D Format
This is only for SECM image data. When this box is checked, the output text data
file will be readable directly by Excel (Microsoft Corp., Redmond, WA) to generate
a 3D surface plot.
To generate Excel 3D surface plots, follow these instructions:
1. Start the Excel Program.
2. Open the target text data file created by the CHI900/CHI900A/CHI900B
program.
3. The "Text Import Wizard - Step 1 of 3" dialog box will appear. Click "Next".
4. The "Text Import Wizard - Step 2 of 3" dialog box will appear. Select
Delimiters to match the data separator used in the output text file format (see above).
Click "Next".
5. The "Text Import Wizard - Step 3 of 3" dialog box will appear. Click "Finish".
A spread-sheet containing the data will appear.
6. Select all data points from the spread-sheet.
7. Click the "ChartWizard" button on the toolbar.
8. Move the mouse cursor to the spread-sheet data area, click the left mouse
button.
9. The "ChartWizard - Step 1 of 5" dialog box will appear. Click "Next".
10. The "ChartWizard - Step 2 of 5" dialog box will appear. Choose "3D Surface"
and click "Next".
11. The "ChartWizard - Step 3 of 5" dialog box will appear. Choose "1" or "2"
and click "Next".
12. The "ChartWizard - Step 4 of 5" dialog box will appear. You should read
"Data series in Row", "Use First 1 Row(s) for Category (X) Axis Labels", "Use First
Column(s) for Series (Y) Axis Labels". Click "Next".
13. The "ChartWizard - Step 5 of 5" dialog box will appear. Decide if you want to
add a legend, a chart title or Axis Titles for X, Y and Z. Click "Finish".
14. A 3D surface plot will appear in the spread-sheet data area. You can resize the
graph by moving the cursor to the corner of the graph until you see the cursor change
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to a small dual arrow connected with a diagonal line. Press down the left button and
drag the mouse. You can see that the graph can be enlarged or reduced.
15. Once the graph selected (click), copy it (using the Copy command under the
Edit menu or click the Copy button on the toolbar). You can then paste the graph into
a word processor for further usage or print. Please be aware that exporting the graph
to a picture format like Bitmap or JPEG in Excel and subsequently inserting the
picture into the word processor document generally reduces the final files’s size.
If the data density is so high that the lines that connect the data points cannot be
seen clearly, set the data point interval to more than 1.
Nanoscope Header
This is only for SECM image data. When this box is checked, a header will be
added to render the text data file readable directly by the Nanoscope software
(Veeco Instruments Inc., Santa Barbara, CA) to create a 3D image. However,
Veeco Instruments regularly updates the Nanoscope software, your generated file
may therefore nit be readable if your version is older than that used in the CHI900B
software.
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Import Text File Command
Use this command to import text files. Currently it will read the CHI text file
format as well as BAS text file format.
This command presents an Import Text File dialog box:
For CHI files, the memo and the parameters are required to import a text file.
Since some BAS parameters are different from the CHI parameters, BAS
parameters will be adjusted to be CHI parameters.
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Print Command
Use this command to print data. The printer output is identical to what is
displayed on the screen. Use the Graph Option command under the Graph menu to
customize the print output.
The paper must oriented as landscape. If a warning pops up, use the Print Setup
command to set the paper orientation properly. This setting will however, will not be
saved once you quit the program. In order to set the paper orientation to landscape
permanently, you need to run the “Printer Manager” in the Main window and execute the
“Printer Setup” command.
This command has a toolbar button:
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Print Multiple Files Command
Use this command to print multiple data files. The printer output is identical to
what is displayed on the screen. Use the Graph Option command under the Graphics
menu to customize the print output.
This command presents a Multiple File Print dialog box:
The following options allow you to specify the name and location of the binary
data files you're about to print:
File Name
Type or select the filename(s) you want to print. This box lists files with the
extension you select in the List Files of Type box. To select multiple files, point the
mouse cursor to the filename(s) you want to select and click the left mouse button
while holding the Ctrl key.
You don't have to type the extension, the system will automatically attach a ".bin"
extension to the filename. Other extensions are not allowed.
List Files of Type
Select the type of file you want to print. Only ".bin" (binary data file) is available.
Drives
Select the drive from which you want to print the file(s).
Directories
Select the directory from which you want to print the file(s).
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Print Setup Command
Use this command to select a printer and a printer connection.
This command presents a Print Setup dialog box:
The following options allow you to select the destination printer and its
connection.
Printer
Select the printer you want to use. Choose the Default Printer; or choose the Specific
Printer option and select one of the currently installed printers available in the box.
You can install printers and configure ports through the Windows Control Panel.
Orientation
Choose Portrait or Landscape. The paper orientation has to be landscape in the CHI
program environment. If a warning pops up, use the Print Setup command to set the
paper orientation properly. This setting will however not be saved once you quit the
program. In order to set the paper orientation to landscape permanently, you need to
set the printer to Landscape globally by changing the printer setting in Windows
Control Panel. Double click the Printer Manager icon to activate the program. Choose
the Print Setup command under the Option Menu. You will be able to set the default
to Landscape. Other softwares may have their own default settings. The global setting
will not affect those programs.
Paper Size
Select the size of the paper that will be used to print documents.
Paper Source
Some printers offer multiple trays with different paper sources. Specify the tray here.
Options
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This displays a dialog box where you can make additional choices about printing,
depending on the specific printer you have selected.
Exit Command
Use this command to end your application session.
Upon exit, some of the system information, such as file directory, system setup,
control status, macro command, data processing options, simulation options, graphics
options, color and font will be saved.
Shortcuts
Mouse:
Keys:
Double-click the application's Control menu button.
ALT+F4
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Technique Command
Use this command to select an electrochemical technique.
This command presents an Electrochemical Techniques dialog box:
The following options allow you to select an electrochemical technique:
Technique Selection
Select the electrochemical technique you want to use. This box lists the techniques
available in the instrument. Double clicking the technique you want to select is equivalent to
selecting the technique and clicking the OK button.
Polarographic Mode
Check this box will enable the polarographic mode. In the polarographic mode, the
mercury drop will be allowed to grow and be dislodged for every data point.
Only a few techniques are allowed to have polarographic mode: Sampling Current
(Staircase) Polarography (SCP), Differential Pulse Polarography (DPP), Normal Pulse
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Polarography (NPP), Differential Normal Pulse Polarography (DNPP), A.C. Polarography
(ACP), and Second Harmonic A.C. Polarography (SHACP).
Once polarographic mode is enabled, stripping mode is disabled. In order to set stripping
mode by using the Stripping Mode command in Control Menu, you have to uncheck the
polarographic mode.
This command has a toolbar button:
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Chapter 4. Setup Menu
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Parameters Command
Use this command to set experimental parameters.
This command presents a Parameter dialog box so you can select the parameters you
want to use.
Depending on the technique, the parameters dialog box will be different. The followings
are the parameters for different techniques:
Parameters for Cyclic Voltammetry
Parameters for Linear Sweep Voltammetry
Parameters for Sampled Current Voltammetry
Parameters for Tafel Plot
Parameters for Chronoamperometry
Parameters for Chronocoulometry
Parameters for Differential Pulse Voltammetry
Parameters for Normal Pulse Voltammetry
Parameters for Differential Normal Pulse Voltammetry
Parameters for Square Wave Voltammetry
Parameters for A.C. Voltammetry
Parameters for 2nd Harmonic A.C. Voltammetry
Parameters for Amperometric i-t Curve
Parameters for Differential Pulse Amperometry
Parameters for Double Differential Pulse Amperometry
Parameters for Triple Pulse Amperometry
Parameters for Integrated Pulse Amperometric Detection
Parameters for Bulk Electrolysis with Coulomtery
Parameters for Hydrodynamic Modulation Voltammetry
Parameters for Sweep-Step Functions
Parameters for Multi-Potential Steps
Parameters for A.C. Impedance
Parameters for Impedance - Time
Parameters for Impedance - Potential
Parameters for Chronopotentiometry
Parameters for Chronopotentiometry with Current Ramp
Parameters for Multi-Current Steps
Parameters for Potentiometric Stripping Analysis
Parameters for Open Circuit Potential - Time
For details of the parameters of each technique, see the description of individual dialog
box of related techniques.
This command has a toolbar button:
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Chapter 4. Setup Menu
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Parameters for Cyclic Voltammetry
In Cyclic Voltammetry (CV), potential is scanned from Init E toward either High E or
Low E depending on the Init P/N. The potential will then scan back. The following diagram
shows the potential waveform applied as the function of time. The current is recorded as the
function of potential.
Potential(V)
High E
Scan Rate (V/s)
Init E
Low E
Segment 1
Segment 2
Segment 3
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Init E (V)
High E (V)
Low E (V)
Init P/N
Scan Rate (V/s)
Sweep Segments
Sample Interval (V)
Quiet Time (sec)
Sensitivity (A/V)
Auto Sens
Scan Complete Cycles
Auxiliary Signal
Recording
Notes:
Range
-10 - +10
-10 - +10
-10 - +10
Positive or Negative
1e-6 - 20000
1 - 1000000
1e-6 - 0.064
0 - 100000
1e-12 - 0.1
Check or Uncheck
Check or Uncheck
Check or Uncheck
Description
Initial potential
High limit of potential scan
Low limit of potential scan
Initial scan direction
Potential scan rate
Sweep segments, each segments is half cycle
Data sampling interval
Quiescent time before potential scan
Sensitivity scale
Automatic sensitivity switching during run
Scan complete cycles
Simultaneously external signal recording
when the scan rate is less than 0.25V/s
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1. High E and Low E should be at least 0.01 V apart.
2. If unreasonable High E and Low E are entered, the system will automatically readjust
them.
3. Depending on the Init E, High E and Low E value, the system will automatically readjust
initial scan direction.
4. The maximum potential scan range is 13.1V.
5. The potential increment is 0.1 mV if the scan rate is below 500 V/s. The potential
increment is 1 mV at the scan rate of 5000 V/s, and 4 mV at 20000 V/s.
6. The sample interval can be 1 mV When the scan rate is below 1000 V/s. The sample
interval is 2 mV at the scan rate of 2000 V/s, 5 mV at 5000 V/s, and 20 mV at 20000 V/s. If
the scan rate is high, the data sampling interval will be automatically increased.
7. When large number of sweep segments are involved, the data sampling interval will be
automatically increased up to 0.02V. If the scan rate is higher than 0.5V/s, the number of
sweep segments will be limited by the memory size (64000 points). If the scan rate is below
0.5V/s, the maximum data length set by the System command will take effect. When the scan
rate is low, the specified sweep segments will be executed, but only limited number of
segments will be stored. Large sweep segments might be useful for conditioning of
electrodes.
8. When scan rate is below 0.01 V/s, the sensitivity scale during run can be automatically
switched according to the current level. When it is activated, the sensitivity selection will
have no effect on the measurement. However, the automatic sensitivity switching range will
be from 1e-8 - 0.1 A/V, instead of 1e-12 - 0.1 A/V. The Picoamp Booster will not work
either. In order to select higher sensitivities, automatic sensitivity switching option needs to
be disabled.
9. Scan Complete Cycles will only work for Sweep Segments at 3, 5, 7, 9, (odd numbers)
and if Initial E is different from High E and Low E. When it works, the last segment will stop
at Initial E instead of High E or Low E.
10. If the scan rate is lower than 0.25V/s, it is possible to record external voltage signal (such
s spectroscopic signal) simultaneously with the voltammogram. Use the 9-pin D-connector
on the real panel for signal input. Check the User's Manual for the pin-out and signal level
requirements.
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Parameters for Linear Sweep Voltammetry
In Linear Sweep Voltammetry (LSV), potential is scanned from Init E toward Final E.
The following diagram shows the potential waveform applied as the function of time. The
current is recorded as the function of potential.
Potential(V)
Final E
Scan Rate (V/s)
Init E
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Init E (V)
Final E (V)
Scan Rate (V/s)
Sample Interval (V)
Quiet Time (sec)
Sensitivity (A/V)
Auto Sens
Auxiliary Signal
Recording
Range
-10 - +10
-10 - +10
1e-6 - 20000
1e-6 - 0.064
0 - 100000
1e-12 - 0.1
Check or
Uncheck
Check or
Uncheck
Description
Initial potential
Final potential
Potential scan rate
Data sampling interval
Quiescent time before potential scan
Sensitivity scale
Automatic sensitivity switching
during run
Simultaneously external signal
recording when the scan rate is less
than 0. 25V/s
Notes:
1. Init E and Final E should be at least 0.01 V apart.
2. The maximum potential scan range is 13.1 V.
3. When the scan rate is high, the data sampling interval will be automatically increased.
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4. The potential increment is 0.1 mV if the scan rate is below 500 V/s. The potential
increment is 1 mV at the scan rate of 5000 V/s, and 4 mV at 20000 V/s.
5. The sample interval can be 1 mV When the scan rate is below 1000 V/s. The sample
interval is 2 mV at the scan rate of 2000 V/s, 5 mV at 5000 V/s, and 20 mV at 20000 V/s. If
the scan rate is high, the data sampling interval will be automatically increased.
6. When scan rate is below 0.01 V/s, the sensitivity scale during run can be automatically
switched according to the current level. When it is activated, the sensitivity selection will
have no effect on the measurement. However, the automatic sensitivity switching range will
be from 1e-8 - 0.1 A/V, instead of 1e-12 - 0.1 A/V. The Picoamp Booster will not work
either. In order to select higher sensitivities, automatic sensitivity switching option needs to
be disabled.
7. If the scan rate is lower than 0.25V/s, it is possible to record external voltage signal (such
s spectroscopic signal) simultaneously with the voltammogram. Use the 9-pin D-connector
on the real panel for signal input. Check the User's Manual for the pin-out and signal level
requirements.
8. Linear polarization resistance plot can be obtained by the Special Plots command under
the Graphics menu.
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Parameters for Staircase Voltammetry
In Staircase Voltammetry (SCV), potential is increment from Init E toward Final E. The
potential may be scanned back. The following diagram shows the potential waveform applied as
the function of time. The current is sampled at every potential increment and recorded as the
function of potential.
Potential(V)
Final E
Incr E
Init E
Sample Width
Step Period
Segment 1
Segment 2
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Init E (V)
Final E (V)
Incr E (V)
Range
-10 - +10
-10 - +10
1e-3 - 0.05
Description
Initial potential
Final potential
Increment potential of each step
Segments
1 - 10000
Number of scan segments
Sampling Width (sec)
Step Period (sec)
Quiet Time (sec)
Sensitivity (A/V)
1e-4 - 50
0.001 - 50
0 - 100000
1e-12 - 0.1
Data sampling width for each point
Potential step period or dropping time
Quiescent time before potential scan
Sensitivity scale
Notes:
1. Init E and Final E should be at least 0.01 V apart.
2. Sampling Width should be no more than half of Step Period, otherwise the system will
automatically readjust Sampling Width.
3. Data sampling always occurs at the end of each step.
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Chapter 4. Setup Menu
________________________________________________________________________
Parameters for Tafel Plot
In Tafel Plot (TAFEL), potential is scanned from Init E toward Final E. The potential
may be scanned back. The following diagram shows the potential waveform applied as the
function of time. The logarithm of current is recorded as the function of potential.
Potential(V)
Final E
Hold Time
Scan Rate (V/s)
Init E
Segment 1
Segment 2
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Init E (V)
Final E (V)
Sweep Segments
Hold Time at Final E (s)
Scan Rate (V/s)
Quiet Time (sec)
Sensitivity (A/V)
Auto Sens
Range
-10 - +10
-10 - +10
1 - 2
0 - 100000
1e-6 - 0.1
0 - 100000
1e-12 - 0.1
Check or
Uncheck
Description
Initial potential
Final potential
Sweep segments, each segments is half cycle
Potential hold time atfer 1st sweep segent
Potential scan rate
Quiescent time before potential scan
Sensitivity scale
Automatic sensitivity switching during run
Notes:
1. Init E and Final E should be at least 0.01 V apart.
2. Corrosion rate calculation can be obtained by Special Analysis command under the
Analysis menu.
4-9
Chapter 4. Setup Menu
________________________________________________________________________
Parameters for Chronoamperometry
In Chronoamperometry (CA), potential is stepped from Init E toward either High E or
Low E depending on the Init P/N. The potential will then step back. The following diagram
shows the potential waveform applied as the function of time. The current is recorded as the
function of time.
Potential(V)
High E
Pulse Width
High E
Pulse Width
Init E
Low E
Step 1
Step 2
0
Step 3
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Init E (V)
High E (V)
Low E (V)
Init P/N
Number of Steps
Pulse Width (sec)
Sample Interval (s)
Quiet Time (sec)
Sensitivity (A/V)
Auxiliary Signal
Recording
Range
-10 - +10
-10 - +10
-10 - +10
Positive or Negative
1 - 320
1e-4 - 1000
1e-6 - 10
0 - 100000
1e-12 - 0.1
Check or Uncheck
Notes:
4-10
Description
Initial potential
High limit of potential scan
Low limit of potential scan
Initial step direction
Number of potential steps
Potential pulse width
Sampling Interval
Quiescent time before potential step
Sensitivity scale
Simultaneously external signal
recording when the sample interval is
greater than 0.005 s
Chapter 4. Setup Menu
________________________________________________________________________
1. High E and Low E should be at least 0.01 V apart.
2. If unreasonable High E and Low E are entered, the system will automatically readjust
them.
3. Depending on the Init E, High E and Low E value, the system will automatically readjust
initial step direction.
4. The maximum potential step range is 13.1 V.
5. Shorter sample interval will increase data density, but will reduce the signal-noise ratio.
If earlier transient data is important, shorter sample interval is recommended. If the later part
of data is of interest, longer sample interval is recommended. However, minimum 100 points
per step are required.
6. If the sample interval is less than 0.002s, the data will not be transferred on the real-time
base. Instead the data will be transferred after the experiment is completed. Cell is turned off
during the data transfer unless the Cell On between Run option is selected. From start of
experiment and data transfer there is a delay. The total number of data points will be limited
to 64K due to internal memory size limitation. Sample interval might be automatically
altered to adjust the data points in the reasonable range.
7. If the sample interval is longer than 0.002s, data will be transferred during experiment.
Maximum 64K total data points are allowed for each step. Sample interval might be
automatically altered to adjust the data points in the reasonable range.
8. If the sample interval is greater than 0.005s, it is possible to record external voltage
signal (such s spectroscopic signal) simultaneously with the current. Use the 9-pin Dconnector on the real panel for signal input. Check the Appendix of the User's Manual for the
pin out.
4-11
Chapter 4. Setup Menu
________________________________________________________________________
Parameters for Chronocoulometry
In Chronocoulometry (CC), potential is stepped from Init E toward Fianl E. The potential
may step back. The following diagram shows the potential waveform applied as the function of
time. The charge passing through the working electrode is recorded as the function of time.
Potential(V)
Final E
Pulse Width
Final E
Pulse Width
Init E
Init E
Step 1
Step 2
0
Step 3
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Init E (V)
Final E (V)
Number of Steps
Pulse Width (sec)
Sample Interval (s)
Quiet Time (sec)
Sensitivity (C or
A/V)
Range
-10 - +10
-10 - +10
1 - 320
1e-4 - 1000
1e-6 - 10
0 - 100000
1e-12 - 0.1
or 1e-9C/V 1e-6 C/V
Description
Initial potential
Final potential
Number of potential steps
Potential pulse width
Sampling Interval
Quiescent time before potential step
Sensitivity scale
Notes:
1. Init E and Final E should be at least 0.01 V apart.
2. The maximum potential step range is 13.1 V.
3. A true integrator (charge-to-voltage converter) can be chosen. In this case, the sensitivity
is 1e-9C/V to 1e-6C/V. If the charge exceeds the 8e-6 coulomb, the capacitor of the
4-12
Chapter 4. Setup Menu
________________________________________________________________________
integrator will be discharged and the new charge will be added to the previous value. This
allows higher charge to be measured with the integrator. There might be discontinuity in
charge-time curve due to the capacitor discharge. The discontinuity should be negligible.
However, if it is significant to the measurement, you may choose to use the current-tovoltage converter and integrate the current measured by software.
4. Current-to-voltage converter is not ideal for chronocoulometry, particularly if the early
transient data is important, such as double layer capacitance, or surface reactions. Charge-tovoltage converter (true integrator) is a better choice.
5. If current-to-voltage converter is selected due to high total charge, shorter sample interval
will increase data density, but will reduce the signal-to-noise ratio. If earlier transient data is
important, shorter sample interval is recommended. If the later part of data is of interest,
longer sample interval is recommended. However, minimum 1000 points per step are
required, unless sampling rate does not allow it.
6. If the sample interval is less than 0.002s, the data will not be transferred on the real-time
base. Instead the data will be transferred after the experiment is completed. Cell is turned off
during the data transfer unless the Cell On between Run option is selected. From start of
experiment and data transfer there is a delay. The total number of data points will be limited
to 64K due to internal memory size limitation. Sample interval might be automatically
altered to adjust the data points in the reasonable range.
7. If the sample interval is longer than 0.002s, data will be transferred during experiment.
Maximum 64K total data points are allowed for each step. Sample interval might be
automatically altered to adjust the data points in the reasonable range.
8. If the current-to-voltage converter is used, during the run, an “Overflow” warning might
appear. This is due to the current transient immediately after the potential step. If the
intercept (that gives information of double layer capacitance and adsorption) of Anson plot
(Q-t1/2 plot) is not your primary interest, you may not worry about it. However, if the data
distortion can be seen visually, you have to lower the sensitivity scale.
Sometimes, you may use i/E converter filter to slow the system down, but make sure that
the time constant of the filter (1/cutoff freq) is much shorter than the pulse width.
In order to reduce noise and enhance the accuracy of the measurement, it is
recommended to use the highest sensitivity scale possible.
4-13
Chapter 4. Setup Menu
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Parameters for Differential Pulse Voltammetry
Potential(V)
In Differential Pulse Voltammetry (DPV), the base potential is incremented from Init E
toward Final E. A potential pulse is applied. The current before the potential pulse and at the end
of the potential pulse are sampled. The difference of these two current samples is recorded as the
function of potential. The following diagram shows the potential waveform applied as the
function of time and the current sampling scheme.
Pulse Width
Amplitude
Final E
Incr E
Init E
Pulse Period
Sample Width
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Init E (V)
Final E (V)
Incr E (V)
Amplitude (V)
Pulse Width (sec)
Sampling Width (sec)
Pulse Period (sec)
Quiet Time (sec)
Sensitivity (A/V)
Range
-10 - +10
-10 - +10
±0.001 - ±0.05
0.001 - 0.5
0.001 - 10
1e-4 - 10
0.01 - 50
0 - 100000
1e-12 - 0.1
Description
Initial potential
Final potential
Increment potential of each point
Potential pulse amplitude
Potential pulse width
Data sampling width
Potential pulse period or dropping time
Quiescent time before potential scan
Sensitivity scale
Notes:
1. Init E and Final E should be at least 0.01 V apart.
2. Pulse Width should be no more than half of Pulse Period, otherwise the system will
automatically readjust Pulse Width.
3. Sampling Width should be no more than half of Pulse Width, otherwise the system will
automatically readjust Sampling Width.
4. When amplitude is negative, the pulse direction is different from the potential scan
direction.
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Chapter 4. Setup Menu
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Parameters for Normal Pulse Voltammetry
Potential(V)
In Normal Pulse Voltammetry (NPV), the base potential is held at Init E. A sequence of
potential pulse with increasing amplitude is applied. The current at the end of the potential pulse
is sampled. This current is recoded as the function of the pulsed potential. The following
diagram shows the potential waveform applied as the function of time and the current sampling
scheme.
Pulse Width
Final E
Incr E
Init E
Pulse Period
Sample Width
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Init E (V)
Final E (V)
Incr E (V)
Pulse Width (sec)
Sampling Width (sec)
Pulse Period (sec)
Quiet Time (sec)
Sensitivity (A/V)
Range
-10 - +10
-10 - +10
0.001 - 0.05
0.001 - 10
1e-4 - 10
0.01 - 50
0 - 100000
1e-12 - 0.1
Description
Initial potential
Final potential
Increment potential of each point
Potential pulse width
Data sampling width
Potential pulse period or dropping time
Quiescent time before potential scan
Sensitivity scale
Notes:
1. Init E and Final E should be at least 0.01 V apart.
2. Pulse Width should be no more than half of Pulse Period, otherwise the system will
automatically readjust Pulse Width.
3. Sampling Width should be no more than half of Pulse Width, otherwise the system will
automatically readjust Sampling Width.
4-15
Chapter 4. Setup Menu
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Parameters for Differential Normal Pulse Voltammetry
Potential(V)
In Differential Normal Pulse Voltammetry (DNPV), the base potential is held at Init E. A
sequence of dual potential pulses are applied. The first pulse will increment its magnitude for
each pulse. The second pulse has the constant amplitude. The current at the end of two potential
pulses are sampled. The difference of these two current is recoded as the function of the first
pulsed potential. The following diagram shows the potential waveform applied as the function of
time and the current sampling scheme.
Pulse Width
Incr E
Pulse Width
Final E
Amplitude
Init E
Pulse Period
Sample Width
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Init E (V)
Final E (V)
Incr E (V)
Amplitude (V)
1st Pulse Width (sec)
2nd Pulse Width (sec)
Sampling Width (sec)
Pulse Period (sec)
Quiet Time (sec)
Sensitivity (A/V)
Open Circuit at Initial E
Range
-10 - +10
-10 - +10
0.001 - 0.05
0.001 - 0.5
0.01 - 10
0.01 - 10
0.001 - 5
0.05 - 50
0 - 100000
1e-12 - 0.1
Check or
uncheck
Description
Initial potential
Final potential
Increment potential of each point
Potential pulse amplitude
First potential pulse width
Second potential pulse width
Data sampling width
Potential pulse period or dropping time
Quiescent time before potential scan
Sensitivity scale
Step 1 could be either held at a constant
potential or open circuit
Notes:
1. Init E and Final E should be at least 0.01 V apart.
4-16
Chapter 4. Setup Menu
________________________________________________________________________
2. In Differential Normal Pulse Voltammetry, the potential of first step is normally held at
Initial E where no electrochemical reaction will occur. The second step is incremented every
cycle. A current sample is taken at the later part of the period. The potential of the third is
also incremented like the second step, but it is more positive (for positive scan) or more
negative (for negative scan) than the second potential by a constant magnitude (amplitude).
The second sample is taken at the later part of the period. The difference between the two
current samples is reported as the function of the second potential.
3. Pulse Width should be no more than half of Pulse Period, otherwise the system will
automatically readjust Pulse Width.
4. Sampling Width should be no more than half of Pulse Width, otherwise the system will
automatically readjust Sampling Width.
4-17
Chapter 4. Setup Menu
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Parameters for Square Wave Voltammetry
Potential(V)
In Square Wave Voltammetry (SWV), the base potential is increment from Init E towards
Final E. A square wave potential is superimposed to the base potential. The base potential
increments after each cycles of the square wave. The current at the end of forward and reverse
steps are sampled. These two current are recoded as the function of the base potential. During the
experiment, only the difference of two current samples is displayed. After experiment, the
forward and reverse current are also available for display. The following diagram shows the
potential waveform applied as the function of time and the current sampling scheme.
Incr E
Final E
Amplitude
Init E
1/Frequency
Sample Width
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Init E (V)
Final E (V)
Incr E (V)
Amplitude (V)
Frequency (Hz)
Quiet Time (sec)
Sensitivity (A/V)
Range
-10 - +10
-10 - +10
0.001 - 0.05
0.001 - 0.5
1 - 100000
0 - 100000
1e-12 - 0.1
Description
Initial potential
Final potential
Increment potential of each point
Square wave amplitude, half peak-to-peak
Square wave frequency
Quiescent time before potential scan
Sensitivity scale
Notes:
1. Init E and Final E should be at least 0.01 V apart.
2. Forward, reverse and difference currents are recorded. Use the Graph Option command
under the Graphics menu to choose data display options.
4-18
Chapter 4. Setup Menu
________________________________________________________________________
Parameters for A.C. Voltammetry
Potential(V)
In AC Voltammetry (ACV), the base potential is increment from Init E towards Final E.
A sequential sine waveform is superimposed to the base potential. The current is sampled when
ac signal is applied and analyzed using a software lock-in amplifier. During the experiment, only
the absolute ac current is displayed. After experiment, the phase-selective current at any phase
angle are also available for display. The following diagram shows the potential waveform
applied as the function of time.
Incr E
Final E
Amplitude
Init E
Sample Period
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Init E (V)
Final E (V)
Incr E (V)
Amplitude (V)
Frequency (Hz)
Sample Period (sec)
Quiet Time (sec)
Sensitivity (A/V)
Bias DC Current
Auto Sens
Range
-10 - +10
-10 - +10
0.001 - 0.05
0.001 - 0.4
0.1 - 10000
1 - 65
0 - 100000
1e-12 - 0.1
off - range - on
Check or
Uncheck
Description
Initial potential
Final potential
Increment potential of each point
A.C. amplitude
A.C. frequency
Data sampling period or dropping time
Quiescent time before potential scan
Sensitivity scale
Enable dc current bias during run
Automatic sensitivity switching during run
Notes:
1. Init E and Final E should be at least 0.01 V apart.
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Chapter 4. Setup Menu
________________________________________________________________________
2. Depending on the frequency range, sometimes the exact frequency can not be obtained. If
this occurs, the closest possible frequency will be applied.
3. When frequency is 2 Hz or lower, Sample Period should be at least 2 seconds, otherwise,
the system will automatically readjust Sample Period.
4. When dc current is high and ac current is low, the sensitivity can not be increased
because dc current will overflow. This problem is more serious when the frequency is
relatively low. By applying dc current bias, it allows higher ac signal amplification. A 16-bit
DAC is used for this purpose. If dc current is not expected to be large and the frequency is
high, one may not want to bias dc current.
5. Both absolute current and phase selective current are available. Use the Graph Option
command under the Graphics menu to choose data display options.
4-20
Chapter 4. Setup Menu
________________________________________________________________________
Parameters for Second Harmonic A.C. Voltammetry
Potential(V)
In Second Harmonic AC Voltammetry (SHACV), the base potential is increment from
Init E towards Final E. A sequential sine waveform is superimposed to the base potential. The
current is sampled when ac signal is applied and its second harmonic components are analyzed
using a software lock-in amplifier. During the experiment, only the absolute second harmonic ac
current is displayed. After experiment, the phase-selective second harmonic current at any phase
angle are also available for display. The following diagram shows the potential waveform
applied as the function of time.
Incr E
Final E
Amplitude
Init E
Sample Period
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Init E (V)
Final E (V)
Incr E (V)
Amplitude (V)
Frequency (Hz)
Sample Period (sec)
Quiet Time (sec)
Sensitivity (A/V)
Bias DC Current
Auto Sens
Range
-10 - +10
-10 - +10
0.001 - 0.05
0.001 - 0.4
0.1 - 5000
1 - 65
0 - 100000
1e-12 - 0.1
off - range - on
Check or Uncheck
Description
Initial potential
Final potential
Increment potential of each point
A.C. amplitude
A.C. frequency
Data sampling period or dropping time
Quiescent time before potential scan
Sensitivity scale
Enable dc current bias during run
Automatic sensitivity switching during run
Notes:
1. Init E and Final E should be at least 0.01 V apart.
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Chapter 4. Setup Menu
________________________________________________________________________
2. Depending on the frequency range, sometimes the exact frequency can not be obtained. If
this occurs, the closest possible frequency will be applied.
3. When frequency is 2 Hz or lower, Sample Period should be at least 2 seconds, otherwise,
the system will automatically readjust Sample Period.
4. When dc current is high and ac current is low, the sensitivity can not be increased
because dc current will overflow. This problem is more serious when the frequency is
relatively low. By applying dc current bias, it allows higher ac signal amplification. A 16-bit
DAC is used for this purpose. If dc current is not expected to be large and the frequency is
high, one may not want to bias dc current.
5. Both absolute current and phase selective current are available. Use the Graph Option
command under the Graphics menu to choose data display options.
4-22
Chapter 4. Setup Menu
________________________________________________________________________
Parameters for Amperometric i-t Curve
Potential(V)
In Amperometric i-t Curve (i-t), a constant potential is applied and the current is recorded
as the function of time. The following diagram shows the potential waveform applied as the
function of time and the sample scheme.
Sample Interval
Init E
0
Run Time
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Init E (V)
Sample Interval (sec)
Run Time (sec)
Quiet Time (sec)
Scales During Run
Sensitivity (A/V)
Auxiliary Signal
Recording
Range
-10 - +10
1e-6 - 50
0.001 - 5e5
0 - 100000
1, 2, 3
1e-12 - 0.1
Check or
Uncheck
High Resolution ADC
Check or
Uncheck
Description
Initial potential
Data sample interval
Total measurement time
Quiescent time before taking data
Number of current display scales
Sensitivity scale
Simultaneously external signal
recording when the sample interval
is greater than 0.005 s
Use high resolution ADC sample
interval is greater than 0.002 s
Notes:
1. The data sample interval should be chosen according to the length of the experiment. The
longer the experiment, the larger the sample interval. Long sample interval will have better
signal averaging and less noise.
2. During experiment, whenever the data exceed the maximum allowed points, the data
storage interval will be doubled automatically. Therefore, data points will not overflow for
an unexpected long experiment.
4-23
Chapter 4. Setup Menu
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3. If the sample interval is greater than 0.005s, it is possible to record external voltage
signal (such s spectroscopic signal) simultaneously with the amperometric i-t response. Use
the 9-pin D-connector on the real panel for signal input. Check the User’s Manual for the
pinout.
4. If the sample interval is greater than 0.002s, High resolution ADC can be used to acquire
data. High resolution ADC usually provide better signal-to-noise ratio. The data quality less
depends on the sensitivity setting because of its higher resolution.
5. When 1 current scale is displayed during run, it will automatically fit the data in scale.
When 2 current scales are displayed during run, they is 1/100 and 1/10 of full scale. When 3
current scales are displayed during run, they is 1/100, 1/10, and 1/1 of full scale.
4-24
Chapter 4. Setup Menu
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Parameters for Differential Pulse Amperometry
In Differential Pulse Amperometry (DPA), a clean potential could be applied for
electrode conditioning with no current sampling. Two potential pulses are applied after the
cleaning step and the current at the end of each pulses are recorded as the function of time.
During the experiment, only the difference of two current samples is displayed. After
experiment, the current responses to the two potential pulses are also available for display. The
following diagram shows the potential waveform applied as the function of time and the current
sampling scheme.
Potential(V)
Data Sampling
Clean E
E1
Init E
E2
Clean T
Cycle 1
T1
Cycle 2
0
T2
Cycle 3
Time (s)
The following are the experimental parameters, their range and descriptions:
Param
Init E (V)
Cleaning E (V)
Cleaning Time (sec)
Pulse E1 (V)
Pulse T1 (sec)
Pulse E2 (V)
Pulse T2 (sec)
Number of Cycles
Quiet Time (sec)
Scales During Run
Sensitivity (A/V)
Open Circuit During
Cleaning
Range
-10 - +10
-10 - +10
0 - 32
-10 - +`0
.01 - 32
-10 - +10
.01 - 32
10 - 100000
0 - 100000
1, 2, 3
1e-12 - 0.1
Check or
Uncheck
Description
Initial potential during quiescent time
Electrode cleaning potential
Electrode cleaning time
First pulse potential
First pulse time
Second pulse potential
Second pulse time
Number of Repetitive Cycles
Quiescent time before taking data
Number of current display scales
Sensitivity scale
Cleaning step could be either held at a
constant potential or open circuit
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Chapter 4. Setup Menu
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Notes:
1. The experimental sequence follows cleaning, first pulse, and second pulse. This sequence
will be repeated until the total number of cycles is reached or interrupted by user. There is no
data acquisition during cleaning step. If the cleaning time is zero, this step will be ignored.
Data are sampled for first and second pulses and the difference is reported.
2. The data is sampled at later ½ period of pulse 1 and 2. The longer the pulse width, the
longer the sample interval. Long sample interval will have better signal averaging and less
noise.
3. During experiment, whenever the data exceed the maximum allowed points, the data
storage interval will be doubled automatically. Therefore, data points will not overflow for
an unexpected long experiment.
4. When 1 current scale is displayed during run, it will automatically fit the data in scale.
When 2 current scales are displayed during run, they is 1/100 and 1/10 of full scale. When 3
current scales are displayed during run, they is 1/100, 1/10, and 1/1 of full scale.
4-26
Chapter 4. Setup Menu
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Parameters for Double Differential Pulse Amperometry
In Double Differential Pulse Amperometry (DDPA), it combines two sets of the
differential pulse amperometry. Two sets of data will be recorded and displayed. Each set
consists of a cleaning potential without current sampling and two pulsed potential with current
sampling. The current at the end of each pulses are recorded as the function of time. During the
experiment, only the difference of two current samples is displayed. After experiment, the
current responses to the two potential pulses are also available for display. The following
diagram shows the potential waveform applied as the function of time and the current sampling
scheme.
Potential(V)
Data Sampling
Clean E1
Data Sampling
Clean E2
E1
E2
Init E
E3
E4
Clean T1
T1
T2
Clean T2 T3
T4
Cycle 1
Cycle 2
0
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
First DPA:
Cleaning E1 (V)
Cleaning Time (sec)
Pulse E1 (V)
Pulse T1 (sec)
Pulse E2 (V)
Pulse T2 (sec)
Open Circuit During
Cleaning
Second DPA:
Cleaning E2 (V)
Cleaning Time (sec)
Range
Description
-10 - +10
0 - 32
-10 - +10
.01 - 32
-10 - +10
.01 - 32
Check or
Uncheck
Electrode cleaning potential
Electrode cleaning time
First pulse potential
First pulse time
Second pulse potential
Second pulse time
Cleaning step 1 could be either held at
a constant potential or open circuit
-10 - +10
0 - 32
Electrode cleaning potential
Electrode cleaning time
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Chapter 4. Setup Menu
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Pulse E3 (V)
Pulse T3 (sec)
Pulse E4 (V)
Pulse T4 (sec)
Open Circuit During
Cleaning
-10 - +10
.01 - 32
-10 - +10
.01 - 32
Check or
Uncheck
First pulse potential
First pulse time
Second pulse potential
Second pulse time
Cleaning step 2 could be either held at
a constant potential or open circuit
Init E (V)
Number of Cycles
Quiet Time (sec)
Scales During Run
Sensitivity (A/V)
-10 - +10
10 - 100000
0 - 100000
1, 2, 3
1e-12 - 0.1
Initial potential during quiescent time
Number of Repetitive Cycles
Quiescent time before taking data
Number of current display scales
Sensitivity scale
Notes:
1. The experimental sequence follows the first DPA cleaning, first pulse, and second pulse,
then the second DPA cleaning, first pulse, and second pulse. This sequence will be repeated
until the total running time is reached or interrupted by user. There is no data acquisition
during cleaning step. If the cleaning time is zero, this step will be ignored. Data are sampled
for first and second pulses and the difference is reported. Two sets of data will be obtained.
2. The data is sampled at later ½ period of pulse 1 and 2. The longer the pulse width, the
longer the sample interval. Long sample interval will have better signal averaging and less
noise.
3. During experiment, whenever the data exceed the maximum allowed points, the data
storage interval will be doubled automatically. Therefore, data points will not overflow for
an unexpected long experiment.
4. When 1 current scale is displayed during run, it will automatically fit the data in scale.
When 2 current scales are displayed during run, they is 1/100 and 1/10 of full scale. When 3
current scales are displayed during run, they is 1/100, 1/10, and 1/1 of full scale.
5. To display data for 1st, 2nd DPA or both, use the Graph Option command under the
Graphics menu to choose data display options.
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Chapter 4. Setup Menu
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Parameters for Triple Pulse Amperometry
In Triple Pulse Amperometry (TPA), three potential pulses are applied. First two pulses
are for electrode conditioning or cleaning. The current is sampled at the end of the third potential
pulse. The current is recorded as the function of time. The third potential pulse could be at a
constant potential, or be incremented after each cycle. The following diagram shows the
potential waveform applied as the function of time and the current sampling scheme.
Potential(V)
Data Sampling
E1
Init E
E3
E3
E3
T1
E2
T2
Cycle 1
T3
Cycle 2
Cycle 3
0
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
E1 (V)
Duration 1 (sec)
Open Circuit
Range
-10 - +10
0 - 32
Check or
Uncheck
Description
First pulse potential
First pulse duration
Step 1 could be either held at a
constant potential or open circuit
E2 (V)
Duration 2 (sec)
-10 - +10
0 - 32
Second pulse potential
Second pulse duration
E3 (V)
Duration 3 (sec)
Incr E (V)
-10 - +10
.01 - 32
0 - 0.2
Third pulse potential
Third pulse duration
Increment potential
Init E (V)
-10 - +10
Final E (V)
Number of Cycles
-10 - +10
10 - 100000
Initial potential during quiescent
time
Final potential for scan
Number of Repetitive Cycles
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Chapter 4. Setup Menu
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Quiet Time (sec)
Scales During Run
Sensitivity (A/V)
0 - 100000
1, 2, 3
1e-12 - 0.1
Quiescent time before taking data
Number of current display scales
Sensitivity scale
Notes:
1. The experimental sequence follows first pulse, second pulse, and third pulse. This
sequence will be repeated until the total running time is reached or interrupted by user. There
is no data acquisition during the first and second. They are used for electrode cleaning
purposes If the first and/or second pulse time is zero, the corresponding step will be ignored.
Data is sampled only for the third pulse.
2. If the increment potential is non-zero, the experiment will start at the E3 and end at the
Final E. E3 and Final E should be at least 0.01 V apart. The number of cycles will have no
effect.
3. The data is sampled at later ½ period of pulse 3. The longer the pulse width, the longer
the sample interval. Long sample interval will have better signal averaging and less noise.
4. During experiment, whenever the data exceed the maximum allowed points, the data
storage interval will be doubled automatically. Therefore, data points will not overflow for
an unexpected long experiment.
5. When 1 current scale is displayed during run, it will automatically fit the data in scale.
When 2 current scales are displayed during run, they is 1/100 and 1/10 of full scale. When 3
current scales are displayed during run, they is 1/100, 1/10, and 1/1 of full scale.
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Chapter 4. Setup Menu
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Parameters for Integrated Pulse Amperometric Detection
In Integrated Pulse Amperometric Detection (IPAD), six segments of potential sweeps or
steps are applied. Current is sampled and integrated during the first four potential segment. The
last two potential steps are for electrode conditioning or cleaning. The integrated current is then
averaged and recorded as the function of time. The following diagram shows the potential
waveform applied as the function of time and the current sampling scheme.
St 1
St 2
St 3
St 4
St 5
St 6
Potential(V)
Oxd E
Peak E
Start E
Return E
Hold E
Integration Time
Red E
Cycle 1
Cycle 2
0
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Step 1: Start
Start E (V)
Hold Time (sec)
Range
Description
-3.276 - +3.276
0.05 - 1
Start potential (constant)
Start potential duration, Current
integration starts 10 msec before the
end of this step
Step2: Forward Scan
Peak E (V)
-3.276 - +3.276
Scan Time (s)
0.15 - 1
Potential is scanned from Start E to
Peak E
Time to scan from Start E to Peak E,
Current integration continues
Step 3: Reverse Scan
Return E (V)
-3.276 - +3.276
Scan Time (s)
0.15 - 1
Potential is scanned from Peak E to
Return E. Often Return E is the same
as Start E
Time to scan from Peak E to Return E,
Current integration continues
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Chapter 4. Setup Menu
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Step 4: Hold
Hold E (V)
Hold Time (sec)
-3.276 - +3.276
0.05 - 1
Hold potential (constant)
Hold potential duration, Current
integration for 10 msec and end
Step 5: Oxidation
Oxd E (V)
-3.276 - +3.276
Oxidation potential for electrode
treatment
Oxidation time duration
Oxd Time (s)
Step 6: Reduction
Red E (V)
0.05 - 1
Red Time (s)
0.05 - 1
Reduction potential for electrode
treatment
Reduction time duration
Number of Cycles
Quiet Time (sec)
Sensitivity (A/V)
5 - 65535
0 - 100000
1e-12 - 0.1
Number of cycles through six steps
Quiescent time before taking data
Sensitivity scale
-3.276 - +3.276
Notes:
1. The experimental sequence follows starting potential, forward potential scan, reverse
potential scan, hold potential, oxidation potential and reduction potential. This sequence will
be repeated until the total number of cycles are reached or interrupted by user.
2. Current is sampled during the last 10 msec of the start potential, forward scan, reverse
scan, and the first 10 msec of the hold potential. The current are integrated and reported.
3. During experiment, whenever the data exceed the maximum allowed points, the data
storage interval will be doubled automatically. Therefore, data points will not overflow for
an unexpected long experiment.
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Chapter 4. Setup Menu
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Parameters for Bulk Electrolysis with Coulometry
Potential(V)
In Bulk Electrolysis with Coulometry (BE), a constant potential is applied and the
integrated charge is recorded as the function of time. The following diagram shows the potential
waveform applied as the function of time and the sample scheme.
A pre-electrolysis may be applied to reduce the interference and background current
before the formal electrolysis.
Data Storage Interval
Electrolysis E
0
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Range
Description
-10 - +10
Electrolysis potential
Electrolysis E (V)
0 - 100
Stop experiment at this current ratio
End Current Ratio (%)
Data display and storage interval
Data Storage Interval (s) 0.01 - 100
-10 - +10
Preelectrolysis potential
Preelectrolysis E (V)
0 - 100000
Preelectrolysis time
Preelectrolysis Time (s)
Notes:
1. Preelectrolysis step is allowed before the regular electrolysis. This is useful to reduce
some residue current. The current at the end of preelectrolysis will be regarded as residue
current and it will be subtracted from the total charge to give net charge. If the preelectrolysis
time is set to zero, this step is ignored. You can stop preelectrolysis at any time by invoke
Stop command. The regular electrolysis will follow immediately.
2. Sensitivity scale will be switched automatically during experiment.
3. The current ratio is referred to the initial current. If the data storage interval is 1 second,
the initial current is the average current of the first second after electrolysis.
4. If the end current ratio is zero, the electrolysis will continue forever. In order to stop the
experiment, the Stop command should be invoked.
5. During the experiment, the data will be updated in a rate same as data storage interval.
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Chapter 4. Setup Menu
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6. The data storage interval should be chosen according to the length of the experiment. The
longer the experiment, the larger the data storage interval. Long data storage interval will
have better signal averaging and less noise. However, for a thin layer cell, short data storage
time should be used in order to observe the detail of the electrolysis process.
7. During electrolysis, whenever the data exceed the maximum allowed points, the data
storage interval will be doubled automatically. Therefore, data points will not overflow for
an unexpected long electrolysis.
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Chapter 4. Setup Menu
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Parameters for Hydrodynamic Modulation Voltammetry
Potential(V)
In Hydrodynamic Modulation Voltammetry (HMV), potential is increment from Init E
toward Final E. The following diagram shows the potential waveform applied as the function of
time. At each potential, the rotating speed of the RDE is modulated. The resulting alternating
current is sampled and analyzed using a software lock-in amplifier. During the experiment, only
the absolute ac current is displayed. After experiment, the phase-selective current at any phase
angle are also available for display. The ac current is sampled at every potential increment and
recorded as the function of potential.
Final E
Init E
Incr E
Rotation speed modulation
& data sampling
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Init E (V)
Final E (V)
Incr E (V)
Rotation Rate (rpm)
Modul Frequency (Hz)
Modul Amplitude (rpm)
Number of Cycles
Quiet Time (sec)
Sensitivity (A/V)
Range
-10 - +10
-10 - +10
0.001 - 0.02
0 – 10000
1–5
0 – 3600
1 – 10
0 - 100000
1e-12 - 0.1
Description
Initial potential
Final potential
Increment potential of each step
Center rotation rate
Modulation frequency
Modulation Amplitude, see note 2
Number of modulation cycles
Quiescent time before potential scan
Sensitivity scale
Notes:
1. Init E and Final E should be at least 0.01 V apart.
2. The actual rotation rate in hydrodynamic modulation is
ω1/2=ωo1/2+∆ω1/2 sin (σt)
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Chapter 4. Setup Menu
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Notice that the modulation function is not a sine wave, but more complicated. On the other
hand, it is still a periodic waveform at frequency σ (Modulation Frequency). The rotation
rate is fluctuated around ωo (Rotation Rate), but the amplitude of the fluctuation is not
symmetric. The input parameter ∆ω (Modulation Amplitude) is really not the amplitude, but
the square of ∆ω1/2 in the above equation.
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Chapter 4. Setup Menu
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Parameters for Sweep-Step Functions
In Sweep Step Functions (SSF), six potential sweeps and six potential steps can be mixed
together. It is somewhat like a arbitrary waveform generator. The following diagram shows the
potential waveform applied as the function of time. One can skip any segment (by default
parameter). It provides better flexibility for waveform control. The current is recorded as
function of time. For sweep segments, it can also be presented as function of potential.
Segments:
Potential(V)
1
Final E
Init E
2
3
4
5
6
7
8
9
10
11
12
Step E
Scan Rate (V/s)
Time (s)
The following are the experimental parameters, their range and descriptions:
Param
Range
Sequence 1, 3, 5, 7, 9, 11
Sweep:
-10 - +10
Init E (V)
-10 - +10
Final E (V)
1e-6 - 50
Scan Rate (V/s)
Description
Initial potential
Final potential
Potential scan rate
Sequence 2, 4, 6, 8, 10, 12
Step
Step E (V)
Step Time (s)
-10 - +10
0 - 10000
Step potential
Step Duration
Init E (V)
Sweep S.I. (V)
Step S.I. (s)
Quiet Time (sec)
-10 - +10
0.001 - 0.05
0.0001 - 1
0 - 100000
Initial potential
Sweep function sample interval
Step function sample interval
Quiescent time before potential scan
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Chapter 4. Setup Menu
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Sensitivity (A/V)
1e-12 - 0.1
Sensitivity scale
Notes:
1. For sweep function, if the difference of Init E and Final E is less than 0.01 V, this
segment will be ignored.
2. For step function, if the step time is less than 0.001 sec, or if the number of points is less
than 3, this segment will be ignored. You need to increase step time or decrease sample
interval.
3. If the scan rate for sweep function is less than 0.5 V/s, data is transferred and displayed
real time.
4. If the sample interval for step function is larger than 0.002 sec, data is transferred and
displayed real time.
5. The potential differences of Init E, Final E and Step E should be less than 13.1 V.
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Chapter 4. Setup Menu
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Parameters for Multi-Potential Steps
In Multi-Potential Steps (STEP), twelve potential steps can be applied and cycled. The
current is recorded as the function of time. The following diagram shows the potential waveform
applied as the function of time.
Potential(V)
Steps:
1 2 3 4 5 6 7 8 9 10 11 12
Cycle 1
Cycle 2
Time (s)
The following are the experimental parameters, their range and descriptions:
Param
Step Sequence 1 – 12:
Step E (V)
Step Time (s)
Init E (V)
No. of Cycles
Smpl Intv (s)
Quiet Time (sec)
Sensitivity (A/V)
Range
Description
-10 - +10
0 - 10000
Step potential
Step Duration
-10 - +10
1 - 10000
0.0001 - 1
0 - 100000
1e-12 - 0.1
Initial potential
Number of cycles
Sample interval
Quiescent time before potential scan
Sensitivity scale
Notes:
1. If the step time is less than 0.001 sec, this step will be ignored.
2. If the step time is shorter than the sample interval, this step will be ignored.
3. Sample interval will be automatically increased if (step time * cycles / sample interval)
exceeds 64K if data is transferred after experiment..
4. If the sample interval is larger than 0.002 sec, data is transferred and displayed real time.
5. The potential differences of Init E, Final E and Step E should be less than 13.1 V.
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Chapter 4. Setup Menu
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Parameters for A.C. Impedance
Potential(V)
In AC Impedance (IMP), the base potential is held constant at Init E. A sine waveform is
superimposed to the base potential. The frequency is scanned from high frequency to low
frequency with 12 components per decade frequency. The current and the potential are sampled
and analyzed to obtain the real and imaginary impedance. During the experiment, Bode plot or
Nyquist plot can be switched by right click the mouse button. After experiment, impedance data
can be presented in various forms. The following diagram shows the potential waveform applied
as the function of time.
Amplitude
Init E
High Freq
Low Freq
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Init E (V)
High Frequency (Hz)
Low Frequency (Hz)
Amplitude (V)
Quiet Time (sec)
Sensitivity Scale Setting
Time (sec, range 1-100 Hz)
Cycles (0.1 - 1 Hz)
Cycles (0.01 - 0.1 Hz)
Cycles (0.001 - 0.01 Hz)
Cycles (0.0001 - 0.001 Hz)
Points (0.1 - 1 Hz)
Points (0.01 - 0.1 Hz)
Points (0.001 - 0.01 Hz)
Range
-10 - +10
0.001 – 100000
0.0001 – 10000
0.001 – 0.4
0 - 100000
Select
1 - 10
1 - 4096
1 - 4096
1 - 256
1 - 16
12, 6, 4, 3, 2, 1
12, 6, 4, 3, 2, 1
12, 6, 4, 3, 2, 1
4-40
Description
Initial potential
High frequency limit
Low frequency limit
A.C. amplitude
Quiescent time before potential scan
Automatic or Manual
Measurement time
Number of cycles at each frequency point
Number of cycles at each frequency point
Number of cycles at each frequency point
Number of cycles at each frequency point
Number of points per decade frequency
Number of points per decade frequency
Number of points per decade frequency
Chapter 4. Setup Menu
________________________________________________________________________
Points (0.0001 - 0.001 Hz)
Points (0.00001 - 0.0001
Hz)
Bias DC Current
12, 6, 4, 3, 2, 1
12, 6, 4, 3, 2, 1
Number of points per decade frequency
Number of points per decade frequency
off - range - on
Enable dc current bias during run
Notes:
1. Above 100 Hz, both current and potential are measured in order to calculate the
impedance. 12 frequency components per decade will be measured. In case of Fourier
transform, each measurement covers a decade of frequency range. Below 100 Hz, the only
current is measured. The applied potential is assumed to have no extra phase shift and be
accurate.
2. When dc current is high and ac current is low, the sensitivity can not be increased
because dc current will overflow. This problem is more serious when the frequency is
relatively low. By applying dc current bias, it allows higher ac signal amplification. A 16-bit
DAC is used for this purpose. If dc current is not expected to be large and the frequency is
high, one may not want to bias dc current.
3. Line frequency (50/60 Hz) can interfere measurements. Use longer measurement time
between 1-100Hz will improve data quality of the given frequency range.
4. The sensitivity scale setting is automatic by default. During the experiment, the system
tests the current size and determines the proper sensitivity scale. It usually works well. The
sensitivity scale setting can also be manually overridden. In certain cases, it may provide
better results. In this case, the sensitivity scale can be set for each decade of frequency range.
The system displays the Manual Sensitivity Setting dialog box:
4-41
Chapter 4. Setup Menu
________________________________________________________________________
Parameters for Impedance - Time
Potential(V)
In Impedance – Time (IMPT), the base potential is held constant at Init E. A sine
waveform is superimposed to the base potential. The current and the potential are sampled and
analyzed to obtain the real and imaginary impedance. The impedance is recorded as the function
of time. The following diagram shows the potential waveform applied as the function of time.
Amplitude
Sample Interval
Init E
Run Time
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Init E (V)
Amplitude (V)
Frequency (Hz)
Sample Interval (sec)
Run Time (sec)
Cycles (below 10 Hz)
Range
-10 - +10
0.001 - 0.25
0.0001 - 100000
5 - 20000
100 - 500000
1 - 100
Quiet Time (sec)
Bias DC Current
Sensitivity (A/V)
0 - 100000
off - range - on
Automatic or
Manual
Description
Initial potential
A.C. amplitude
A.C. frequency
Data sampling interval
Total experiment time
Number of repetitive cycles at each
frequency
Quiescent time before sampling data
Enable dc current bias during run
Sensitivity scale
Notes:
1. If the sample interval is smaller than the actual time required for sampling, it will be
automatically adjusted.
2. The more the cycles, the better signal-to-noise ratio. However, it will take longer for the
experiment.
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Chapter 4. Setup Menu
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3. When dc current is high and ac current is low, the sensitivity can not be increased
because dc current will overflow. This problem is more serious when the frequency is
relatively low. By applying dc current bias, it allows higher ac signal amplification. A 16-bit
DAC is used for this purpose. If dc current is not expected to be large and the frequency is
high, one may not want to bias dc current.
4. The sensitivity scale setting is automatic by default. During the experiment, the system
tests the current size and determines the proper sensitivity scale. It usually works well. The
sensitivity scale setting can also be manually overridden. In certain cases, it may provide
better results.
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Chapter 4. Setup Menu
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Parameters for Impedance - Potential
Potential(V)
In Impedance - Potential (IMPE), the base potential is increment from Init E towards
Final E. A sequential sine waveform is superimposed to the base potential. The current and the
potential are sampled and analyzed to obtain the real and imaginary impedance. The impedance
is recorded as the function of potential. The following diagram shows the potential waveform
applied as the function of time.
Incr E
Final E
Amplitude
Init E
One Cycle
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Init E (V)
Final E (V)
Incr E (V)
Amplitude
Frequency (Hz)
Cycles (below 10 Hz)
Range
-10 - +10
-10 - +10
0.001 - 0.25
0.001 - 0.4
0.0001 - 100000
1 - 100
Quiet Time (sec)
Bias DC Current
Sensitivity (A/V)
0 - 100000
off - range - on
Automatic or
Manual
Description
Initial potential
Final potential
Increment potential
A.C. amplitude
A.C. frequency
Number of repetitive cycles at each
frequency
Quiescent time before sampling data
Enable dc current bias during run
Sensitivity scale
Notes:
1. When dc current is high and ac current is low, the sensitivity can not be increased
because dc current will overflow. This problem is more serious when the frequency is
relatively low. By applying dc current bias, it allows higher ac signal amplification. A 16-bit
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Chapter 4. Setup Menu
________________________________________________________________________
DAC is used for this purpose. If dc current is not expected to be large and the frequency is
high, one may not want to bias dc current.
2. The sensitivity scale setting is automatic by default. During the experiment, the system
tests the current size and determines the proper sensitivity scale. It usually works well. The
sensitivity scale setting can also be manually overridden. In certain cases, it may provide
better results.
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Chapter 4. Setup Menu
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Parameters for Chronopotentiometry
In Chronopotentiometry (CP), two current levels can be controlled to pass the working
electrode. The switch of current polarity can be controlled by time or by potential. The potential
is recorded as the function of time. The following diagram shows the current waveform applied
as the function of time.
Current (A)
Anodic Current
Cathodic Time
Anodic Time
Cathodic Current
Cathodic Current
Segment 1
Cathodic Time
Segment 2
0
Segment 3
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Cathodic Current (A)
Anodic Current (A)
High E Limit (V)
Low E Limit (V)
Cathodic Time (sec)
Anodic Time (sec)
Initial Polarity
Data Storage Intvl (sec)
Number of Segments
Current Switching Priority
Auxiliary Signal Recording
Range
0 - 0.25
0 - 0.25
-10 - +10
-10 - +10
0.05 - 100000
0.05 - 100000
Cathodic or Anodic
0.0001 - 32
1 - 1000000
Potential or Time
Check or Uncheck
4-46
Description
Controlled cathodic current
Controlled anodic current
High potential limit value
Low potential limit value
Cathodic run time
Anodic run time
Polarity for the first segment
Data storage interval
Number of half cycles
Current polarity switching control
Simultaneously external signal
recording when the sample
interval is greater than 0.0005 s
Chapter 4. Setup Menu
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Notes:
1. Cathodic current is for reduction, and anodic current is for oxidation. During the course
of reduction, if the Low E limit is reached, the current polarity will be automatically
switched to anodic. Similarly, if the High E Limit is reached during oxidation process, the
current will be automatically switched to cathodic. The number of current polarity switching
depends on the Number of Segments. When the number of segments is reached, the
experiment stops.
2. The initial current polarity is determined by the Initial Polarity parameter.
3. During the experiment, the data will be updated in a rate same as data storage interval.
4. In general, the data storage interval should be chosen according to the length of the
experiment. The longer the experiment, the larger the data storage interval. Whenever the
data exceed the maximum allowed points, the data storage interval will be doubled
automatically. Therefore, data points will not overflow for an unexpected long experiment.
5. Though large number of segments is possible, the data will be stored only for first 400
segments. The later segments will be displayed during the run, but will not be stored.
6. The current polarity can be switched either at the specified potential or at the specified
time. Cathodic and anodic time setting can be different. On the other hand, even with time
priority selected, if the limiting potential is reached, the current polarity will still be reversed
in order to protect the electrode.
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Chapter 4. Setup Menu
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Parameters for Chronopotentiometry with Current Ramp
In Chronopotentiometry with Current Ramp (CPCR), a current ramp can be applied to
the working electrode. The potential is recorded as the function of time. The following diagram
shows the current waveform applied as the function of time.
Current (A)
Final Current
Scan Rate (A/s)
Init Current
Time (s)
The following are the experimental parameters, their range and descriptions:
Param
Init Current (A)
Final Current (A)
Scan Rate (A/s)
Sample Interval (sec)
High E Limit (V)
Low E Limit (V)
Data Storage Intvl (sec)
Range
-0.25 - +0.25
-0.25 - +0.25
1e-10 - 0.01
0.0025 - 32
-10 - +10
-10 - +10
0.0001 - 32
Description
Initial current
Initial current
Current scan rate
Sampling interval
High potential limit value
Low potential limit value
Data storage interval
Notes:
1. Initial Current and Final Current should be at least 1e-9A apart.
2. Positive current is for reduction, and negative current is for oxidation. During the course
of reduction, if the High E or Low E limit is reached, the experiment stops.
3. At least 10 points are required to run the experiment. Otherwise, you have to reduce the
current scan rate or reduce the sampling interval.
4. During the experiment, the data will be updated in a rate same as data storage interval.
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Chapter 4. Setup Menu
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5. In general, the data storage interval should be chosen according to the length of the
experiment. The longer the experiment, the larger the data storage interval. Whenever the
data exceed the maximum allowed points, the data storage interval will be doubled
automatically. Therefore, data points will not overflow for an unexpected long experiment.
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Chapter 4. Setup Menu
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Parameters for Multi-Current Steps
In Multi-Current Steps (ISTEP), twelve current steps can be applied and cycled. The
potential is recorded as the function of time. The following diagram shows the current waveform
applied as the function of time.
Steps:
Current (A)
1 2 3 4 5 6 7 8 9 10 11 12
Cycle 1
Cycle 2
Time (s)
The following are the experimental parameters, their range and descriptions:
Param
Step Sequence 1 - 12:
Step i (A)
Step Time (s)
High E Limit (V)
Low E Limit (V)
No. of Cycles
Smpl Intv (s)
Range
Description
-0.25 - +0.25
0 - 10000
Step current
Step duration
-10 - +10
-10 - +10
1 - 10000
0.0001 - 1
Potential high limit
Potential low limit
Number of cycles
Sample interval
Notes:
1. If the step time is less than 0.001 sec, this step will be ignored.
2. If the step time is shorter than the sample interval, this step will be ignored.
3. Sample interval will be automatically increased if (step time * cycles / sample interval)
exceeds 128K and if data is transferred after experiment..
4. If the sample interval is larger than 0.002 sec, data is transferred and displayed real time.
5. The experiment will stop if the potential reaches either High E Limit or Low E Limit.
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Chapter 4. Setup Menu
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Parameters for Potentiometric Stripping Analysis
Potenital (V) or Current (A)
In Potentiometric Stripping Analysis (PSA), a potential-controlled deposition step is
applied first. After deposition, the elements cumulated at the electrode surface is stripped out by
applying a constant current. The potential is recorded as the function of time. The following
diagram shows the potential waveform during the deposition stage and the current waveform
during the stripping stage.
Data Storage Interval
Stripping Current
Deposition E
Deposition Time
0
Time (s)
The following are the experimental parameters, their range and descriptions:
Parameters
Deposition E (V)
Deposition Time (sec)
Final E (V)
Stripping Current (A)
Sample Interval (sec)
Quiet Time (sec)
Range
-10 - +10
0 - 100000
-10 - +10
-0.25 - +0.25
0.0001 - 50
0 - 100000
Description
Deposition potential
Deposition time
Final potential, see note 2
Controlled stripping current
Sampling interval
Quiescent time before taking data
Notes:
1. If sample interval is less than 0.002 s, Total 64K data points are allowed. The data
density equals to the Run Time / 64000.
2. If the final potential is reached, the experiment will automatically stop.
3. If the controlled stripping current is set to zero, the counter electrode is actually not
connected.
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Chapter 4. Setup Menu
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4. If the controlled stripping current is smaller than 1.0e-10A, no current will flow during
experiment.
5. You do not have to worry about the current polarity. The system will automatically
assign the current polarity according to the deposition potential and the final potential.
Positive current is for reduction. Negative current is for oxidation.
6. In general, the data storage interval should be chosen according to the length of the
experiment. The longer the experiment, the larger the data storage interval.
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Chapter 4. Setup Menu
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Parameters for Electrochemical Noise Measurement
In Electrochemical Noise Measurement (ECN), no waveform is applied to the
electrochemical cell. The working electrode is at the zero-resistance ammeter. Its potential is at
virtue ground (very close to ground but can not be connected to true ground). To measure
electrochemical noise, an identical electrode to the working electrode should be connected to the
instrument ground (black banana jack on the real panel labeled as GND), and immerse these two
electrodes in the same solution. The electrochemical noise current pass through these two
electrodes will be measured. If the potential noise needs to be measured, a reference electrode
can be added to the solution and connected to the reference clip. The counter electrode will not
be used.
The system displays an Electrochemical Noise Measurement Parameters dialog box:
The following are the experimental parameters, their range and descriptions:
Parameters
Sample Interval (sec)
Run Time (sec)
Quiet Time (sec)
Sensitivity (A/V)
Potential Gain
Measurement Mode
Range
0.1 - 10
10 - 100000
0 - 100000
1e-12 - 0.1
1, 10, 100, 1000
i, E or both
Description
Sampling interval
Experiment running time
Quiescent time before sampling data
Sensitivity scale
Gain Setting for potential noise measurement
Measurement mode
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Chapter 4. Setup Menu
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Parameters for Open Circuit Potential - Time
In Open Circuit Potential – Time (OCPT), the working and reference electrodes are
connected and the potential difference between these two electrodes is recorded as the function
of the time. Since the counter electrode is not connected to the external cell, no current is pass
through the working electrode, except the bias current of the measuring amplifiers, which is in
picoamperes range.
The system displays an Open Circuit Potential - Time Parameters dialog box:
The following are the experimental parameters, their range and descriptions:
Parameters
Run Time (sec)
Sample Interval (sec)
High E Limit (V)
Low E Limit (V)
Range
0.1 - 500000
0.0025 - 50
-10 - +10
-10 - +10
Description
Experiment running time
Sampling interval
High potential limit
Low potential limit
Notes:
1. If high or low potential limit is reached, a warning will be given.
2. In general, the data storage interval should be chosen according to the length of the
experiment. The longer the experiment, the larger the data storage interval.
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Chapter 4. Setup Menu
________________________________________________________________________
System Command
Use this command to set up the serial communication port, current polarity, potential axis
and current axis.
This command presents a System Setup dialog box:
The following options allow you to set up your system:
Communication Port
Select the communication port to link the PC to the instrument.
Com Port Speed
Select the communication port speed to link the PC to the instrument. Standard is
guaranteed to work with any computer. Fast may or may not work with a particular
computer. When Fast is chosen, the real time data transfer will be done at higher scan rate or
shorter sample interval.
Current Polarity
You can either select cathodic current as positive current or anodic current as positive
current. You should set this before experiment, otherwise the experimental results (peaks and
waves) will not be reported properly.
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Chapter 4. Setup Menu
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Potential Axis
You can set positive potential axis either left or right. This is meaningful only for
voltammetric or polarographic modes.
Current Axis
You can set positive current axis either up or down.
Line Frequency
Set line frequency according to what is applied. This helps set default sample interval in
certain techniques to reduce the interference from the line frequency.
Windows
if you are using English Windows, please choose English. If you are using Chinese,
Japanese, or Korean Windows, check Oriental. Oriental Windows shows slightly bigger
letters than English Windows. The Technique selection field may be truncated if you select
English Windows. Also oriental Windows does not support certain symbols. For instance,
symbol "µ" will not be displayed properly. Choose oriental Windows will use "u" instead of
"µ".
Data Length
The default data length is 128K. The longer the data length, the more computer resource
will be used. It is recommended not to use long data length unless necessary. Using long data
length will need large computer memory such as 256M, 512M RAM or more. It will also
slow down the system and prohibit other programs to run.
After you change the data length setting in the System Setup command, please exit the
program and restart the program so that the data length can be set properly. Otherwise the
program may crash.
If the data is acquired and saved with long data length setting, but read back with shorter
data length setting, the program may crash. Therefore once you used long data length setting,
you should not set to shorter data length later. Please think carefully before you decide to
increase the data length.
Save retrieve data during run
Check this option will allow data to be saved on the hard drive during run. In case
experiment does not complete due to external interference or interruption, miss
communication, partial data can be recovered. This is useful for very slow experiments.
Hours of experimental data can be recovered.
This option is not active by default. If you do not run very slow experiments, you can rerun the experiment if the experiment is interrupted by accident.
To retrieve experimental data of last run, you should use Retrieve command under the
File menu.
Present Data Override Warning
If your experimental data is not saved before running a new experiment or opening an
existing file on the disk, your unsaved data will be overridden. This option will allow system
to issue a warning before the data is lost.
Save Text File As Well
Normally only binary data files is saved. Binary file contains more information
(including experimental control information) but small in size. This option allows you to
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Chapter 4. Setup Menu
________________________________________________________________________
save text file as well whenever you save the binary data. This is useful for those who want to
export data to other software, such as spreadsheet software.
Erase ADC Calibration Coefficients
The analog-to-digital converter (ADC) calibration coefficients are stored in the
instrument non-volatile memory. ADC calibration is carried out in CH Instruments before the
instrument is shipped. You use this command only if you want to recalibrate the ADC. After
you erase ADC calibration coefficients, you will see a prompt of ADC calibration when you
run next hardware test or experiment.
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Chapter 4. Setup Menu
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Hardware Test Command
Use this command to test the system hardware. The system will test digital and analog
circuitry.
After the test, the system will display the Hardware Test Results dialog box:
Digital Circuitry Test
The software version and the last revision date for the Flash ROM is shown.
Potential and current offset test
If test is failed, the error message will be given.
Sensitivity scale test
If test is failed, the error message will be given. Most times the error is related to leakage
current.
Gain test
There are 3 gain stages. If test is failed, the error message will be given.
Analog Test Summary
The test results of analog circuitry are summarized. A message of “Analog circuitry test
OK.” will appear if no error is detected, otherwise an error message will appear. In case there
is error and the cause is due to the analog-to-digital converters, it will also be reported.
If you see analog test error, please repeat the test several times and see if the error is
consistent. Record the error message and contact the factory for servicing.
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Run Command
Use this command to run experiment.
This command is also used to skip Quiet Time, Deposition Time and
Preconditioning. In the middle of Quiet Time, Deposition Time and Preconditioning, you
can use this command to go to next step.
Before run, the instrument will check the data link. If link fails, the command is
terminated, and an error message will appear.
The software will also check the combination of experimental parameters. If
illegal combination is encountered, the command is terminated, and an error message will
appear.
In most cases, real time data display is possible. However, when the data
acquisition speed is higher than the data transmission rate, the data will be displayed
immediately after the experiment.
You can stop running experiment by invoking the Stop command.
You can copy the graphics during run to the clipboard.
This command has a toolbar button:
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Chapter 5. Control Menu
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Pause/Resume Command
Use this command to pause and resume experiment.
This command does not work for time based experiments, such as CA, CC, BE, it, DPA, DDPA, TPA, IMP, IMP-t, CP, PSA, and etc.
This command has a toolbar button:
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Chapter 5. Control Menu
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Stop Run Command
Use this command to stop running experiment.
You can also use this command to stop repetitive runs and macro command while
running experiment.
This command has a toolbar button:
Reverse Scan Command
Use this command to reverse the potential scan direction during cyclic
voltammetry experiment.
Each time this command is invoked, sweep segment counter increments.
If this command is used during experiments, some data analysis features will not
work, such as peak search.
This command does not work for other techniques.
This command has a toolbar button:
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Chapter 5. Control Menu
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Run Status Command
Use this command to check and change certain status related to running
experiment, such as iR compensation, smoothing, purge, stir, and prerun mercury drops,
enable or disable automatic smoothing after running each experiment.
This command presents a Run Status dialog box:
The following options allow you to change certain status related to running
experiment:
Calibration before Run
When this box is checked, the potential and current offset will be measured and
will be compensated. Disable this option will reduce the time delay before running
each experiments.
Check Connection before run
When this box is checked, the connection of the counter and reference electrodes
will be checked. If one of the electrodes is not connected, a warning message will
appear. This can prevent accidental damage of working electrode due to open loop of
the potentiostat. You should check the connection or you may ignore the warning.
Disable this option will reduce the time delay before actual running of experiments.
Use Open Circuit E as Init E
When this box is checked, the system will test open circuit potential before
running the experiment, and use the open circuit potential as initial potential.
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Chapter 5. Control Menu
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External Trigger Run
When this box is checked, Run will be initiated by the external trigger signal from
the Cell Control port on the rear panel. See appendix for the pin assignment.
iR Comp for Next Run
When this box is checked, the iR compensation for next run is enabled. You may
not be able to enable iR compensation if the automatic compensation is set and the iR
compensation test is not conducted or the sensitivity scale is altered. Certain
techniques, such as TAFEL, BE, IMP, CP and PSA, do not allow iR compensation.
This option can also be turned on or off from iR Compensation command under
Control menu.
Smooth After Run
When this box is checked, the automatic smoothing after run is enabled. Certain
techniques, such as TAFEL, BE and IMP, do not allow smoothing. This option can
also be turned on or off from Smoothing command under DataProc menu.
There are two types of digital smoothing available: the least square and Fourier
transform smoothing. To set the mode of smoothing, use Smoothing command under
DataProc menu.
Purge Between Runs
Check this item will allow purge between runs. This item can also be turn on or
off from Purge command under Control menu.
Stir Between Runs
Check this item will allow stir between runs. This item can also be turn on or off
from Stir command under Control menu.
Rotate during Deposition Time
Check this item will turn the rotator on during the deposition time in the stripping
analysis. This item can also be turn on or off from Rotating Disk Electrode command
under Control menu.
Rotate during Quiet Time
Check this item will turn the rotator on during the quiet time. This item can also
be turn on or off from Rotating Disk Electrode command under Control menu.
Rotate during Run
Check this item will turn the rotator on when experiment is running. This item can
also be turn on or off from Rotating Disk Electrode command under Control menu.
Rotate between Runs
Check this item will turn the rotator on between runs. This item can also be turn
on or off from Rotating Disk Electrode command under Control menu.
Rotation Speed (rpm)
This parameter set the speed of the rotating disk electrode. The parameter range is
0 - 10000.
SMDE Drops Before Run
The default value of this parameter is 1. Normally the system will issue a
combined dispense and knock signal before running experiment to allow a new drop
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Chapter 5. Control Menu
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to be formed when the static mercury drop electrode (SMDE) is used. You can
change this default condition. The parameter range is 0 - 20. If the prerun drop is set
at 0, the same drop used in the previous experiment will be used for the next
experiment. More than one prerun drops might be useful if the SMDE occasionally
traps little air bubble in the capillary and loses contact.
This option can also be varied from Cell command under Control menu.
Abort Experiment at Level
Experiment will be terminated automatically if the current or charge level reaches
the specified value (or overflow). It allows electrode over-current protection. If No is
selected, experiment will end normally.
Current Display during Quiet Time
You can display current during quiet time either numerically or graphically. The
sensitivity scale will be switched automatically in order to read current properly. If
No is selected, current will not be displayed and the sensitivity will be the same as
what used in the experiment.
Abort Quiet Time
Quiet time before data acquisition will be terminated automatically if the current
or charge level reaches the specified value (or overflow). If No is selected,
experiment will end normally.
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Chapter 5. Control Menu
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Repetitive Runs Command
Use this command to run a series of experiments.
During repetitive runs, the instrument will check the data link. If link fails, the
command is terminated, and an error message will appear.
The system will also check the combination of experimental parameters. If illegal
combination is encountered, the command is terminated, and an error message will
appear.
This command presents a Repetitive Runs dialog box:
The following options allow you to define parameters for repetitive runs:
Number of Runs
Enter the number of runs. The parameter range is 1 - 9999.
Time Interval Between Runs
This parameter allows a delay time between two successive runs. The parameter
range is 0 - 32767.
This parameter is not effective, if Prompt Before Each Run is enabled.
Prompt Before Each Run
When Manual is selected, a prompt will be issued before each run (except the 1st
run). The instrument will wait until you respond.
When External Trigger is selected, the instrument will wait for external trigger
signal. External trigger is an active low signal and can be applied to the Pin 13 of the
Cell Control port on the rear panel.
When Manual or External Trigger is selected, Time Interval Between Runs has no
effect.
Base Filename
Enter the base filename. Maximum 5 characters are allowed. After run, the data is
saved. The run number will be attached to the base filename, i.e., filenameN, where N
is the run number from 1 to 999. If the base filename is not specified, a warning will
be given. If you continue, the system will run experiments without saving the data.
The browse button allows user to choose the base filename from different
directory.
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Chapter 5. Control Menu
_____________________________________________________________________________________
Data Averaging When Done
When this item is checked, the data of repetitive runs will be averaged and saved
as filename0.
5-8
Chapter 5. Control Menu
_____________________________________________________________________________________
Multiplexer Command
Use this command to run a series of experiments using multiplexer. The hardware
requirement is the CHI684 Multiplexer. The minimum channel for the CHI684 is 8. The
channel increment is 8. The maximum channels are 64.
The multiplexer switches four lines (working, sensing, reference, and counter
electrodes). You can have maximum 64 cells, but only one cell can be connected at a
time.
This command presents a Multiplexer dialog box:
The following options allow you to define parameters for repetitive runs:
Channel Selection
You can select any channel by checking that channel. Uncheck any channel will
disable it. If you select a channel that is beyond your CHI684 channel number, it will
be ignored.
Prompt Before Each Run
When Manual is selected, a prompt will be issued before each run (except the 1st
run). The instrument will wait until you respond.
When External Trigger is selected, the instrument will wait for external trigger
signal. External trigger is an active low signal and can be applied to the Pin 13 of the
Cell Control port on the rear panel.
Base Filename
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Chapter 5. Control Menu
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Enter the base filename. Maximum 5 characters are allowed. After run, the data is
saved. The run number will be attached to the base filename, i.e., filenameN, where N
is the run number from 1 to 99999. If the base filename is not specified, a warning
will be given. If you continue, the system will run experiments without saving the
data.
The browse button allows user to choose the base filename from different
directory.
Immediate Channel Set
It allows you to set arbitrary channel immediately. You can then exit the dialog
box and run experiment for that particular channel.
Run Multiplexer
Press this button will run experiment in a sequence of selected channels using the
CHI684 Multiplexer. If you provide the base file name, the file will automatically
saved after each run as base filename+channel number.bin. For instance, if you set
base filename as "test", and you select channels 3, 8, 23, and 58, Run Multiplexer will
run 4 experiments and save data as test3.bin, test8.bin, test23.bin, and test58.bin.
Before execution, the system will check the filename. If existing data files have a
same base filename, an override warning will be issued. The experimental conditions
should be set before this command is executed.
Multiplexer related Macro Command
There are also two Macro command for multiplexer. One is "mch:##". This macro
comamnd allow you to set individual channel. The other macro command is "mchn".
This is used in For...Next loop. It will select the channel according to the For...Next
loop counter. However, "mchn" will run in 1,2,3,4... sequence. You can not skip
channels when you use For...Next loop.
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Chapter 5. Control Menu
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Macro Command
Use this command to execute a series of commands in the order you specified.
This is particularly useful if a sequence of action needed to be taken.
This command presents a Macro Command dialog box:
The following options allow you to edit, load, save and execute macro command:
Read
You can read in macro command that you saved as a disk file before.
This command presents a Open dialog box so you can select your file.
Save
You can save the macro command that you edited to a disk file. You can retrieve
it later.
This command presents a Save As dialog box so you can name your file.
Run Macro
Press this button will execute the macro command. Before execution, the system
will check the validity of the command and parameters. If error is detected, the system
will terminate the macro and issue a warning message.
Macro Command Editor
Type in commands in the editor box. Each command occupies one line. The
command is case insensitive. Space will be ignored. If a parameter is required
following the command, a colon ":" or a equal sign "=" is used to separate the
command and parameter.
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Chapter 5. Control Menu
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The following are the legal commands:
command
parameter
explanation
tech
run
save
string
for
next
delay
purge
stir
cellon
celloff
rdeon
rdeoff
mch
mchn
1 - 999
ei
eh
el
ef
eio
-10
-10
-10
-10
e2
e2on
e2off
v
incre
pn
-10 - +10
cl
si
1 - 10000
.001 - .064
sens
sens2
autosens
qt
ht
pw
amp
sw
st
prod
freq
iratio
bepe
bept
rpm
i
ic
1e-12 - .1
1e-12 - .1
string
1 - 32000
1 - 32000
1 - 32000
1 - 64
-
+10
+10
+10
+10
1e-6 - 2e4
.01 - .05
'p' or 'n'
0 - 100000
0 - 100000
1e-4 - 1e3
.001 - .5
1e-4 - 50
.001 - 5e5
.01 - 50
1 - 100000
0 - 100
-10 - +10
0 - 100000
0 - 10000
0 - 0.25
0 - 0.25
select an electrochemical technique
run experiment
save data to a disk file; In case of For…Next
loop, the filename will be truncated to 5 letters.
The loop number (1-999) will be added to the
filename
for…next loop, only one layer is allowed
for…next loop
delay between commands
purge for a given time
stir for a given time
cell on between runs
cell off between runs
turn on RDE
turn off RDE
select multiplexer channel
multiplexer channel selection according to the
For…Next loop
initial potential
high limit of potential in CV, CA, CP
low limit of potential in CV, CA, CP
final potential for single sweep tech and PSA
use open circuit potential as init E. This flag will
be turned off after a new init E is entered
potential for the second working electrode
turn on the second working electrode
turn off the second working electrode
scan rate
increment potential
initial potential change direction in CV, CA;
initial current polarity in CP
number of segments in CV and CP
sample interval or data storage interval in BE,
CP
sensitivity
sensitivity for the second working electrode
automatic sensitivity for slow CV or LSV
quiescent time before run
hold time at final E in TAFEL
pulse width
a.c. or pulse amplitude
sampling width
total sample time in I-t curve
sampling period
frequency
end current ratio in BE
pre-electrolysis potential in BE
pre-electrolysis time in BE
rotation rate of RDE
controlled current in PSA
cathodic current in CP
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Chapter 5. Control Menu
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ia
tc
ta
priot
prioe
fl
fh
mt
0 - 0.25
0.05 - 100000
0.05 - 100000
cl1
cl2
cl3
cl4
cl5
depeon
depeoff
depe
dept
pcon
pcoff
pce1
pce2
pce3
pct1
pct2
pct3
ei1
ei2
ei3
ei4
ei5
ei6
ef1
ef2
ef3
ef4
ef5
ef6
v1
v2
v3
v4
v5
v6
es1
es2
es3
es4
es5
es6
st1
st2
st3
st4
1
1
1
1
1
.0001-10000
.001-100000
1 - 1024
-
4096
4096
256
256
16
-10 - +10
1 - 100000
-10 - +10
-10 - +10
-10 - +10
0 - 6400
0 - 6400
0 - 6400
-10 - +10
-10 - +10
-10 - +10
-10 - +10
-10 - +10
-10 - +10
-10 - +10
-10 - +10
-10 - +10
-10 - +10
-10 - +10
-10 - +10
1e-4 - 10
1e-4 - 10
1e-4 - 10
1e-4 - 10
1e-4 - 10
1e-4 - 10
-10 - +10
-10 - +10
-10 - +10
-10 - +10
-10 - +10
-10 - +10
0 - 10000
0 - 10000
0 - 10000
0 - 10000
anodic current in CP
cathodic time in CP
anodic time in CP
time priority in CP
potential priority in CP
low frequency in IMP
high frequency in IMP
measuring time when freq is above 10Hz in
IMP
measuring cycles when freq is 1-10 Hz in IMP
measuring cycles when freq is .1-1 Hz in IMP
measuring cycles when freq is .01-.1 Hz in IMP
measuring cycles if .001-.01 Hz in IMP
measuring cycles if .0001-.001 Hz in IMP
deposition potential on in stripping mode
deposition potential off in stripping mode
deposition potential
deposition time
turn on preconditioning
turn off preconditioning
potential of the 1st stage of preconditioning
potential of the 2nd stage of preconditioning
potential of the 3rd stage of preconditioning
time of the 1st stage of preconditioning
time of the 2nd stage of preconditioning
time of the 3rd stage of preconditioning
initial potential 1 in SSF
initial potential 2 in SSF
initial potential 3 in SSF
initial potential 4 in SSF
initial potential 5 in SSF
initial potential 6 in SSF
final potential 1 in SSF
final potential 2 in SSF
final potential 3 in SSF
final potential 4 in SSF
final potential 5 in SSF
final potential 6 in SSF
scan rate 1 in SSF
scan rate 2 in SSF
scan rate 3 in SSF
scan rate 4 in SSF
scan rate 5 in SSF
scan rate 6 in SSF
step potential 1 in SSF and STEP
step potential 2 in SSF and STEP
step potential 3 in SSF and STEP
step potential 4 in SSF and STEP
step potential 5 in SSF and STEP
step potential 6 in SSF and STEP
step time 1 in STEP
step time 2 in STEP
step time 3 in STEP
step time 4 in STEP
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Chapter 5. Control Menu
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st5
st6
0 - 10000
0 - 10000
step time 5 in STEP
step time 6 in STEP
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Chapter 5. Control Menu
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Open Circuit Potential Command
Use this command to measure the open circuit potential.
The open circuit potential is the potential between the working electrode and
reference electrode while no current flows through the cell. This is an important
parameter. It tells you what is the initial state before you start experiment. You can then
figure out if the compound under study is oxidizable or reducible.
After the measurement, the system will display the open circuit potential value
through the Open Circuit Potential dialog box. Click OK to close the dialog box after you
read it.
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Chapter 5. Control Menu
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iR Compensation Command
Use this command to test the solution resistance and the cell time constant, as
well as to enable or disable automatic or manual iR compensation.
This command presents an iR Compensation dialog box:
The following options allow you to set iR compensation parameters:
iR Comp Test Results
If you click the iR Test button, the system will engage solution resistance and cell
time constant test. The result will be reported here.
After that the system will test the stability by gradually increase the compensation
level until the desired compensation level is reached or if the system is no longer
stable. The actually allowed compensation level and the uncompensated resistance
will be displayed. The uncompensated resistance is calculated from the measured
resistance and the allowed compensation level.
Please note that the maximum allowed resistance compensation may also be
limited to the feedback resistor of the i/E converter.
iR Comp Test
Before start iR compensation test, you should check the test parameters.
Test E is the test potential where no electrochemical reaction will occur. When
the system is doing test, it applies a potential step around the test potential. The test
result is good only if the electrochemical cell can be equivalent to a solution
resistance in series with a double layer capacitor. The range of Test E is -10V - +10V.
You may adjust the potential step amplitude. The larger the amplitude, the higher
the signal-to-noise ratio. However, too large amplitude may cause faradaic current to
flow. A step amplitude of 0.05V is recommended. The range of Step Amplitude is
0.01 - 0.25 V.
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The compensation level is the percentage of resistance you want to compensate
based on the measured solution resistance. The range of this parameter is 0 - 200%.
The default value is 100%.
Overshoot level is the criterion of the stability test. As the amount of positive
feedback increases, the system might become unstable. Before the potentiostat start to
oscillate, the overshoot in current response to the potential pulse will appear. The
higher the allowed overshoot level, the higher the possible compensation level, but
the worse the system stability. The range of this parameter is 0 - 100%. The default
level is 2%.
If you click the iR Test button, the system will engage solution resistance and
stability test. The result will be reported in the iR Comp Test Results Box.
For more details about the iR compensation, please see “Intelligent, Automatic
Compensation of Solution Resistance”, P. He, and L. R. Faulkner, Anal. Chem., 58,
517-523 (1986).
iR Compensation for Next Run
When this box is checked, the iR compensation for next run is enabled. You may
not be able to enable iR compensation if the automatic compensation is set and the iR
compensation test has not been conducted or the sensitivity scale has been altered.
This option can also be turned on or off from Run Status command under Control
menu.
iR Comp Enable
If the option "Once" is chosen, the iR compensation will only be applied to next
run and then disabled. If you want the same compensation conditions to be applied to
the consecutive runs, choose "Always" option. Click the proper radio button to select
the option.
iR Comp Mode
You can choose automatic iR compensation or manual iR compensation. The
automatic iR compensation will be based on the iR compensation test results. You
can also choose manual iR compensation by entering the resistance value you want to
compensate. Click the proper radio button to select the option.
Manual Compensation Resistance
If you select manual iR compensation, you should enter the resistance value that
you want system to compensate. Be careful about the compensation level. If the
compensation level is close or exceeds the actual solution resistance, the potentiostat
will oscillate. Please also notice that the maximum allowed resistance compensation
may be limited to the feedback resistor of the i/E converter.
This parameter has no effect if automatic iR compensation is selected.
This command has a toolbar button:
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Filter Setting Command
Use this command to set potential and current filters.
The potential filter is used to filter the potential waveforms. It is a second order
Bessel low-pass filter. It can be used to filter out transient components. An application is
to convert the staircase ramp to linear sweep.
A capacitor might be connected to the feedback resistor of the i/E converter to
form a low-pass RC filter. It can remove the high frequency noise at the first hand.
The signal filter is employed before the gain stage. It is a second order Bessel
low-pass filter.
The filters are useful in reducing the noise during measurement.
This command presents a Filter Selection dialog box:
The following options allow you to set filter parameters:
If you are not familiar with the concept and parameters, please choose automatic
setting.
Potential Filter
This box displays the actual potential filter setting.
Selection
Select the potential filter cutoff frequency. This is a 2nd order Bessel filter. The
setting of this filter depends on the type of experiment and the time scale of the
experiment. Choosing automatic will give you the default setting. This filter is used
to shape the waveforms. In ac impedance measurement, it filters out the high
frequency components to avoid aliasing. In linear sweep voltammetry, it convert the
staircase ramp to true linear potential sweep.
i/E Conv. Filter
This box displays the actual current-to-voltage converter filter setting.
Selection
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Select the i/E converter filter cutoff frequency. This is an RC filter in conjunction
with the current-to-voltage (i/E) converter. The setting of this filter depends on the
type of experiment and the time scale of the experiment. Choosing automatic will
give you the default setting.
Sometimes certain cutoff frequency can not be selected, because for a given
sensitivity scale, the feedback resistor of i/E converter is determined and the
combination of RC can not make up the cutoff frequency you selected. This could
happen if you want to select a relatively low cutoff frequency but use a low
sensitivity scale, or if you want to select a relatively high cutoff frequency but use a
high sensitivity scale. You may be able to set to the proper cutoff frequency by
altering the sensitivity scale.
Signal Filter
This box displays the actual signal filter setting.
Selection
Select the signal filter cutoff frequency. This is a 2nd order Bessel filter. The
setting of this filter depends on the type of experiment and the time scale of the
experiment. Choosing automatic will give you the default setting.
This command has a toolbar button:
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Cell Command
Use this command to control purge, stir, and electrochemical cleaning. You can
also set signal level of stir line, mercury drop collection, prerun drops, and stabilizing
capacitor.
This command presents a Cell Control dialog box:
The following options allow you to set the cell control:
Control Level of Stir Line
The stir line control signal can be either active high or active low. BAS uses an
active high control signal, whereas PAR uses an active low signal. You can click the
radio button to select the proper control level.
Immediate Stir
You can enter immediate stir time. The parameter range is between 1 - 32767.
Press the Stir button will activate immediate stir.
Immediate Purge
You can enter immediate purge time. The parameter range is between 1 - 32767.
Press the Purge button will activate immediate purge.
Immediate Cell On
You can enter the cell potential (range from -10 to +10) and the cell on time
(range from 1 to 32767). Press the Cell On button will poise the electrode at the given
potential for a given amount of time.
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Mercury Drop Collection
This is a useful option for you to collect and then weigh mercury drops. Enter the
number of drop you want to collect (range from 1 to 1000) and the time interval
between drops (range from 0.5 to 10). Press Collect pushbutton will activate the
collection process.
Stir Between Runs
Check this item will allow stir between runs. This item can also be turned on or
off from Run Status command under Control menu.
Purge Between Runs
Check this item will allow purge between runs. This item can also be turned on or
off from Run Status command under Control menu.
Stir and Purge Simultaneously
Check this item will couple stir and purge.
Test with Internal Dummy Cell
Internally there is a 1K ohm resistor as dummy cell. When this option is checked,
the cell will not be turned on, instead the internal dummy cell will be used to run
experiment. This option is useful for instrument test.
SMDE Drops Before Run
The default value of this parameter is 1. Normally the system will issue a
combined dispense and knock signal before running experiment to allow a new drop
to be formed when the static mercury drop electrode (SMDE) is used. You can
change this default condition. The parameter range is 0 - 20. If the prerun drop is set
at 0, the same drop used in the previous experiment will be used for the next
experiment. More than one prerun drops might be useful if the SMDE occasionally
traps little air bubble in the capillary and loses contact.
This option can also be changed from Run Status command under Control menu.
Stabilizing Capacitor
There is a 0.1 µF stabilizing capacitor that might be connected between the
counter and reference electrodes. This capacitor can stabilize the potentiostat but
somewhat slow the system down. This is particularly useful when the double layer
capacitance of working electrode is large, such as in bulk electrolysis, or in case high
degree of iR compensation is required.
The default for this stabilizing capacitor is automatic setting. You can disable the
automatic setting and then enable or disable the stabilizing capacitor by clicking one
of the radio buttons.
4 Electrodes
Check this will set the potentiostat at 4-electrode configuration.
It can be used for liquid/liquid interface measurements. In this case, the red clip is
connected to the counter electrode in phase I. The white clip is connected to the
reference electrode of the same phase. The green clip is connected to the counter
electrode in phase II. The black clip is connected to the reference electrode of phase
II.
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The 4th electrode can also be used for sensing the voltage drop due to the contact
resistance of electrode clip, connector, relay, and circuit board traces. The contact
resistance could be about 0.2 - 0.3 ohm. It can cause 50 - 75 mV voltage drop if the
current is at 250 mA. It also makes low impedance cell (such as battery) measurement
impossible. With the 4th electrode introduced, the effect of contact resistance can be
eliminated and low impedance cell can be readily measured.
You should turn the 4th electrode off if you do not use 4-electrode configuration.
Otherwise the potential will be out of control if the sensing electrode is left
unconnected. This could damage the electrodes.
Cell On Between Runs
By default, the cell will be turned on during run and turned off after run. Check
this will make the cell connected after run. Caution should be take when this item is
checked. Connect or disconnect the cell in an improper sequence could damage the
electrodes when the cell is on. It is recommended to connect the reference and
counter electrodes first. When disconnect, disconnect the working electrode first.
Return to Initial E after Run
Check this will let the potential return to the Initial E after run. Otherwise, the
potential will remain at the end value of the previous run. This will make sense only
if Cell On Between Runs is checked.
This command has a toolbar button:
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Step Functions Command
Use this command to generate a contineous square waveform. This command can
be used for electrode conditioning (or cleaning), or other purposes.
No data will be collected and displayed.
The system displays the Step Functions dialog box so you can set the step
conditions and run the step function generator:
The following options allow you to set set the step potentials, duration and
segments:
Param
Range
Description
-10 - +10
Starting potential
Start E (V)
0 - 100000
Duration at Start E
Duration (s)
-10 - +10
First step potential
Step E1 (V) / i1 (A)
.0001 - 100000
Duration of each step
Step Time 1 (s)
-10 - +10
Second step potential
Step E2 (V) / i2 (A)
.0001 - 100000
Duration of each step
Step Time 2 (s)
1 - 2000000000
Step segments, each segments is half cycle
Step Segments
Galvanostatic Mode Check or Uncheck Select potentiostatic or galvanostatic mode
Notes:
1. The potential range among Start E, Step E1 and Step E2 should be less than 13.1
V.
2. If the Duration at Start E is less than 0.001 sec, the Start E will be ignored.
3. The step is in a sequence of Step E1, Step E2, Step E1, Step E2, ... The ending
potential is at Step E1 for odd number of segments, at Step E2 for even number of
segments.
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Run
Press the Run button will activate the step function generator. A status box will be
displayed showing the number of steps completed, the remaining steps and the
remaining time. You can cancel this function by pressing the Stop pushbutton.
No data will be collected and displayed.
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Preconditioning Command
Use this command to condition working electrode before running an experiment.
This can be useful for cleaning the electrode or other usages. Preconditioning occurs
before the deposition or quiet time.
This command presents a Preconditioning before Run dialog box:
You can program the conditioning in three steps. The following options allow you
to set preconditioning:
Enable Preconditioning
Preconditioning occurs before the deposition or quiet time. Uncheck this box will
bypass the proconditioning step.
Potential
The parameter range is between -10 - 10.
Time
The parameter range is between 0 - 6400. If preconditioning time for a particular
step is zero, this step will be bypassed. If the time setting is less than 1 msec, the time
control may not be accurate.
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Rotating Disk Electrode Command
(Model 630B/650B/660B)
Use this command to set the rotation rate for the rotating disk electrode. You can
also control the rotator on and off in various cases.
This command presents a Rotating Disk Electrode Control dialog box:
The following options allow you to set the rotating disk electrode control:
Rotation Speed (rpm)
This parameter set the speed of the rotating disk electrode. The parameter range is
0 - 10000. There are banana jacks on the rear panel of the instrument that will output
a 0 - 10 V voltage that corresponds to 0 - 10000 rpm rotation rate.
Rotate during Deposition Time
Check this item will turn the rotator on during the deposition time in the stripping
analysis. This item can also be turn on or off from Run Status command under
Control menu.
Rotate during Quiet Time
Check this item will turn the rotator on during the quiet time. This item can also
be turn on or off from Run Status command under Control menu.
Rotate during Run
Check this item will turn the rotator on when experiment is running. This item can
also be turn on or off from Run Status command under Control menu.
Rotate between Runs
Check this item will turn the rotator on between runs. This item can also be turn
on or off from Run Status command under Control menu.
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Stripping Mode Command
Use this command to enable of disable the stripping mode and set the deposition
condition. The stripping mode command is only available to LSV, SCV, DPV, NPV,
SWV, ACV and SHACV. It is also not available if a polarographic mode is chosen.
This command presents a Stripping Control dialog box:
The following options allow you to set stripping mode control:
Stripping Mode Enabled
When this item is checked, the stripping mode is enabled. When it is enabled, a
deposition step will be inserted before quiescent time step while running experiment.
The deposition potential and time can be selected in this dialog box.
After deposition period and before quiescent time, the potential will be set back to
initial potential. The potential scan during stripping step will start from initial
potential.
Purge During Deposition
When this item is checked, the system will purge solution during deposition
period.
Stir During Deposition
When this item is checked, the system will stir solution during deposition period.
Deposition Potential
You can have a choice of using initial potential or some other potential as
deposition potential, by clicking one of the radio button. If you choose not to use
initial potential as deposition potential, you have to enter the Deposition E as
described below.
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Deposition E
Enter the deposition potential that is different from initial potential. This value
will have no effect if initial potential is chosen as deposition potential.
Deposition Time
Enter the deposition time. The parameter range is from 0 to 100000.
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Present Data Plot Command
Use this command to plot the currently active data.
Use this command to zoom out the plot.
You can rescale the X and Y axis by moving the mouse cursor to the axis and see
the cursor change to ↔ (X axis) or ¦ (Y axis). You can then hold down the left mouse
button and drag the mouse. When you release the mouse button, the axis will be rescaled.
It provides a convenient way to zoom out further than the default scale. It can be
particularly useful when plots are overlaid if some of the files have a higher range than the
default range.
If you double click the axis, an Axis Options dialog will be brought up:
You can change the axis settings. Please see also Graph Options, Color and Font
descriptions. The unique selections here are Axis Label Expression, Long Divisions and
Short Ticks. If you choose Scientific Expression, the axis label is in floating format. For
instance, one microampere will be expressed as 1e-6A. If you choose Engineering
Expression, one microampere will be expressed as 1 µA. However, if you use Oriental
Windows versions (such as Chinese, Japanese, Korean), the “micro” symbol will not
appear properly, you need to set Windows by using the System command under the Setup
menu. The “micro” symbol will then be expresses as “u”. The Long Divisions and Short
Ticks will allow you to customize the ticks. You should freeze the axis scale when you try
to use manual setting of ticks.
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You can also enter text into the data field by double clicking. An Insert Text dialog
box will be brought up:
You can enter the text you want to display in the “Text” field. You can erase the
text field by clicking the Erase button. You can change the X and Y position of the text.
The X and Y position is the position of the mouse button before you bring up the dialog
box by double-clicking. This will also be the position of the upper-left corner of the first
letter. You can rotate the letter to any angle between 0 and 360 degrees by 1-degree
increments. You can change the font of the inserted text. The font is a global setting. It
affects all inserted text displayed. If you uncheck Text Display Enabled, the text you enter
will remain, but will not be displayed.
You can alter the existing text, its position or rotation angle, or simply erase it. You
need to move the mouse close to the upper-left corner of the first letter of the text. Doubleclicking that location will select the existing text. You can change the setting. If you clear
the Text field, the existing text will be gone when you exit the dialog box.
The entered text will also be saved with the data when you save the data file.
Depending on the techniques, the data can be displayed in various formats:
Technique
CV
TAFEL
CA
CC
SWV
Data Display Formats
sweep segment
log current ~ potential
current ~ potential
current density ~ potential
i~t
i ~ t -1/2
Q~t
Q ~ t1/2
forward current
reverse current
forward and reverse current
difference of forward and reverse current
sum of forward and reverse current
forward, reverse, and summation current
forward, reverse, and difference current
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ACV
PSACV
BE
IMP
IMP-t or IMP-E
IMP-E
CP, PSA
absolute current
phase selective current
resistance
capacitance
absolute current
phase selective current
resistance
capacitance
charge ~ time
current ~ time
current ~ log (time)
Bode: log Z ~ log (freq)
Bode: phase ~ log (freq)
Bode: log Z” & Z’ ~ log (freq)
Bode: log Y ~ log (freq)
Nyquist: Z” ~ Z’
Admittance: Y” ~ Y’
Warburg: Z” & Z’ ~ w -1/2
Z’ ~ w Z”
Z’ ~ Z”/w
cot (phase) ~ w1/2
log Z ~ t or E
phase ~ t or E
Z ~ t or E
Z' ~ t or E
Z" ~ t or E
Z' & Z" ~ t or E
log (Z' & Z") ~ t or E
log Y ~ t or E
Y ~ t or E
Y' ~ t or E
Y" ~ t or E
Y' & Y" ~ t or E
log (Y' & Y") ~ t or E
Rs ~ E
Cs ~ E
Rp ~ E
Cp ~ E
1 / (Cs×Cs) ~ E
(Mott-Schottky)
1 / (Cp×Cp) ~ E
(Mott-Schottky)
potential ~ time
dE/dt ~ time
dt/dE ~ potential
Potential ~ charge
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To select the data display format, the Graph Option command should be invoked.
When the data is saved to the disk, the display format is also saved. When the data
is retrieved, it will be displayed just like before it is saved. This is also true for Overlay
Plots, Parallel Plots, and Print Multiple Files.
The Graph Option, Color and Legend, and Font commands allow you customize
your data plot.
This command is disabled if there is no currently active data.
This command has a toolbar button:
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Overlay Plots Command
Use this command to plot multiple sets of data in a single plot. This is particularly
useful for data comparison. The color and legend will be displayed together with the
corresponding filenames. You can select the data files you want to plot along with the
currently active data. Multiple files can be selected. To select multiple files, point the
mouse cursor to the filename you want to select and click the left mouse button one at a
time, while holding the Ctrl key.
This command will allow you select multiple files in the same directory. In order to
overlay data in the different directory or disks, use the Add Data to Overlay command.
This command presents an Overlay Data Display dialog box:
The plot will be scaled according to the currently active data. This command does
not check the type of data. If both X and Y values fall into the plot scale, the data point
will be plotted.
The Graph Option, Color and Legend, and Font commands allow you customize
your data plot. The color and legend of each traces can be specified by Color and Legend
command.
This command is disabled if there is no currently active data.
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Add Data to Overlay Command
This command is complementary to the Overlay Plots command. It allows you to
add more data to the overlay plots without reselecting all the files. It also allows you to
overlay data from different directories or from floppy disks. Multiple files can be selected.
To select multiple files, point the mouse cursor at the filename you want to select and click
the left mouse button one at a time, while holding the Ctrl key.
This command presents an Add Data to Overlay dialog box:
The plot will be scaled according to the currently active data. This command does
not check the type of data. If both X and Y values fall into the plot scale, the data point
will be plotted.
The Graph Option, Color and Legend, and Font commands allow you customize
your data plot. The color and legend of each trace can be specified by Color and Legend
command.
This command is disabled if there is no currently active data. This command is also
disabled unless the current plot is an overlay plots.
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Parallel Plots Command
Use this command to plot multiple sets of data in a parallel mode. This is
particularly useful to view data obtained with different techniques and for data
comparison. You can select the data files you want to plot along with the currently active
data. Multiple files can be selected. To select multiple files, point the mouse cursor to the
filename you want to select and click the left mouse button one at a time, while holding the
Ctrl key.
This command will allow you to select multiple files in the same directory. In order
to parallel plot data from a different directory or from a floppy disk, use the Add Data to
Parallel command.
This command presents a Parallel Data Display dialog box:
Each plot will be automatically scaled according to each data set read from the
disk, unless the scale is frozen. In the latter case, all the plots will have the same frozen
scale. To freeze the scale, use the Graph Option command.
The Graph Option, Color and Legend, and Font commands allow you customize
your data plot.
This command is disabled if there is no currently active data.
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Add Data to Parallel Command
This command is complementary to the Parallel Plots command. It allows you to
add more data to the parallel plots without reselecting all the files. It also allows you to
parallel plot data from different directories or floppy disks and control the sequence of the
data in the plot. Multiple files can be selected. To select multiple files, point the mouse
cursor to the filename you want to select and click the left mouse button one at a time,
while holding the Ctrl key.
This command presents an Add Data to Parallel Plot dialog box:
The plot will be scaled according to the currently active data. This command does
not check the type of data. If both X and Y values fall into the plot scale, the data point
will be plotted.
The Graph Option, Color and Legend, and Font commands allow you customize
your data plot.
This command is disabled if there is no currently active daya. This command is
also disabled unless the current plot is a parallel plots.
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Zoom In Command
Use this command to zoom in the data plot.
This is a toggle switch. A check mark appears next to the menu item when the
zoom in function is enabled. The Zoom In toolbar button will be pressed in. When you
move the mouse cursor in the data plot area, an upper arrow cursor appears.
To zoom in, press the mouse button at one corner, drag it to the diagonal corner of
the area you want to have a closer view at and release the mouse button.
To zoom out click the Zoom In command again. This also disables the zoom
function.
This command has a toolbar button:
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Manual Result Command
Use this command to report peaks or wave potentials, currents and area manually.
You can determine the baseline for a peak or wave visually.
This is a toggle switch. A check mark appears next to the menu item when the
manual result function is enabled. The Manual Result toolbar button will be pressed in.
When you move the mouse cursor in the data plot area, an upper arrow cursor appears.
In order to report a peak or wave correctly, you have to define the peak shape with
the Peak Definition command. The peak shape can be Gaussian, diffusive, or sygmoidal.
You can also determine if you want to report peak (or wave) potential, half peak (or wave)
potential, peak (or wave) currents or peak area.
For a Gaussian peak, the baseline is determined by two points at each sides of the
peak. Press the mouse button at one point, drag it and release it at the other point. A
vertical line that connects the peak and the baseline will appear. The numerical report is
shown at the right side of the plot.
For a diffusive peak, the baseline is determined by extending the foot before the
peak. To determine the baseline, press the mouse button at the foot, drag it and release it
after passing the peak potential. A vertical line that connects the peak and the baseline will
appear. The numerical report is shown at the right side of the plot. Notice that when peak
area is reported, it is the half peak area.
For a sygmoidal wave, two baselines are needed. One is at the foot of the wave and
the other is at the plateau of the wave. To determine the baselines, press the mouse button,
drag it and release it. A vertical line that connects two baselines and crosses the middle of
the wave will appear. The numerical report is shown at the right side of the plot.
The following is a typical result from manual peak search:
This command has a toolbar button:
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Peak Definition Command
Use this command to define the peak shape ( Gaussian, diffusive, or sygmoidal).
You can also determine if you want to report peak (or wave) potential, half peak (or wave)
potential, peak (or wave) currents or peak area.
The peak definition is used for both automatic and manual result reports.
This command presents a Peak Definition dialog box:
The following options allow you to define the peak shape and determine what
parameters need to be reported:
Peak Shape
You can select the peak shape according to the property of your data. The peak
shape can be Gaussian, diffusive or sygmoidal. The peak shape is assumed from the
electrochemical technique. Each time you change the technique, a default value is assigned
to the peak shape. However, you can change this setting.
Report Option
You can determine if you want to report peak (or wave) potential, half peak (or
wave) potential, peak (or wave) currents or peak area.
Peak or Wave Search Potential Range
Depending on the peak shape, the peak search potential range can be adjusted. For
a broader peak or wave, the search potential range should be larger, and vice versa. The
search potential range includes both sides of the peak or wave.
This parameter is only meaningful for automatic result report.
For cyclic voltammetry data, select the segment by the Graph Options command
under the Graphics menu.
This command has a toolbar button:
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XY Plot Command
Use this command to make an X-Y plot of your own data. You can also do linear
curve fitting to the data.
After you edit the data, click the OK button to do the plot. The X-Y plot is
temporary and it disappears if other data display commands are invoked. However you can
use Graph Option, Color and Legend and Font commands to customize your plot.
The command presents the X-Y Plot dialog box:
The following options allow you to edit data and enter plot options:
XY Data Array Editor
Enter your own X Y data points. Use comma or space as separator. Each pair of
data occupies one line:
x1, y1
x2, y2
x3, y3
......
Read
Use this command to read the data you saved.
Save
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Use this command to save your data. XY titles, units, header and note will be saved
along with the data.
Overlay Plot
Use this command to overlay several data plots. If you want to have both symbols
and lines to connect symbols, save you data with two different names and select proper
legends by using Color and Legend command. To freeze the scale, use the Graph Option
command.
The system displays the Overlay Data Display dialog box so you can select the data
files you want to plot along with the data in the XY Data Array Editor. Multiple files can
be selected.
The plot will be scaled according to the data in the XY Data Array Editor. If both X
and Y values fall into the plot scale, the data point will be plotted.
Parallel Plot
Use this command to plot multiple sets of data in a parallel mode.
The system displays the Parallel Data Display dialog box so you can select the data
files you want to plot along with the data in the XY Data Array Editor. Multiple files can
be selected.
Each plot will be automatically scaled according to each data set read from the
disk, unless the scale is frozen. In the latter case, all the plots will have the same frozen
scale. To freeze the scale, use the Graph Option command.
Plot
Use this command to plot the XY Data Array Editor.
The plot will be automatically scaled according to the data range. To freeze the
scale, use the Graph Option command.
XY Title
Enter the X and Y titles.
Unit
Enter the unit or dimension of the customized X and Y axis titles.
Header
This is the header text editor box. Enter your header here. To display the header on
top of the plot, check the Header box using the Graph Option command.
Note
This is the note text editor box. Enter your note here. The note is not displayed on
the plot, but will be saved in the data file. It allows you to put more comments about the
data and remind you later about the purpose and the conditions of the experiment.
Linear Curve Fitting
Checking this box will allow the data to be fit linearly by the least square method.
A best fit straight line will also appear on the plot.
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Peak Parameter Plot Command
Use this command to plot the peak current versus scan rate, peak current versus
square root of the scan rate, or peak potential versus the logarithm of the scan rate. For a
reversible surface reaction, the peak current is proportional to the scan rate. For a
reversible diffusive system, the peak current is proportional to the square root of the scan
rate. The peak potential should be independent to the scan rate for a reversible reaction. A
shift of peak potential as a function of scan rate indicates either slow kinetics or chemical
complexity.
You can also do linear curve fitting of the data.
This command works only for cyclic voltammetric or linear sweep voltammetric
data. For CV data, the system only searches for the currently active data segment.
After you set the potential window for peak and select the proper files, click the
OK button to display the plot. The X-Y plot is temporary and it disappears if other data
display commands are invoked. However you can use Graph Option, Color and Legend,
and Font commands to customize your plot.
The system displays the Peak Parameter vs. Scan Rate Plot dialog box:
The following options allow you to set the potential window for peak and select
data files:
Peak Potential Window
Enter the possible peak potential range. The system only searches for peaks in the
specified potential range. Once the first peak in this potential range is found, it will be used
for plotting.
Type of Plot
You can plot the peak current versus scan rate, peak current versus square root of
the scan rate or peak potential versus the logarithm of the scan rate.
Linear Curve Fitting
Checking this box will allow the data to be fit linearly by the least square method.
A best fit straight line will also appear on the plot.
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Select Files
In order to plot data, you have to select files. Only CV or LSV data will be read.
Data obtained with other techniques will be ignored. Select at least three data files
obtained at a different scan rate.
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Semilog Plot Command
Use this command to display a current-potential semilog plot. This plot is useful in
data analysis for steady state responses. One can also convert a diffusive or peak shaped
response by semi-integral or full integral to a sygmoidal curve and display a semilog plot.
For a reversible reaction, the intercept on the potential axis is the half wave potential and
the slope should be 0.059/n V. Any discrepancy from the expected slope indicates slow
kinetics or complexity of the electrode reaction.
You can also do linear curve fitting to the data.
After you set the options, click the OK button to display the plot. The X-Y plot is
temporary and disappears if other data display commands are invoked. However you can
use Graph Option, Color and Legend, and Font commands to customize your plot.
The system displays the Current-Potential Semilog Plot dialog box:
The following options allow you to set the plot parameters:
Potential Window
Enter the potential window for the data to be plotted. The potential window should
be around the half wave potential and within ±0.059/n V. Data points ouside the
specified potential window will be ignored.
Linear Curve Fitting
Checking this box will allow the data to be fit linearly by the least square method.
A best fit straight line will also appear on the plot.
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Special Plot Command
Use this command to display special plots if available.
For linear sweep voltammetry (LSV), the special plot is the Polarization Resistance
Plot. After this command is invoked, the program will check the potential at zero current.
If it is found, it will be used as E (V, I=0). Otherwise, a warning "Potential at zero current
not found" will be issued. A Polarization Resistance Plot dialog box will appear.
After entering the center potential and the potential range, click OK and a
polarization resistance plot will be constructed. Polarization resistance and correlation will
be reported.
The polarization resistance plot is temporary and disappears if other data display
commands are invoked. However you can use Graph Option, Color and Legend, and Font
commands to customize your plot.
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Graph Options Command
Use this command to select graphic plot options.
The graphic options allow you to selectively turn on or off the plot captions, XY
grid, and XY axis inversion. You can also freeze the XY axis, customize the XY axis titles
and write memos that can be saved together with the data.
Most of the parameters will be saved when you end the program and reloaded when
you restart the program.
This command presents a Graph Options dialog box:
The following options allow you to select graphic plot options:
Screen
You can selectively turn on or off header, axis, baseline, parameters and results on
the screen.
The header is the caption shown on top of the plot. The header text can be typed in
the Header text area.
The baseline is drawn to visually define a peak or wave.
The screen options are independent of printer options as described below.
Printer
You can selectively turn on or off header, axis, baseline, parameters and results on
the printer.
The printer options are independent of screen options as described above.
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Grid and Inv
You can selectively turn on or off XY grid and XY inversion.
XY inversion will allow you to change the X Y axis polarity. This is only for
temporary. If you want to invert the X Y axis polarity permanently, use the System
command in the Setup menu.
XY Freeze
You can freeze the XY axis by checking the item(s) and enter the freezing scale. X
and Y axis can be controlled independently.
When X Y axis freeze is not checked, the X Y scale will have the value that was
used in the present plot.
Sometimes the XY axis can not be frozen at the exact scale you entered in order to
have an integer number of ticks on the X Y axis.
XY Title
For each electrochemical technique, the system provides default X Y axis titles. If
you want to customize them, check the items and enter the title you want to appear.
Unit
You can enter the unit or dimension of customized XY axis titles.
XY scale
You can change the size of the plot by changing the XY scale. The default XY
scale is 1 that is full size.
This is particularly useful when you want to print the plot for publication, or when
you want to paste the plot into a word processor.
Data
You can choose the data set to be plotted. Depending on the technique, the
selection varies. See the Present Data Plot command description.
Cursor Lock to Data Points
The cursor could be either locked to data points or free of movement.
Current Density
If this item is checked, the current density will be displayed.
Electrode Area
The electrode area is used to calculate the current density.
E vs Reference Electrode
By default, the potential axis title is “Potential / V”. If this item is checked, the type
of reference electrode used in the experiment will be attached to the potential axis title.
For instance, the potential axis title might be “Potential / V vs SCE”. You can enter the
type of the reference electrode in the edit box after the “Ref Electrode:” prompt.
Header
This is the header text editor box. Enter your header here. To display the header on
top of the plot, check the Header box in the Screen and/or Printer options.
Note
This is the note text editor box. Enter your note here. The note is not displayed on
the screen, but will be shown as data information and saved in the data file. It allows
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you to put more comments about the experiment and remind you later about the
purpose and the conditions of the experiment.
This command has a toolbar button:
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Color and Legend Command
Use this command to edit graphic plot color and legends.
You can change the color of the background, the axis, the grid and thedata curve.
You can also change the legend of the data curve and the grid.
The color and legend will be saved when you exit the program and will be reloaded
when you restart the program.
To change the text color, please use the Font command.
This command presents a Color Selection dialog box:
The following options allow you to select the colors and the legends of the plot:
Curve #
Curve 0 represents the currently active data. Curves 1-9 are for Overlay Plots. The
overlapped curves use the color in the order defined here.
Color
You can select the color of the data curve, the grid, the axis and the background. To
change these colors, click the Change button. The system displays the Color dialog box
so you can select a color. For more information about the Color dialog box, refer to
your Windows User's Manual.
To change the color of the text, use the Font command.
Legend
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You can select the legend of the data curve and the grid. The legend can be line,
point, circle or any other pattern.
When a point is chosen for the curve or the grid legend, it may not be displayed by
certain printers or plotters. For instance, HP LaserJet IV will not draw a dot in the
HPGL mode, but it will draw a dot in the raster mode. Properly configuring your
printer may help.
Size
You can specify the size of the legend or the thickness of the line.
Interval
You can change the data density for the plot. The original data density is 1. Larger
interval lowers your data point density. This is useful when you use Overlay Plots and
different legends.
Default
Pressing this button will reset all the colors and legends to the system default.
This command has a toolbar button:
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Font Command
Use this command to select the font of the text used in the plot. You can define the
font, the style, the size and the color.
You can also rotate the Y axis title for printing.
The font will be saved when you exit the program and will be reloaded when you
restart the program.
This command presents a Font Selection dialog box:
To change the font, style, size or color of the text, press the Change button of the
corresponding item.
The Y axis title should go from bottom to top. However, different printers define
the character rotation angles differently. For instance, HP LaserJet IV defines the desired
rotation as 90 degrees, but IBM Lexmark 4039 12R defines it as 270 degrees. If you find
that the Y axis title goes from top to bottom, change the selection until the desired result is
attained.
The system displays the Font dialog box so you can select the font. For more
information about Font dialog box, refer to your Windows User's Manual.
Pressing the Default button will reset all fonts to the system default.
This command has a toolbar button:
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Copy to Clipboard Command
Use this command to copy the plot to clipboard. You can then paste it into a word
processor or any other windows based prgram.
This command will work during a run or a digital simulation.
This command has a toolbar button:
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Smoothing Command
Use this command to smooth the currently active data.
This command presents a Smoothing dialog box:
To perform the smoothing, click the OK button.
The following options allow you to select the mode and parameter for smoothing:
Method Selection
Select the smoothing method: least square or Fourier transform smoothing.
Least Square Point
The Savitzky and Golay algorithm is used in this technique. An odd number of
points from 5 to 49 should be used for smoothing. The more points, the better the
smoothing effect will be, but it may cause larger distortion.
For more detail about Savitzky and Golay algorithm, please see "Smoothing and
Differentiation of Data by Simplified Least Squares Procedures", Anal. Chem., 36,
1627-1639 (1964).
FT Cutoff (1/s or 1/V)
Specify the filter cutoff frequency. For a time based experiment including CA,
CC, TB..., 1/s or Hz is the unit. For voltammetry, the unit is 1/V. Its physical meaning
is how many signal cycles are allowed in one volt of potential range. The lower the
cutoff, the better the smoothing effect will be, but it may also cause more distortion.
Fourier transform smoothing is done by a procedure proposed by D.E. Smith et al.
For more detail about the algorithm, please see "Some Observations on Digital
Smoothing of Electroanalytical Data Based on the Fourier Transformation", Anal.
Chem., 45, 277-284 (1973).
In general, Fourier transform smoothing is very effective. The distortion may be
minimal, if the signal band is well separated from the noise band. On the other hand,
this method is relatively more time-consuming.
Smooth After Run
When this box is checked, automatic smoothing after run is enabled. Certain
techniques, such as TAFEL, BE and IMP, do not allow smoothing. This option can
also be turned on or off from the Run Status command under the Control menu.
Override Present Data
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When this box is checked, the currently active data will be replaced by smoothed
data. Otherwise, the smoothed data will be displayed, but will not override the
currently active data. In this case, when the Present Data Plot command under the
Graphics menu is invoked, the original data reappears.
This command has a toolbar button:
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Derivatives Command
Use this command to calculate the derivative of the currently active data.
After performing a first order derivative, the Y axis has a unit of Y unit / X unit.
For voltammetry, it is A/V. For an i-t curve, it is A/s. The new unit is not explicitly
expressed, but you should be aware of it.
This command presents a Derivative dialog box:
To calculate the derivative, click the OK button.
The following options allow you to select the order and parameter for derivative:
Order Selection
Select the derivative order: first, second, third, fourth, or fifth order.
Least Square Point
The Savitzky and Golay algorithm is used to calculate the derivative. An odd
number of points from 5 to 49 should be used. Since the derivative tends to amplify
high frequency noise, a relatively large number of points should be considered. The
more the points, the less noisy the derivative data will appear, but it may cause larger
distortion.
For more detail about the Savitzky and Golay algorithm, please see "Smoothing
and Differentiation of Data by Simplified Least Squares Procedures", Anal. Chem.,
36, 1627-1639 (1964).
Override Present Data
When this box is checked, the currently active data will be replaced by the
derivative data. Otherwise, the derivative data will be displayed, but will not override
the currently active data. In this case, when the Present Data Plot command under the
Graphics menu is invoked, the original data reappears.
This command has a toolbar button:
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Integration Command
Use this command to integrate the currently active data.
After performing integration, the Y axis has a unit of Y unit × X unit. For
voltammetry, it is AV. For an i-t curve, it is As (coulomb). The new unit is not explicitly
expressed, but you should be aware of it.
This command presents an Integration dialog box:
To perform integration, click the OK button.
The following options allow you to select the parameters for integration:
Override Present Data
When this box is checked, the currently active data will be replaced by the
integrated data. Otherwise, the integrated data will be displayed, but will not override
the currently active data. In this case, when the Present Data Plot command under the
Graphics menu is invoked, the original data reappears.
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Semiinteg and Semideriv Command
Use this command to perform semi-integral or semi-derivative treatments to the
currently active data.
Semi-derivative and semi-integral are useful. You can convert a diffusive peak to
a Gaussian peak by using semi-derivative. This gives a better resolution and makes
measurements easier. You can also convert a diffusive peak to a sygmoidal wave. This
gives a time-independent steady state current plateau. In polarographic theory, the
current-potential semilog analysis can be used to interpret the data.
This command presents a Convolution dialog box:
To perform semi-integral or semi-derivative treatments, click the OK button.
The following options allow you to select the order and parameters for
convolution:
Order Selection
Select either semi-integral or semi-derivative.
Override Present Data
When this box is checked, the currently active data will be replaced by the
convoluted data. Otherwise, the convoluted data will be displayed, but will not
override the currently active data. In this case, when the Present Data Plot command
under the Graphics menu is invoked, the original data reappears.
This command has a toolbar button:
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Interpolation Command
Use this command to insert more data points to the currently active data.
This command presents an Interpolation dialog box:
To perform interpolation, click the OK button.
The following options allow you to select the parameters for interpolation:
Data Insertion Density
The larger the number, the higher the final data density will be. When the number
of data points exceeds the allowed memory size, a warning will be given and the
command is terminated. The data insertion density can only be a power of 2. Fourier
transform is used in this case.
Override Present Data
When this box is checked, the currently active data will be replaced by the
interpolated data. Otherwise, the interpolated data will be displayed, but will not
override the currently active data. In this case, when the Present Data Plot command
under the Graphics menu is invoked, the original data reappears.
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Baseline Fitting & Subtraction Command
Use this command to fit the baseline and subtract the fitting curve from the
currently active data. This is very useful for peak evaluation.
In order to perform Baseline Fitting and Subtraction, you need to specify the
potential on the two sides of the peak base. You also need to specify the algorithm and
orders of fitting.
Baseline Fitting and Subtraction only works for certain peaks, it does not work for
all the techniques.
This command presents a Baseline Fitting & Subtraction dialog box:
If there is more than one segment of data available, such as CV data, you can
choose the set of data to operate on by using the Graph Option command under the
Graphics menu.
The following options allow you to select the fitting parameters and the way of
the data will be saved:
Two sides of Peak Foot
When fitting the baseline, the data points corresponding to peaks should be
ignored. You need to provide the two sides of the peak foot. If the baseline fitting is
not ideal, you may need to adjust the peak foot values or the polynomial orders.
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If there are several peaks, you may need to enter several sets of peak feet. You
can also specify the whole potential or time range that you do not want to use for the
baseline fitting.
A maximum 5 sets of peak feet can be entered.
Baseline Fitting Algorithm and Orders
You also need to specify the algorithm and orders of fitting. There are two fitting
algorithms used: Orthogonal Least Square or Least Square. Both are based on
polynomial fittings. The order of polynomials is related to the shape of the baseline.
First order stands for linear fitting, aX+b. Second order stands for aX2+bX+c fitting
and so on. You need to adjust the fitting algorithm and polynomial orders for best
fitting results. You may also need to adjust the potential of the peak foot.
Save to Override Original Data
When the OK button is clicked, if “No Action” is selected, the graphical screen
will show the original data and the fitted baseline. The original data remains
unchanged. If “Difference” is selected, the original data will be replaced by the
difference data. The difference data is obtained by subtracting the baseline data from
the original data. If “Baseline” is selected, the fitted baseline data will be saved.
View Baseline
This button will allow the user to view the original data and the fitted baseline
together to evaluate the fitting results. This is important because you need to be sure
that the fitting is ideal and correct. If the peak defining lines affect your vision, you
can turn off the “Screen Baseline” option by using the Graph Options command
under the Graphics menu.
The original data remains unchanged. When the Present Data Plot command
under Graphics menu is invoked, the original data reappears.
View Difference
This button will allow the user to view the difference data by subtracting the fitted
baseline from the original data. This is helpful when evaluating the fitting results.
The original data remains unchanged. When the Present Data Plot command
under the Graphics menu is invoked, the original data reappears.
This command has a toolbar button:
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Linear Baseline Correction Command
Use this command to visually correct the baseline of the currently active data.
You can compensate a sloping baseline and shift the DC level of the curve.
The linear baseline correction command will be activated only once. In order to
compensate or shift the baseline more than once, invoke this command repeatedly.
This command presents a Baseline Correction dialog box:
To perform baseline correction, click the OK button first. The mouse cursor now
changes to an upper arrow cursor.
To compensate a sloping baseline, press the mouse button at the starting point,
drag the mouse and extend to the point that forms the baseline. When the mouse
button is released, this line is subtracted from your data. The range of compensation
in X coordinate is the range at which the line is drawn.
To shift the DC level, use the mouse to draw a horizontal line. This line will be
the new zero of the curve. The DC level shift applies to the whole curve. You don't
have to draw a line to cover the entire X range.
If there is more than one segment of data available, such as CV data, you can
choose the set of data to operate on by using the Graph Option command under the
Graphics menu.
The baseline correction command will be activated only once. In order to
compensate or shift the baseline more than once, invoke this command repeatedly.
The following option allows you to determine if the currently active data will be
replaced by the baseline corrected data:
Override Present Data
When this box is checked, the currently active data will be replaced by the
baseline corrected data. Otherwise, the baseline corrected data will be displayed, but
will not override the currently active data. In this case, when the Present Data Plot
command under the Graphics menu is invoked, the original data reappears.
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Data Point Removing Command
Use this command to remove unwanted data points from the currently active data.
You can only remove data points from the beginning or at the end.
This command presents a Data Point Removing dialog box:
To remove unwanted data points, click the OK button.
The following options allow you to select the parameters for data point removing:
Remove Beginning Data Points
In order to remove the points at the beginning of the data, check this box. You
should also enter the number of data points to be removed in the edit box. If the check
box is unchecked or if the number of data points to be removed is zero, no action will
be taken.
Remove Ending Data Points
In order to remove the points at the end of the data, check this box. You should
also enter the number of data points to be removed in the edit box. If the check box is
unchecked or if the number of data points to be removed is zero, no action will be
taken.
Override Present Data
When this box is checked, the currently active data will be replaced by the new
data after data points removal. Otherwise, the new data will be displayed, but will not
override the currently active data. In this case, when the Present Data Plot command
under the Graphics menu is invoked, the original data reappears.
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Data Point Modifying Command
Use this command to visually modify the data points of the currently active data.
You can correct data points due to bad mercury drop or any other reason.
This command presents a Data Point Modifying dialog box:
To modify data points, click the OK button first. The mouse cursor now changes
to an upper arrow cursor.
When you move the mouse cursor in the data display region, a hair-cross cursor
will appear at the data point corresponding to the X axis position of the mouse cursor.
Move the mouse horizontally to select the data point you want to modify. When the
hair-cross cursor appears at the selected point, press the mouse button. Drag the
mouse up or down in the direction you want to move the data point. The hair-cross
cursor will move up or down correspondingly. When the hair-cross cursor is located
at the position where you want the modified data point to be, release the mouse
button. The old point will be erased and a new point will appear at the new position.
The following option allows you to select the data set you want to modify and to
determine if the currently active data will be replaced by the modified data:
Data Set (Segment)
Choose the data set you want to modify. This selection depends on the
electrochemical technique used.
Override Present Data
When this box is checked, the currently active data will be replaced by the
modified data. Otherwise, the modified data will be displayed, but will not override
the currently active data. In this case, when the Present Data Plot command under the
Graphics menu is invoked, the original data reappears.
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Bkgnd Subtraction Command
This command allows you to calculate the difference between two data sets. First
you have to measure the blank solution, save the data file. Then run the sample. You can
now use this command to do a background subtraction.
In order to do a background subtraction, the background data should be the same
type of experiment and the same X data array. Otherwise an error message will be issued,
and the command will be terminated.
This command presents a Background Subtraction dialog box so you can select
the background data file that will be subtracted from the currently active data.
The following options allow you to specify the file to select:
File Name
Type or select the filename. You don't have to type the extension. The system
will automatically attach an extension to the filename.
List Files of Type
Select the type of file. Only “.bin” (binary data file) is available.
Drives
Select the drive in which the system stores the file.
Directories
Select the directory in which the system stores the file.
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Signal Averaging Command
Use this command to perform signal averaging to the currently active data and the
disk data file(s). The currently active data will always participate. Several sets of data are
added together, and then divided by the number of data sets. If any set of data has
different X array from the currently active data, an error message will be issued and this
set of data will be ignored.
This command presents a Signal Averaging dialog box so you can select the data
file(s) for signal averaging.
The following options allow you to specify the file to select:
File Name
Type or select the filename. You don't have to type the extension. The system
will automatically attach an extension to the filename. To select multiple files, point
the mouse cursor to the filename you want to select and click the left mouse button
one at a time, while holding the Ctrl key.
List Files of Type
Select the type of file. Only “.bin” (binary data file) is available.
Drives
Select the drive in which the system stores the file.
Directories
Select the directory in which the system stores the file.
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Mathematical Operation Command
Use this command to perform mathematical operations to the currently active
data. You can work on both X and Y arrays. The allowed operations include addition,
subtraction, multiplication, division, exponential, logarithm, square, square root, and
reciprocal.
This command presents a Math Operation dialog box:
To perform mathematical operations, click the OK button.
The following options allow you to choose the type of operation and the
destination of the data array:
Operation Selection
Select the operation you want to apply to the data. If addition, subtraction,
multiplication or division is chosen, you have to provide the operand.
Data Selection
You can choose either the X data array or the Y data array for operation.
Override Present Data
When this box is checked, the currently active data will be replaced by the
mathematically operated data. Otherwise, the mathematically operated data will be
displayed, but will not override the currently active data. In this case, when the
Present Data Plot command under the Graphics menu is invoked, the original data
reappears.
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Fourier Spectrum Command
Use this command to obtain the Fourier spectrum of the currently active data.
This command presents a Fourier Spectrum dialog box:
To calculate a Fourier spectrum, click the OK button.
The following options allow you to select the parameters to calculate a Fourier
spectrum:
X Scale
The X data array of the Fourier spectrum can just be the nth component, a 1/s
scale or a 1/V scale. An nth component scale is generally used. It is available for all
techniques. Its physical meaning comes from experimental parameters. The 1/s and
1/V scales have a clear physical meaning. For time-based experiments, the 1/s scale
should be used, and the 1/V is invalid; for voltammetric experiments, the 1/V should
be used since the 1/s scale may not be valid. Cyclic Voltammetry and Linear Sweep
Voltammetry are special, both 1/s and 1/V scales can be used.
Y Scale
The Y data array is the Fourier coefficients. You can choose either the linear scale
or the logarithmic scale.
Override Present Data
When this box is checked, the currently active data will be replaced by the
Fourier spectrum data. Otherwise, the Fourier spectrum will be displayed, but will not
override the currently active data. In this case, when the Present Data Plot command
under the Graphics menu is invoked, the original data reappears.
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Calibration Curve Command
Use this command to make a calibration curve.
The system displays the Calibration Curve dialog box:
The following options allow you to enter the data for calibration curve calculation
or plotting:
Standard #
Enter the concentration and peak height/current obtained from standard solutions.
Unknown
Enter the unknown peak height if available for unknown concentration
calculation.
X Axis Title
Enter the X axis title (such as Concentration) to be plotted.
X Axis Unit
Enter the X Axis unit or dimension (such as ppm, or M) to be plotted.
Y Axis Title
Enter the Y axis title (such as Peak Current) to be plotted.
Y Axis Unit
Enter the signal unit or dimension (such as A) to be plotted.
Header
This is the header text editor box. Enter your header here. To display the header
on the top of the plot, check the Header box using the Graph Option command.
Note
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This is the note text editor box. Enter your note here. The note can not be
displayed on the plot, but will be saved in the data file. It allows you to put more
comments about the data and remind you later about the purpose and the conditions
of this experiment.
Read
Use this command to read the data you saved.
Save
Use this command to save your data. XY titles, units, header and note will be
saved along with the data.
Calculate
Use this command to calculate the slope, intercept and correlation of the
calibration curve. If the unknown peak height is give, the unknown concentration will
also be calculated.
Plot
Use this command to plot the calibration curve.
The plot will be automatically scaled according the data range. To freeze the
scale, please use the Graph Option command.
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Standard Addition Command
Use this command to calculate the unknown concentration by standard addition.
The system displays the Standard Addition dialog box:
In standard addition, the unknown is measured first and the peak height is
recorded. Then the standard solutions are added. After each addition, the peak height
is measured again. Usually, the added volume is much smaller than the total volume
in order to maintain the sample compositions and have the same matrix effect. The
increment concentration should be comparable to the unknown.
The following options allow you to enter the data for unknown concentration
calculation or plotting:
Unknown
Enter the unknown peak height for unknown concentration calculation.
Addition #
Enter the concentration and peak height/current after adding the standard solution.
X Axis Title
Enter the X axis title (such as Concentration) to be plotted.
X Axis Unit
Enter the X Axis unit or dimension (such as ppm, or M) to be plotted.
Y Axis Title
Enter the Y axis title (such as Peak Current) to be plotted.
Y Axis Unit
Enter the Y Axis unit or dimension (such as A) to be plotted.
Header
This is the header text editor box. Enter your header here. To display the header
on the top of the plot, check the Header box using the Graph Option command.
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Note
This is the note text editor box. Enter your note here. The note is not displayed on
the screen, but will be saved in the data file. It allows you to put more comments
about the data and remind you later about the purpose and the conditions of the
experiment.
Read
Use this command to read the data you saved.
Save
Use this command to save your data. XY titles, units, header and note will be
saved along with the data.
Calculate
Use this command to calculate the slope, correlation of the standard addition
curve. The unknown concentration will also be calculated.
Plot
Use this command to plot the standard addition curve.
The plot will be automatically scaled according to the data range. To freeze the
scale, please use the Graph Option command.
8-4
Chapter 8. Analysis Menu
_____________________________________________________________________________________
Data File Report Command
Use this command to generate a report for stored data files.
The system presents the Data File Report dialog box:
The following options allow you to enter the peak potential windows, slope and
intercept of calibration curves, and select the data files for report:
Compound
Enter the names of the determined compounds. A maximum of four compounds
can be searched and reported.
Ep From and Ep To
Enter the peak potential range. Ep From and Ep To cannot be equal. When the
program searches for peaks, the first peak in the specified range will be selected. For
a different compound, different values should be entered.
Slope
Enter the slope of the calibration curve for the compound. It will be used to
calculate the concentration of the compound. Each compound has its own slope. If
Conc. report is selected and the slope is zero, a warning will be given.
Intercept
Enter the intercept of the calibration curve for theat compound. It will be used to
calculate the concentration of the compound. Each compound has its own intercept.
Peak Shape
You can select the peak shape according to the property of your data. The peak
shape can be Gaussian, diffusive or sygmoidal.
8-5
Chapter 8. Analysis Menu
_____________________________________________________________________________________
Data Type
You can select original data, semi-derivative or first derivative to report the
concentration.
Number of Species
Enter the number of species for the data file report.
Concentration Unit
Enter the concentration unit or dimension (such as ppm or M).
Report Filename
Enter the report filename if you want to save the report text file. If the name
already exists, an override warning will be issued. If no filename is specified, the
report will be shown but not saved.
Report Data Type
You can report concentration or peak current.
Header
This is the header text editor box. Enter your header here. To display the header
on top of the plot, check the Header box using the Graph Option command.
Note
This is the note text editor box. Enter your note here. The note will be saved in
the data file. It allows you to put more comments about the data and remind you later
about the purpose and the conditions of the experiment.
Read
Use this command to read the data you saved.
Save
Use this command to save your data. XY titles, units, header and note will be
saved along with the data.
Report
Use this command to generate the data file report.
8-6
Chapter 8. Analysis Menu
_____________________________________________________________________________________
Time Dependence Command
Use this command to generate a report or plot for time dependence of peaks or
concentrations from stored data files.
This command reads data from stored files and searches for peaks. The peak
height or concentration will be used for the time dependence report. All the valid data
files, i.e., containing the peak specified are sorted according to the experiment run time.
The first one is assigned to the start time. The time of the other experiments are obtained
by subtracting the start time.
The system displays the Time Dependence dialog box:
The following options allow you to enter the peak potential windows, slope and
intercept of calibration curves, and select the data files for time dependence report or
plot:
Ep From and Ep To
Enter the peak potential range. Ep From and Ep To cannot be equal. When the
program searches for peaks, the first peak in the specified range will be selected.
Slope
Enter the slope of the calibration curve for that compound. It will be used to
calculate the concentration of the compound. Each compound has its own slope. If
Conc. report is selected and the slope is zero, a warning will be given.
Intercept
Enter the intercept of the calibration curve for that compound. It will be used to
calculate the concentration of the compound. Each compound has its own intercept.
Peak Shape
You can select the peak shape according to the property of your data. The peak
shape can be Gaussian, diffusive or sygmoidal.
Data Type
8-7
Chapter 8. Analysis Menu
_____________________________________________________________________________________
You can select original data, semi-derivative or first derivative to report the
concentration.
Y Axis Title
Enter the Y axis title (such as Concentration or Peak Current) to be plotted.
Conc. Unit
Enter the concentration unit or dimension (such as ppm or M).
Report Name
Enter the report filename if you want to save the time dependence report text file.
If the name already exists, an override warning will be issued. If no filename is
specified, the report will be shown but not saved.
Report Data Type
You can report concentration or peak current.
Header
This is the header text editor box. Enter your header here. To display the header
on top of the plot, check the Header box using the Graph Option command.
Note
This is the note text editor box. Enter your note here. The note will be saved in
the data file. It allows you to put more comments about the data and remind you later
about the purpose and the conditions of the experiment.
Read
Use this command to read the data you saved.
Save
Use this command to save your data. XY titles, units, header and note will be
saved along with the data.
Report
Use this command to generate the time dependence report.
Plot
Use this command to generate the time dependence plot.
8-8
Chapter 8. Analysis Menu
_____________________________________________________________________________________
Special Analysis Command
Currently this command is only active for TAFEL measurements. You can use
this command to calculate the corrosion rate from the Tafel experiment results. If you
have the TAFEL data available, invoking this command will display the Corrosion rate
Calculation dialog box:
The following options allow you to enter the parameters that will be used to
calculate the corrosion rate:
Data Segment
If you have more than one segment of data, you need to specify which segment of
data you want to use to calculate the corrosion rate.
Equilibrium E
The program will search for the potential value where the current is closest to
zero or a minimum value and assign that corresponding potential as the equilibrium
potential. You can change the default value reported by the program.
Cathodic Tafel Slope Potential Range
By default, the cathodic Tafel slope potential range starts at 60 mV more negative
than the equilibrium potential and has a range of 100 mV. You can change this
potential range.
Anodic Tafel Slope Potential Range
By default, the anodic Tafel slope potential range starts at 60 mV more positive
than the equilibrium potential and extend the range for 100 mV. You can change this
potential range.
Calculate
8-9
Chapter 8. Analysis Menu
_____________________________________________________________________________________
Once you think the data segment, equilibrium potential, anodic and cathodic
potential ranges are properly set, you can click this button to calculate the cathodic
and anodic Tafel slope, the linear polarization resistance (in ohms) and the corrosion
current (in amperes).
8-10
Chapter 9. Simulation Menu
_____________________________________________________________________________________
Mechanism Command
A digital cyclic voltammetry (CV) simulator and digital impedance (IMP)
simulator software is integrated as well as a fitting program for impedance data.
The following pages (9-1 to 9-10) relate to the CV simulator only. For
instructions for the impedance simulator and the fitting program, please refer to a later
portion of this chapter (pages 9-11).
Mechanism Command for CV simulator
Use this command to set the reaction mechanism, the concentration of each
involved species, the kinetic and experimental parameters and some other variables
before your perform a simulation. You can store all the parameters needed for simulation
into a disk and read from it. You can also check the equilibrium concentration.
This command presents a Digital Simulation dialog box:
The following options allow you to set the reaction mechanism, the concentration
of each involved species, the kinetic parameters, the experimental parameters and
some other variables. You can store all the parameters needed for simulation on a
disk or read them from a disk. You can also check the equilibrium concentration.
9-1
Chapter 9. Simulation Menu
_____________________________________________________________________________________
Mechanism Edit
This edit box allows you to edit the reaction mechanism. You may check the
Mechanism Select box to see if the mechanisms you want to study are predefined. If
so, click the mechanism in the Mechanism Select box, the mechanism will appear in
this edit box. Only certain high end models will work with edited reaction mechanism
even if the user-specified mechanism is identical to the predefined one. Whenever
you try to type into this edit box, the Mechanism Select box changes the selection to
"User Input".
For user input, use only one letter (A-Z) to represent each chemical species. The
letter "e" is dedicated to electron transfer process. Upper case and low case letters are
interchangeable. Spaces will be ignored. The software can simulate any reasonable
combination of electron transfer, 1st and 2nd order chemical reactions. A maximum
of 11 steps and 9 chemical species will be accepted. The following are legal format:
A+e=B
(reduction)
A-e=B
(oxidation)
A=B
(chemical reaction)
A=B+C
(chemical reaction)
A+B=C
(chemical reaction)
A+B=C+D
(chemical reaction)
If you don't follow the convention, an error message will appear before you take
any other action.
Mechanism Select
There are 10 predefined reaction mechanisms. These are the most common
reaction mechanisms. The first item is "User Input". Only certain high end models
will accept user defined mechanisms.
You can obtain other mechanisms from the predefined mechanisms. For instance,
the EEC, ECC and CEC mechanisms can be obtained from an ECEC mechanism by
defining some of the kinetic parameters as zero. If you set the heterogeneous electron
transfer rate ko to zero, the corresponding electron transfer step will have no effect.
Similarly if you define the forward and reverse rate constants of a chemical reaction
to zero, the corresponding chemical reaction will be ignored.
When you click the predefined reaction mechanism, the mechanism will appear in
the Mechanism Edit box. If "User Input" is clicked, the Mechanism Edit box will be
emptied.
System under Study
The software will simulate either diffusive or adsorptive system. The diffusive
system assumes planar diffusion. The adsorptive system assumes that the adsorption
obeys the Langmuir isotherm and that both oxidized and reduced forms are strongly
adsorbed.
Dimensionless Current
9-2
Chapter 9. Simulation Menu
_____________________________________________________________________________________
Checking this box will allow the system to calculate the dimensionless current.
This might be useful when comparing a particular simulation to other theoretical
results. When this box is unchecked, the current will be calculated according to the
concentration, electrode area and time scale of the experiment.
Initial Concentration at the Equilibrium
Checking this box will make the system calculate and use the concentration at the
equilibrium when starting a simulation. The equilibrium state is calculated according
to the kinetic parameters and input concentrations. If this box is unchecked, the
simulation will use the input concentration as an initial condition.
Display Concentration Profile during Run
Checking this box will make the system to display the concentration profile along
with the voltammogram during the simulation. This is very helpful to understand the
reaction mechanism and very instructive when teaching to students.
In voltammograms, the current display scale is determined by the sensitivity scale
that is selected in the Parameters command. If the current axis scale is too high, the
voltammogram may appear as a flat line. If the current axis scale is too low, the data
point will be too scattered. However, the post-run data display will always autoscale
the voltammogram and makes it readable. You may want to change the sensitivity
scale for next run according to the post-run display.
In concentration profiles, relative concentrations and relative distances are used.
The total concentration of all the involved species is set to unity. The concentrations
of each species during simulation are referred to this value. The unity distance is set
to 6*sqrt(Dt), where D is the diffusion coefficient and t the total time involved in the
given experiment. To change the scales for concentration and distance, see the two
items below.
Conc. Range
Enter the concentration scale for the concentration profile display. The range is
0.001 to 100000. The default is 1.
Dist. Range
Enter the distance scale for the concentration profile display. The range is 0.001
to 10. The default is 1.
Time Delay Loop
The speed of digital simulation depends on the problem you want to study and the
type of computer used. If the simulation is performed at a fast speed, you may not be
able to see the progress or the change in concentration profiles clearly. You can insert
time delay loops between the computation of two points to slow down the system.
The range of this parameter is 0 to 1e6. The optimal delay loop duration depends on
the problem you want to study and the speed of the computer used.
Read Command
You can read proviously saved *.sim files. These files contain all the parameters
needed for a simulation.
An Open dialog box will be displayed, so you can select your file.
Save Command
9-3
Chapter 9. Simulation Menu
_____________________________________________________________________________________
You can save all the parameters needed for a simulation to the disk by invoking
this command. The file will have a *.sim extension.
The Save As dialog box will be displayed, so you can name your file.
Exp. Param Command
Press this button to set the experimental parameters of the simulation.
You can also change the experimental parameters through the Parameter
command under the Setup menu.
The Cyclic Voltammetry Parameters dialog box will be displayed, so you can
select the parameters you want to use.
Kinetics Command
This command allows you to enter the electron transfer kinetic parameters, such
as standard heterogeneous rate constant, standard redox potential or charge transfer
coefficient. It also allows you to enter the forward and backward rate constant of
chemical reactions.
The Potentials and Rate Constants dialog box will be displayed, so you can enter
the kinetic parameters.
Conc Command
This command allows you to enter the concentrations and diffusion coefficients of
each chemical species involved.
The Concentration and Diffusion Coefficients dialog box for a diffusive system,
or the Surface Concentration dialog box for an adsorptive system will be displayed,
so you can specify the concentration and diffusion coefficients.
Equilibrium Command
This command allows you to view the concentration of each chemical species
involved under the given kinetic conditions.
The Concentration at Equilibrium dialog box will be displayed, so you can view
the equilibrium state.
Variables Command
This command allows you to enter certain variables such as temperature and
electrode area.
The Simulation Variables dialog box will be displayed, so you can enter the
variables.
9-4
Chapter 9. Simulation Menu
_____________________________________________________________________________________
Potentials and Rate Constants dialog box
This dialog box allows you to enter the kinetic parameters.
On the left side of the panel, the reaction mechanism is listed. This will remind
you of each step. On the right side of the panel, either 2 or 3 parameter boxes are shown
depending on the type of reaction considered. Enter the proper value into the edit box.
If the reaction involves an electron transfer, enter the heterogeneous rate constant
ko, the standard redox potential Eo and the charge transfer coefficient alpha.
If a chemical reaction is involved, enter the forward and backward rate constants
for this reaction.
Sometimes you may notice that some of the kinetic parameters are
"predetermined". This because the concentrations of n species can be determined by n-1
reactions plus the initial conditions. It often occurs that there are more equations than the
number of species. Therefore some of the equations must be linearly correlated. The
equilibrium constants of some reactions are overdetermined and should not be assigned
arbitrarily, otherwise the system will never be able to reach an equilibrium. The software
will look for such dependences and properly assign the kinetic parameters. Put the
reactions whose kinetic parameters you know best on the top and. those you know less
accurately at the bottom and let the software determine the proper kinetic parameters. If
the overdetermined equilibrium constant involves a chemical reaction, the backward rate
constant will be determined by the system. The forward constant must still be entered. If
an electron transfer process is involved, the standard redox potential will be determined
by the system. The heterogeneous rate constant and the alpha coefficient must still be
entered.
9-5
Chapter 9. Simulation Menu
_____________________________________________________________________________________
Concentration and Diffusion Coefficients dialog box
This dialog box allows you to enter the concentrations and diffusion coefficients.
On the left side of the panel, the reaction mechanism is listed. This will remind
you of each step. The species involved in the reaction are also listed. On the right side of
the panel, you can enter the concentrations and diffusion coefficient corresponding to
each species.
9-6
Chapter 9. Simulation Menu
_____________________________________________________________________________________
Surface Concentration dialog box
This dialog box allows you to enter the surface concentrations.
On the left side of the panel, the reaction mechanism is listed. This will remind
you of each step. The species involved in the reaction are also listed. On the right side of
the panel, you can enter the surface concentrations corresponding to each species.
9-7
Chapter 9. Simulation Menu
_____________________________________________________________________________________
Concentration at Equilibrium dialog box
This dialog box allows you to view the concentrations at the equilibrium.
On the left side of the panel, the reaction mechanism is listed. This will remind
you of each step. The species involved in the reaction are also listed. On the right side of
the panel, the concentrations at equilibrium corresponding to each species are listed.
9-8
Chapter 9. Simulation Menu
_____________________________________________________________________________________
Simulation Variables dialog box
This dialog box allows you to change some simulation variables:
Temperature
Enter the temperature in Celsius here. Both thermodynamic and kinetic
parameters are a function of temperature.
Electrode Area
Enter the area of the electrode in square centimeters here. The current is
proportional to the electrode area in planar diffusion situations or for surface reactions.
Capacitance
Enter the electrode double layer capacitance in microfarads here. Charging
currents will be added to the total current reported during the simulation.
9-9
Chapter 9. Simulation Menu
_____________________________________________________________________________________
Simulate Command
Use this command to perform the digital simulation.
Set the mechanism, the concentrations, the kinetic parameters and the
experimental parameters before you click this command.
In order to perform a simulation, connect the instrument to the computer and turn
it on. The hardware only needs be tested once after you start the program.
You can copy the screen graphics to the clipboard during the simulation.
The user input mechanism will work only for high-end instrument models.
9-10
Chapter 9. Simulation Menu
_____________________________________________________________________________________
AC Impedance Simulator and Fitting Program
An impedance simulator is integrated into the software. To use the impedance
simulator, you need to set the Technique to AC Impedance (IMP) and then use the
Mechanism command to enter the equivalent circuitry. Once the Mechanism command is
invoked, the original toolbar will be replaced by a new one. The new toolbar contains
symbols of components and commands. The following screenshot shows the toolbar and
the mechanism edit field:
Here is the explanation of the toolbar buttons:
Undo
Redo
Rearrange the components
Move components left, right, up and down
Clear all the components in the edit field
Cut a component or connection
Add a resistor in Ohm
Add a capacitor in Farads
Add an inductor in Henry
Add a Warburg impedance
Add a constant phase element
9-11
Chapter 9. Simulation Menu
_____________________________________________________________________________________
Change simulation parameters such as frequency range
Open an equivalent circuit file for a simulation or a fit
Save the current equivalent circuit
Run the impedance simulator
Run the impedance fitting program
Stop the fitting in progress
Exit the mechanism editor simulation environment
The equivalent circuitry drawing is visual. To add a component, click the
component symbol on the tool bar and then click the edit field. The component will
appear in the edit field. If you double click the component you placed in the edit field,
you can name the component and enter the value of the component.
You can connect two components by moving the mouse to the left or to the right
of a component. When the mouse cursor is close to the left or right side of a component,
a black dot will appear. Press the left mouse button when the dot appears and drag the
mouse while holding the left mouse button down. A trace will appear as you drag the
mouse. Drag the mouse to the left or to the right of the other component connect. If a
black dot appears on the left or right side of the other component, release the left mouse
button. A connection should then be made between the two components.
To remove a component, select the component by clicking it. The component’s
color will change to red. Then click the Cut button on the toolbar. When a component is
deleted, the corresponding connections are deleted with it. You can also remove a
component by moving the mouse to the component, holding down the left button and
dragging it out of the edit field.
To remove a connection wire, select the wire by clicking the trace (will turn to
red) and use the Cut command on the toolbar.
You can move components and wires around. Select a component or a trace, drag
it while holding the left mouse button. After you move the component or the trace to a
desired location, release the left mouse button. You can thus make the circuit drawing
more readable.
You can use the Move button on the toolbar to move all components left, right, up
or down.
You can also use the Rearrange button on the toolbar to rearrange components
and connection wires. However, there are only four modes and they may not create an
ideal diagram. You may have to redraw the diagram manually.
To finish the equivalent circuit drawing, you need to connect the two big dots on
the left and the right sides of the edit field. If you do not connect those two dots, the
program will not know what the two terminals of your circuit are and can not perform
simulation.
You might find the command buttons on the toolbar useful. You can undo or redo
your actions. You can clear the edit field by removing all the components and connection
wires. You can change the impedance simulation parameters such as frequency range and
number of data points per decade of frequency.
Please notice that the equivalent circuit you draw can be used for both simulation
and fitting. To perform a simulation, click the Sim button. After that, the program will
9-12
Chapter 9. Simulation Menu
_____________________________________________________________________________________
exit the equivalent circuit edit field and display the simulated data on the screen. Be
aware that unsaved data will be erased when a new simulation starts. Save your existing
data before starting a simulation.
To start fitting, you need to have a set of impedance data first. The impedance
data can be obtained by running impedance measurements or by a simulation. You also
need to draw the circuit that would match the equivalent circuit of your actual system.
If the equivalent circuit does not match the mechanism of the actual data, the data
may not fit very well. You may need to revise your circuit.
The fitting program may not be perfect. Sometimes, it does not fit very well even
with a known (simulated) data set. You may also find that fitting results be affected are
dependent on the initial value of the components. If you experience problems, please email us the data. We will try to study it and improve it, but cannot guarantee better
results. Efficient fitting algorithms are difficult and complicated to obtain.
Press the Fit button on the toolbar to start the fitting process. During fitting, the
elapsed time, fitting error and evolution of component parameters will be diaplyed. When
the values stop changing, the fitting ends. You can then see the fitting results (value of
component parameters as well as the fitting error). In order to stop the fitting process,
click the Exit button on the toolbar. The original data and the fitted data will be overlaid
and displayed.
You can save your equivalent circuit drawing to a disk file and read it back later.
To exit the circuit editing field, click the Exit button. You need to exit first to use
other commands of the program.
Notes:
Before you run the fitting program by pressing the Fit button, connect the
instrument. The program will check for the proper instrument model. It only needs to
check once after the program is started. After the first fit, you do not need to have the
instrument connected anymore.
When you do impedance simulation and fitting, please do not enter other
technique or read data files other than impedance measurements. Otherwise the
equivalent circuit editing field will go wrong.
Dimensions and Ranges of Components
Name
Resistor R
Capacitor C
Inductor L
Warburg Impedance W
Constant Phase Element Q
Dimension
Ohms
Farad
Henry
Siemens•sec1/2
Siemens•secn
9-13
Range
0.001 - 1e12
1e-12 - 1
1e-12 - 1
1e-6 - 1
1e-12 - 1000
Chapter 9. Simulation Menu
_____________________________________________________________________________________
Property of Components
Component Impedance
Resistor R:
ZR = R
Capacitor C: ZC = -j/ωC
Inductor L: ZL = jωL
Warburg Impedance W:
ZW = (1/Yo)(jω)-1/2
Constant Phase Element Q:
ZQ = (1/Yo)(jω)-n
Conductance
YR = 1/R
YC = jωC
YL = -j/ωL
Phase
frequency-independent
ϕ=π/2
ϕ=-π/2
YW = Yo(jω)1/2
ϕ=π/4
YQ = Yo(jω)n
ϕ = nπ / 2, 0 < n < 1
9-14
Chapter 10. View Menu
_____________________________________________________________________________________
Data Information Command
Use this command to view the information of the currently active data.
This command presents a Data Information dialog box:
The following items allow you to view the information of the currently active
data:
Filename
This non-editable box displays the filename of the currently active data. If it has
not been stored, the filename is "Unsaved".
Data Source
This box displays the data source that is either experimental or simulated.
Model
This box displays which instrument model was used when the data was acquired.
Date
This box displays the date that the data was acquired.
Time
This box displays the time that the data was acquired.
Data Proc Performed
This list box displays the type of data processing performed. If several types of
data processing have been executed, multiple item will be checked. This reminds you
what you have done to this set of data in the past.
10-1
Chapter 10. View Menu
_____________________________________________________________________________________
Header
This box displays the header. The header can appear on the data plot.
Note
This box displays the note about the experiment. The note can remind you about
the purpose and the conditions of the experiment.
10-2
Chapter 10. View Menu
_____________________________________________________________________________________
Data Listing Command
Use this command to list the experimental conditions, results, and numerical
value of the currently active data.
The format of the listing can be altered by the Text File Format command under
the File menu.
The system displays the Data List dialog box so you can view the numerical data.
Use scroll bar to view the listing if necessary. If the listing is too long, the later part of
the data will be truncated.
10-3
Chapter 10. View Menu
_____________________________________________________________________________________
Equations Command
Use this command to view the equations relating to the electrochemical technique
currently invoked.
The following is a list of equations available. For more details about the equations
and how to use them, please refer to "Electrochemical Methods", A.J. Bard and L.R.
Faulkner, Wiley, New York, 1980.
Equations
General equations
Symbols and Units
Linear Sweep Voltammetry and Cyclic Voltammetry
Staircase Voltammetry
Tafel Plot
Chronoamperometry
Chronocoulometry
Differential Pulse Voltammetry
Normal Pulse Voltammetry
Square Wave Voltammetry
A.C. Voltammetry
2nd Harmonic A.C. Voltammetry
i-t Curve
Bulk Electrolysis
Hydrodynamic Modulation Voltammetry
A.C. Impedance
Chronopotentiometry
Potentiometric Stripping Analysis
10-4
Chapter 10. View Menu
_____________________________________________________________________________________
Clock Command
Use this command to view the current date and time.
This command presents a Clock dialog box so you can view the date and time.
The time will be updated constantly.
10-5
Chapter 10. View Menu
_____________________________________________________________________________________
Toolbar Command
Use this command to display and hide the Toolbar, which includes buttons for
some of the most common commands in the system, such as File Open. A check mark
appears next to the menu item when the Toolbar is displayed.
The toolbar is displayed across the top of the application window, below the
menu bar. The toolbar provides quick mouse access to many tools used in the program,
To hide or display the Toolbar, choose Toolbar from the View menu.
Status Bar Command
Use this command to display and hide the Status Bar, which describes the action
to be executed by the selected menu item or depressed toolbar button, the file status and
the currently active technique. A check mark appears next to the menu item when the
Status Bar is displayed.
The status bar is displayed at the bottom of the application window. To display or
hide the status bar, use the Status Bar command in the View menu.
The left area of the status bar describes actions of menu items as you use the
arrow keys to navigate through menus. This area similarly shows messages that describe
the actions of toolbar buttons as you depress them, before releasing them. If after
viewing the description of the toolbar button command you wish not to execute the
command, then release the mouse button while the pointer is off the toolbar button.
The right areas of the status bar indicate the file status and the currently active
technique:
Indicator
Technique
Description
The currently active technique.
3 or 4 electrode configuration
10-6
Chapter 11. Help Menu
_____________________________________________________________________________________
Help Topics Command
Use this command to display the opening screen of Help. From the opening
screen, you can jump to step-by-step instructions on how to use the program as well as
various types of reference information.
There is a Context Help for buttons in the toolbar, Use the Context Help
command to obtain help on some portion of the program. When you choose the toolbar's
Context Help button, the mouse pointer will change to an arrow and question mark. Then
click anywhere in the application window to obtain help on the item you’ve picked.
11-1
Chapter 11. Help Menu
_____________________________________________________________________________________
About Command
Use this command to display a copyright notice, the version number, the software
revision date and the manufacturer’s contact information:
11-2
Appendix
________________________________________________________________________
Cables and Connections
1. Electrode connection (Video connector)
Pin
Function
1
Working electrode
2
Sensing electrode
3
N/C
4
Reference electrode
5
Counter electrode
6
Analog Ground
(Green)
(Black)*
(White)
(Red)
*:
This electrode is used for 4-electrode configuration. It can be used for liquid/liquid interface
measurements. In this case, the red clip is connected to the counter electrode in phase I. The white clip is connected
to the reference electrode of the same phase. The green clip is connected to the counter electrode in phase II. The
black clip is connected to the reference electrode of phase II.
The 4-electrode configuration also helps to eliminate contract resistance (due to clip, connector, switching
relay) and the resistance of circuitry traces. It is very important for large current (> 100mA) measurements and low
impedance cell (< 1 ohm). However, it is not recommended for low current measurement (< 100mA) and high
impedance cell.
To use 4-electrode configuration, please check the "4-Electrode" option use the Cell command under the
Control menu. If the purpose of using the 4-electrode configuration is to eliminate contact resistance, you should
connect the Sensing electrode together with the Working electrode.
If you do not use 4-electrode configuration, please make sure that the "4-Electrode" option in Cell Control
dialog box is unchecked. Otherwise noise and other problems may occur.
If you use 3-electrode configuration, please leave the Sensing electrode unconnected.
2. RDE Control connection (Banana jacks)
Red
Signal
Black
Analog Ground
3. Signal Output on Rear Panel (9-pin D connector)
1
Current Output*
2
Reserved for Current 2 (bipotentiostat)
3
Potential Output
4
External Signal Input**
5
External Potential Input***
6
Ground
7
Ground
8
Ground
9
Ground
*:
The current can be calculated by
Current Output Reading (V) * sensitivity (A/V)
**:
The input voltage range is ±10 V. The input impedance of the input stage is 10K ohm. For signals with
high voltages, a resistor divider should be used. For signal with small voltage range (< 0.1V), it is possible to
amplify the signal by factor 10 or 100. If the amplification is needed, please contact CH Instruments for
instructions.
***:
The external Potential Input is disabled. To enable it, you need to set the jumper inside the instrument.
Please contact CH Instruments for details.
A-1
Appendix
________________________________________________________________________
4. Comm Port connection (DB-25 connector)
Pin
Function
2
Receive
3
Transmit
7
Digital Ground
5. Cell Control connection (DB-25 connector)
Pin
Function
1
2
3
4
Analog Ground
5
-15V
(<20 mA load)
6
+5V
(<100 mA load)
7
Digital Ground
8
Stir
(active level can be set in Cell Control)
9
Knock
(active low pulse)
10
External Device Sense 1
11
External Device Sense 2
12
External Device Control 1
13
External Device Sense 3 (external trigger input, TTL signal, active low)
14
Reserved
15
Reserved
16
17
+15V
(<20 mA load)
18
19
External Device Control 2
20
External Device Control 3
21
Purge
(active low level)
22
23
External Device Control 4
24
External Device Control 5
25
Reserved
The Cell Control port can be used to control stir, knock and purge. Please check the
manual of your cell stand for compatibility. Customized jumper or connection cable might be
needed.
A-2
Appendix
________________________________________________________________________
Instructions of Software Update
Instrument control software has two portions. One is the software on the PC side. There
is also software inside the instrument. Sometimes software update will only involve the software
on the PC side, but occasionally software inside the instrument is also involved. The software
inside the instrument is stored in the flash memory. You can get updated software on both PC
side and instrument side from CH Instruments. The software installation on the PC side us
described in Chapter 2. The software on the instrument side is a hexadecimal file
(CHI6xxC.HEX, where 6xxC is the model number). In order to update the software inside the
instrument, use the "Update Instrument Program" command under the File menu to bring up the
following dialog box:
You can type in the hexadecimal file name and path in the “Filename” field. Or you can
use "Browse" button to select the hexadecimal filename.
Click "Update" button to upload the program to the instrument flash memory.
During upload, please be patient and wait. Please do not activate any other program. It
could cause the upload to fail and mess up the flash memory and instrument will not be useable.
One has to do force programming. Please contact CH Instruments if this occurs.
If download failed, you will get an error message. You may need to turn off the
instrument and wait for 5-10 seconds and turn the instrument on. You may need to exit the PC
program and restart the program. You can then try again.
If the download is successful, you will get a confirmation message. You can now use the
instrument.
A-3
Appendix
________________________________________________________________________
Trouble Shooting
Problem
link failed
Possible Cause
power is not on
cable is not connected
bad cable
comm port setting does not
match the port in use
computer problem
static discharge
program does not
respond mouse action
lengthy computation
process
communication failed
Windows application
error
hardware test error
no current response
noisy data
electrode leads is not
connected or broken leads
unreliable data transfer
reference electrode
impedance too high
electrically noisy
environment
instability of potentiostat
due to large double layer
capacitance
signal is too weak
A-4
Action
turn on the instrument power
connect the cable
check and change cable
use System command under
Setup menu to set the port
make sure no network card or
fax/modem card in the
computer system. If there is
one, unplug it and try again. If
the problem persists, try a few
more computers.
turn off and turn on the
instrument again. You may
also have to reset the computer
wait
reset the instrument and the
computer
restart the program or reset the
computer
repeat the hardware test,
record the error message, and
contact CHI for service
check the electrode leads
If the data reading exceeds 10
× sensitivity scale, the problem
could be due to comm port.
Make sure the network is
disconnected. Try another
computer.
check if air bubble is trapped
at the reference electrode tip;
change to reference electrode
with vicor tip
use Faraday cage; also see
chapter 2, "Useful Tips"
use Cell command under
Control menu to manually set
the stabilizing capacitor on
use the highest sensitivity scale
Appendix
________________________________________________________________________
computer problem
data recorded is out
of range
sensitivity scale is too high
hardware problem
overflow warning
sensitivity scale is too high
during the experiment
Y axis title rotate in a printer driver
wrong angle
incompatibility
unreasonable default
conditions
simulation program
does not run
as possible, set filter
make sure no network card or
fax/modem card in the
computer system. If there is
one, unplug it and try again. If
the problem persists, try a few
more computers.
lower the sensitivity scale
use Hardware Test command
under Setup menu to test the
hardware
lower the sensitivity scale
use Font command under
Graphics menu to toggle the Y
axis title rotation
different version of software delete old *.cfg file, a new
and the configure file
configure file will be generated
automatically
could not find the hardware connect and turn on the
instrument
user input mechanism is not try to use the predefined
available to the instrument
mechanism, or you may have
model
to give up
A-5
Appendix
________________________________________________________________________
Maintenance and Service
The recommended operating temperature is 15-28°C.
Since the instrument is a sophisticated equipment, you should not try to service it
yourself. If the instrument does not work properly, please run the hardware test and contact the
factory for service.
Limited Warranty
This CH Instruments product is warranted against defects in workmanship and material.
If any failure, resulting from a defect of workmanship or material, shall occur under normal use
within one year from the date of purchase as shown on the purchase receipt, CH Instruments
will, at its option, either repair the defective product without charge for parts and labor, or
provide a replacement in exchange for the defective product.
In order to obtain service under this warranty, customer must notify CH Instruments
before the expiration of the warranty period and make arrangements for the service. Customer
shall be responsible for packing and shipping the defective product with shipping charges
prepaid. CH Instruments shall pay for the return of the product to customer if the shipment is
within the United States. Customer shall be responsible for paying all shipping charges, duties,
taxes, and any other charges for products returned to outside of the United States.
Warranty service does not include repair of failures caused by misuse, accident,
modification, unsuitable physical or operating environment, improper maintenance and service
of the product by unauthorized personnel.
In no event shall CH Instruments be liable, or in any way responsible, for any lost profits,
lost savings, incidental damage, or other economic consequential damages. This is true even if
you advise CHI of the possibility of such damages.
A-6
Appendix
________________________________________________________________________
Safety
Section 1: LVD Notes for manual Safety issues and protection of instrument against
damage
1. The unit described in this manual is designed to be operated by trained personnel with
some reasonable background knowledge of electrochemistry. Any adjustments, maintenance or
repair must be carried out as defined by this manual (please refer to appendix sections) and by a
person qualified and aware of the hazards involved.
2. (a) It is essential that operating personnel employ a safe system of work, in addition to
the detailed instructions specified in this manual.
2. (b) The instrument should be placed in a position where the likelihood of the ingress of
a chemical spill is kept to an absolute minimum. Efforts should also be made to avoid contact of
the instrument, with for instance, corrosive vapor. The electrochemical cell should not be placed
on top of the unit due to the risk of leakage and the possibility of the cell contents entering the
instrument. If chemicals do enter the unit then it should be switched off immediately and the
nearest dealer/CH Instruments, Inc (contact details at the front of this manual) contacted.
Routine cleaning of the chassis of the instrument is not necessary. A spill onto the outer casing
that does not enter the instrument should be wiped off with a dry cloth, making sure to wipe
away from any instrument connections. Likewise the PC used to operate the instrument should
be protected from the possible exposure to chemicals.
2.(c) Despite the customers best efforts corrosion of the electrode leads can occur.
This condition is best diagnosed by running a CV from -1 V to +1 V on a 1 M Ohm resistor;
sensitivity set at 1.e-6. An Ohmic plot through the origin should be obtained
with maximum currents of +/-1 uA. Working contacts (green and black) are connected to one
side of the resistor and counter (aux) and reference (red and white) to the other. Noticeable
divergence from this behavior (i.e., linearity through origin) may suggest faulty leads.
2. (d) Erroneous data/behavior in an actual electrochemical experiment may be due to
factors such a faulty cell connections, poor reference electrode contact or poor condition of the
working electrode. Reference and working electrodes are consumable items and are freely
available from CH Instruments, Inc or your local dealer (see Appendix for a description of the
range of accessories available). Where a customer uses his/her own electrodes it is recommended
that experimental data is compared against know standards from time to time.
3. The cover of the unit should only be removed by competent personnel on direction of
CH Instruments, Inc.
4. Reference should always be made to the health and safety data supplied with any
chemicals used. Generally accepted laboratory procedures for the safe handling of chemicals
should always be employed.
5. Evidence of any fault condition should immediately be reported to CH Instruments, Inc
or the local distributor – Whichever is applicable. Faults with the hardware are usually diagnosed
through the instruments own self test procedure (see Troubleshooting in the Appendix).
6. As the instrument operates by a data coupling to a PC we recommend that sufficient
space (at least 2 m of linear bench) is set aside in order to avoid cluttering the work area and to
ensure easy access of the cell. There should be some free space around the vents and fan exhaust
of the instrument for effective cooling.
7. Connection of the cell by the crocodile clip connections should be made in such a way
A-7
Appendix
________________________________________________________________________
as to avoid shorting of the contacts.
Section 2. Power configuration
On unpacking the instrument the presence of the following should be noted.
1.
Mains cable
2.
Cell Lead
3.
Instrument instruction manual
4.
Optional accessories (e.g., cells, electrodes, etc.) if ordered
The unit is designed to operate at 110V or 230 V AC power @ 50-60 Hz. Please check
the rear panel label for the input voltage setting. If wrong ac voltage is connected, fuse will blow
and instrument may be damaged.
The correct voltage and line frequency for your region have been set prior to shipment at
our factory.
The standard 2 meter (or 6 foot) mains cable is fitted with an IEC type connector which
can be plugged directly into the power input on the rear panel of your instrument. The mains fuse
(250V L 0.4A) is housed within the power socket. When replacing the fuse, the user should fully
disconnect the instrument from the power supply.
In the event of repeat failure of the fuse the user should consult with CH Instruments, Inc
a correct course of action before proceeding further.
The unit should be placed within 1.5 m of an earthed mains power supply.
When the instrument is powered on, the indicator light on the front panel will be
illuminated.
Rear Panel of instrument
1.
2.
3.
4.
Power switch
On/off Switch of unit
Fuse
State fuse value here
Power input Socket IEC type connection socket for mains cable
Cooling fan
Fuse rating = 0.8 A for 110V AC input, 0.4 A for 230V AC input
Power cord rating = 15A for 110V AC input, 10A for 230V AC input
All other features are clearly labeled on the rear panel itself.
A-8
Appendix
________________________________________________________________________
Abbreviation of Electrochemical Techniques
ACV:
BE:
CA:
CC:
CP:
CPCR:
CV:
DDPA:
DNPV:
DPA:
DPV:
HMV:
IMP:
IMP-t:
IMP-E:
IPAD:
ISTEP:
i-t:
LSV:
NPV:
OCPT:
PSA:
QCM:
SCV:
SHACV:
SSF:
STEP:
SWV:
TAFEL:
TPA:
A.C. Voltammetry (including Phase Selective A.C. Voltammetry)
Bulk Electrolysis with Coulometry
Chronoamperometry
Chronocoulometry
Chronopotentiometry
Chronopotentiometry with Current Ramp
Cyclic Voltammetry
Double Differential Pulse Amperometry
Differential Normal Pulse Voltametry
Differential Pulse Amperometry
Differential Pulse Voltammetry
Hydrodynamic Modulation Voltammetry
Impedance Spectroscopy
Impedance - Time
Impedance - Potential
Integrated Pulse Amperometric Detection
Multi-Current Steps
Amperometry i-t Curve
Linear Sweep Voltammetry
Normal Pulse Voltammetry
Open Circuit Potential - Time
Potentiometric Stripping Analysis
Quartz Crystal Microbalance
Staircase Voltammetry
Second Harmonic A.C. Voltammetry (including Second Harmonic Phase
Selective A.C. Voltammetry)
Sweep-Step Functions
Multi-Potential Steps
Square Wave Voltammetry
Tafel Plot
Triple Pulse Amperometry
A-9
Appendix
________________________________________________________________________
Model 400A Time-Resolved Electrochemical
Quartz Crystal Microbalance
The quartz crystal microbalance (QCM) is a variant of acoustic wave microsenseors that are capable of
ultrasensitive mass measurements. Using a crystal with a 7.995-MHz fundamental frequency (as used in our
measurements) as an example, a net change of 1 Hz corresponds to 1.34 ng of materials adsorbed or desorbed onto
the crystal surface of an area of 0.196 cm2.
QCM and the combination of QCM with electrochemistry (EQCM) have been widely employed for the
determination of metals deposited onto the crystal, studies of ion-transport processes in polymer films, biosensor
developments, and investigations of the kinetics of adsorption/desorption of adsorbate molecules. In EQCM
experiments, the measurements of the various electrochemical parameters, such as potential, current and charge at
the working electrode, and the acquisition of the corresponding frequency change, are conducted simultaneously.
Such simultaneous measurements were made possible by employing an experimental setup shown in the Figure 1 on
the next page. For any model in the CHI400A series, the application of a specific potential waveform (e.g.,
triangular potential waveform for cyclic voltammetric experiments), and the subsequent measurement of the current,
and the frequency counting were carried out with a potentiostat/frequency counter, which is, in turn, controlled by a
computer.
The CHI400A series contains a quartz crystal oscillator, a frequency counter, a fast digital function
generator, a high-resolution and high-speed data acquisition circuitry, a potentiostat, and a galvanostat (Model 440A
only). The QCM is integrated with potentiostat and galvanostat, making the EQCM study simple and convenient.
Instead of measuring the frequency directly, the CHI400A series uses time-resolved mode. The frequency signal of
the QCM is subtracted from a standard reference frequency. The difference is then measured by reciprocal
technique. This technique greatly reduces the time need for sampling the QCM signal and gives much better time
resolution for the QCM signal. With direct counting method, a 1 Hz QCM resolution requires 1 second of sampling
time, and a 0.1 Hz resolution requires 10 seconds sampling time. The time-resolved mode allows QCM signal to be
measured in milliseconds with much better resolution. The QCM data can be recorded while the scan rate is at 1
V/s.
The EQCM cell consists of three round Teflon pieces (see Figure 1 on next page). The total height is 37
mm with a diameter of 35 mm. The top piece is the cell top to hold reference and counter electrodes. There are also
two 2mm holes for manual purging. The center piece is the cell body for solution. The bottom piece is for mounting
purpose. Four screws are used to tighten the bottom piece and center piece together. The quartz crystal is located
between the center and bottom pieces. The seal is through two O-rings that are pressed together by the four screws
mentioned above. The diameter of the quartz crystal is 13.7 mm. The gold electrode diameter is 5.1 mm.
Specifications
Potentiostat
Galvanostat (Model 440A)
Potential range: -10 to 10V
Potentiostat rise time: < 2 µs
Compliance voltage: ±12 V
3- or 4-electrode configuration
Current range: 250 mA
Reference electrode input impedance: 1×10-12 ohm
Sensitivity scale: 1×10-12 - 0.1 A/V in 34 ranges
Input bias current: < 50 pA
Current measurement resolution: < 1 pA
Minimum potential increment in CV: 100 µV
Potential update rate: 1 MHz
Data acquisition: 16 bit @ 200 kHz
Frequency resolution: < 0.1 Hz
QCM maximum sampling rate: 500 Hz
Automatic and manual iR compensation
Low-pass signal filters, automatic and manual setting
CV and LSV scan rate: 0.000001 to 2000 V/s
Potential increment during scan: 0.1 mV @ 100 V/s
CA and CC pulse width: 0.0001 to 1000 sec
CA and CC Steps: 320
DPV and NPV pulse width: 0.0001 to 10 sec
SWV frequency: 1 to 100 kHz
ACV frequency: 0.1 to 10 kHz
SHACV frequency: 0.1 to 5 kHz
Automatic potential and current zeroing
RDE rotation control output: 0 - 10 V (430A and up)
Potential and current analog output
Cell control: purge, stir, knock
Data length: 128K-4096K selectable
Chassis dimension: 12.5”(W) × 11”(D) × 4.75”(H)
Oscillator box (external):
4.75"(L) × 2.6" (W) × 1.55" (H)
Weight: 15 Lb.
A-10
Appendix
________________________________________________________________________
Techniques for the Model 400A Series
Techniques
400A
410A
420A
430A
440A
Cyclic Voltammetry (CV)
Linear Sweep Voltammetry (LSV) &
Staircase Voltammetry (SCV) #,&
Tafel Plot (TAFEL)
Chronoamperometry (CA)
Chronocoulometry (CC)
Differential Pulse Voltammetry (DPV) #,&
Normal Pulse Voltammetry (NPV) #,&
Differential Normal Pulse Voltammetry (DPNV)#,&
Square Wave Voltammetry (SWV) &
AC Voltammetry (ACV) #,&,$
2nd Harmonic AC Voltammetry (SHACV) #,&,$
Amperometric I-t Curve (I-t)
Differential Pulse Amperometry (DPA)
Double Differential Pulse Amperometry (DDPA)
Triple Pulse Amperometry (TPA)
Bulk Electrolysis with Coulometry (BE)
Hydrodynamic Modulation Voltammetry (HMV)
Sweep-Step Functions (SSF)
Multi-Potential Steps (STEP)
Chronopotentiometry (CP)
Chronopotentiometry with Current Ramp (CPCR)
Potentiometric Stripping Analysis (PSA)
Open Circuit Potential - Time (OCPT)
Quartz Crystal Microbalance (QCM)
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
Galvanostat
RDE control (0-10V output)
Full version of CV simulator
Limited version of CV simulator
iR Compensation
z
z
z
z
z
z
z
#: Corresponding polarographic mode can be performed.
&: Corresponding stripping mode can be performed.
$: Phase selective data are available.
Figure 1. EQCM setup
A-11
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
Appendix
________________________________________________________________________
Techniques for the Model 600C Series
Electrochemical Analyzer
Techniques
CV
LSV &
SCV #,&
TAFEL
CA
CC
DPV #,&
NPV #,&
DNPV #,&
SWV &
ACV #,&,$
SHACV #,&,$
i-t
DPA
DDPA
TPA
IPAD
BE
HMV
SSF
STEP
IMP
IMP-t
IMP-E
CP
CPCR
ISTEP
PSA
OCPT
600C
z
z
602C
z
z
604C
z
z
606C
z
z
608C
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
610C
z
z
620C
z
z
z
z
z
z
z
z
z
630C
z
z
z
z
z
z
z
z
650C
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
#: Corresponding polarographic mode can be performed.
&: Corresponding stripping mode can be performed.
$: Phase selective data are available.
Dynamic Range of Some Experimental Parameters
Parameters
Potential (V)
Current (A)
Sensitivity (A/V)
Sampling Rate
Scan rate (V/s)
Pulse width (sec)
Pulse width (sec)
Sampling width (sec)
Frequency (Hz)
Frequency (Hz)
Frequency (Hz)
Frequency (Hz)
Model 6××B
-10 to +10
0 to ±0.25
1x10-12 to 0.1
1 M Hz at 16-bit resolution
0.000001 to 20000
.0001 - 1000
0.001 to 10
0.0001 to 10
1 to 100000
1 to 10000
1 to 5000
0.0001 to 100000
A-12
Techniques Involved
CV, LSV
CA, CA
DPV, NPV
DPV, NPV
SWV
ACV
SHACV
IMP
660C
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
Appendix
________________________________________________________________________
Techniques for the Model 700C Series Bipotentiostat
Techniques
CV
LSV &
SCV #,&
TAFEL
CA
CC
DPV #,&
NPV #,&
DNPV #,&
SWV &
ACV #,&,$
SHACV #,&,$
i-t
DPA
DDPA
TPA
IPAD
BE
HMV
SSF
STEP
IMP
IMP-t
IMP-E
CP
CPCR
ISTEP
PSA
OCPT
700C
z
z
701C
z
z
z
z
z
z
710C
z
z
720C
z
z
730C
z
z
z
z
z
z
z
z
750C
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
760C
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
#: Corresponding polarographic mode can be performed.
&: Corresponding stripping mode can be performed.
$: Phase selective data are available.
Dynamic Range of Some Experimental Parameters
for Model 700C Series
Parameters
Potential (V)
Current (A)
Current (A)
Sensitivity (A/V)
Sampling Rate
Scan rate (V/s)
Pulse width (sec)
Pulse width (sec)
Sampling width (sec)
Frequency (Hz)
Frequency (Hz)
Frequency (Hz)
Frequency (Hz)
Range
-10 to +10
0 to ±0.25 (one channel only)
0 to ±0.125 (dual channel)
1x10-12 to 0.1 (both channel)
1 M Hz at 16-bit resolution
0.000001 to 20000
.0001 - 1000
0.001 to 10
0.0001 to 10
1 to 100000
1 to 10000
1 to 5000
0.0001 to 100000
Techniques Involved
CV, LSV
CA, CA
DPV, NPV
DPV, NPV
SWV
ACV
SHACV
IMP
Dual channel measurements apply to CV, LSV, SCV, CA, DPV, NPV, DNPV, SWV, and i-t.
A-13
Appendix
________________________________________________________________________
Techniques for the Model 800B Series
Electrochemical Detector
Techniques
CV
LSV &
CA
CC
DPV #,&
NPV #,&
SWV &
i-t
DPA
DDPA
TPA
BE
SSF
STEP
PSA (Zero Current)
CP
CPCR
ISTEP
OCPT
800B/802B
z
z
810B/812B
z
z
820B/822B
z
z
z
z
z
z
z
z
z
z
z
830B/832B
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
840B/842B
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
#: Corresponding polarographic mode can be performed.
&: Corresponding stripping mode can be performed.
Dynamic Range of Some Experimental Parameters
for Model 800B Series
Parameters
Potential (V)
Current (A)
Sensitivity (A/V)
Scan rate (V/s)
Pulse width (sec)
Pulse width (sec)
Sampling Interval (sec)
Frequency (Hz)
Range
-10 to +10
0 to ±0.010
1x10-12 to 0.001
0.000001 to 25
0.001 - 1000
0.001 to 10
.00005 to 100
1 to 10000
Techniques Involved
CV, LSV
CA, CA
DPV, NPV
i-t
SWV
Model 8××B: Single (8×0B) or dual (8×2B) channel electrochemical detection. High sensitivity and low noise.
Fast 16-bit A/D converter and 24-bit high resolution A/D converters. Bipotentiostat can also be used for RRDE.
The Model 800B is the upgrade version of the Model 800 and 800A series. It is more sensitive than the 800
series and has wider potential range.
New features include high data acquisition rate, iR compensation, current re-zeroing circuitry, low-pass
filters with lower cutoff frequencies, 0-10V RDE control output, and galvanostat (model 840B/842B).
A-14
Appendix
________________________________________________________________________
CHI900B/910B Scanning Electrochemical Microscope
The scanning electrochemical microscope (SECM) was introduced in 19891 as an instrument that
could examine chemistry at high resolution near interfaces. It is based on reactions that occur at a small
electrode (the tip) as it is scanned in close proximity to a surface. SECM can be employed to obtain
chemical reactivity images of surfaces and also in quantitative measurements of reaction rates. Numerous
studies with the SECM have now been reported from a number of laboratories all over the world and the
instrument has been used for a wide range of applications, including studies of corrosion, biological
systems (e.g., enzymes, skin, leaves), membranes and liquid/liquid interfaces2. Trapping and
electrochemical detection of single molecules with the SECM has also been reported. With the
introduction of the CH Instruments SECM, developed in collaboration with the University of Texas
group, this technique now becomes available to any laboratory.
1. A. J. Bard, F.-R. F. Fan, J. Kwak, and O. Lev, Anal. Chem. 61, 132 (1989); U.S. Patent No. 5,202,004 (April 13, 1993).
2. A. J. Bard, F.-R. Fan, M. V. Mirkin, in Electroanalytical Chemistry, A. J . Bard, Ed., Marcel Dekker, New York, 1994, Vol.
18, pp 243-373.
CHI900B/910B SECM Specifications
Micropositioner:
Other Features:
X, Y, Z resolution:
1.6 nm (combination of Stepper
motors and Piezos, CHI910B has a closed-loop Piezo
controller)
X, Y, Z total distance: 2.5 cm or 5.0 cm
Windows-based software
Amperometric and potentiometric detection
Constant height and constant current mode
Real time absolute and relative distance display
Real time probe and substrate current display
Current vs. X plot
Current vs. Y plot
Current vs. Z Plot
Bipotentiostat:
Probe Potential: ± 10 V
Substrate Potential: ± 10 V
Compliance Voltage: ± 12 V
Current Sensitivity: 10-12 A/V to 10-3 A/V
Maximum Current: ± 10 mA
Fast A/D Converter: 16-bit @ 25 K Hz
ADC Resolution: 20-bit @ 1kHz, 24-bit @ 10 Hz
Applications:
Electrode surface studies
Corrosion
Biological samples
Solid dissolution
Liquid/liquid interfaces
Membranes
Type of Measurements:
SECM Imaging
Probe Scan and Approach Curves
Surface Patterned Conditioning
CV, CA, DPV, SWV, i-t, DPA, DDPA, TPA, BE, SSF,
STEP, CP, CPCR, ISTEP, and E-t
Probe Approach Curve
8.00E-10
150
0
80
40
Y / um
i/A
6.00E-10
100
0
0.00E+00
-2.00E-10
-4.00E-10
-6.00E-10
-8.00E-10
50
i/A
SECM Image
4.00E-10
2.00E-10
0.00E+00
-60
X / um
-40
-20
Distance / um
A-15
0
Appendix
________________________________________________________________________
Model 1000 Series Multi-Potentiostat
CHIl0×× series is a computerized 8 channel potentiostat. The system contains a digital function generator,
a multiplexed data acquisition circuitry, a multi-potentiostat with eight working electrodes, one common reference
electrode and one common counter electrode. The instrument is designed so that eight working electrodes are in the
same electrochemical cell. The potential control range is ±3.276 V for the primary channel and ±2.0 V for the rest
of the seven channels. Any of these seven channels can also be set at the identical potential as the primary channel
with potential range of ±3.276 V, so that they can sweep or step potentials together with the primary channel. Each
electrode can be individually controlled, including on/off control, potential and sensitivity settings. However, the
primary channel is always on during ran. The current range is ±10 mA. The instrument is capable of measuring
current down to picoamperes.
Besides the commonly used cyclic voltammetry, amperometric i-t measurements, many other
electrochemical techniques are available. All eight channels work for various electrochemical techniques, except
open circuit potential measurements. The parameters for all the channels should be set before running experiments.
You can not alter the parameter setting during experiments. During run, you can alter display mode between single
data set display and multi-set data display (either parallel or overlay plots). After run, you can choose data sets of
any channels as parallel plots or overlay plots.
Techniques for the Model 1000 Series Multi-Potentiostat
Techniques
CV
LSV &
CA
CC
DPV #,&
NPV #,&
SWV &
i-t
DPA
TPA
SSF
STEP
OCPT
1000
z
z
1010
z
z
1020
z
z
z
z
z
z
z
z
z
z
z
z
1030
z
z
z
z
z
z
z
z
z
z
z
z
z
#: Corresponding polarographic mode can be performed.
&: Corresponding stripping mode can be performed.
Specifications
8-Channel potentiostat
Potential range (primary channel): ±3.275 V
Potential range (channel 2-8): ±2.0 V
Compliance voltage: ±12 V
Current range (each channel): 10mA
Reference electrode input impedance: IX1012 ohm
Sensitivity scale: I x 10-9 - 0.001 A/V in 7 ranges
Input bias current: < 50 pA
Current measurement resolution: < 5 pA
Data acquisition: 16 bit @ 5 kHz maximum
A-16
CV and LSV scan rate: 0.000001 to 5 V/s
CA and CC pulse width: 0.01 to 1000 s
CA and CC Steps: 320
DPV and NPV pulse width: 0.005 to 10 s
SWV frequency: 1 to 250 Hz
Current low-pass filters
Potential and current analog output
Cell control: purge, stir, knock
Maximum data length: 128000 points each channel
Chassis dimension: 12.5"(W) x I I "(D) x 4.75"(H)
Appendix
________________________________________________________________________
Model 1100A Series Power Potentiostat / Galvanostat
The Model 1100A series power potentiostat/galvanostat is designed for electrochemical applications that
require relatively large current and high compliance voltage, such as battery, corrosion, electrolysis and
electroplating. The current range is ± 2 A. The compliance voltage is ± 25 V. Instrument contains a digital function
generator, a data acquisition system, filters for the current signals, iR compensation circuitry, a potentiostat, and a
galvanostat (Model 1140A). The potential control range is ± 10 V. Similar features can also be obtained by using
the combination of the CHI600B series and the CHI680 Amp Booster. However, the CHI1100A series is more
compact and lower cost. This series is capable of measuring current down to tens of picoamperes. The instrument is
reasonably fast. For instance, the scan rate in cyclic voltammetry can be up to 2000 V/s.
Specifications
Potentiostat
Galvanostat (Model 1140A)
Potential range: -10 to 10 V
Potentiostat rise time: < 2 µs
Compliance voltage: ± 25 V
3- or 4-electrode configuration
Current range: ± 2 A
Ref. electrode input impedance: 1×1012 ohm
Sensitivity scale: 1×10-10 - 0.1 A/V in 10 ranges
Input bias current: < 100 pA
Potential update rate: 1 MHz
Data acquisition: 16 bit @ 200 kHz
Automatic and manual iR compensation
CV and LSV scan rate: 0.000001 to 2000 V/s
Potential increment during scan: 0.1 mV if below 100V/s
CA and CC pulse width: 0.001 to 1000 s
CA and CC Steps: 320
DPV and NPV pulse width: 0.001 to 10 s
SWV frequency: 1 to 100 kHz
Automatic potential and current zeroing
Signal low-pass filters, covering 8-decade frequency range,
Automatic and manual setting
Potential and current analog output
Cell control: purge, stir, knock
Maximum data length: 128K-4096K selectable
Chassis dimension: 12.5”(W) × 11”(D) × 4.75”(H)
Differences of 1100A Series Models
Techniques
1100A
1110A
1120A
1130A
1140A
Cyclic Voltammetry (CV)
Linear Sweep Voltammetry (LSV) &
Staircase Voltammetry (SCV) #,&
Tafel Plot (TAFEL)
Chronoamperometry (CA)
Chronocoulometry (CC)
Differential Pulse Voltammetry (DPV) #,&
Normal Pulse Voltammetry (NPV) #,&
Differential Normal Pulse Voltammetry (DPNV)#,&
Square Wave Voltammetry (SWV) &
AC Voltammetry (ACV) #,&,$
2nd Harmonic AC Voltammetry (SHACV) #,&,$
Amperometric i-t Curve (i-t)
Differential Pulse Amperometry (DPA)
Double Differential Pulse Amperometry (DDPA)
Triple Pulse Amperometry (TPA)
Bulk Electrolysis with Coulometry (BE)
Sweep-Step Functions (SSF)
Multi-Potential Steps (STEP)
Chronopotentiometry (CP)
Chronopotentiometry with Current Ramp (CPCR)
Potentiometric Stripping Analysis (PSA)
Open Circuit Potential - Time (OCPT)
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
Galvanostat
Full version of CV simulator
Limited version of CV simulator
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
#: Corresponding polarographic mode can be performed. &: Corresponding stripping mode can be performed.
Model 1200A Series Hand-held
A-17
Appendix
________________________________________________________________________
Potentiostat / Bipotentiostat
The Model 1200A series is a computerized hand-held potentiostat/bipotentiostat. The instrument consists
of a digital function generator, a data acquisition system, a potentiostat/bipotentiostat. The potential range is ± 2.4
V. The current range is ± 2 mA. This series is capable of measuring current down to 100 pA. The steady state
current of a 10 µm disk electrode can be readily measured. The size of the instrument is 7” (L) × 4.5” (W) × 1” (H).
The instrument is powered by the PC computer through the USB port. The instrument can be used for
electroanalysis and sensor studies. Due to its small size, light weight, and low cost, it is particularly useful for field
applications and teaching laboratories.
The CHI1200A series provides various instrument models to meet different applications and budget. The
instrument offers potentiostat version and bipotentiostat version. The CHI1200A, 1210A, 1220A, 1230A, and
1240A are potentiostat, whereas the CHI1202A, 1212A, 1222A, 1232A, and 1242A are bipotentiostat.
Specifications
Potentiostat / bipotentiostat
Potential range: ± 2.4 V
Compliance voltage: ± 7.5 V
Current range: ± 2 mA
Reference electrode input impedance: 1×1012 ohm
Sensitivity scale: 1×10-10 - 0. 01 A/V in 7 ranges
Input bias current: < 100 pA
Current measurment resolution: < 5 pA
Data acquisition: 16 bit @ 10 kHz
CV and LSV scan rate: 0.000001 to 10 V/s
CA and CC pulse width: 0.001 to 1000 s
CA and CC Steps: 1 - 320
DPV and NPV pulse width: 0.001 to 10 s
SWV frequency: 1 to 5000 Hz
ACV frequency: 0.1 to 2000 Hz
Low pass filter for current measurements
Maximum data length: 128000
Chassis dimension: 7” (W) × 4.5 (D) × 1 (H)
Differences of 1200A Series Models
Techniques
1200A
/1202A
1205A
/1206A
1207A
/1208A
1210A
/1212A
1220A
/1222A
1230A
/1232A
Cyclic Voltammetry (CV)
Linear Sweep Voltammetry (LSV) &
Chronoamperometry (CA)
Chronocoulometry (CC)
Differential Pulse Voltammetry (DPV) &
Normal Pulse Voltammetry (NPV) &
Differential Normal Pulse Voltammetry (DPNV) &
Square Wave Voltammetry (SWV) &
Amperometric i-t Curve (i-t)
Differential Pulse Amperometry (DPA)
Double Differential Pulse Amperometry (DDPA)
Triple Pulse Amperometry (TPA)
Open Circuit Potential - Time (OCPT)
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
Full version of CV simulator
Limited version of CV simulator
z
&:
Note:
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
z
Corresponding stripping mode can be performed.
1200A/1205A/1207A/1210A/1220A/1230A are single potentiostat.
1202A/1206A/1208A/1212A/1222A/1232A are bipotentiostat.
A-18
Appendix
________________________________________________________________________
CHI200(B) Picoamp Booster and Faraday Cage
With CHI200(B) Picoamp Booster and Faraday Cage, the current down to a few picoamperes can
be readily measured. CHI200 is compatible with Model 600/A, 700/A series of instruments. CHI200B is
compatible with Model 600B/C, 700B/C, and 800B series. When used with 700/A/B/C and 800B series
bipotentiostat, Picoamp Booster will have effect on the primary channel only.
The internal sensitivity of the 600C series is the same as the Picoamp Booster (1×10-12 A/V).
However, the bias current of the 600C series input can be as high as 50 pA. The Picoamp Booster has
lower bias current, and it also bring the preamplifier close to the electrode that results in lower noise. It is
also necessary to have Faraday Cage in case of small current yet relatively fast measurements.
Before connecting the Picoamp Booster, turn the instrument power off. Connect the din connector
of the Picoamp Booster to the “Electrodes” connector at the rear panel of the instrument. Also connect the
DB-25 connector of the Picoamp Booster to the “Cell Control” connector at the rear panel of the
instrument with a straight through DB-25 cable (come with PBFC). You can then turn the power on.
DB-25 connector provides power supplies and control lines (see Cables and Connections in
Appendix). If DB-25 connector is not connected, you can still do experiments as Picoamp Booster is
disabled. In this case, the faraday cage is effective.
To purge inert gas, you may unscrew one of the screws on the back of the faraday cage. This will
open a hole for inert gas tubing.
When the Picoamp Booster is connected and the sensitivity scale is at or below 1e-8 A/V, the
Picoamp Booster will be enabled. Otherwise it will be disabled. The sensing of the Picoamp Booster
existence and the enable/disable switching are automatic.
Picoamp Booster will be disabled for techniques using automatic sensitivity switching, such as
TAFEL, BE, IMP, IMP-t, and IMP-E. You do not need to disconnect it to run these techniques. However,
for galvanostatic techniques, such as CP, CPCR and PSA, Picoamp Booster has to be disconnected.
If the Picoamp Booster is not used, please disconnect the DB-25 cable.
CHI684 Multiplexer
CHI684 is a multi-channel multiplexer for the model 400, 400A, 600A, 600B, 600C, 700A,
700B, 700C, 800B, 900B and 1100A series. The multiplexer switches four lines (working, sensing,
reference, and counter in case of single potentiostat; working, 2nd working, reference and counter in case
of bipotentiostat). You can have maximum 64 cells, but only one cell can be connected at a time.
The multiplexer is controlled from the "Mulrtiplexer" command under the Control menu. You can
select any channels and run experiment in a sequence of selected channels. The files will automatically
saved after each run. You can also set prompt before each channel run.
It is allowed to set arbitrary channel immediately. You can run experiment for that particular
channel.
Two Macro commands are available for the multiplexer. One is "mch:##". It allows to set individual
channel. The other macro command is "mchn". This is used in For...Next loop. It will select the channel
according to the For...Next loop counter.
The minimum channels for the CHI684 are 8. The channel increment is 8. The maximum channels
are 64.
A-19
Appendix
________________________________________________________________________
CHI680 Amp Booster
With the CHI680 Amp Booster, the current can be measured up to 2A. The CHI680 is compatible
with Model 600, 60A/B/C series of instruments. You can stack the CHI6×× and the CHI680 together.
Before connecting the Amp Booster, turn the instrument power off. Connect the 6-pin din
connector of the CHI680 to the “Electrodes” connector on the rear panel of the CHI6××C. Also connect
the “Cell Control” ports of both instruments with a straight through 3-ft DB-25 cable (come with the
CHI680). You can then turn the power on for both CHI6××C and CHI680. It is generally a good practice
to turn on the CHI6××A/B/C first and then CHI680. When the power is turned off, reverse the order.
The cell connector is a 6-pin connector with four cell leads. The clip with green cover is for
working electrode, The white one is for reference electrode. The red one is for counter electrode. The
black one is for sensing electrode of the 4-electrode configuration. The 4-electrode configuration can be
turned on or off by check or uncheck the "4 Electrodes" box using the Cell command under the Control
menu. When the 4-electrode option is on, you should connect the black lead to the working electrode
(short the green and black leads together). The 4-electrode configuration is useful for liquid/liquid
interface measurements, or when the current is relatively high. It helps eliminate the resistance (about 0.20.3 ohm) due to the connectors, relays, and printed circuit board traces.
With the Amp Booster connected, the cell control signals such as purge, knock and stir are
disabled.
The Amp Booster will also allow low current measurements. The current down to 10 pA can be
measured. It is comparable with the CHI6××A/B alone. You may need to use Faraday cage to eliminate
line frequency noise when the scan rate is above 50 mV/s.
The frequency responses of the Amp Booster is somewhat lower than the CHI6××A/B/C
instruments. In case of high speed experiments (such as impedance measurements), the Amp Booster
should be disconnected.
If you think there might be something wrong with the hardware, please do hardware test with
Amp Booster disconnected. If the CHI6××A/B/C passes the test, you can then connect the Amp Booster
and test the Amp Booster with a standard resistor. You can use CV to see if you obtain a straight line with
a slope of voltage / resistance.
CHI682 Liquid/Liquid Interface Adapter
Liquid/liquid interface study is very important in understanding the charge transfer, chemical
sensor, drug release, solvent extraction, and others. Liquid/liquid interface study usually involves two
reference electrodes and two auxiliary electrodes. The modified potentiostat controls the potential
difference of the two reference electrodes in two phases, while measuring the current passing through two
auxiliary electrodes. The CHI682 Liquid/Liquid Interface Adapter is compatible with our model 700A
series. It is fully automatic and transparent to users. Most electrochemical techniques can be used.
However, it does not have galvanostat and bipotentiostat functions.
Please notice that for model 400, 600A, 600B, 600C, 700B, 700C, 800B, 900B, 1100, 1100A
series, 4-electrode configuration will allow liquid/liquid interface measurement to be made directly
without using CHI682 Liquid/Liquid Interface Adapter.
A-20
Appendix
________________________________________________________________________
Accessories
Part No.
CHI101
CHI101P
CHI102
CHI102P
CHI103
CHI104
CHI104P
Description
2 mm dia. Gold Working Electrode
2 mm dia. Gold Working Electrode
2 mm dia. Platinum Working Electrode
2 mm dia. Platinum Working Electrode
2 mm dia. Silver Working Electrode
3 mm dia. Glassy Carbon Working
Electrode
3 mm dia. Glassy Carbon Working
Electrode
Unit
1
3/pk
1
3/pk
1
1
Part No.
CHI117
25 µm dia. Platinum SECM Tip
Unit
1
CHI117P
25 µm dia. Platinum SECM Tip
3/pk
CHI118
3/pk
CHI127
CHI128
CHI129
1-5 µm dia. Platinum SECM Tip
Electrode Polishing Kit 2
Polished, Bounded, Mounded 100A Cr
+ 1000 A Gold Crystal for EQCM
EQCM Cell
Reference Electrode for EQCM Cell
Pt Wire Counter Electrode for EQCM
Cell
Thin-Layer Flow Cell
GC Working Electrode for Flow Cell
Au Working Electrode for Flow Cell
Pt Working Electrode for Flow Cell
Reference Electrode for Flow Cell
25 um Spacer for Flow Cell
Spectroelectrochemical Cell
Calomel Reference Electrode
Mercury/Mercurous Sulfate Reference
Electrode
Alkaline/Mercurous Oxide Reference
Electrode
Electrode leads for a particular
instrument model number
Picoamp Booster and Faraday Cage 3
Picoamp Booster
Faraday Cage
Simple Cell Stand 4
Cell Top (including Pt wire counter
electrode, not a replacement part for
the CHI200 cell stand) 5
Glass Cell
Teflon Cap 5
CHI105
10 µm dia. Gold Microelectrode
1
CHI105P
10 µm dia. Gold Microelectrode
3/pk
CHI106
25 µm dia. Gold Microelectrode
1
CHI106P
25 µm dia. Gold Microelectrode
3/pk
CHI107
10 µm dia. Platinum Microelectrode
1
CHI107P
10 µm dia. Platinum Microelectrode
3/pk
CHI108
25 µm dia. Platinum Microelectrode
1
CHI108P
25 µm dia. Platinum Microelectrode
Ag/AgCl Reference Electrode
Ag/AgCl Reference Electrode
Non-Aqueous Ag/Ag+ Reference
Electrode 1
Non-Aqueous Ag/Ag+ Reference
Electrode 1
Platinum Wire Counter Electrode
3/pk
CHI111
CHI111P
CHI112
CHI112P
CHI115
CHI116
CHI116P
1
3/pk
1
3/pk
10 µm dia. Platinum SECM Tip
1
1
10 µm dia. Platinum SECM Tip
3/pk
CHI120
CHI125
CHI130
CHI131
CHI132
CHI133
CHI134
CHI135
CHI140A
CHI150
CHI151
CHI152
CHI172Model #
CHI200
CHI201
CHI202
CHI220
CHI221
CHI222
CHI223
Description
1
1
1
1
1
1
1
1
1
1
1
4/pk
1
1
1
1
1
1
1
1
1
1
1
1
Notes:
1. A Ag+ solution (typical 10 mM) should be prepared with the supporting electrolyte and AgNO3 (not included).
This solution is then filled into the reference electrode compartment using a syringe (not included). The
instructions will come with the components.
2. The electrode polishing kit contains 1 bottle of 1.0 micron Alpha alumina powder, 1 bottle of 0.3 micron Alpha
alumina powder, 3 bottles of 0.05 micron Gamma alumina powder, 2 glass plates for polishing pads, 5 pieces of
73 mm diameter 1200 grit Carbimet disks (grey in color), 5 pieces of 73 mm diameter Mastertex polishing pads
(white in color), and 10 pieces of 73 mm diameter Microcloth polishing pads (brown in color).
3. Picoamp Booster and Faraday Cage allows the current measurement down to 1 pA. It is fully automatic and
compatible with Model 6xxC and 7xxC series instruments. However, it only works for the primary channel of the
7xxC series .
4. Made of stainless steel and Teflon (see figure below). Not remote-controllable. Four glass cells are included.
5. Not a replacement part for the CHI220 Cell Stand.
A-21
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