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1. I Chronopotentiometry CH a WEE af E WC SCH E ie PS E Gg KE A ooo Es a Buk Bectrolysis with Coulometry BE E ral z a It H We Eat A i ER ES It Ge i H ew al RES 2014 CH Instruments Inc 254 CH Instruments Model 900D Series Reference Auxiliary Potentiostat Galvanostat H Frequency Counter Cell Body Computer Dorrean A Cell Bottom Crystal EQCM setup 2014 CH Instruments Inc Appendix 12 9 Model 600E Series Electrochemical Analyzer Techniques 604E 606E 660E E aan IPAD B H l Cc PCI STEP IMP t IMP E ISTEP 2 Corresponding polarographic mode can be performed S Corresponding stripping mode can be performed Phase selective data are available aa SC ee ee ee ee EEN ee ee Fi ee TE eee a ee ees eed eed fee a ae ee E ee a ee E Ye Set Deg ST C E EN EE ee EE E Kees EE e EC ee Ed EE BC EE E EE eS EE E ee ee e ee ee EE E ee BEE E ee EC EC ME EE DEE Ee it ES ee es ees ees Be ee ee PA a EE WEEN DEEN ees DPA LI DEE eee DE eee PA LL EE EE ee S E ER ER DE De E E a ai DEE ee ae EE MV E EE E D E SF a ae ae ae ee DEE EE PER bf EE DE DEER a MP Eo EE EE EEN DEE E Eee a DEE BE LL HERE DE BEE P Ooo o T EE E DEA E Kee EE EH DEER EES BEE EE ET DE EE A ae E EE EE GE Ee CN ae E es ee ee eee CPT ES eee WEE EC e EEN EES Dynamic Range of S
2. ss ssssssuussnunnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnn mennan nnmnnn 152 6 2 Overlay Plots COMMANG cccceeeeceeeee ence ee eeeeeeeee ee eeeeeeeeeeeeeeeeeeseeeseeeseeneeesseesaeeseeneeeesseeeseeses 156 6 3 Add Data to Overlay COMIMANGC cceceeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeaeeeeeeeeeseeseeeseeeseeeeeeeseeeeeeeaes 157 6 4 Replot Overlay COMMANG ececeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeseeeeeeseeeseeeseeeeeeeseeeeeeeaes 158 6 5 Manage Overlay command eeeeeREEERRRREEERRRR KEE RRE KEREN KEE EEEE RRE mnnn nnnm mennan nnmnnn 159 6 6 Parallel Plots COMMANG cceececeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeseaeeeeeseeeeeesseeseeeseaeeeeeseeeeeeees 160 6 7 Add Data to Parallel COMIMANG cccceeeeeceee ee eeeeeeeeeeeeeeee ee eeesee ee eeseeeeeeseeeaaeessaeeeeesseeeeeeses 161 6 8 Replot Parallel COMIMANGA ccceeeeeeeeeee KEREN KEE eeeeeeeeeeeeeeeeeeeeeeseeeseeeesesseeeeeseeeneeesseeneeeses 162 6 9 Manage Parallel COMMANG cccceeeeceeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeseseeeseeeseeneeeeseeeeeeeses 163 6 10 Zoom IN COMMANGL i cecccecececccecnsenceccnecectcnadecteceeencucaneesstecaeeescecerccsteccecsuecausrsceceverstecausecctans 164 6 11 Manual Results COMMANGC cccceeeseeeeeeeeeeeeeeeeeeeeeeseeeeeeeseeeeeeeseeeeeeseeeeeeseeeeeeeseeeeeeeneesenens 165 6 12 Peak Definition COMIMANG cceeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeneeseeeeeeeseeeaeeeseeeeeeseeeeeeeseeeae
3. 2014 CH Instruments Inc 134 CH Instruments Model 900D Series Test E is the test potential at which no electrochemical reaction will occur When the system is performing the test it applies a potential step relative to the test potential The test is passed only if the electrochemical cell can be considered equivalent to a solution resistance in series with a double layer capacitor The allowed range of the Test E parameter is 10V to 10V Step Amplitude refers to the magnitude of the applied potential step The larger the amplitude the higher the signal to noise ratio However too large of an amplitude may cause faradaic current to flow A step amplitude of 0 05V is recommended The allowed range of the Step Amplitude parameter is 0 01V to 0 25 V The compensation level Comp Level is the percentage of resistance you want to compensate based on the measured solution resistance The allowed range of this parameter is 0 to 200 default 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 starts to oscillate an overshoot in current in response to the potential pulse will be observed 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 Click the Test button to perform the solution resistan
4. 5 k a Init E Sample Width Step Period Segment 1 Segment 2 Time s Parameter Range Description Init E V 10 10 Initial potential Final E V 10 10 Final potential Incr E V te 3 0 05 Increment potential of each step Segments 1 1000 Number of scan segments Sampling Width s 1e 4 50 Data sampling width for each point Step Period s 0 001 50 Potential step period or dropping time Quiet Time sec 0 100000 Quiescent time before potential scan Sensitivity A V 1e 12 0 1 Sensitivity scale Electrode 2 Potential V 10 10 Second working electrode potential if not scan Sensitivity A V 1e 12 0 1 Sensitivity scale for second electrode On Check or Uncheck Second electrode at constant potential Scan Check or Uncheck Scan the second electrode potential Notes e Init E and Final E should be at least 0 01 V apart e Sampling Width should be no more than half of Step Period otherwise the system will automatically readjust the former e Data sampling always occurs at the end of each step e When the second electrode is in Scan mode it will have the same potential as the primary electrode throughout the experiment The potential of the second electrode is therefore not independent 2014 CH Instruments Inc ER CH Instruments Model 900D Series 4 2 4 Tafel Plot Parameters dialog box In the Tafel Plot technique TAFEL the potential is scanned from Init E toward Final E The potential may be
5. You can also use the scroll bar to move the piezo Every click on the left or right arrow on the scroll bar will move 1 100 of the full scale 2014 CH Instruments Inc Graphics Menu 151 Chapter 6 Graphics Menu The Graphics menu offers the following commands Present Data Plot Overlay Plots Add Data to Overlay Replot Overlay Parallel Plots Add Data to Parallel Replot Parallel Zoom In Manual Results Peak Definition XY Plot Peak Parameter Plot Semilog Plot Special Plots Graph Options Color and Legend Font Copy to Clipboard 2014 CH Instruments Inc Plot current data graphically Plot multiple data sets in a single graph Add data sets to existing overlay plot Show most recent overlay plot Plot multiple data sets in side by side graphs Add data sets to existing parallel plots Show most recent parallel plots Magnify graph region Report results manually Define peak or wave parameters Input custom data for plotting Plot peak current or potential versus scan rate Generate current potential semilog plot Generate special plots Set graph options Set color and legend options Set graph font options Copy graph to clipboard 152 CH Instruments Model 900D Series 6 1 Present Data Plot command Use this command to plot the currently active data You can rescale the Xor Y axis by hovering over it changing the mouse cursor to a double headed arrow Left click and drag to resca
6. 0 001 e 0 24 i i fo F Quiet Time s 2 H R n 3 f Sensitivity A V 1e 6 S oJ i i f Segment 1 Z i i i Ep 0 163V H E ip 9 619e 6A 5 0 Ss i F Ah 6 068e 6C d S i i E Segment 2 0 4 i i Ep 0 163V 064 i E ip 9 619e 6A RK 4 d d Ah 6 068e 6C d d 0 8 pq tert esq E t 0 50 045 040 035 030 025 020 015 010 0 0 0 0 05 0 10 Potential V For Help pri CN Hemna The fitting potential range will be bracketed graphically with the fitted data plotted in green and your input data plotted in red Fitting error and the time elapsed are also displayed in the top left The fitting process will end when the specified Error is reached alternatively it can be terminated at any time by clicking the Stop button or by pressing the Esc key The resulting fitted kinetic parameters will be then be displayed 2014 CH Instruments Inc View Menu 227 Chapter 10 View Menu The View menu offers the following commands Data Information View data information Data Listing View current data as a text list Equations View equations related to the selected technique Clock View current date and time Toolbar Shows or hides the toolbar Status Bar Shows or hides the status bar 2014 CH Instruments Inc 28 CH Instruments Model 900D Series 10 1 Data Information command This command opens the Data Information dialog box Use this command to view the information of the currently active data inc
7. 10 10 Final potential Incr E V 0 001 0 05 Increment potential of each pulse Amplitude V 0 001 0 5 Potential pulse amplitude Pulse Width s 1e 3 10 Potential pulse width Sample Width s 1e 4 10 Data sampling width Pulse Period s 0 01 50 Potential pulse period or dropping time Quiet Time s O 100000 Quiescent time before potential pulses begin Sensitivity A V 1e 12 0 1 Sensitivity scale Electrode 2 Potential V 10 10 Second working electrode potential if not step Sensitivity A V 1e 12 0 1 Sensitivity scale for second electrode On Check or Uncheck Second working electrode at constant E Scan Check or Uncheck Scan the second electrode potential Notes e Init E and Final E should be at least 0 01 V apart e Pulse Width should be no more than half of Pulse Period otherwise the system will automatically readjust Pulse Width Sample Width should be no more than half of Pulse Width otherwise the system will automatically readjust Sample Width When Amplitude is negative the pulse direction will in the opposite direction of the potential scan When the second electrode is set to Scan its potential will be the same as the primary electrode it is not independent 2014 CH Instruments Inc CH Instruments Model 900D Series 4 2 8 Normal Pulse Voltammetry Parameters dialog box In Normal Pulse Voltammetry NPV the base potential is held at Init E and a sequence of potential pulses with increasing am
8. 2 Controlled stripping current Sample Interval s 0 0001 50 Sampling interval Quiet Time s O 100000 Quiescent time before taking data Notes If sample interval is less than 0 002 s a total of 64K data points is allowed The data density is equal to Run Time 64000 If the final potential is reached the experiment will automatically stop H the controlled stripping current is set to zero the counter electrode is actually not connected If the controlled stripping current is smaller than 1 0e 10A no current will flow during experiment 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 and negative current correspond to reduction and oxidation respectively In general the data storage interval should be chosen according to the length of the experiment The longer the experiment the longer the data storage interval should be 2014 CH Instruments Inc Setup Menu 4 2 30 Parameters for Open Circuit Potential vs Time dialog box In the Open Circuit Potential Time technique OCPT the working and reference electrodes are connected and the potential difference across them is recorded as a function of time Since the counter electrode is not connected to the external cell no current passes through the working electrode except the bias current of the measuring amplifiers which is in the picoa
9. Control Level of Stir Line The stir line control signal can be specified as active high BAS or active low PAR Immediate Stir Specify the immediate stir time from 1 32767 Click the Stir button to activate immediate stirring Immediate Purge Specify the immediate purge time from 1 32767 Click the Purge button to activate immediate purging 2014 CH Instruments Inc 13 CH Instruments Model 900D Series Immediate Cell On Specify the cell potential from 10 to 10 and the cell on time from 1 to 32767 Click the Cell On button to poise the electrode at this potential for the specified amount of time SMDE Drops Before Run When using the static mercury drop electrode SMDE specify the number of mercury drops to be dispensed before the experiment Normally the system will issue a combined dispense and knock signal before running the experiment to allow a new drop to be formed This parameter should be between 0 20 default 1 if set to 0 the same drop used in the previous experiment will be used for the next experiment It may be useful to use more than one prerun drop if the SMDE occasionally traps little air bubbles in the capillary and loses contact Stabilizing Capacitor There is a 0 1 pF stabilizing capacitor that can be connected between the counter and reference electrodes This capacitor can stabilize the potentiostat but slows the system down somewhat This is particularly useful when the double lay
10. In this technique the potential of the substrate electrode which should be about the same size and positioned close to the probe is first swept or stepped to adsorb or electrochemically generate a species of interest with the probe electrode at open circuit Then the substrate electrode is disconnected at open circuit and the probe electrode potential is swept or stepped to electrochemically generate a titrant from a reversible redox mediator This titrant reacts in situ with the species generated during the first step resulting in a transient positive feedback loop until the adsorbate is consumed completely The current response is recorded The program presents the following dialog box Surface Interrogation SECM Parameters q SSES Substrate Electrode MEM WAERME Segments Quiet Time sec Probe Electrode t m SE IEN 0 Final EW 0 me Segments 0 0 0 2 Ber E Quiet Time sec 2 Sensitivity A V 1 e 006 e Sensitivity AT 1 e 006 D Sweep Sweep Scan Rate V s for Scan Rate Wil for Sample Interval 0 001 Sample Interval hl 0 001 Step Step Action between Two Runs Pilse Witdh s 1 Pilse Witdh s 1 Sample Interval s 0 002 Sample Interval s 0 002 Delay jO C Manual e Sweep Step e Sweep Step C ocp 10 Parameter Range Description Substrate Electrode Init E V 10 10 Initi
11. lt 50 pA Potential and signal low pass filters 8 decade freq Current measurement resolution lt 1 pA range auto manual Potential update rate 10 MHz Potential and current analog output Data acquisition 16 bit 1 MHz Cell control purge stir knock External voltage signal recording channel Flash memory for quick softw are update External potential input USB or serial port selectable for data communication Automatic and manual iR compensation Data length 128K 4096K selectable Potential and current analog output Chassis dimensions 14 2 W x 9 2 D x 4 7 H RDE control voltage output 0 10 V selected models Techniques for Model 1100C Series 1100c_ 1110c 1120c 1130c 1140c 1150C clic Voltammetry C Linear Sw eep Voltammetry LSV amp CC i oeo STe S oe e ee oee e Se DE SN EE ET EES EES 178 ET E EC eeh ee EE EE EE ET EE EECH Ghronocoulometry Il ll Differential Pulse Voltammetry DPv ITT CS E EE EE e e EE SS EE WEE E E EE EE E ee ee ee Be WR EE EE EE D Differential Normal Pulse Voltammetry DNPV Square Wave Voltammetry SWV AC Voltammetry ACV amp 2nd Harmonic AC Voltammetry SHACV 365 Amperometric i t Curve i t V Normal Pulse Voltammetry N S 2014 CH Instruments Inc Differential Pulse Amperometry DPA Double Differential Pulse Amperometry DDPA Triple Pulse Amperometry TPA Bulk Electrolysis w ith Coulometry BE d A ions
12. rdedepositionoff rdequieton rdequietoff rderunon rderunoff rdebetweenrunon rdebetweenrunoff rpm 0 rpmincr 0 rpmsart 0 rpmsqrtincr 0 afit fiti 0 HG 0 flt3 0 H 0 flt5 0 mch 1 mchn ei 10 eh 10 el 10 ef 10 eio eho elo efo eioei 10 eioef 10 eiocenter 2014 CH Instruments Inc 10 10 10 10 10 Control Menu enable internal dummy cell disable internal dummy cell turn on RDE turn off RDE RDE on during deposition RDE off during deposition RDE on during quiet time RDE off during quiet time RDE on during run RDE off during run RDE on between runs RDE off between runs RDE rotation rate in rpm RDE rotation rate increment in rpm square root of rotation rate square root of rotation rate increment automatic filter setting potential filter O none 1 150KHz 2 15KHZz UV converter O none 1 32kHz 2 3 2kHz signal filter O none 1 150KHz 2 15KHZz 2nd channel UV O none 1 32kKHz 2 3 2kHZz 2nd channel signal filter O none 1 150KHZz select multiplexer channel multi channel selection according to 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 OCP as init E disabled after new init E is specified by ei use OCP as high E disabled by eh command use OCP as low E disabled by el
13. 10 10 High potential limit Low E Limit V 10 10 Low potential limit No of Cycles 1 10000 Number of cycles Smpl Intv s qe 5 1 Sampling interval Notes e A step with duration less than 0 001 sec or shorter than the sampling interval will be ignored e f the sampling interval is longer than 0 002 sec data will be transferred and displayed in real time e The experiment will stop if the potential reaches either High E Limit or Low E Limit e The sampling interval will be automatically increased if step time cycles sample interval exceeds 128K if data is to be transferred after the experiment 2014 CH Instruments Inc 9 CH Instruments Model 900D Series 4 2 29 Potentiometric Stripping Analysis Parameters dialog box In Potentiometric Stripping Analysis PSA a constant potential deposition step is first applied after which the species accumulated at the electrode surface are stripped out by applying a constant current Potential is recorded as a 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 Potential V or Current A Deposition Time 0 Time s Parameter Range Description Deposition E V 10 10 Deposition potential Deposit Time s 0 1000000 Deposition time Final E V 10 10 Final potential see Notes Stripping Curr A 0
14. Automatically detect Com port Automatically detect Com port When this option is checked the program will detect a compatible instrument and assign its Com port number automatically This requires that the instrument be powered on and connected to your computer Set Com Port Press this button to assign your instrument s Com port number This will take the Automatically detect Com port setting into account If the Com port assignment does not succeed the dialog will not be closed To assign your Com port number and close the dialog regardless of whether the change succeeds use the OK button instead 2014 CH Instruments Inc 108 CH Instruments Model 900D Series 4 4 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 test results in the Hardware Test Results dialog box The Self Test command tests the digital and analog circuitry in the instrument This command presents the following dialog box Hardware Test Results Digital circuitry test results ROM version 1 04 ROM revision date 18 Jul 2003 Hel Check Code 0 0 He Potential and current offset test OK x Sensitivity test OK Gain stages test OK Analog circuitry test OK Review the Self Test results carefully In the case of an analog test error please repeat the test several times to see if the error is consistent Record th
15. To adjust text color use the Font command instead Legend Specify the style legend of the marker line style for the data curves and grid e g line point circle When the legend is chosen to be point data curves curve or the grid may not print correctly This has been found to be a printer specific problem Please consult your printer documentation or choose a different legend if this occurs Size Specify the marker size line thickness Interval Setting this value to N plots every Nth data point default 1 A larger value of Interval lowers your data point which is useful for Overlay Plots or different legends Default Clicking this button will reset all colors and legends to the program s default values 2014 CH Instruments Inc 178 CH Instruments Model 900D Series 6 19 Font command This command opens the Font Selection dialog box Use this command to adjust the appearance of the text used in the plot The font style size and color can be adjusted separately for all text elements You can also rotate the Y axis title for printing Font options will be saved when you exit the program and will be reloaded when you restart the program This command has a toolbar button The Font command presents a dialog box FontSeecion D ee a Items Axis Label Aral Narrow Axis Title Times New Roman Header arial Parameter Arial Results Arial Numerical Courier New Y axis Title Rotation
16. bin DI Cancel G Ge To select multiple files for conversion point the mouse cursor to the filenames you want to select and click the left mouse button while holding the Ctrl key or left click on two files while holding the Shift key to select a range of files or left click and drag To quickly convert the currently active file use the Save As command instead The following options allow you to specify the name and location of the binary file s that will be converted to text format File name Type or select the filename s you want to convert The box above lists files with the extension you select in the Files of type box Multiple files can be selected for conversion You don t have to type the extension The program will automatically attach an extension of bin to the filename Other extensions are not allowed Files of type Select the type of file you want to convert Only the bin type binary data file will be available 2014 CH Instruments Inc File Menu 3 8 TextFile Format command This command opens the Text File Format dialog box Use this command to specify text formatting options for non binary files generated by the Save As and File Conversion commands The Text File Format command presents this dialog box Le pe x Separator Dk Memg G Comma Cancel Iw Parameter C TAB z Help V Results C Space V Numeric Date C Linefeed Number of Significant Figures Data Point Interv
17. the other hand if the DC current is not expected to be large and the frequency is high a DC current bias may be unnecessary Automatic sensitivity scale is used by default During the experiment the system tests the current size and determines the proper sensitivity scale This usually works pretty well The sensitivity scale setting can also be manually overridden which may yield better results in certain cases 2014 CH Instruments Inc Setup Menu 4 2 25 Impedance Potential Parameters dialog box In the Impedance Potential technique IMPE the base potential is incremented from Init E toward Final E onto which a sequential sine waveform is superimposed Current and potential are sampled and analyzed to obtain the real and imaginary parts of the impedance as a function of potential The following diagram shows the potential waveform applied as a function of time Incr E TT Final E Amplitude xX Potential V Init E One Cycle Time s Parameter Range Description Init E V 10 10 Initial potential Final E V 10 10 Final potential Incr E V 0 001 0 25 Increment potential Amplitude V 0 001 1 5 A C amplitude Frequency Hz 0 0001 1e5 A C frequency Cycles lt 10 Hz 1 100 Number of repetitive cycles at each frequency Quiet Time s O 100000 Quiescent time before sampling data Bias DC Current off range on Enable DC current bias during run Sensitivity Scale 1e 12 0 1 Sensiti
18. when it appears This should install files in two locations Restart your computer if prompted to do so 4 Finally power on and connect your instrument to your computer Windows should now recognize the instrument automatically 5 Please note that the latest driver requires our software version 12 04 or newer Part 2 Instrument Installation Installation Procedure Complete the USB Driver Installation Procedure from Part 1 above Disconnect the instrument from your PC if applicable Connect the instrument to your PC and turn the power on Wait for any automatic system installation tasks to complete Open Device Manager right click My Computer gt Manage gt Device Manager Double click the category Ports COM amp LPT to display OO P Go bh 2014 CH Instruments Inc Getting Started 23 24 Device Manager BAX File Action View Help 8 l A Wil Batteries iY Computer Disk drives Display adapters 3 DVD CD ROM drives Human Interface Devices 4 IDE ATA ATAPI controllers Si IEEE 1394 Bus host controllers d i Infrared devices 5 gt Keyboards Mice and other pointing devices b Modems Monitors B i Network adapters S i 1394 Net Adapter S i Intel R PRO 100 VE Network Connection fH Intel R PRO Wireless LAN 2100 38 Mini PCI Adapter J EI CP2101 USB to UART Bridge Controller COMS a7 ECP Printer Port LPT1 7
19. which provide comprehensive context sensitive help via the Shift F1 keyboard shortcut and in dialog boxes Legacy documentation is also available in Microsoft s old WinHelp hlp file format and the program can switch dynamically between chm and hlp files when the latter are available This is particularly useful when using newer software versions with older instrument models However our old WinHelp files may be out of date and their use is discouraged Moreover starting with Windows Vista Microsoft has also dropped out of the box support for 32 bit hlp files although strangely 16 bit hlp files from the Windows 3 x era are still supported This issue can be resolved by installing WinHlp32 exe from the Microsoft website refer to article KB917607 for more information To install the software insert the software CD Double click the set exe file on the CD to extract the files to your hard drive The default extraction directory is C CHI The installation simply copies all files to the extraction directory After installation you should find chi exe the program executable chi chm HTML help file and some test data files bin in this directory Administrative rights are not required to run the program and UAC permissions introduced in Vista should not be an issue If the executable is copied or moved say to D My Prog exe it must be accompanied by a help file with the same name say D My Prog chm for the comprehensi
20. 1000 1500 hours or 125 200 days for average usage of 8 hours per day At 50V it will last 30 000 hours or about 10 years It is recommended to keep the motor controller turned off when the piezo block is not going to be used in the next hour or longer It is also recommended to image by scanning X and Y from zero in the positive direction At the end of imaging set the tip to return to the origin This will ensure low piezo voltage between experiments extending the lifetime of the piezo which is a relatively expensive part to replace 2014 CH Instruments Inc Getting Started 21 The program will issue a warning if a high piezo voltage is detected for too long If this happens you should either move the piezo back to zero or start the next experiment 2014 CH Instruments Inc 22 CH Instruments Model 900D Series 2 2 USB Driver Installation Part 1 Driver Installation System Requirements e Windows XP Vista 7 8 e CH Instruments Software version 12 04 or newer If your system does not meet the requirements above please visit our website for instructions and downloads for all versions of Windows starting from Windows 98 Installation Procedure 1 Do not connect the instrument to the computer yet 2 Double click the USB Driver installer on your software CD 3 Follow the on screen instructions accepting all default options in the affirmative Make sure the Launch the CP210x VCP Driver Installer option is checked
21. 1e 12 0 1 Sensitivity scale for second electrode E2 On Check or Uncheck Second working electrode on off control i2 On Check or Uncheck Second working electrode current measurement on off Notes The data sampling interval should be chosen according to the length of the experiment The longer the experiment the longer the sampling interval should be A longer sampling interval results in more signal averaging and less noise During an 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 unexpectedly long experiment It is possible to record external voltage signals eg spectroscopic signals simultaneously with the amperometric i t response minimum sampling interval may be limited Use the 9 pin D connector on the rear panel for signal input Consult the User s Manual for the pin out and signal level requirements When only 1 current scale is displayed during a run the data will be automatically scaled to fit When 2 current scales are displayed during a run they will be 1 100 and 1 10 of full scale When 3 current scales are displayed they will be 1 100 1 10 and 1 1 of full scale E2 On will turn the 2nd electrode potential control on without current sampling This is useful if the 2nd electrode is used for some kind of generator electrode In order to measure current from the 2nd channel check i2 On 2014 CH Instrument
22. 1e 3 1e 9 1e 3 1e 9 1e 3 1e 9 1e 3 1e 9 1e 3 1e 9 1e 3 1e 9 1e 3 1e 9 1e 3 Explanation initial potential for channel 1 potential for channel 2 potential for channel 3 potential for channel 4 potential for channel 5 potential for channel 6 potential for channel 7 potential for channel 8 sensitivity scale for channel 1 sensitivity scale for channel 2 sensitivity scale for channel 3 sensitivity scale for channel 4 sensitivity scale for channel 5 sensitivity scale for channel 6 sensitivity scale for channel 7 sensitivity scale for channel 8 turn on channel 1 turn on channel 2 turn on channel 3 turn on channel 4 turn on channel 5 turn on channel 6 turn on channel 7 turn on channel 8 turn off channel 1 turn off channel 2 turn off channel 3 turn off channel 4 turn off channel 5 turn off channel 6 turn off channel 7 turn off channel 8 scan or step channel 2 with primary channel scan or step channel 3 with primary channel 2014 CH Instruments Inc Control Menu 131 e4scan scan or step channel 4 with primary channel e5scan scan or step channel 5 with primary channel e6scan scan or step channel 6 with primary channel e7scan scan or step channel 7 with primary channel e8scan scan or step channel 8 with primary channel eiincr 1 1 increment e1 in for next loop should be reset to zero after loop e2incr 1 Al increment e2 in for loop should be reset to 0 after e3incr 1 1 increment e3 in for loop s
23. Controlled anodic current High E Limit V 10 10 High potential limit High E Hold T s 0 100000 High potential hold time Low E Limit V 10 10 Low potential limit Low E Hold T s 0 100000 Low potential hold time Cathodic Time s 0 005 100000 Cathodic run time Anodic Time s 0 005 100000 Anodic run time Initial Polarity Cathodic Anodic Polarity for the first segment Data Stor Intvl s 0 0001 500 Data storage interval Num of Segments 1 1000000 Number of half cycles Curr Switch Prior Potential or Time Current polarity switching control Aux Signal Rec Check or Uncheck Simult record external signal when samp interval gt 0 0005 s Notes Cathodic and anodic currents correspond to reduction and oxidation respectively When the Low E limit is reached during reduction the current polarity will automatically be switched to anodic Similarly when the High E Limit is reached during oxidation current will automatically be switched to cathodic When the number of current polarity switches Segments is reached the experiment stops The Initial Polarity parameter specifies the initial current polarity During the experiment data update and storage rates will be the same i e dictated by the Data Storage Intv parameter The data sampling interval should be chosen according to the length of the experiment The longer the experiment the longer the sampling interval should be During an experiment whenever the
24. Example usage A e B reduction A e B oxidation A B isomerization A B C dissociation A B C combination 2014 CH Instruments Inc 212 CH Instruments Model 900D Series A B C D general reaction Mechanism Select There are 10 pre defined mechanisms covering the most commonly encountered reactions The first item is User Input Only Model 630 and Model 660 will accept the user defined mechanism Some mechanisms not listed can still be obtained from the pre defined mechanisms For instance EEC ECC and CEC mechanisms can be obtained from the ECEC mechanism by setting the appropriate kinetic parameters to null If you define the heterogeneous electron transfer rate ko to zero the corresponding electron transfer step will have no effect If you define the forward and reverse rate constants of a chemical reaction to zero the corresponding chemical reaction will have no effect Clicking on a pre defined reaction mechanism will automatically fill out the Mechanism Edit box If User Input is selected the Mechanism Edit box will be empty System under study A diffusive or adsorptive system can be simulated For diffusive systems planar diffusion is assumed For adsorptive systems it is assumed that the adsorption obeys the Langmuir isotherm and both oxidized form and reduced form are strongly adsorbed Dimensionless current When this box is checked the program will calculate the dimensionless current which is useful
25. Input 5 External Signal Input 6 Ground 7 Ground 8 Ground 9 Ground The input voltage range is 10 V and the input impedance of the input stage is 10K ohms For signals with high voltages a resistor divider should be used For signals with a small voltage range lt 0 1 V it is possible to amplify the signal by a factor of 10 or 100 please contact info chinstruments com for details The external potential input is disabled by default To enable it you need to change a jumper setting inside the instrument Please contact info chinstruments com for details 2014 CH Instruments Inc Com Port connection DB 25 connector i Function Receive Transmit Digital Ground d be ss Cell Control connection DB 25 connector Pin Function 1 2 Stepper motor control line 1 3 Stepper motor control line 2 4 Analog Ground 5 15 V lt 20 mA load 6 5 V lt 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 Stepper motor control line 15 Piezo positioner control line 16 Piezo positioner control line 17 15 V lt 20 mA load 18 Piezo positioner control line 19 External Device Control 2 20 External Device Control 3 21 Purge active low level 22 23 External Device Control 4 24 External D
26. Multi Potential Steps STEP AC Impedance IMP l Impedance Potential IMPE Chronopotentiometry CP Sw eep Step Functions SSF Impedance Time IMPT B Chronopotentiometry w ith Current Ramp CPCR Potentiometric Stripping Analysis PSA Open Circuit Potential Time OCP Galvanostat Full version of CV simulator Limited version of CV simulator Impedance simulation and fitting program Corresponding polarographic mode can be performed amp Corresponding stripping mode can be performed Phase selective data are available 2014 CH Instruments Inc CH Instruments Model 900D Series 12 15 Model 1200B Series Handheld Potentiostat Bipotentiostat The model 1200B series instrument is a computerized hand held potentiostat bipotentiostat The system contains a digital function generator a data acquisition system and a potentiostat bipotentiostat and it is w ell suited for electroanalysis and sensor studies The potential range is 2 4 V and the current range is 2 mA This series is capable of measuring current dow n to 100 pA The steady state current of a 10 umdisk electrode can be readily measured The size of the instrument is 7 W x 4 5 D x 1 H and it is pow ered through a USB port without any need for an AC adapter or batteries The instrument can be used for electroanalysis and sensor studies Due to its small size light w eight and low cost it is particularly useful for field applications and teach
27. SES EE EES SEELEN 6 1 4 System Require Ment ccccccceecececeeeeeeeeeeeeeeeeeeeseeeeeeseeeeeeseeeeeeeseeeeeeeseeeaeeeseeeeeeeseeeseeneesseees 9 1 5 Hardware Specifications ccccccecceeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeseeseeeeeeeeeeseeeseeseaeeeeeseeeseeeees 10 Chapter 2 Getting Started 11 21 ICT E Le EE 12 p Wa DRA Parts List aE OE E ect cctecseccctncdieseceenateneeseetesivedei E steeencrsedesectunes 13 2 1 2 Software 22133 Farduw ANG E E E T E E T T T E T 16 2 1 4 Nanopositioner Stepper Motors and Piezo s n nsusnnnnnnsnnnnnnrunnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnn ennn 19 2 2 USB Driver Installaton SEENEN EEN eee REENEN EEN EEN nennen nenna 22 23 gt TO SUMO BE 25 24 Some Usefull Tips eege ES eesti ewceeeeen scenes dss iv net sien cane tae SES NEE ELE ee 27 Chapter 3 File Menu 29 3 1 Open COMMA DE 30 ER E Lu RE 32 3 3 Delete command ee dee SEENEN SEENEN e EEN Ee Ee Ee EE 34 3 4 Retri ves COM MAN oisceneccsecccescccceveccaccccasscceneecteeccoetaetsectaecceoustesteceta EE ENER 35 3 5 Update Instrument Program COMMANA ccceeececeeeeeeeeeeeeeeeeeeeeeeeeeeeeseeeeneeseeeeenseeeeneeneeeeeees 36 Sp List Data Fil command eai aea ENEE EENEG NES 37 3 7 Convert to Text commande EEREEE RRE REENEN eee ence mnnn nn nnmnnn mnnn nessa eeeeaseeeeeseeeeeees 38 3 8 Text File Format COMMANGA c ccseccee cece eee eee REENEN ENEE ENEE EEN 39 3 9 Import Text File COMMANGA cccceeeceeee
28. SSlESESESES ES ES ES SSES NES S S S S S S S S S S ololololjolol ajo o NINIS E U U Notes Part No Description Unit Polished Bounded Mounded 100A Ti CH 1000 A Gold Crystal for EQCM Kee Pt Wire Counter Electrode for EQCM Cell a c c CI cH150 BE a Hectrode Hectrode ICHI202 a CHI172 Hectrode leads for a particular Model instrument model number Faraday Cage 1 Simple Cell Stand 4 SES C Cell Top including Pt w ire counter 1 electrode not a replacement part for the CHI200 cell stand 5 Glass Cell CHI223 Teflon Cap 5 CHI202 HI 20 HI 20 H 272 HI 23 HD 24 HD A0 HI SO HD 51 HI200 HI201 HI220 HI221 HI222 1 Ag solution typically 10 mM should be prepared w ith the supporting electrolyte and AgNO not included and filled into the reference electrode compartment using a syringe not included Detailed instructions are included w ith the components 2 The electrode polishing kit contains 1 bottle of 1 0 micron Alpha alumina pow der 1 bottle of 0 3 micron Alpha alumina pow der 3 bottles of 0 05 micron Gamma alumina pow der 2 glass plates for polishing pads 5 pieces of 73 mm diameter 1200 grit CarbiMet disks grey colored 5 pieces of 73 mm diameter Mastertex polishing pads w hite colored and 10 pieces of 73 mmdiameter Microcloth polishing pads brow n colored 3 The Picoamp Booster and Faraday Cage allow current measurements down to 1 pA Usag
29. The Faraday cage also makes it possible to make relatively fast measurements of small currents When the Picoamp Booster is connected and the sensitivity scale is at or below 1e 8 A V the Picoamp Booster will be automatically enabled Otherwise it will be disabled Detection and enabling disabling of the Picoamp Booster are fully automatic and do not require user intervention The Picoamp Booster will be disabled for techniques using automatic sensitivity switching such as Tafel plots TAFEL and bulk electrolysis BE and galvanostatic techniques For galvanostatic techniques such as chronopotentiometry CP chronopotentiometry with Current Ramp CPCR Multi Current Steps ISTEP and Potentiometric stripping analysis PSA the Picoamp Booster will not work However it works with AC impedance IMP In addition to allowing weak signal measurements the Faraday cage is useful for eliminating electrical interference especially line frequency noise If the electrochemical cell is picking up electrical noise from the environment the additional use of the Faraday cage is strongly recommended Before connecting the Picoamp Booster turn the instrument power off Connect the Picoamp Booster to the 6 pin Electrodes connector on the rear panel of the instrument Also connect the DB 25 connector of the Picoamp Booster to the Cell Control connector on the rear panel of the instrument with the straight through DB 25 cable included then turn the
30. V 10 10 Second working electrode potential Sensitivity A V 1e 12 0 1 Sensitivity scale for second electrode On Check or Uncheck Second working electrode at constant E Pulse Check or Uncheck Step the second electrode potential Notes e The experimental sequence consists of three pulses This sequence is repeated until the total number of cycles is reached or the experiment is interrupted by the user There is no data acquisition during 2014 CH Instruments Inc Setup Menu the first two pulses which are used for electrode cleaning purposes data are sampled only for the third pulse If the first or second pulse time is zero the corresponding step will be ignored If the increment potential is non zero the experiment will start at E3 and end at Final E E3 and Final E should be at least 0 01 V apart The number of cycles will have no effect Data sampling occurs during the second half period of pulse 3 The longer the pulse width the longer the sample interval will be resulting in better signal averaging and less noise During an 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 unexpectedly long experiment When only 1 current scale is displayed during a run the data will be automatically scaled to fit When 2 current scales are displayed during a run they will be 1 100 and 1 10 of full scale When 3 current sca
31. V s with a 0 1 mV potential increment or 5000 V s with a 1 mV potential increment The potentiostat galvanostat uses a 4 electrode configuration allow ing it to be used for liquid liquid interface measurements and eliminating the effect of the contact resistance of connectors and relays for high current measurements The data acquisition systems allow an external input signal such as spectroscopic to be recorded simultaneously w ith electrochemical data Similar features can also be obtained using the combination of the model 600E series and the CHI680C Amp Booster How ever the model 1100C series is more compact and less expensive Specifications Potentiostat CV and LSV scan rate 0 000001 to 5000 V s Galvanostat Model 1140C Potential increment during scan 0 1 mV 1000 V s Potential range 10 to 10 V CA and CC pulse w idth 0 0001 to 1000 sec Applied potential resolution 0 0015 of potential range CA and CC Steps 320 Applied potential accuracy 2 mV 0 02 of scale DPV and NPV pulse width 0 001 to 10 sec Potentiostat rise time lt 2 us SWV frequency 1 Hz to 100 kHz Compliance voltage 25 V CA and i t sample interval minimum 1 us 3 or 4 electrode configuration ACV frequency 0 1 Hz to 10 kHz Current range 2 A SHACV frequency 0 1 Hz to 5 kHz Reference electrode input impedance 10 12 ohm IMP frequency 0 00001 Hz to 10 kHz Sensitivity scale 10 12 0 1 A V in 12 ranges Automatic potential and current zeroing Input bias current
32. Y amp Y torE log Y amp Y torE IMP E Rs E Cs E Rp E Cp E Mott Schottky 1 CsxCs E Mott Schottky 1 CpxCp E CP PSA potential time dE dt time dt dE potential Potential charge 2014 CH Instruments Inc 156 CH Instruments Model 900D Series 6 2 Overlay Plots command Use this command to plot multiple sets of data in a single graph This is particularly useful for data comparison A multi colored legend will be automatically generated from the data filenames To view a saved overlay plot use the Replot Overlay command This command presents the following dialog box Overlay Data Display E 2 x Lookin l cht Jo Eich E fs MP1 EJ IMPE1 Ewe Elwpe EJocpTi EJ IMPE4 EJ Psao gt Filename LSVO BIN nun BIN CV3 BIN CVO BIN Files of type Data Files bin DI Cancel Select the data files you want to overlay 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 while holding the Ctrl key down to select files one at a time This command allows you select multiple files in the same directory In order to overlay data files located in a different directory or drive use the Add Data to Overlay command The plot will be automatically scaled to fit the currently active data If both X and Y values fall into the plot scal
33. a Gaussian peak This allows higher resolution and facilitates measurement A diffusive peak can also be converted to a sigmoidal wave to yield a time independent steady state current plateau In polarographic theory current potential semilog analysis can be used to interpret the resulting data This command has a toolbar button The Semiinteg and Semideriv command presents this dialog box Semi derivative and Semi integral OK ee Beem Ste Cancel Semi Integral Help Je Override Present Data Order Selection Both semi derivative and semi integral can be computed Override Present Data Check this box to replace the currently active data with the resulting convoluted data If this box is not checked the convoluted data will only be displayed without overriding the currently active data and invoking the Present Data Plot command will display the original data 2014 CH Instruments Inc DataProc Menu 187 7 5 interpolation command This command opens the Interpolation dialog box Use this command to insert additional data points into the currently active data The Interpolation command presents this dialog box Interpolation J x Data Insertion fz DI IV Override Present Data Cancel Help Data Insertion Density The larger the multiplier the more points will be inserted between the existing data points When the number of data points exceeds the available memory size a warning
34. and between runs e step functions multiple cycles of step function generator for electrode cleaning or other purposes e iR compensation automatic and manual compensation solution resistance double layer Capacitance and stability test e SECM probe control calibration and move probe in three dimensions Graphical Display 2014 CH Instruments Inc General Information present data plot data plot with header filename parameters and results re scaling and labeling axis expression re scaling and text insertion overlay plots plot multiple data sets on the same graph for comparison parallel plots plot multiple data sets side by side for comparison Zoom in visually selected zoom area manual results visually selected baseline peak definition shape width and report options X Y Plot import arbitrary data sets peak parameter plot ip v ip v1 2 Ep log v plots semilog plot current potential semilog plot graph options display 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 of axis labels axis titles header parameters and results copy to clipboard for pasting graphics in third party applications word processors etc 3d plotting NEW interactive visualization of im
35. any channel for parallel or overlay plotting Techniques for Model 1000C Series ___Techniques_ 1000c _ 1010C _ 1020c IT 1030c 1040C Oooo o owo oo oe ee I e o oe IESSE amp Corresponding stripping mode can be performed Specifications 8 channel potentiostat DPV and NPV pulse width 0 001 to 10 sec 8 independent cells or a multi WE cell SWV frequency Potential range all channels 10 V e 1 Hz to 100 kHz sequential scan Applied potential accuracy 1 mV 0 01 of e 1 to 3125 Hz 8 channel simultaneous scan scale ACV frequency Compliance voltage 12 V e 1 to 10000 Hz sequential scan 2014 CH Instruments Inc Current range each channel 10 mA Reference electrode input impedance 10 ohm Sensitivity scale 10 0 001 A V in 7 ranges Minimum current resolution 0 0015 of current range min 0 3 pA Input bias current lt 50 pA Fast waveform update 5 MHz 16 bit Fast data acquisition up to 1 MHz 16 bit CV and LSV scan rate e 0 000001 to 5000 V s sequential scan e 0 000001 to 25 V s 8 channel simultaneous scan e Potential increment during scan 0 1 mV 1 000 V s CA and CC pulse width 0 0001 to 1000 sec CA and CC sample interval e 1e 6 to 50 s sequential step e 8e 5 to 50 s 8 channel simultaneous step 2014 CH Instruments Inc e 1 to 312 Hz 8 channel simultaneous scan SHACV frequency e 1 to 5000 Hz sequential scan e 1 to 250 Hz 8 channel simultaneous scan FTACV
36. as Long Return to Origin 2014 CH Instruments Inc Range 10 10 1 100000 1e 12 0 1 10 0 1 10 1e 12 Description First probe potential Quiescent time before data sampling Probe sensitivity scale Substrate potential Substrate sensitivity scale Check or Uncheck Substrate potential on off Check or Uncheck Substrate electrode imaging on off 50000 50000 0 0001 100 0 002 60 Select 5e 12 1e8 0 01 5 0 0001 10 1 1000000 0 0001 0 7 50000 Probe travel distance in X direction 50000 Probe travel distance in Y direction Probe distance increment during scan Probe time increment Sampling time Amperometry constant height potentiometry constant current or impedance Constant current control value Allowed current tolerance for constant current control Maximum allowed Z step size for current adjustment AC frequency AC amplitude Check or Uncheck Bias DC current during measurement to increase AC gain Check or Uncheck Enable automatic sensitivity scale impedance only Select Select Auto stepper or piezo Specify long move direction Check or Uncheck Move probe back to origin after imaging 104 CH Instruments Model 900D Series Notes A maximum of 512 x 512 pixels per image is allowed If the number of data point in a dimension exceeds 512 its increment distance will be automatically adjusted When E2 On is checked the substrate potential will be turned on
37. but no current will be measured When i2 On is checked the substrate potential will be turned on and current will be measured X Y distance cannot be zero H both X and Y distances are within the X and Y piezo range automatic motor selection will choose the piezo positioner Otherwise the stepper motors will be used If the piezo positioner is selected but the X or Y distance exceeds the piezo range the stepper motors will be used instead To reduce interference from the power line frequency the sampling period via Incr Time should be a multiple of the reciprocal of the line frequency For instance if the line frequency is 60 Hz an Incr Time of 0 01667 0 03333 0 05 0 06667 0 08333 0 1 etc is recommended If the line frequency is 50 Hz an Incr Time divisible by 0 02 is recommended If the line frequency is 50 Hz Incr Time of 0 02s and its multiples are recommended In Constant Current mode negative positive height indicates that the tip has moved upward downward Before the measurement the Z piezo will be set to its middle position and the specified constant current level will be reached with a combination of stepper motor and piezo movements Once the scan starts only the Z piezo will be adjusted to keep the current constant Since the Z piezo has a maximum range of about 80 microns and its start position is at the middle its maximum adjustable range is 40 microns If a Z move exceeds 40 microns a warning will appear and
38. by this command which fully supersedes the Import Text File command When a file is read the program places its data in memory and updates the display technique and experimental parameters some of which are only available in binary data files You can only open files generated by this or an older version of the software Use the Window menu to switch among the multiple open documents See Window 1 2 command You can create new blank documents with the New command This command has a toolbar button The Open command presents this dialog box Open ee Look in Sy chi lo e ES Pe IMPO fs MP1 Ein EJ IMPE1 PALsva ad IMPE2 fd NPVO EJ IMPE3 EJocpTi EJ IMPE4 EJ Psao H File name evo Files of type Binary Data Files bin DI Cancel Binary data files and text files saved from the program can both be read directly by the Open command which fully supersedes the Import Text File command The following options allow you to specify which file to open File name Type or select the name of the file s to be opened The box above lists files with the extension you select in the Files of type box You don t have to type the extension the program will automatically attach the selected extension in the Files of type box to the filename or the default bin if All Files is selected Multiple file names in the File name field are enclosed by quotation marks and 2014 CH Instr
39. checked the Fourier spectrum data will only be displayed without overriding the currently active data and invoking the Present Data Plot command will display the original data 2014 CH Instruments Inc Analysis Menu 197 Chapter 8 Analysis Menu The Analysis menu offers the following commands Calibration Curve Plot a calibration curve Standard Addition Determine concentration by Standard Addition Data File Report Generate report file Time Dependence Plot time dependence of concentration Special Analysis Perform special analysis for select techniques if available 2014 CH Instruments Inc 198 CH Instruments Model 900D Series 8 1 Calibration Curve command This command opens the Calibration Curve dialog box which allows you to specify options for calibration curve calculation and or plotting The Calibration Curve command presents this dialog box Calibration Curve Concentration Peak Height OK Standard 1 ho mem E Standard 2 po 4 782e 007 Standard 3 300 7 023e 007 Slope 22785 005 Bee Standard 4 Im 3 272e 007 Intercept 1 65199e 008 Read Standard 5 Im IS Correlation fossssat Sg Standard 6 zz pooo x Axis Title Concentration x Axis Unit ppb Y Axis Title Peak Current Y Axis Unit a Header Cu in waste water Note M ooo Standard Enter the concentration and peak height current obtained from standard solutions Unknown Enter th
40. closely Release the mouse button to zoom in To zoom back out and exit zoom mode click the Zoom In command or toolbar button again 2014 CH Instruments Inc Graphics Menu 16 6 11 Manual Results command Use this command to report peaks wave potentials currents and area manually You can determine the linear baseline s for a peak or wave graphically This command has a toolbar button To enter manual mode either click on the toolbar button or on its entry in the Graphics menu When manual mode is enabled the menu entry and toolbar button will both be marked Once in manual mode the mouse cursor will appear as an up arrow in the data plot area In order to report a peak or wave correctly you must use the Peak Definition command to define the peak shape as Gaussian diffusive or sigmoidal You can also choose between reporting peak or wave potential half peak or wave potential peak or wave currents and or peak area For a Gaussian peak the baseline is determined by two points straddling the peak Left click at one point drag to the other point and release the left mouse button A vertical line from peak to baseline will appear with corresponding numerical values reported at the right side of the plot For a diffusive peak the baseline is determined by extending the foot before the peak Left click at the foot drag past the peak potential and release the left mouse button A vertical line from peak to ba
41. columns apply to dual channel measurements If you are unsure what settings to choose please select Automatic Potential Filter The grayed out box displays the actual potential filter setting Choose the potential filter cutoff frequency from the list The potential filter is a 2nd order Bessel filter used to shape the waveforms The appropriate setting for 2014 CH Instruments Inc 136 CH Instruments Model 900D Series this filter should take the type and time scale of the experiment into account For instance the Automatic setting will filter out high frequency components to avoid aliasing in AC impedance measurements whereas in linear sweep voltammetry it will convert the staircase ramp to a true linear potential sweep i E Conv Filter The grayed out box displays the actual current to voltage converter filter setting Choose the i E converter filter cutoff frequency from the list The i E converter filter is an RC filter in conjunction with the current to voltage i E converter The appropriate setting for this filter should take the type and time scale of the experiment into account In certain cases some cutoff frequencies cannot be selected This is because for a given sensitivity scale the feedback resistor of i E converter is fixed and when this is combined with the RC filter it may be impossible to reach certain cutoff frequencies For instance a low high sensitivity scale could preclude the selection of a r
42. data exceed the maximum allowed points the data storage interval will be doubled automatically Therefore data points will not overflow for an unexpectedly long 2014 CH Instruments Inc Setup Menu experiment e A large number of segments can be specified but data will only be stored for the first 400 segments Later segments will be displayed during the run but not stored e The current polarity can be switched when either the specified potential or the specified time has been reached The switching time can be different for cathodic and anodic switching Note however that even with Time switching selected if the limiting potential is reached the current polarity will still be reversed in order to protect the electrode 2014 CH Instruments Inc CH Instruments Model 900D Series 4 2 27 Chronopotentiometry with Current Ramp Parameters dialog box In the Chronopotentiometry with Current Ramp technique CPCR a current ramp is applied to the working electrode and potential is recorded as a function of time The following diagram shows the current waveform applied as a function of time Final Current Current A Scan Rate A s Time s Parameter Range Description Init Current A 2 2 Controlled cathodic current Final Current A 2 2 Controlled anodic current Scan Rate A s te 12 0 1 Current scan rate High E Limit V 10 10 High potential limit Low E Limit V 10 10 Low potential limit Data
43. data for the first or second DPA or both use the Graph Option command under the Graphics menu 2014 CH Instruments Inc CH Instruments Model 900D Series 4 2 17 Triple Pulse Amperometry Parameters dialog box In Triple Pulse Amperometry TPA three potential pulses are applied The first two pulses are for electrode conditioning or cleaning Current is sampled at the end of the third potential pulse and recorded as a function of time The third potential pulse can be constant or incremented after each cycle The following diagram shows the potential waveform applied as a function of time and the current sampling scheme Data Sampling kK E1 Potential V Parameter Range Description E1 V 10 10 First pulse potential Duration 1 s 0 32 First pulse duration Open Circuit Check or Uncheck Hold step 1 at open circuit or constant potential E2 V 10 10 Second pulse potential Duration 2 s 0 32 Second pulse duration E3 V 10 10 Third pulse potential Duration 3 s 0 01 32 Third pulse duration Incr E V 0 0 02 Increment potential for third step Init E V 10 10 Initial potential during quiescent time Final E V 10 10 Final potential for scan Number of Cycles 10 100000 Number of Repetitive Cycles Quiet Time sec 0 100000 Quiescent time before taking data Scales During Run 1 2 3 Number of current display scales Sensitivity A V 1e 12 0 1 Sensitivity scale Electrode 2 Potential
44. ee eeeeeeeeeeseeeeeeseeeseeeseeeseeeseeeeeeeaes 200 8 3 Data Report COMMANG cccceeeece cece ee ee eee ee eens KEE RRE KEREN EEEE ERR EEEE RRE nnn ERR EEE mennan REENEN EEN 202 8 4 Time Dependence COMMANGA cccceececeeeeeeeeeeeeeeeeeeeeeeeeeeeeseeeeeeeseeeseeeseeseeeseeeseeeseeeseeeneeeees 205 8 5 Special Analysis COMIMANG ccccceeeeeeeee eee eeeeeeeeeeeeee ee eeeeee ee eeeeeeeeeeseeeeeeseeeseeeseeeseeeseeeeeeeaes 207 Chapter 9 Sim Menu 9 1 9 2 9 3 9 4 Chapter 10 View Menu Mechaniem commande keNdNE EENS KN ENNEN NEEN EE NEEN SEN ENEE ENNER ENNER Tt Digital Simulation dialog DOK T r E a Ea aa a aE aA ra aaae da eae Aaaa 9 1 2 Potentials and Rate Constants dialog DOX cessscseeeeesseeseeeseeseesseesseeseeeseees 9 1 3 Concentration and Diffusion Coefficients dialog box 9 1 4 Surface Concentration dialog DOX sscescsecsseeseesseeeseeseeeseeseeeseessensneneeseeneeeseees 9 1 5 Concentration at Equilibrium dialog box cece seestsseeeseesesseeseeseeseeseeseesoevesseeseeseesoesessessevseeenennens 9 1 6 Simulation Variables dialogi box ixni inn ainiai iaaiaee adei ina aaa aaaea aa aiaa AC Impedance Simulator and Fitting Program sccccceeeeeeeeeeeeeeseeeeeeseeeeeeeeeeeeeeeeeeneeees CV Simulate Got maps ge Eege ENEE SN Ne SERA deeg CV Fitting COMIMANGA cccceeeceeeeeeeeeeeeeeeeeeeeeeeeeeeeeeseeeeeeeseeeeeeeseeeaeeeseeeeenseeeeeenseeeeeeeseeeanees 10 1 Data Information
45. for comparison with other theoretical predictions When this box is not checked current will be calculated according to the concentration electrode area and time scale of the experiment Initial Concentration at the equilibrium When this box is checked the program will first calculate equilibrium concentrations and then use the computed values as the initial conditions for the simulation The equilibrium state is calculated according to the kinetic parameters and input concentrations When this box is unchecked the program uses input concentrations as initial condition Display concentration profile during run When this box is checked the program will display the concentration profile along with the voltammogram during the simulation This is very helpful to understand the reaction mechanism and is ideal for teaching purposes For voltammograms the current axis scale is determined by the sensitivity scale selected under the Parameters command If the current axis scale is too high the voltammogram will appear as a flat line If the current axis scale is too low the data points will be scattered everywhere However the post run data display will always autoscale the voltammogram to maximize readability The sensitivity scale can be adjusted for the next simulation run according to the post run display For concentration profiles relative concentrations and relative distances are used The total concentration of all involved species is
46. frequency simultaneously acquire 1st 2nd 3rd 4th 5th and 6th harmonics data e 0 1 to 50 Hz Sequential scan e 0 1 to 34 Hz 8 channel simultaneous scan Current low pass filters Current analog output Cell control purge stir knock Data length 128K 4096K each channel Dimensions 14 2 W x 9 2 D x 4 7 H ER CH Instruments Model 900D Series 12 14 Model 1100C Series Power Potentiostat Galvanostat The Model 1100C series pow er potentiostat galvanostat is designed for electrochemical applications that require relatively large current and high compliance voltage such as battery studies corrosion electrolysis and electroplating The potential control range is 10 V the current range is 2 A and the compliance voltage is 25 V The instrument contains a high speed digital function generator a fast data acquisition system current signal filters iR compensation circuitry a potentiostat anda galvanostat 1140C only The function generator can update at a 10 MHz rate and the maximum sampling rate is 1 MHz at 16 bit resolution This series is capable of measuring current dow n to tens of picoamperes The 1100C series is capable of measuring current dow n to tens of picoamperes The steady state current of a 10 amp mu m disk electrode can be readily measured without external adapters The instrument provides a very wide dynamic range of experimental time scales For instance the scan rate in cyclic voltammetry can be up to 1000
47. general SECM experiment the probe electrode is scanned across the XY plane and a probe response is recorded and plotted as a function of X and Y to yield an SECM image Typically the image will be generated from the probe electrode response but the substrate electrode response can also be used in amperometry mode The probe and substrate electrode potential and current sensitivity can be controlled independently time and distance increments and the scan distance can also be specified Several measurement modes are available When performed in the Xor Y direction amperometry potentiometry and impedance modes maintain constant probe height Amperometry measure probe current as a function of position Potentiometry measure probe potential as a function of position Constant current measure probe height as a function of position e Height Z will be adjusted automatically to maintain current constant e If the sample or substrate is an insulator the resulting plot yields topographic information e Current value and tolerance must be specified Impedance measure probe impedance as a function of position e AC frequency and amplitude must be specified e In aZdirection scan the impedance will increase sharply when approaching the surface thus allowing a close probe approach without a redox mediator in solution During an SECM experiment the program will display a greyscale or color coded 2 d plot of the XY plane in real time Interact
48. has lowered the priority of the serial port interrupt Other devices such as disk access screen saver virus scan internet connection etc will all generate interrupts that could interfere with the serial port data communication Please disable your screen saver disconnect from the internet disable any virus scanners and try again You should also not use a network card which will generate a background interrupt that interferes with data transfer between the PC and the instrument Disconnect the connector to the network card If you continue to encounter get Link Failed messages after all these efforts please try a different computer Once the instrument and PC can communicate properly you can connect the electrode leads to the rear panel The green clip is for the working electrode white is for reference and red is for counter The black clip is a sensing electrode 2014 CH Instruments Inc 13 CH Instruments Model 900D Series The Cell Control port on the rear panel is used for stepper and motor control when the nanopositioner is used for SECM or other scanning probe techniques This port can also be used to control purge stir and mercury drop dislodge Please see the Appendix for more information If you have a Pine Instrument AFMSRX or AFMSREC Rotator for RDE it is possible for the instrument to control the RDE with the instrument select models Two banana jacks on the rear panel will provide a voltage of 0 10
49. held there and then scanned back The following diagram shows the potential waveform applied as a function of time The logarithm of current is recorded as a function of potential Potential V Parameter Init E V Final E V Incr E V Sweep Segments Scan Rate V s Quiet Time sec Sensitivity A V Auto Sens Notes Final E Hold Time Scan Rate V s Segment 1 Segment 2 Time s Range Description 10 10 Initial potential 10 10 Final potential te 3 0 05 Increment potential of each step 1 2 Sweep segments each segment is half cycle te 6 0 01 Potential scan rate O 100000 Quiescent time before potential scan te 12 0 1 Sensitivity scale Check or Uncheck Automatic sensitivity switching during run e Init E and Final E should be at least 0 01 V apart e Corrosion rate calculations can be performed using the Special Analysis command under the Analysis menu 2014 CH Instruments Inc Setup Menu s 4 2 5 Chronoamperometry Parameters dialog box In Chronoamperometry CA the potential is stepped from Init E to either High E or Low E depending on the Init P N and may then be stepped back The following diagram shows the potential waveform applied as a function of time Current is recorded as a function of time E 5 Pulse Width Pulse Width A 0 Time s Parameter Range Description Init E V 10 10 Initial potential High E V 10 10 Upper limit of pote
50. in Sy chi lo ef ES Pe IMPO fs MP1 Ein EJ IMPE1 PALsvo sd IMPE2 fd NPVO EJ IMPE3 EJocpTi EJ IMPE4 EJ Psao DI Files of type Data Files P br sl Cancel i The following options allow you to specify the name and location of the file you re about to delete permanently File name Type or select the filename s you want to delete permanently You don t have to type the extension the system will automatically attach the selected extension in the Files of type box to the filename The box above lists files with the extension you select in the Files of type box To delete multiple files permanently point the mouse cursor to the files you want to select and click the left mouse button while holding down the Ctrl key You will be prompted for confirmation before the files are deleted permanently Files of type Select the type of file you want to delete permanently 2014 CH Instruments Inc File Menu 35 3 4 Retrieve command Use this command to retrieve data saved on the PC hard drive during an experimental run In case your experiment does not run to completion e g due to external interference interruption or missed communication data can be recovered partially This is useful for very slow experiments hours of experimental data can be recovered For performance reasons this command is not enabled by default For fast experiments it may prove more expedient to simply re run the exper
51. not be entered Click OK in the Digital Simulation dialog box to bring up the CV Fitting Parameter dialog box This dialog box allows you to specify parameters for the CV Fitting program CV Fitting Parameter 4 EI Fitting Potential Range Fit_eh v 0 254 Cancel Fix Fit_elfv 0 1 42 Capacitance uF H D Potentials and Rate Constants Reactions Fix Fix Fix A e B ko fil s P xs es The previously selected reaction mechanism and its associated potentials and rate constants will be shown You do not need to enter kinetic parameters A well chosen initial value may reduce the time needed for fitting although this is not required You can also assign and fix any kinetic parameters whose correct values are known beforehand Checking Fix for any variable will prevent its value from being changed during the fitting process reducing the total number of unknown variables and thus the time needed for fitting The initial values for the fitting potential range is determined automatically from the peak potentials but the positive and negative limits can also be specified manually in the Fit_eh v and Fit_el v fields respectively The fitting procedure will generate a fitted curve over the entire potential range but the goodness of fit will only be measured on the Fitting Potential Range subinterval This is because toward more extreme potentials there tend to be significant contributions from residual or backgr
52. not compatible with the AC Impedance simulator e Toolbar settings are saved locally in your ini file as an alternative to clicking the Reset button simply delete your ini file to restore the default toolbar Beware that manually editing the ini file may result in unexpected behavior 2014 CH Instruments Inc View Menu 235 10 7 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 pressed toolbar button and keyboard latch state A checkmark appears next to the menu item when the status bar is displayed CV The status bar is displayed at the bottom of the program 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 press 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 area of the status bar indicates the currently active technique 2014 CH Instruments Inc Help Menu 237 Chapter 11 Help Menu The Help menu offers the following commands which provide you assistance with this application Help Topics Offers you an index to topics o
53. obtain Click the Fit button on the toolbar to start the fitting process During fitting the elapsed time fitting error and evolution of circuit element parameters will be displayed The fitting process is complete when the component values have converged the resulting values value of circuit elements as well as fitting error will be displayed To stop the fitting process click the Exit button on the toolbar The original and fitted data will be overlaid and displayed To exit the circuit editor and return to the main program click the Exit button Notes Before you run the fitting program make sure the instrument is correctly connected to your PC e g by running the Self Test command The program will verify that your instrument model is supported This check only needs to be performed once after the program is started After the first fit you do not need to have the instrument connected anymore When carrying out impedance simulation and fitting do not run other techniques or read data files other than impedance measurements Otherwise the circuit editor may not function correctly Circuit Element Notation and Ranges Circuit Element Abbrev Units Range Resistor R Ohm 0 001 to 1e12 Capacitor C Farad te 12 to 1 Inductor L Henry 1e 12 to 1 Warburg Impedance W Siemens sec 1e 6 to 1 Constant Phase Q Siemens sech 1e 12 to 1000 Cole Cole CC Ohm 0 001 to 1e12 Cole Davidson CD Ohm 0 001 to 1e12 Finite Layer Diffusion FD Siemen
54. of Cycles 10 100000 Number of Repetitive Cycles Quiet Time s O 100000 Quiescent time before potential pulses begin Scales During Run 1 2 3 Number of current display scales Sensitivity A V 1e 12 0 1 Sensitivity scale Notes e The experimental sequence consists of the first DPA cleaning a first pulse and a second pulse followed by a second DPA cleaning a third pulse and a fourth pulse This sequence is repeated until 2014 CH Instruments Inc Setup Menu the total number of cycles is reached or the experiment is interrupted by the user There is no data acquisition during the cleaning steps if the cleaning time is zero the cleaning step will be ignored Data are sampled for first and second pulses and the difference is reported Data sampling occurs during the second half period of pulses 1 and 2 The longer the pulse width the longer the sample interval will be resulting in better signal averaging and less noise During an 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 unexpectedly long experiment When only 1 current scale is displayed during a run the data will be automatically scaled to fit When 2 current scales are displayed during a run they will be 1 100 and 1 10 of full scale When 3 current scales are displayed they will be 1 100 1 10 and 1 1 of full scale To specify options to display
55. on Printer 270 degree e To change the font style size or color of the text click the Change button to the right of the corresponding item The Y axis title should read from bottom to top However different printers have been found to follow different character rotation conventions so you may have to adjust the rotation angle to obtain the correct orientation for your printer Pressing the Default button will reset all font settings to the program defaults 2014 CH Instruments Inc Graphics Menu 179 6 20 Copy to clipboard command Use this command to copy the currently displayed plot to the clipboard You can then paste it into a word processor or any other Windows based program This command will work during a run or a digital simulation Alternatively use the Alt PrtScn system keyboard shortcut This command has a toolbar button 2014 CH Instruments Inc DataProc Menu is Chapter 7 DataProc Menu The DataProc menu offers the following commands Smoothing Smooth data by least squares or bandwidth filtering Derivatives Compute numerical derivatives of data up to 5th order Integration Integrate data numerically Semiinteg and Semideriv Take semi integral or semi derivative Interpolation Insert interpolated data points Baseline Fitting amp Subtract Fit and subtract a polynomial baseline from data Linear Baseline Correction Correct baseline visually Data Point Removing Remove data po
56. or higher It is easy to install and use The user interface uses the classic Microsoft design so if you are familiar with Windows applications you can likely use the software without referring at all to this user manual or the comprehensive context sensitive help files that are included with the instrument software The commands parameters and options have been written using terminology that most chemists are familiar with A customizable toolbar allows quick access to the most commonly used commands The instrument provides many powerful functions such as straightforward file handling extensive experimental control flexible graphics various data analyses and efficient digital simulation Additional features include macro commands working electrode conditioning color legend and font selection data interpolation visual baseline correction data point removal visual data point modification signal averaging Fourier spectrum and a convenient technique specific electrochemical equation viewer This model series includes a USB port default and a serial port for data communication with the PC with hot switching capabilities available on the rear panel of the instrument Firmware is now stored in flash memory and as a result instrument firmware upgrades can be downloaded electronically and installed immediately instead of the inconvenient shipment and installation of EPROM chips 1 A J Bard F R F Fan J Kwak and O Lev Anal
57. s Parameter Range Description Init E V 10 10 Initial potential Final E V 10 10 Final potential Incr E V 0 001 0 02 Increment potential of each step Rot Rate rpm O 10000 Center rotation rate Modul Freq Hz 1 5 Modulation frequency Modul Amp rpm 0 3600 Modulation amplitude see Notes or Equations Quiet Time s O 100000 Quiescent time before potential pulses begin Sensitivity A V 1e 12 0 1 Sensitivity scale Notes e Init E and Final E should be at least 0 01 V apart e The actual rotation rate in hydrodynamic modulation is given by A sin t e The modulation function is a periodic waveform with modulation frequency but more complicated than a sine wave The rotation rate oscillates about rotation rate but the amplitude of this oscillation is not symmetric The input parameter A modulation frequency is not really the amplitude but the square of A in the equation above 2014 CH Instruments Inc so CH Instruments Model 900D Series 4 2 21 Sweep Step Function Parameters dialog box In the Sweep Step Functions technique SSF the instrument alternates between six potential sweeps and six potential steps somewhat like an arbitrary waveform generator The following diagram shows the potential waveform applied as a function of time One can skip any segment by setting parameters sufficiently small allowing enhanced flexibility for waveform control Current is recorded as a fu
58. sampling rate exceeds 3 KHz data will be be displayed at the end of the experiment instead of in real time The total measurement time in seconds is equal to the total number of points points per sine wave frequency The potential scan rate in turn is equal to the specified potential range divided by the total measurement time The absolute AC current DC current first second third and fourth harmonic components and the complete response spectrum can be plotted using the Graph Option command under the Graphics menu 2014 CH Instruments Inc CH Instruments Model 900D Series 4 2 14 Amperometric i t Curve dialog box In the Amperometric i t Curve technique i t a constant potential is applied and current is recorded as a function of time The following diagram shows the potential waveform applied as a function of time and the current sampling scheme Sample Interval Init E Potential V Time s Parameter Range Description Init E V 10 10 Initial potential Sample Interval s 1e 6 50 Data sampling interval Run Time s 0 001 500000 Total measurement time Quiet Time s O 100000 Quiescent time before potential step Scales During Run 1 2 3 Number of current display scales Sensitivity A V 1e 12 0 1 Sensitivity scale Aux Signal Rec Check or Uncheck Record external signal when sample interval gt 0 005 s Electrode 2 Potential V 10 10 Second working electrode potential Sensitivity A V
59. selected in the Electrochemical Techniques dialog box This command has a toolbar button The following parameter dialog boxes available for your instrument series are listed below For details about each technique please refer to the description of each dialog box Parameters for Cyclic Voltammetr Parameters for Linear Sweep Voltammetr Parameters for Staircase Voltammetr 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 FT 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 Coulometry 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 fo
60. the File menu The Data List command presents this dialog box Aug 10 1994 14 11 32 Cyclic Yoltammetry File cv1 bin Data Source Experiment Instrument Model CHIO Data Proc Smoothing Header 0 5 mM Ferrocene in 0 1M LiCIO4 CH3CN 2mm Pt disk Note Init E V 0 1 Scan Rate V s 10 Segment 2 Sample Interval Vv 0 001 Quiet Time sec 2 Sensitivity A V 1e 4 Potential Current A This dialog box lists the experimental conditions results and numerical values of the currently active data with scroll bars if necessary If the list is too long the later part of the data will be truncated 2014 CH Instruments Inc View Menu 231 10 3 Equations command This command opens the help browser to view equations related to the electrochemical technique currently invoked The following is a list of available equations 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 1st ed 2001 2nd ed Equations General equations Symbols and Units Linear Sweep Voltammetry LSV and Cyclic Voltammetry CV Staircase Voltammetry SCV Tafel Plot TAFEL Chronoamperometry CA Chronocoulometry CC Differential Pulse Voltammetry DPV Normal Pulse Voltammetry NPV Square Wave Voltammetry SWV AC Voltammetry ACV Second Harmonic A C Voltammetry GSHACV Amperometric Curve i t Bulk Electrolysis with Co
61. the rotator on during quiet time This option can also be found in the Run Status command under the Control menu Rotate during Run Check this box to turn the rotator on during the experiment This option can also be found in the Run Status command under the Control menu Rotate between Runs Check this item to turn the rotator on between experiments This option can also be found in the Run Status command under the Control menu 2014 CH Instruments Inc Control Menu 1 5 18 Other command This command opens the Other Controls dialog box Use this command to control the cooling fan and working electrode static discharge protection The Other command presents this dialog box Other Controls xi m Fan Control OK I Fan On between Runs WE Static Discharge Protection Dff at High Sensitivity C OnAll Times Fan Control The instrument as all electronics will generate heat Most components consume minimal power but the voltage regulators buffer amplifiers and some other amplifiers may grow warm particularly when higher currents are passing through the cell Turning the fan on will help help to dissipate this heat and cool the instrument However the fan will also generate mechanical noise and electrical interference When current sensitivity is set to 0 01 A V or lower or if automatic sensitivity is employed the fan will be turned on automatically Check the appropriate box to turn the f
62. the scan will be terminated At the end of a scan in Constant Current mode the Z piezo will be moved back to its zero position 2014 CH Instruments Inc Setup Menu 10 4 3 System command This command opens the System Setup dialog box Use this command to set up the serial communication port current polarity potential axis and current axis You can choose any convention for the potential and current axis The System command presents this dialog box System Setup r Communication Port C Coml Line Frequency Cancel GC Gen eee Lei Com 3 C 50Hz Help C Com4 E Comp E rm Potential Axis C Comp C Com Positive Left e Ca C Postve Righi C Com C Com11 Ze Positive Up Com 12 Positive Down Com Port Speed j e Cumert Pi Se Erase ADC Calibration Coefficients e Standard Cathodic Positive C Fast C Anodic Posi Data Length 128K D I Save retrieve data during run m Windows E Present Data Override Warning dek Siena I Save Text File As Well The following options allow you to set up your system Communication Port Select the PC communication port to which the instrument is linked This setting is required to establish communication between your PC and your instrument If it is not set correctly you will not be able to control your instrument Available ports should be listed in the Windows Device Manager If you are using the Automatic
63. user defined mechanisms e Impedance simulation and fitting program SECM Image i A 2014 CH Instruments Inc Other Techniques Amperometric Lt Curve i t Differential Pulse Amperometry DPA Double Differential Pulse Amperometry DDPA Triple Pulse Amperometry TPA Integrated Pulse Amperometric Detection IPAD Bulk Hectrolysis w ith Coulometry BE Hydrodynamic Modulation Voltammetry HMV Sw eep Step Functions SSF Multi Potential Steps STEP Electrochemical Noise Measurement ECN Open Circuit Potential Time OCPT Various Stripping Voltammetry Potentiometry Experimental Parameters CV LSV scan rate 0 000001 to 10 000 V s two channels simultaneously Potential increment during scan 0 1 mV 1 000 V s CA and CC pulse w idth 0 0001 to 1000 sec e CA minimum sample interval 1 us both channels e CC minimum sample interval 1 us e True integrator for CC DPV and NPV pulse w idth 0 001 to 10 sec SWV frequency 1 Hz to 100 kHz e i t sample interval minimum 1 us both channel e ACV frequency 0 1 Hz to 10 kHz e SHACV frequency 0 1 Hz to 5 kHz e FTACV frequency 0 1 to 50 Hz simultaneous acquire 1st 2nd 3rd 4th 5th and 6th harmonics ACV data e IMP frequency 0 00001 Hz to 1 MHz IMP amplitude 0 00001 V to 0 7 V RMS Probe Approach Curve Distance um 20 CH Instruments Model 900D Series 12 13 Model 1000C Series Multi Potentiostat The model 1000C series instrument is a co
64. waveform is superimposed Current is sampled when the AC signal is applied and e second harmonic component is analyzed using a software lock in amplifier During the experiment only the absolute second harmonic AC current is displayed After the experiment the phase selective second harmonic current at any phase angle will also be available for display The following diagram shows the potential waveform applied as a function of time Incr E TT Final E Amplitude xX Potential V Init E J k Sample Period Time s Parameter Range Description Init E V 10 10 Initial potential Final E V 10 10 Final potential Incr E V 0 001 0 05 Increment potential of each pulse Amplitude V 0 001 0 5 AC amplitude Frequency Hz 0 1 10000 AC frequency Sample Period s 0 1 50 Data sampling period or dropping time Quiet Time s O 100000 Quiescent time before potential pulses begin Sensitivity A V 1e 12 0 1 Sensitivity scale Bias DC Current off range on Enable DC current bias during run Auto Sens Check or Uncheck Automatic sensitivity switching during run Notes e Init E and Final E should be at least 0 01 V apart e Depending on the frequency range it may not be possible to generate the requested AC frequency in this case the closest available frequency will be applied When the AC frequency is 2 Hz or lower the Sample Period parameter should be at least 2 seconds if not the system will automatic
65. will be given and the command will terminate The multiplier can only be a power of 2 Fourier transform is used in this case Override Present Data Check this box to replace the currently active data with the resulting interpolated data If this box is not checked the interpolated data will only be displayed without overriding the currently active data and invoking the Present Data Plot command will display the original data 2014 CH Instruments Inc CH Instruments Model 900D Series 7 6 Baseline Fitting amp Subtraction command This command opens the Baseline Fitting amp Subtraction dialog box 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 both sides of the peak base the algorithm and the order of fit Baseline Fitting and Subtraction only works for certain peaks and experimental techniques If more than one segment of data is available such as CV data you can choose the segment to operate on with the Graph Option command under the Graphics menu This command has a toolbar button GI The Baseline Fitting amp Subtraction command presents this dialog box Baseline Fitting amp Subtraction m Two Sides of Peak Foot From To jo c i From fo To jo SC From fo To o E e From fo To fo View Baseline From Io To fo V
66. 0 2014 CH Instruments Inc General Information 1 Chapter 1 General Information This chapter contains general information about your instrument Introduction Electrochemical Techniques Software Features System Requirements Hardware Specifications 2014 CH Instruments Inc 2 CH Instruments Model 900D Series 1 1 Introduction The scanning electrochemical microscope SECM was introduced in 1989 as an instrument that could examine chemistry at high resolution near interfaces By detecting reactions that occur at a small electrode the tip as it is scanned in close proximity to a surface the SECM can be employed to obtain chemical reactivity images of surfaces and to make 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 interfaces The trapping and electrochemical detection of single molecules by SECM has also been reported The model 900D 920D Scanning Electrochemical Microscope consists of a digital function generator bipotentiostat high resolution data acquisition circuitry three dimensional nanopositioner positioner controller and a sample cell holder as shown in the Figure below The three dimensional nanopositioner has a spatial resolut
67. 0 Initial potential Final E V 10 10 Final potential Incr E V 0 001 0 05 Increment potential of each pulse Amplitude V 0 001 0 5 AC amplitude Frequency Hz 0 1 5000 AC frequency Sample Period s 0 1 50 Data sampling period or dropping time Quiet Time s O 100000 Quiescent time before potential pulses begin Sensitivity A V 1e 12 0 1 Sensitivity scale Bias DC Current off range on Enable DC current bias during run Auto Sens Check or Uncheck Automatic sensitivity switching during run Notes e Init E and Final E should be at least 0 01 V apart e Depending on the frequency range it may not be possible to generate the requested AC frequency in this case the closest available frequency will be applied When the AC frequency is 2 Hz or lower the Sample Period parameter should be at least 2 seconds if not the system will automatically readjust the Sample Period Both absolute current and phase selective current are available Use the Graph Option command under the Graphics menu to specify data display options e When DC current is high and AC current is low sensitivity cannot be increased because the DC current will overflow This problem is more serious when the frequency is relatively low The application of a DC current bias allows higher AC signal amplification A 16 bit DAC is used for this purpose On the other hand if the DC current is not expected to be large and the frequency is high a DC current bias may b
68. 0 V selected models CV simulation and fitting program Cell control purge stir knock Data length 128K 4096K selectable Chassis dimensions 14 25 W x 9 25 D x 4 75 H Oscillator box external 4 75 L x 2 6 W x 1 55 H Weight 12 Ib 2014 CH Instruments Inc Appendix 253 Techniques for Model 400C Series 00C 450C Linear Sw eep Voltammetry LSV amp Staircase Voltammetry SCV amp Tafel Plot TAFEL Chronoamperometry CA Chronocoulometry CC Differential Pulse Voltammetry DPV 8 Normal Pulse Voltammetry NPV Ht is 2nd Harmonic AC Voltammetry SHACV 8 Amperometric Lt Curve Differential Pulse Amperometry DPA Square Wave Voltammetry SWV Double Differential Pulse Amperometry DDPA AC Voltammetry ACV 283 Wi Triple Pulse Amperometry TPA Hydrodynamic Modulation Voltammetry HMV Differential Normal Pulse Voltammetry DNPV amp Impedance Time IMPT Impedance Potential IMPE amp Sw eep Step Functions SSF Chronopotentiometry w ith Current Ramp CPCR ions Multi Potential Steps STEP AC Impedance IMP Cc Potentiometric Stripping Analysis PS Open Circuit Potential Time OCPT Quartz Crystal Microbalance QCM Ee Impedance simulation and fitting program iR Compensation Corresponding polarographic mode can be performed amp Corresponding stripping mode can be performed Phase selective data are available
69. 0000 Probe travel Incr Dist um 0 001 100 Probe increment distance during scan Incr Time s 0 002 60 Increment or sampling time Quiet Time s O 100000 Quiescent time before probe move Notes When E2 On is checked the substrate potential will be turned on but no current will be measured When i2 On is checked the substrate potential will be turned on and current will be measured The probe can be stopped either manually or at an absolute current level depending on the selection made in the Probe Stop at Current Level area The travel distance cannot be set to zero The options in the Probe E Pulse before Sampling area can be used for electrode cleaning purposes during an experiment If E1 Pulse On is unchecked this feature will be ignored If both X and Y distances are within the X and Y piezo range automatic motor selection will choose the piezo positioner Otherwise the stepper motors will be used If the piezo positioner is selected but the X or Y distance exceeds the piezo range the stepper motors will be used instead To reduce interference from the power line frequency the sampling period via Incr Time should be a multiple of the reciprocal of the line frequency For instance if the line frequency is 60 Hz an Incr Time of 0 01667 0 03333 0 05 0 06667 0 08333 0 1 etc is recommended If the line frequency is 50 Hz an Incr Time divisible by 0 02 is recommended In Constant Current mode negative positive heig
70. 2014 CH Instruments Inc CH Instruments Model 900D Series Use this command to generate the data file report 2014 CH Instruments Inc Analysis Menu 205 8 4 Time Dependence command This command opens the Time Dependence dialog box Use this command to generate a report or plot for the time dependence of peak heights or concentrations from stored data files The program will search for peak height or concentration in each data file sorted in chronological order relative to the earliest experiment The Time Dependence command presents this dialog box LT x EpFrom v foz OK Ep To ME us Cancel Slope 22739 Help Intercept 1 65268 Peak Shape Gausian zl Report Data fue Read Save Data Type Original DI Cone C Current Report Name Joel Bt Report PAPE Y Axis Title Concentration Y Axis Unit ppb Plot Header Waste Water Batch 16 Note The following options allow you to specify peak potential windows slope intercept of calibration curves and select the data files whose time dependence is to be reported or plotted 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 Ranges should not overlap for different species Slope Enter the slope of the calibration curve for each species to calculate the concentration of the compound A value must be specified fo
71. 4 2 8 Normal Pulse Voltam metry Parameters dialog DOX n snnnnnnsunnnnnunnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnennnnnnnnnnnenn nna 64 4 2 9 Differential Normal Pulse Voltam metry dialog DOX n n nnnnnnunnnnnsunnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnenn nna 65 4 2 10 Square Wave Voltam metry Parameters dialog DOX s nnnnnsunnnnnsnnnnnnrnnnnnnnnnnnnnnnnnnnnnnnnnennnnnnnnnnnnnn nna 66 4 2 11 AC Voltam metry Parameters dialog DOX s s nnnsnsnnnnnunnnnnnurunnnnnnnnnnnnnnnnnnnnnnnnnnnnnennnnnnnnnnnnnennnnnnnnn aneneen 67 4 2 12 2nd Harmonic AC Voltam metry Parameters dialog DOX s s nnnnnnunnnnnnnnnnnunnnnnnnnnnnnnnrnnnnnnnnnnnnnnnnnnnnna 68 4 2 13 FT AC Voltam metry Parameters dialog box 69 4 2 14 Amperometric i t Curve dialog DOX s s snnsusnnnnnnsnnnnnnrnnnnnnrnnnnnnnnnnnnnnnnnnrnnennnnnnnnnnnnnnnnnnnnnnennnnnnnnn nennen 70 4 2 15 Differential Pulse Amperometry Parameters dialog DOX s n nnnsnnnnnnnnnnnnusnnnnnnrnnnnnnrnnnnennnnnnnnnnnenn nna 71 4 2 16 Double Differential Pulse Amperometry dialog DOX s nnnnnsunnnnnrununnnrnnnnnunnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnenn nna 72 4 2 17 Triple Pulse Amperometry Parameters dialog DOX s n nsnsnnnnnnsnnnnnnnnnnnnnnnnnnnnnnnnnnnrnnnnennnnnnennnnenn nna 74 4 2 18 Integrated Pulsed Amperometric Detection Parameters dialog DOX ssussussunnurnnnnnrenrennnnnnnnnnnen 76 4 2 19 Bulk Electrolysis with Coulometry Parameters dialog DOX s nsnsnnnnnnsnnnnnunnnnnnnrnnnnnnrnnnnn
72. 900D Series Click the Change button to specify the style size color and font of the inserted text This setting will be applied to all text inserted in the current plot Text Display Enabled Uncheck this option to hide all text messages the messages will not be deleted Default Set the current font as the default for all data files Monochrome Set the text color to black Depending on the active technique data can be displayed in various formats Tech Data Display Formats CV sweep segment TAFEL log current potential current potential current density potential CA i t i EN t12 CC Q t Q SN t 2 SWV 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 ACV absolute current phase selective current resistance capacitance PSACV absolute current phase selective current resistance capacitance BE charge time current time current log time IMP Bode log Z log freq Bode phase log freq Bode log Z amp Z log freq Bode log Y log freq Nyquist Z Z Admittance Y Y Warburg Z amp Z wi Z wZ Z Z w 2014 CH Instruments Inc Graphics Menu 155 cot phase wl IMP t IMP E log Z torE phase t or E Z torE Z torE Z torE Z amp Z torE log Z amp Z torE logY torE Y torE Y torE Y torE
73. COMMANG ccceeee cece ee ence ee ee ee ee ee eee ence ee eeee ee eeee REENEN EEN EEN 228 10 2 Data Listing Gommand euEEENNEEEEEENE EEN EEEE ENEE SENGES ENEE SSES runan KENS 230 10 3 Equations command xisi rieien annain ENNAN EN area EEANN EN EEA ANKEA REAA EANNA EEA KUNNEN 231 E DW e ee eu E Le DEET 232 10 5 Toolbar COMMA 22 scx sco0 ccece edanen oneei nee Tapae SEEEE dE eaa aiaiai 233 10 6 Add or Remove Buttons COMMANGA cccceeceee ence eee cence EEN ENEE REENEN EEN EEN 234 10 7 Status Bar Commands ege kee ee ENEE ENNEN ENEE SEENEN EENS 235 Chapter 11 Help Menu 237 11 1 Help Topics Comma nd ii scccccsccceccete cect cccseatec eeeccatece st ccceccendcceensencecestcccuauewdcceusteceteeerecs 238 11 2 Old Help Comma nde ee EES 239 11 3 About cM MANO ice aes cas cece edecaa thee daeseeeee ca eege Eed deeg 240 Chapter 12 Appendix 241 12 1 Cables and Connections 20ccccseceeeee cee ee cee cece ee eeceeeeeaaeeceeeeeeeseeeaa sees dama tana aidien aineid 242 12 2 Firmware Update INStructions cccccceeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeseaeeeeseeeseeeseeeneeeees 244 12 3 Trouble Shooting orainn a e the ects este ance cee Dee eats ede cde ceae ee ceetebeet cde ieee tet tds 245 2014 CH Instruments Inc Contents 12 4 Maintenance and Service secececceeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeseeeeeeeseeeeeeaseeeeeeeeeseeeeeeeseeeneeeses 246 12 5 Limited Watantin nina eana aE ERE OE
74. 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 2014 CH Instruments Inc 4 CH Instruments Model 900D Series 1 2 Electrochemical Techniques Scanning Probe Techniques e SECM Imaging constant height constant current potentiometric e Probe Approach Curves e Probe Scan Curve amperometric constant current potentiometric e Surface Patterned Conditioning Sweep Techniques e Cyclic Voltammetry e Linear Sweep Voltammetry e Rotating Disk Electrode Voltammetry e Tafel Plot e Sweep Step 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 Sweep Step 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 Stri
75. Determine the COM number for the newly installed CP2101 USB to UART Bridge Controller or similarly named device In the figure above this is COM5 8 Assign this COM number using the System command under the Setup menu in our software 9 Run the Hardware Test command under the Setup menu to confirm that the instrument and computer are communicating properly This completes instrument installation Part 3 Additional Information In the future if you encounter the Can not open com port message when starting the program please check Device Manager again and see what com port number is currently assigned to the instrument If the com port number assignment has changed you need to set the com port number using the System command accordingly If you do not see the CP2101 device listed in under Ports COM amp LPT please make sure your instrument is turned on and the USB cable is properly connected The USB driver needs to be installed only once on your computer Multiple instruments can be connected to the same computer and Windows automatically assign them to different COM ports USB communication is achieved using a USB serial port converter chip inside the instrument Our software will behave as if this device is connected to a serial port even though the physical connection is by USB Thus you need to use Device Manager as described above to determine what serial port number is assigned to this device You can double click o
76. E EE EE ENEE 247 12 6 Sate ty ii i a eaaa apa a ta ted an Ea SSES EENS ENEE EN 248 12 7 Abbreviations of Electrochemical Techniques ccccceeeeceeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeseeeeeeeees 251 12 8 Model 400C Series Time Resolved Electrochemical Quartz Crystal Microbalance 252 12 9 Model 600E Series Electrochemical Analyzer Techniques ccccsseceeeeeeeeeeeeeeeeeeeeeeeeeees 255 12 10 Model 700E Series Bipotentiostat TeChniques ccceessececneeeeeeeeeeeeeeeeeseeeeneeeeeeeeenseeeanees 256 12 11 Model 800D Series Electrochemical Detector Techniques sssccceeeeeeeeeeeseeeeeeeneenenees 257 12 12 Model 920D Scanning Electrochemical MicroSCope cccsesceceeeeeeeeeeeeeeeeeeeeeeeeeeeneeenenees 258 12 13 Model 1000C Series Multi Potentiostat cccceeeeseeeeeeeeeeeeeeeeeeeeeeeseeeeeeseeeeeeeseeeeeeeneeeeeees 260 12 14 Model 1100C Series Power Potentiostat Galvanostal cccccceeeeseeeeeeeeeeeeeeeeeeeeeeeeeeeeees 262 12 15 Model 1200B Series Handheld Potentiostat Bipotentiostat ccceesseeeeeeeeeeeeeeeeeeeeeees 264 12 16 Model 1550A Pico Liter Solution DiSpenset 0s cccceeeeseeeeeeeeeeeeeeeseeeeeeseeeeeeeseeeeeeeneeeeeees 265 12 17 Picoamp Booster Faraday Cage and MultiplexXer ccccceesseeeeeeeeeeeeeeeeeeeeeeeeeeeeeeseeneeees 267 12 18 Amp Booster and Liquid Liquid Interface Adaptel cceeesseceeeeeseeeeeeseeeeeeeseeeenenneeneeees 269 12 19 WE 27
77. Figure Micropositioner and sample stand System requirements Operating System Windows 95 98 NT Me 2000 XP Vista 7 8 Communication between PC and instrument USB or RS 232 serial port Hardware Specifications Micropositioner Jetting Device Three high resolution stepper motors Nozzle 60 microns e Maximum range of motion 50 mm Droplet size 100 200 picoliters e Motor resolution 8 nm Control voltage 0 150 V e Stall Load 50 N Protective holder e Maximum Speed 4 mm sec Three translation stages e Maximum range of motion 25 mm e Angular deviation lt 200 microrad e Load capacity 156 N e Load capacity vertical 67 N 2014 CH Instruments Inc 12 17 Picoamp Booster Faraday Cage and Multiplexer CHI200 B Picoamp Booster and Faraday Cage With the CHI200 B Picoamp Booster and Faraday Cage current down to a few picoamperes can be readily measured The CHI200 is compatible with the model 600 A 700 A series of instruments while the CHI200B is compatible with the model 600B C D E and 700B C D E series When used with the 700 A B C D E series bipotentiostat the Picoamp Booster will affect only the primary channel The internal sensitivity of the 600E series is the same as the Picoamp Booster 101 A V However the bias current of the 600E series input can be as high as 50 pA The Picoamp Booster has a lower bias current and it also brings the preamplifier close to the electrode resulting in lower noise
78. 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 Hectroanalytical Chemistry A J Bard Ed Marcel Dekker New York 1994 Vol 18 pp 243 373 Model 900D 920D SECM Specifications Nanopositioner X Y Z resolution 1 6 nm with Piezo positioner closed loop control 8 nmwith stepper motor positioner X Y Z total distance 50 mm Potentiostat Biptentiostat Zero resistance ammeter 2 or 3 or 4 electrode configuration Floating isolated from earth or earth ground Maximum potential 10 V for both channels Maximum current 250 mA continuous sum of two current channels 350 mA peak Compliance Voltage 13 V Potentiostat rise time lt 1 ms 0 8 ms typical Potentiostat bandw idth 3 dB 1 MHz Applied potential ranges V 0 01 0 05 0 1 0 65 3 276 6 553 10 Applied potential resolution 0 0015 of potential range Applied potential accuracy 1 mV 0 01 of scale Applied potential noise lt 10 mV rms Measured current range 10 pA to 0 25 A in 12 ranges Measured current resolution 0 0015 of current range minimum 0 3 fA Current measurement accuracy 0 2 if current range gt 1e 6 A V 1 otherwise Input bias current lt 20 pA Galvanostat Galvanostat applied current range 3 nA 250 mA Applied current accuracy 20 pA 0 2 if gt 3e 7 A 1 otherw ise Applied current resolution 0 03 of applied current ra
79. MMANGA cccceeeeceeeee ence eeee eee eeee ee eeeeee en eeeeee ae eeeeeeseeeseaeseeaeeeseeeeeeeseeeeeeeseeeseees 123 Macro Command COMMANGA cccceeeeceeeee eee eeeeeeeeeeeeeeeeeeeeeeeeeeeeseeeeeaeseeeeeeseeeaeaaseeeeeenseeeseens 125 Open Circuit Potential COMMANGA cecceeeeeeeeeeeeeeeeeeeeeseeeeeeeeeeeeneeseeeeeeseeeeneeseeeeeeneeeeeeees 132 IR Compensation COMMANA cccceececeeeeeeeeeeee ee eeeeee ee eeeeee se RRER EE ERER EEN ERER EE nnmnnn nnnm mnnn 133 Filter Setting COMMANG eecececeeeeeeeeeee eee eeee ee eeeeee ee RRE EEERER EE ERER EEN ERER mennun nnmnnn nnmnnn 135 2014 CH Instruments Inc Contents In 5 14 Cell commanda seeesgeeieeeEEeEAEERduEAAE ENEE EENS a ENEE RAAS Enana A RANEE RAISA SRTA 137 5 15 Step Functions COMMANGA ccceeeeceeeee eee eeeeeeeeeeeeeeeeeeeeeeseeeeeeeseeeaeeseeeeeeseeeaeeeseeeeeeeneessnees 140 5 16 Preconditioning COMMANGA c ceeeceeeeeeeeeeeeeeeeeeeeeneeeeeeeeseeeeeeeseeeeeeeseeeeeeseeeeeeeseeeeeeeseeseeees 142 5 17 Rotating Disk Electrode COMMANGA c ccceeeeseeeeeeeeeeeeeeeseeeenenseeeeneneeeeeeseeeeeeeseeeeneeseenenees 144 5 19 Other command D 145 5 19 Stripping Mode COMMANGA cccceeeseeeeeeeeeeeeeeeeeeeeeeeeeeeeeeseeeeeeeseeeeeeeseeaeeeseeeeeeeseeeeeeeseeseeens 146 5 20 SECM Probe commMand s sssssssssnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnn mennun nennum nnna 148 Chapter 6 Graphics Menu 151 6 1 Present Data Plot command
80. Model 900D Series Scanning Electrochemical Microscope User Manual HICH Instruments CH Instruments Model 900D Series User Manual 2014 CH Instruments Inc All rights reserved No parts of this work may be reproduced in any form or by any means graphic electronic or mechanical including photocopying recording taping or information storage and retrieval systems without the written permission of the publisher Products that are referred to in this document may be either trademarks and or registered trademarks of the respective owners The publisher and the author make no claim to these trademarks While every precaution has been taken in the preparation of this document the publisher and the author assume no responsibility for errors or omissions or for damages resulting from the use of information contained in this document or from the use of programs and source code that may accompany it In no event shall the publisher and the author be liable for any loss of profit or any other commercial damage caused or alleged to have been caused directly or indirectly by this document Printed August 2014 in Austin Texas Contents i Table of Contents Chapter 1 General Information 1 Ved Introduction ransana eeaeee ara ain aia aeae aaae aaae aeaaea aaaea anacan iaaea Anana 2 1 2 Electrochemical Techniques cccescecceeeeseeeeeeeeeeeeeeeseeeeeeseeeeeeeseeeeeeeseeeeeeeseeeanenseeeeeeneeeaeees 4 1 3 Software T A E S
81. O ring seal betw een the bottom and center pieces w ith the quartz crystal sandw iched betw een them The diameter of the quartz crystal is 13 7 mm The gold electrode diameter is 5 1 mm Specifications Potentiostat Galvanostat Model 440C 2 3 or 4 electrode configuration Potential range 10 to 10 V Applied potential accuracy 1 mV 0 02 of scale Potentiostat rise time lt 2 us Compliance voltage 12 V Maximum current 250 mA continuous 350 mA peak Reference electrode input impedance 10 12 ohm Sensitivity scale 10 12 0 1 A V in 12 ranges Input bias current lt 50 pA Current resolution 0 0015 of current range min 0 3 fA Minimum potential increment in CV 100 pV Fast w aveform update 10 MHz 16 bit Data acquisition 16 bit 1 MHz External signal recording channel QCM Frequency resolution lt 0 1 Hz QCM maximum sampling rate 1 kHz Automatic and manual iR compensation CV and LSV scan rate 0 000001 to 5000 V s Potential increment during scan 0 1 mV 1000 V s CA and CC pulse width 0 0001 to 1000 sec CA and CC minimum sample interval 1 us CA and CC Steps 320 DPV and NPV pulse width 0 0001 to 10 sec SWV frequency 1 Hz to 100 kHz i t sample interval minimum 1 us ACV frequency 0 1 Hz to 10 kHz SHACV frequency 0 1 Hz to 5 kHz IMP frequency 0 00001 Hz to 10 kHz Low pass signal filters automatic and manual setting Potential and current analog output RDE rotation control output 0 1
82. Probe command This command opens the SECM Probe Control dialog box Use this command to control the SECM probe position You can calibrate the probe movement distance or move the probe directly Current and distances in absolute and relative coordinates will be displayed The SECM Probe command presents this dialog box SECM Probe Control x m Stage Home and Reset r Stepper Stage Position Set and Relocate Le Position 1 Position 2 Position 3 Position 4 Bs BY Be Oe Cancel a X 124999 936 20661 403 0 000 jo 000 _ Cancel Reset y Jo o00 Risen Hep Z 424999 936 9868 051 0 000 fo 000 Stepper Stage Moving Speed um sec pe 7 dg Set Set Set Set Scan Piezo 200 I Max Speed Goto Goto Goto Goto _SeanPiezo IV Closed loop Piezo r Stepper Stage Position Absolute um Relative um Absolute Move um Relative Move um x 20756 655 4243 28 Zero Io mm Move 500 000 Move Left al B gt Right Y Z fo o00 Move 500 000 Move Rear Al gt Front Z o 000 Move 500 000 Move Up af B gt Down Stop m Piezo Stage Calibration Piezo Stage Position Full Range um Absolute um Relative um Travel um x Joen XCaib x 40 000 bom Zero fio Move Left All gt Right y Isto Y Calib SE fo 000 fo 000 Zero fio Move Rea 1 sn z 894 ZCaib z eo foo00 Zero fio Move Up gt Down Stage Reset Execute this command when the instrument is first used or if the position
83. Quiet Time if applicable Abort Experiment at Level r Abort Quiet Time Current Bias No EE C Current A ON ent gt No C Current Overflow fo C Current A lt Before Run C Current 4 gt 2 C Current A lt bo Current Display during Quiet Time gt C After Quiet Time C Charge C gt 100000 No C Manual A fo 10s Change lt 0 C Numerical Graphical Calibration Before Run When this box is checked the potential and current offsets will be measured and compensated before running the experiment Disable this option to allow the experiment to start faster Check Connection Before Run When this box is checked the program will verify that the counter and reference electrodes are connected before running the experiment If one of the electrodes is not connected a warning message will appear proceed with the experiment at your own caution This option can prevent accidental damage to the working electrode due to an open loop Disable this option to allow the experiment to start faster Use Open Circuit E as Init E When this box is checked the program will measure the open circuit potential before running the 2014 CH Instruments Inc Control Menu no experiment and use this value as the initial potential External Trigger Run When this box is checked the experiment will be initiated by an external trigger signal from the Cell Control port on the rear panel Consult the a
84. Stor Intvl s 0 0001 500 Data storage interval Notes Initial Current and Final Current should be at least 1e 9A apart Cathodic and anodic currents correspond to reduction and oxidation respectively If the High E or Low E limit is reached during reduction the experiment stops At least 10 points are required to run the experiment Reduce the current scan rate or reduce the sampling interval as needed to meet this requirement During the experiment data update and storage rates will be the same i e dictated by the Data Storage Intv parameter The data sampling interval should be chosen according to the length of the experiment The longer the experiment the longer the sampling interval should be During an 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 unexpectedly long experiment 2014 CH Instruments Inc Setup Menu 4 2 28 Multi Current Steps Parameters dialog box In the Multi Current Steps technique ISTEP up to twelve current steps can be applied and cycled Potential is recorded as a function of time The following diagram shows the current waveform applied as a function of time Steps 4 lolslalslelz7ielo holia T 5 O Time s Parameter Range Description Step Seq 1 12 Step i A 2 2 Step current Step Time s 0 10000 Step duration High E Limit V
85. This command has a toolbar button The Graph Options command presents this dialog box Graph Options x Screen Printer Grid and Inv Je Header IV Header Je Axis IV Axis x en Cancel IV Baseline IV Baseline v an Hel 7 X Invert Hep V Param IV Param M Result IV Result J Y Invert I X Freeze poi To U o Cursor Lock to Data Points I Y Freeze 4 5e005 To 35e005 C Lock Free J X Title ul J Current Density T Y Title OoOo O ue Electrode Area a x Scale fi Y Scale iz Vv E Segments 1 To 2 Ref Electrode Ag AgCl Header 0 5 mM Ferrocene in 0 1M LCDA CH3CN 2mm Pt disk Note Depending on the currently selected experimental technique specialized options may also be available For context specific details click the Help button in the currently open dialog box The following options are available for all techniques Screen Uncheck the corresponding box to hide the header axis baseline parameters or results on screen The header is the title shown at the top of the plot entered in the Header field in this dialog box The baseline is drawn to visually define a peak or wave 2014 CH Instruments Inc CH Instruments Model 900D Series Screen options are independent of the printer options described below Printer Uncheck the corresponding box to hide the header axis baseline parameters or results on printed output Printer options are indepen
86. V corresponding to a rotation rate of O 10 000 rpm This instrument is also capable of controlling a Pine Instrument AFMSRX or AFMSREC Rotator for RDE 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 2014 CH Instruments Inc Getting Started In 2 1 4 Nanopositioner Stepper Motors and Piezo Nanopositioner Assembly Figure 2 3 Nanopositioner and Cell sample holder When the instrument is shipped all stages are dismounted Please carefully follow the instruction video included on the software CD to assemble the positioner Follow the video exactly to assemble the nanopositioner and cell sample holder as shown in Figure 2 3 Please call or e mail us if you have any questions Make sure not to unscrew the screws that are part of the stages The XY Z stages will all be mounted on top of the supporting stainless steel plate with the Y stage under the X stage The cell sample holder will also be mounted to the stainless steel base First mount the Z stage on the Z stand Tighten the four cap screws on the rear panel of the Z stand Be sure to place the Z stage as high as possible This is important Otherwise when the Z stage moves 2014 CH Instruments Inc CH Instruments Model 900D Series down it will collide with the Y stage This may cause the motor to stop and lose track of its position as well as reducing the travel distance for the Z s
87. a Point Interval This option allows you to store or display a subset of the data points For example when the value is changed to 3 only every 3rd data point will be stored or displayed This option is useful for quick examination of data or file size reduction However some details might be lost DigiSim Format for CV and LSV Data This option applies only to CV and LSV data When this box is checked the text data file will be directly readable by DigiSim Bioanalytical Systems West Lafayette IN software Excel 3D Format This option applies only to SECM image data CHI 900 series When this box is checked the output text data file can be read directly by Excel Microsoft Corp Redmond WA to generate a 3D surface plot To generate Excel 3D surface plots follow these instructions Start the Excel Program Open the target text data file created by the CHI900 CHI900A CHI900B program The Text Import Wizard Step 1 of 3 dialog box will appear Click Next The Text Import Wizard Step 2 of 3 dialog box will appear Change the Delimiters setting to match the data separator used in the output text file Click Finish A spreadsheet containing the data will appear Select all data points in the spreadsheet Click the Chart command in the Insert menu The ChartWizard Step 1 of 4 dialog box will appear Choose Surface and click Next The ChartWizard Step 2 of 4 dialog box will appear C
88. age occurs i e will be dictated by the data storage interval The data sampling interval should be chosen according to the length of the experiment The longer the experiment the longer the sampling interval should be A longer sampling interval results in more signal averaging and less noise However for a thin layer cell a short data storage time should be chosen in order to observe the electrolysis process in detail During an 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 unexpectedly long experiment 2014 CH Instruments Inc Setup Menu 4 2 20 Hydrodynamic Modulation Voltammetry Parameters dialog box In Hydrodynamic Modulation Voltammetry HMV the potential is incremented from Init E toward Final E The following diagram shows the potential waveform applied as a 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 the experiment the phase selective current at any phase angle will also be available for display The AC current is sampled at every potential increment and recorded as a function of potential Final E J k Incr E Rotation speed modulation amp data sampling Potential V Init E Time
89. aging You don t have to type the extension The program will automatically attach an extension of bin to the filename Other extensions are not allowed Files of type Select the type of file you want to convert Only the bin type binary data file will be available 2014 CH Instruments Inc Databroc Menu 1 7 12 Mathematical Operation command This command opens the Math Operation dialog box Use this command to perform mathematical operations on the currently active data The allowed operations are addition subtraction multiplication division exponential logarithm square square root and reciprocal applicable to both X and Y data values The Mathematical Operation command presents this dialog box Operation Selection Data Selection OK de Subtraction Multiplication C amp Data Array Y Data Array Cancel di Help C Division Exponential Add fo C Logarithm Sub fo C Square Mul H Square Root Div ft Reciprocal Je Override Present Data 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 second operand in the appropriate field Data Selection Select either the X data array or the Y data array as the target of the mathematical operation Override Present Data Check this box to replace the currently active data with the operated data If t
90. ake sure that the motor controller is turned off when powering up or powering down the bipotentiostat Otherwise very high voltages will be applied to the piezo block greatly reducing the lifetime of the piezo The instrument communicates with the PC through an RS 232 serial port default or USB port but not both If your computer has a free serial port 9 pin male connector it can directly communicate with the instrument without installing any drivers using a 9F 25M serial cable not included You may need to change the instrument software com port setting default COM1 using the System command under the Setup menu You don t have to worry about the baud rate After changing the COM port setting exit and re launch the program If you have a free serial port available on your PC we recommend its use over a USB port This is because we implement USB connectivity using a USB to serial chip on the instrument i e a physical USB port is used on the PC but the USB data are converted to serial by the driver software supplied by the USB chip vendor 2014 CH Instruments Inc Getting Started USB communication is achieved using a USB to serial chip built into the instrument allowing serial communication to occur through the USB port using drivers provided by the chip vendor It therefore provides no specific advantages over the serial port besides the difference in physical connectivity and both the instrument and the PC will intera
91. al DigiSim Format for CY and LSY Data Excel 3D Format for SECM Data Nanoscope Header for SECM data 3 column impedance data Segment Separator Charge Time Memo Check this box to include date time technique name labels and notes in the output text file Parameters Check this box to include experimental parameters in the output text file Results Check this box to include experimental results such as peak wave potential current and electrode area in the output text file To select the item to be displayed on screen when an experiment is complete execute the Peak Definition command in the Graphics menu Numeric Data Check this box to include numeric data points in the output text file 2014 CH Instruments Inc 40 CH Instruments Model 900D Series Separator Select the separator comma TAB space or linefeed to be used between data columns For two data points Xand Y the resulting output will be Separator Output Comma X Y TAB X Y Space XY Linefeed X Y This allows you to make the data format compatible with other commercial software such as spreadsheet or database handlers Number of Significant Figures This option allows you to set the data precision of the text file up to a maximum of 10 significant digits figures A larger number of significant digits will of course result in larger data files The default setting of 4 significant digits is sufficiently precise for most applications Dat
92. al E should be at least 0 01 V apart e Pulse Width should be no more than half of Pulse Period otherwise the system will automatically readjust Pulse Width Sample Width should be no more than half of Pulse Width otherwise the system will automatically readjust Sample Width In Differential Normal Pulse Voltammetry consists of three steps constant potential levels per cycle The potential of the first step is normally held at Initial E where no electrochemical reaction will occur The second step and third steps are incremented by Incr E every cycle with the third step always more positive negative for a positive negative scan than the second potential by Amplitude Current samples are taken every cycle at the end of the second and third steps and the difference between the two current samples is reported as a function of the second potential 2014 CH Instruments Inc ER CH Instruments Model 900D Series 4 2 10 Square Wave Voltammetry Parameters dialog box In Square Wave Voltammetry SWV the base potential is incremented from Init E towards Final E A square wave potential is superimposed onto the base potential which increments after each cycle of the square wave Current is sampled at the end of the forward and reverse steps and recorded as a function of the base potential During the experiment only the difference between the two current samples is displayed After the experiment the forward and reverse currents will also b
93. al data array equations convenient compilation of general and technique specific equations clock toolbar status bar Help comprehensive context sensitive HTML help on the fly switching between HTML help and legacy WinHelp using help about the application 2014 CH Instruments Inc General Information 9 1 4 System Requirements Operating System Windows 98 NT Me 2000 XP Vista 7 8 Communication between PC and instrument USB or RS 232 serial port Output device any printer or plotter supported by Windows 2014 CH Instruments Inc 10 CH Instruments Model 900D Series 1 5 Hardware Specifications Micropositioner Piezo positional resolution 1 6 nm Stepper motor resolution 4nm X Y Z total distance 50mm Bipotentiostat Probe Potential 10 V Substrate Potential 10 V Current 250 mA Compliance Voltage 12 V Input Impedance of Reference Electrode 10 Current Measurement Range 10 0 1 A V in 12 ranges Low Current Measurability 1 pA Maximum Sampling Rate 1 MHz 16 bit Waveform update rate 10 MHz maximum Cell Control purge stir and knock RDE Rotation Rate Control 0 10V voltage output for 0 10000 rom Other Features External voltage input recording channel Automatic and manual iR compensation 2014 CH Instruments Inc Getting Started 11 Chapter 2 Getting Started This chapter contains information about how to get started using your instrument Installation Testi
94. al substrate electrode potential Final E V 10 10 Final substrate electrode potential Segments 1 320 Number of half cycles Quiet Time s O 50000 Quiescent time before run Sensitivity A V 1e 12 0 1 Substrate sensitivity scale Sweep Step Select Potential control linear sweep or pulsed step Scan Rate V s le6 3 Potential scan rate Sweep only Sample Int V 0 001 0 02 Data sampling interval Sweep only Pulse Width s 0 01 1000 Duration of potential step Step only Sample Int s 0 0005 10 Data sampling interval Step only Probe Electrode Init E V 10 10 Initial probe electrode potential Final E V 10 10 Final probe electrode potential Segments 1 100 Number of half cycles Quiet Time s 10 10 Quiescent time before run Sensitivity A V 1e 12 0 1 Probe sensitivity scale 2014 CH Instruments Inc Setup Menu 1 Sweep Step Select Potential control linear sweep or pulsed step Scan Rate V s le6 3 Potential scan rate Sweep only Sample Int V 0 001 0 02 Data sampling interval Sweep only Pulse Width s 0 01 1000 Duration of potential step Step only Sample Int s 0 0005 10 Data sampling interval Step only Action b w Two Select Runs Delay O 10000 Delay in seconds OCP 10 10 Initiate second run at Open Circuit Potential 2014 CH Instruments Inc 102 CH Instruments Model 900D Series 4 2 36 Scanning Electrochemical Microscope Parameters dialog box In the
95. allow you to add reorder and remove files from a multi file plot The Manage Overlay or Manage Parallel command presents this dialog box This dialog box displays a list of all files being plotted with the current file As in older versions of the program the current file is always the first plot so it cannot be moved or removed Click OK to confirm all changes Add Clicking this button has the same effect as the Add Data to Overlay or Add Data to Parallel command Move Up Down Select multiple files by holding down Ctrl or Shift key and left clicking You can then to move your selection up or down in the list by clicking the appropriate Move button The current file is always the first plot so you will not be able to move your selection above it Remove Select file s as when using Move Up Down Once you click Remove these files will be removed from your plot 2014 CH Instruments Inc 164 CH Instruments Model 900D Series 6 10 Zoom In command Use this command to magnify the data plot This command has a toolbar button To enter zoom mode either click on the toolbar button or on its entry in the Graphics menu A check mark appears next to the menu item when zoom mode is enabled and its toolbar button will be depressed Once in zoom mode the mouse cursor will appear as an up arrow in the data plot area To zoom in left click and drag between diagonal corners of the box containing the area you want to view more
96. ally detect Com port option you will not need to change this setting Com Port Speed Set the communication speed between the PC and the instrument The Fast setting allows real time data transfer at higher scan rate and or shorter sampling interval The Standard setting is included for greater compatibility This setting is not available on older instruments 2014 CH Instruments Inc we CH Instruments Model 900D Series Current Polarity Assign anodic or cathodic current as positive valued This sign convention must be chosen before running an experiment otherwise experimental results peaks waves will not be reported properly Potential Axis Assign left or right as the positive direction for the potential axis only applicable to voltammetric or polarographic techniques Current Axis Assign up or down as the positive direction for the current axis Line Frequency Select the correct power line frequency for your geographic region This will reduce interference from the line frequency by adjusting the default sampling interval in certain techniques Windows Select the language used by your Windows operating system Oriental covers Chinese Japanese and Korean Windows The Technique selection field may be truncated if you select English Windows Oriental Windows uses shows slightly bigger letters than English Windows and does not support certain symbols For instance the symbol u may not be displayed properly in Or
97. ally readjust the Sample Period Both absolute current and phase selective current are available Use the Graph Option command under the Graphics menu to specify data display options e When DC current is high and AC current is low sensitivity cannot be increased because the DC current will overflow This problem is more serious when the frequency is relatively low The application of a DC current bias allows higher AC signal amplification A 16 bit DAC is used for this purpose On the other hand if the DC current is not expected to be large and the frequency is high a DC current bias may be unnecessary 2014 CH Instruments Inc ER CH Instruments Model 900D Series 4 2 12 2nd Harmonic AC Voltammetry Parameters dialog box In Second Harmonic AC Voltammetry SH JACV the base potential is incremented from Init E toward Final E and a sequential sine waveform is superimposed Current is sampled when the AC signal is applied and e second harmonic component is analyzed using a software lock in amplifier During the experiment only the absolute second harmonic AC current is displayed After the experiment the phase selective second harmonic current at any phase angle will also be available for display The following diagram shows the potential waveform applied as a function of time Incr E TT Final E Amplitude xX Potential V Init E J k Sample Period Time s Parameter Range Description Init E V 10 1
98. an on during or between experiments WE Static Discharge Protection The working electrode input amplifier is automatically protected from static discharge protection However the protection circuit generates extra leakage current at the input stage This leakage current is normally less than 50 pA and is therefore not noticeable if the current is at nanoamperes or higher For low current measurements you may want to turn off discharge protection when the sensitivity is high However if you are doing electrochemical detection for electrophoresis it is advisable for the protection circuit to be connected at all times to prevent possible high voltage feedthrough 2014 CH Instruments Inc 46 CH Instruments Model 900D Series 5 19 Stripping Mode command This command opens the Stripping Control dialog box Use this command to enable disable the stripping mode and specify deposition conditions This command is only available for the following techniques LSV SCV DPV NPV SWV ACV SHACV It is not available in polarographic mode The Stripping Control command presents this dialog box x Stripping Control OK M Purge During Depostion Cancel d Jh Stir During Deposition Help r Deposition Potential Ge Initial E Deposition E m Quiet Potential Initial E C Quiet E Deposition E 0 Deposition Time 15 Quiet E Mi fo Stripping Mode Enabled Check this box to enable stripping mode in
99. arameters Alternatively use the Parameter command under Setup menu The system displays the Cyclic Voltammetry Simulator Parameters dialog box so you can select the parameters you want to use Kinetics This button allows you to enter the electron transfer kinetic parameters such as standard heterogeneous rate constant the standard redox potential the charge transfer coefficient It also allows you to enter the forward and backward rate constant for chemical reactions The system displays the Potentials and Rate Constants dialog box so you can enter the kinetic parameters Conc This button allows you to enter the diffusion coefficient and concentration of all chemical species in the system Clicking this button displays the Concentration and Diffusion Coefficients dialog box for diffusive systems or the Surface Concentration dialog box for adsorptive systems Equilibrium Command This button allows you to view the concentration of each involved chemical species under the given kinetic conditions Clicking this button displays the Concentration at Equilibrium dialog box so you can view the equilibrium state 2014 CH Instruments Inc 24 CH Instruments Model 900D Series Variables Command This button allows you to specify values for other parameters such as temperature and electrode area Clicking this button displays the Simulation Variables dialog box so you can enter values for the appropriate variables 2014 CH I
100. arate the command and parameter Any text following a semicolon or pound symbol on a line will be ignored inline comments Run Macro Files from Command Line chi660e exe runmacro C CHli test mcr Legal Commands common Command Parameter Explanation tech string select an electrochemical technique folder string specify where to save files e g c chi test run run experiment save string save data to file when used in for next loop filename will be truncated to 5 letters and loop number 1 999 will be added to filename tsave string save data as text file fileoverride allow file override without warning macrotest check macro without execution end end of macro lines below will be ignored beep sound notification for 1 999 for next loop only one layer is allowed next end of for next loop delay 1 32000 delay between commands purge 1 32000 purge for specified time stir 1 32000 stir for specified time trigon turn on trigger before run trigoff turn on trigger before run knockon turn on drop knocker also used to send trigger pulse to external device before run knockoff turn off drop knocker no pulse before run qcmon QCM mode on qcmoff QCM mode off auxon turn on auxiliary signal recording channel auxoff turn off auxiliary signal recording channel cellon cell on between runs celloff cell off between runs 2014 CH Instruments Inc dummyon dummyoff rdeon rdeoff rdedepositionon
101. arly useful for electrochemical detection This command can only be used while an Amperometric i t Curve experiment is in progress and it cannot be used for other techniques It has a toolbar button 2014 CH Instruments Inc Control Menu 117 5 6 Zero Time command During an Amperometric i t Curve experiment the Zero Time command set the time to zero throwing away all previous data points This command can facilitate the time reading and reduce the number of unusable data points and is particularly useful for electrochemical detection This command can only be used while an Amperometric i t Curve experiment is in progress and it cannot be used for other techniques 2014 CH Instruments Inc ns CH Instruments Model 900D Series 5 7 Run Status command This command opens the Run Status dialog box Use this command to adjust certain options related to the currently running experiment including iR compensation automatic smoothing purge stir and prerun mercury drops The Run Status command presents this dialog box Run Status BEE x goeesssssesesesososssssasesesesossssescssessssssessos a Calibration Before Ruri OK Ken re ed eh fuere IT Check Connection Before Run Cancel J Use Open Circuit E as Init E Help I External Trigger Run L7 iR Comp for Next Run Bun J Smooth After Run SMDE Drops Before Buer iz J Purge Between Runs IT Stir Between Runs ddal T E2 Off During
102. artially This is useful for very slow experiments hours of 2014 CH Instruments Inc Setup Menu 107 experimental data can be recovered For performance reasons this command is not enabled by default If a fast experiment is accidentally interrupted it may prove more expedient to simply re run the experiment instead of using the Retrieve command which is located 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 By default the program only saves binary data files which contain extra system information including experimental control information This option allows you to save your data in text format as well whenever you save a binary data file This is useful for exporting data to read into other software e g spreadsheets Check Com port while idling Allow the program to periodically check that a valid and available Com serial port number has been assigned If so then COM OK will be displayed in the Status Bar This will not check for a compatible instrument connected to the Com port In particular COM OK will be displayed for any traditional serial ports or external USB serial converters even if there is no instrument attached at all This check box is deprecated in favor of
103. at 4 2 22 Multi Potential Steps Parameters dialog box In the Multi Potential Steps technique STEP twelve potential steps can be applied and cycled Current is recorded as a function of time The following diagram shows the potential waveform applied as a function of time Steps ze lt lelslalslel7 s lg holil Z T g O A Time s Parameter Range Description Step Seq 1 12 Step E V 10 10 Step potential Step Time s 0 10000 Step duration Init E V 10 10 Initial potential No of Cycles 1 10000 Number of cycles Smpl Intv s 0 0001 1 Sampling interval Quiet Time s O 100000 Quiescent time before potential scan Sensitivity A V 1e 12 0 1 Sensitivity scale E1 On Check or Uncheck Working electrode 1 on off control Notes e A step will be ignored if its step time is less than 0 001 sec or shorter than its sampling interval e f the sampling interval for a Step sequence is larger than 0 002 sec data will be transferred and displayed in real time e The sampling interval will be automatically increased if step time cycles sample interval exceeds 64K if data is to be transferred after the experiment e f the sampling interval is larger than 0 002 sec data will be transferred and displayed in real time e The potential difference between Init E Final E and Step E should be less than 13 1 V 2014 CH Instruments Inc ER CH Instruments Model 900D Series 4 2 23 A C Impedance Paramet
104. at will be subtracted from the currently active data File name Type or select the filename you want to subtract This box lists files with the extension you select in the Files of type box You don t have to type the extension The program will automatically attach an extension of bin to the filename Other extensions are not allowed Files of type Select the type of file you want to subtract Only the bin type binary data file will be available 2014 CH Instruments Inc 194 CH Instruments Model 900D Series 7 11 Signal Averaging command This command allows you to perform signal averaging between the currently active data and files saved on disk The currently active data is always included in the averaging which is computed by simply adding together several sets of data and dividing the result by the number of data sets Data sets whose X values differ from the currently active data will be ignored This command presents the following dialog box 21x Lookin l cht lo KE Pe IMPO fs MP1 Pd ito EJ IMPE1 EJ Lsyo EJ IMPE2 EJ NPVO EJ IMPE3 EJocpTi EJIMPE4 EJ pPsao A Files of type Data Files bin DI Cancel Z This allows you to select the files that will be averaged with the currently active data File name Type or select the filename s you want to average The box above lists files with the extension you select in the Files of type box Multiple files can be selected for aver
105. ate analytical report in text format up to four species of interest time dependence calculate the unknown concentration as a function of time from saved data files based on user defined peak potential range and calibration information report and or plot concentration as a function of time corrosion rate calculation CV Simulation and Fitting fast implicit finite difference algorithm reaction mechanisms 10 predefined mechanisms in select models any combination involving electron transfer first and second order chemical reactions system diffusive or adsorptive 2014 CH Instruments Inc e CH Instruments Model 900D Series 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 display of simulation data concentration profiles dimensionless current equilibrium data automatic detection and calculation of over determined equilibrium constants AC Impedance Simulation and Fitting visually equivalent circuit input automatic equivalent circuit parameters fitting View data information date time filename data source instrument model data processing performed header and notes data listing data information and numeric
106. aveform applied as a function of time and the sampling scheme A preelectrolysis step can be applied to reduce interference and background current Z Sample Interval ae eeee inte O A Time s Parameter Range Description Electrolysis E V 10 10 Electrolysis potential End Current Ratio 0 100 Upper limit of potential step Data Stor Int s 0 01 100 Data display and storage interval Preelec E V 10 10 Preelectrolysis potential Preelec T s O 1000000 Preelectrolysis time Notes Before electrolysis a preelectrolysis step can be performed which is useful for reducing residual current Any current at the end of preelectrolysis will be regarded as residual current and be subtracted from the total charge to give the net charge If preelectrolysis time is set to zero this step is ignored You can stop preelectrolysis at any time by invoking the Stop command and the regular electrolysis will follow immediately The sensitivity scale will be switched automatically during the experiment The current ratio is reported relative to 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 begins If the specified end current ratio is zero electrolysis will continue forever In order to stop the experiment the Stop command should be invoked During the experiment the data will be updated at the same rate that data stor
107. avel a distance of 50 mm in all three directions with 0 1 micrometer resolution allowing high precision patterning This is particularly important when multiple overlapping solution components need to be dispensed The jetting device can dispense single drops of solutions with viscosity less than 40 centipoise and surface tension in the range of 0 02 0 07 N m Solutions with properties outside these limits can be jetted if changes to the properties can be achieved with solvents or changes in temperature With a default nozzle size of 60 microns the jetting device can produce drops ranging from 100 200 picoliters in volume depending on the operating parameters and solution composition The CHI1550A solution dispenser control software is very user friendly for creating binary ternary and quaternary arrays of spots containing mixtures of solutions Instead of using a manually created look up table for solution dispensing patterns pattern creation is facilitated by our software which can also provide commonly used patterns as a default for binary ternary and quaternary arrays The positioner can memorize certain critical positions such as the solution loading point and first dispensing point allowing the jetting device to go to these positions easily and quickly The array pattern can be examined graphically and it will also be displayed during the dispensing process 2014 CH Instruments Inc 2 CH Instruments Model 900D Series
108. can be connected at a time The minimum number of channels for the CHI684 is 8 The channel increment is 8 The maximum number of channels is 64 The Multiplexer command presents this dialog box m Channel Selection OK VMiw2 M3 M4 M5 WME M7 WB x Cancel CatwtnutaEIatutmstI Sie Caz 8 O19 OC 2a rier 23 24 __tep Tar 27 af ar ar af af 32 Run Mutiplexer C 3a 34 ar ar ar af at a rar ar 43 AT ef ef arr as rasp attert 54 set 56 TC steet et eof 61 M 62 M e3r 64 m Prompt Before Each Run Immediate Channel Set e None Manual Extemal Trigger Channel fi Set Base Filename Tesi Browse SC Channel Selection Click a channel to enable it and uncheck to disable If you select a channel beyond your CHI684 channel number it will be ignored Prompt Before Each Run If Manual is selected you will have to click on a message box before each run except the 1st run The instrument will wait until you respond If External Trigger is selected the instrument will wait for an external trigger signal before each run The trigger signal is an active low signal and can be applied to Pin 13 of the Cell Control port on the rear panel Base Filename 2014 CH Instruments Inc 14 CH Instruments Model 900D Series Click Browse or type directly in this field to specify the filename prefix up to 5 characters Data will be saved after each run The run number will be attached to the base filename i
109. ccess to the cell There should be enough free space around the vents and fan exhaust of the instrument to prevent overheating 7 Connections to the cell by crocodile clips should be made in such a way as to avoid shorting of the contacts 2014 CH Instruments Inc Section 2 Power configuration On unpacking the instrument the presence of the following should be noted 1 Mains cable 2 Cell Lead 3 User Manual 4 Optional accessories if ordered cells electrodes etc The instrument is designed to operate at 110V or 220 V 20 AC power 50 60 Hz Please check the rear panel label for its input voltage setting If an incorrect AC voltage is connected the fuse will blow and the instrument may be damaged The correct voltage and line frequency for your region have been set at our factory prior to shipment 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 fuse failure the user should consult CH Instruments Inc before proceeding further The unit should be placed within 1 5 m of a grounded mains power supply When the instrument is powered on the indicator light on the front panel will be illuminated Rear panel of instrum
110. ce and stability test The result will be reported in the iR Comp Test Results Box For more details about iR compensation please refer to 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 iR compensation will be enabled for the next run You may be unable to enable iR compensation if automatic compensation has been set but the iR compensation test has not been conducted or if the sensitivity scale has been altered This option can also be turned on or off from the Run Status command under the Control menu iR Comp Enable If the Once option is selected iR compensation will be applied only to the next run and subsequently disabled If you want the same compensation conditions to be applied to consecutive runs select the Always option iR Comp Mode Specify the mode of iR compensation Automatic iR compensation will be based on the iR compensation test results Manual iR compensation uses the resistance value you specify in the Resistance field below Manual Compensation Resistance Specify the resistance value that you want system to compensate this value is used only for manual iR compensation Choose this value with care if the compensation level is close to or exceeds the actual solution resistance the potentiostat will oscillate Please also notice that the maximum allowed resistance compensation may b
111. ck or Uncheck Return probe to origin after conditioning Motor Selection Select Auto Stepper or Piezo Long Travel Dir XorY Select the long move direction Notes In this technique a new pattern needs to be created by using the Create New Pattern button The pattern size and pixel size are determined by the XY distances and the increment distance in the Probe Travel section The Create New Pattern button can also be used to clear an existing pattern A new pattern is created with all dark pixels Left click and drag to create a trace of bright pixels To erase bright pixels right click and drag You can create a bitmap pattern for surface conditioning this way A dark pixel represents 0 It puts the probe and substrate if turned on at their respective first potentials E1 for Hold Time 1 A bright pixel represents 1 It puts the probe and substrate if turned on at their respective second potentials E2 for Hold Time 2 Sensitivity should be chosen high enough so that the current at each pixel can be displayed correctly during a run but not so high that overflow occurs Overflow will affect the accuracy of potential control and it is safer to set a relatively low sensitivity If the sensitivity setting is too low the current reading may not be accurate Nevertheless this will not affect the surface patterned conditioning results H both X and Y distances are within the X and Y piezo range automatic motor selection will choose the pi
112. command use OCP as final E disabled by ef command use OCP this value as init E disabled by ei use OCP this value as final E disabled by ei use OCP as center potential shifts high and low E limits on both sides of OCP 127 12 CH Instruments Model 900D Series eiincr efincr ehincr elincr fullcycleon fullcycleoff efon efoff sens sens2 autosens qt ht smodeon smodeoff depeon depeoff depe dept quieteon quieteoff quiete pcon pcoff pcon2 pcoff2 initeon initeoff pce pce2 pce3 DCH DCH pct3 1 1 1 1 1 1 1 1 1e 12 1 te 12 1 O 100000 O 100000 10 10 1 100000 10 10 10 10 10 10 10 10 0 6400 0 6400 0 6400 increment init E in for next loop should be reset to zero after loop increment final E in for next loop should be reset to zero after loop increment high E in for next loop should be reset to zero after loop increment low E in for next loop should be reset to zero after loop CV full cycle on CV full cycle off Final E on Final E off sensitivity scale sensitivity for 2nd working electrode if applicable automatic sensitivity if applicable quiescent time before run if applicable hold time at final E if applicable turn on stripping mode turn off stripping mode turn on deposition potential in stripping mode turn off deposition potential in stripping mode deposition potential deposition time in secon
113. ct as if connect by a serial connection The reason we include USB support is that newer computers may not include a serial port and it may be impractical or impossible to add a serial port card To use a USB port for data communication you must first install the USB driver included on the software CD also available from www chinstruments com Depending on your model you may also need to change a jumper setting inside the instrument see below If there is no available serial port on your computer you can use a USB port for communication instead To do so you need to change a jumper setting inside the instrument Figure 2 2 and install the driver software on your PC oe a gt t KZ d e i ba KM j FF ten Aen Ae f GR e Figure 2 2 Serial port or USB port switch selection using two jumpers indicated by arrows Left RS 232 serial port jumper setting Right USB jumper setting USB driver installation will be described in detail later in this chapter If you consistently encounter Link Failed messages try a different PC The instrument we delivered was turned on for a week and tested In nearly all cases consistent Link Failed messages are caused by the PC either by port settings or problems You may occasionally notice unreliable data communication This could be due to background tasks that generate interrupts since serial port data communication is interrupt based In recent versions Microsoft Windows
114. ction 1e 6 10000 Potential scan rate 1 1000000 Sweep segments each is half cycle 0 001 0 064 Data sampling interval O 100000 Quiescent time before potential scan te 12 0 1 Sensitivity scale Check or Uncheck Automatic sensitivity switching during run Check or Uncheck Allow potential scan to end at Final E Check or Uncheck Record external signal 10 10 Second working electrode potential 0 2 0 2 Potential difference with 1st channel if Diff Scan is enabled te 12 0 1 Sensitivity scale for second electrode Select or deselect Second working electrode turned off Select or deselect Hold second electrode at constant potential Select or deselect Scan 2nd channel with 1st channel Select or deselect Scan 2nd channel at constant potential difference with 1st channel s CH Instruments Model 900D Series The potential increment is 0 1 mV when the scan rate is below 1000 V s 1 mV at 5000 V s and 2 mV at 10000 V s High E and Low E should be at least 0 01 V apart e f unreasonably values for High E or Low E are entered the system will automatically readjust them Depending on the Init E High E and Low E values the system will automatically readjust the initial scan direction The maximum potential scan range is 13 1V The sampling interval can be 1 mV when the scan rate is below 1000 V s 2 mV below 2000 V s 5 mV below 5000 V s and 10 mV below 10000 V s The data sampling interval will be automatically increased at
115. current is not sampled Two potential pulses are applied after the cleaning step and the current at the end of each pulse is recorded as a function of time During the experiment only the difference between the two current samples is displayed After the experiment the current responses to the two potential pulses will also be available for display The following diagram shows the potential waveform applied as a function of time and the current sampling scheme Data Sampling Data Sampling Clean E1 ES ern E2 e e T EI S Ki E2 o Init E E3 D E4 Clean T1 T1 T2 Clean T2 T3 T4 Cycle 1 Cycle 2 0 Time s Parameter Range Description First DPA Cleaning E1 V 10 10 Electrode cleaning potential Cleaning Time s 0 32 Electrode cleaning time Pulse E1 V 10 10 First pulse potential Pulse T1 s 0 01 32 First pulse time Pulse E2 V 10 10 Second pulse potential Pulse T2 s 0 01 32 Second pulse time Open Circ Clean Check or Uncheck Cleaning step held at constant or open circuit potential Second DPA Cleaning E2 V 10 10 Electrode cleaning potential Cleaning Time s 0 32 Electrode cleaning time Pulse E1 V 10 10 First pulse potential Pulse T1 s 0 01 32 First pulse time Pulse E2 V 10 10 Second pulse potential Pulse T2 s 0 01 32 Second pulse time Open Circ Clean Check or Uncheck Cleaning step held at constant or open circuit potential Init E V 10 10 Initial potential Number
116. d X Axis Unit Enter the X Axis unit or dimension e g ppm or M to be plotted Y Axis Title Enter the desired Y axis title e g Peak Current to be plotted 2014 CH Instruments Inc Analysis Menu Y Axis Unit Enter the signal unit or dimension such as A to be plotted Header Enter the desired title header for the data To display the header on the top of the plot check the Header box using the Graph Option command Note Enter any comments about the plot The note will not be displayed on the plot but will be saved in the data file It allows you to put additional comments about the data and is well suited for a brief description of the purpose and conditions of the experiment Read Use this command to read data from file Save Use this command to save data to file XY titles units header and note will be saved along with the data Calculate Use this command to calculate the slope intercept and correlation coefficient of the standard addition curve If the unknown peak height is given the unknown concentration will also be calculated Plot Use this command to plot the standard addition curve The plot will be automatically scaled according the data range To freeze the scale please use the Graph Option command 2014 CH Instruments Inc 22 CH Instruments Model 900D Series 8 3 Data Report command This command opens the Data File Report dialog box Use this command to genera
117. dance Time technique IMPT the base potential is held constant at Init E onto which a sine waveform is superimposed Current and potential are sampled and analyzed to obtain the real and imaginary parts of the impedance as a function of time The following diagram shows the potential waveform applied as a function of time Sample Interval K Amplitude we Init E Potential V ke Run Time Time s Parameter Range Description Init E V 10 10 Initial potential Amplitude V 0 0001 1 5 A C amplitude Frequency H2 0 0001 1te6 A C frequency Sample Interval s 1 20000 Data sampling interval Run Time s 1 500000 Total experiment time Cycles lt 10 Hz 1 100 Number of repetitive cycles at each frequency Quiet Time s O 100000 Quiescent time before sampling data Bias DC Current off range on Enable DC current bias during run Sensitivity Scale 1e 12 0 1 Sensitivity scale automatic or manual Notes H the sampling interval is smaller than the actual time required for sampling it will be automatically adjusted More cycles result in a better signal to noise ratio but also a longer experiment run time When DC current is high and AC current is low sensitivity cannot be increased because the DC current will overflow This problem is more serious when the frequency is relatively low The application of a DC current bias allows higher AC signal amplification A 16 bit DAC is used for this purpose On
118. de to the solution and connected it to the reference clip The counter electrode will not be used The system displays the following dialog box Sample Interval sec Io Run Lime sec 400 Quiet Time see 2 Sensitivity LAT 1e006 Potential Gain C1 C10 100 1000 m Measurement Mode Ge Curent Potential Both Parameter Range Description Sample Interval s 0 1 10 Sampling interval Run Time s 10 100000 Experiment running time Quiet Time s O 100000 Quiescent time before potential pulses begin Sensitivity A V 1e 9 0 1 Sensitivity scale Potential Gain 1 10 100 1000 Gain setting for potential noise measurement Meas Mode i E or both Measurement mode 2014 CH Instruments Inc Setup Menu 93 4 2 32 Surface Patterned Conditioning Parameters dialog box This technique is used to condition the SECM substrate surface with a pattern e g for micromachining For instance the SECM probe can be scanned across the surface and held at either E1 or E2 at rectilinear grid points as dictated by the specified pattern If a reaction occurs at E1 but not E2 or vice versa then deposition etching will occur at the patterned points The Create New Pattern button opens the graphical pattern editor please refer to the Notes below for more details The program presents a Surface Patterned Conditioning Parameters dialog box Surface Patterned Conditioning Paramet
119. dent of the screen options described above Grid and Inv Uncheck the corresponding box to hide the X or Y grid or to disable axis inversion Check Xor Y inversion to flip the Xor Y axis temporarily To invert axis polarity permanently use the System command in the Setup menu X Y Freeze Freeze the Xor Y axis range by checking the corresponding box and enter the desired min and max The X and Y axis can be frozen independently When the corresponding box is unchecked the X or Y scale will revert to the original scale of the present plot In SECM mode the Z axis can also be frozen similarly Due to the program requirement for an integer number of ticks an axis may be unable to be frozen at the scale you entered X Y Title The program automatically provides default axis titles for each electrochemical technique To override these defaults check the corresponding box and enter the desired title Unit Specify the units or dimensions of customized axis titles X Y Scale These values change the size of the plot the default full size value is 1 This is particularly useful when you want to print the plot for publication or paste the plot into a word processor Cursor Lock to Data Points This option controls the behavior of the mouse cursor in the plot area The X and Y coordinates of the cursor will be displayed in both modes When Lock is selected the cursor will be locked to data points when you move the mouse in the X d
120. dependent 2014 CH Instruments Inc Setup Menu e 4 2 9 Differential Normal Pulse Voltammetry dialog box In Differential Normal Pulse Voltammetry DNPV the base potential is held at Init E and a sequence of dual potential pulses is applied The magnitude of the first pulse increments after every iteration and the second pulse has a constant amplitude relative to the first Current is sampled at the end of both potential pulses and the difference of these two values is recorded as a function of the first pulse potential The following diagram shows the potential waveform applied as a function of time and the current sampling scheme gt Pulse Width Pulse Width g J k 2 E C xX S Incr E Amplitude D WS a 4 k AkAR Pulse Period Sample Width Time s Parameter Range Description Init E V 10 10 Initial potential Final E V 10 10 Final potential Incr E V 0 001 0 05 Increment potential of each pulse Amplitude V 0 001 0 5 Potential pulse amplitude 1st Pulse Width s 0 001 0 02 First potential pulse width 2nd Pulse Width 0 001 0 02 Second potential pulse width Sampling Width s 0 001 0 5 Data sampling width Pulse Period s 0 05 50 Potential pulse period or dropping time Quiet Time s O 100000 Quiescent time before potential pulses begin Sensitivity A V 1e 12 0 1 Sensitivity scale Open Circuit Check or Uncheck Hold Step 1 at open circuit or constant potential Notes e Init E and Fin
121. ds turn on quiet potential in stripping mode turn off quiet potential in stripping mode quiescent potential in stripping mode turn on preconditioning turn off preconditioning turn on preconditioning for channel 2 turn off preconditioning for channel 2 return to initial potential after run remain at final potential after run potential for 1st stage of preconditioning potential for 2nd stage of preconditioning potential for 3rd stage of preconditioning time for 1st stage of preconditioning time for 2nd stage of preconditioning time for 3rd stage of preconditioning 2014 CH Instruments Inc Control Menu 1 noabort abortov abortigt abortilt abortq abort10s abortchgt bcela bceib bce2a bce2b bce3a bce3b bce4a bce4b bceda bce5b bcorder bcalgor note header forcequit 0 2 0 2 O 100000 0 1 1 3600 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 1 19 0 1 string string yesiamsure do not abort experiment during run abort experiment if current overflow abort experiment if current gt specified value abort experiment if current lt specified value abort experiment if charge gt specified value abort experiment if signal change in 10 seconds is less than specified value revise abort10s to specified time interval Baseline Correction BC a k a baseline fitting and subtraction 1st peak foot from potential BC 1s
122. e filenameN where N is the channel number 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 If a base filename is not specified a warning will be given If you continue the system will run the experiments without saving any data Before execution the program will check for existing data files with a same base filename issuing an overwrite warning if found Immediate Channel Set This allows you to select an arbitrary channel immediately You can then exit the dialog box and run an experiment for that particular channel Run Multiplexer Click this button to run experiments for the selected channels using the CHI684 Multiplexer Experimental conditions should be set before this command is executed Side Note Multiplexer Related Macro Commands Two Macro commands are available for the CHI684 multiplexer The macro comamnd mch allows you to select an individual channel The macro command mchn is used in For loops to select the channel given by the For loop counter Note that this macro command will run in 1 2 3 4 sequence you cannot skip channels in a For loop 2014 CH Instruments Inc Control Menu 125 5 10 Macro Command command This command opens the Macro Command dialog box Use this command to execute a series of other commands This is analogous to batch file
123. e the data point will be plotted The Graph Option Color and Legend and Font commands allow you customize your overlay plot This command does not check the type of data and it is up to the user to ensure the meaningfulness of the overlay plot 2014 CH Instruments Inc 6 3 Add Data to Overlay command Graphics Menu 157 This command complements the Overlay Plots command allowing you to add more data to an existing overlay plot This allows you to overlay data files from multiple directories or drives This command presents the following dialog box Add Data to Overlay 2 x Lookin lc zo a File name eJ MPO fs MP1 EJ IMPE1 EJ IMPE2 FJ IMPE3 ad IMPE4 C4 BIN CV3 BIN CV2 BIN Files of type Data Files TF bm DI Cancel E ITO Lsvo NPVO OCPT1 PSAQ E 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 while holding the Ctrl key down to select files one at a time The plot will be automatically scaled to fit the currently active 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 overlay plot This command does not check the type of data and it is up to the user to ensure the meaningfulness of the overlay plot It is disabled if there is no currently active data or if the c
124. e Fitting Checking this box will generate a linear least squares best fit line on the plot 2014 CH Instruments Inc CH Instruments Model 900D Series 6 16 Special Plot command Use this command to display special plots if available For linear sweep voltammetry LSV this command opens the Polarization Resistance Plot dialog box The resulting plot is temporary and will disappear if other data display commands are invoked You can use the Graph Option Color and Legend and Font commands to customize your plot The Special Plot command presents this dialog box for the LSV technique Polarization Resistance Plot EN Potential Window EM mee jo Cancel Window hl o 03 Hel nep After this command is invoked the program will check for a potential with zero current If found this potential is set as E V l 0 Otherwise a warning Potential at zero current not found will be issued After specifying the center potential and potential range click OK to construct the polarization resistance plot 2014 CH Instruments Inc Graphics Menu 173 6 17 Graph Options command This command opens the Graph Options dialog box Use this command to selectively turn on or off plot captions grids axis inversion You can also freeze axes customize axis titles and write notes that can be saved together with the data Most other parameters will be saved when you exit the program and reloaded when you restart the program
125. e available for display The following diagram shows the potential waveform applied as a function of time and the current sampling scheme a a er mm UR D Final E Potential V A kd k 1 Frequency k Sample Width Time s Parameter Range Description Init E V 10 10 Initial potential Final E V 10 10 Final potential Incr E V 0 001 0 05 Increment potential of each pulse Amplitude V 0 001 0 5 Square wave amplitude Frequency H2 1 100000 Square wave frequency Quiet Time s O 100000 Quiescent time before potential pulses begin Sensitivity A V 1e 12 0 1 Sensitivity scale Electrode 2 Potential V 10 10 Second working electrode potential if not scan Sensitivity A V 1e 12 0 1 Sensitivity scale for second electrode On Check or Uncheck Second working electrode at constant E Scan Check or Uncheck Scan the second electrode potential Notes e Init E and Final E should be at least 0 01 V apart e Forward reverse and difference currents are recorded Use the Graph Option command under the Graphics menu to specify data display options e When the second electrode is set to Scan its potential will be the same as the primary electrode it is not independent 2014 CH Instruments Inc Setup Menu 4 2 11 AC Voltammetry Parameters dialog box In Second Harmonic AC Voltammetry SH JACV the base potential is incremented from Init E toward Final E and a sequential sine
126. e error message and contact the factory for servicing Digital Circuitry Test Results e Firmware version number and revision date e ROM test result if applicable e RAM test result if applicable Potential and current offset test If this test has been failed an error message will be given Sensitivity scale test If this test has been failed an error message will be given This error is usually is related to leakage current Gain test If this test has been failed an error message will be given There are 3 gain stages 2014 CH Instruments Inc Setup Menu 1 Analog Test Summary If no error has been detected the message box will simply read Analog circuitry test OK Errors caused by the analog to digital converters will also be reported here In the case of an analog test error please repeat the test several times to see if the error is consistent Record the error message and contact the factory for servicing 2014 CH Instruments Inc Control Menu 11 Chapter 5 Control Menu The Control menu offers the following commands Run Experiment Start running an experiment Pause Resume Pause or unpause an experiment Stop Run Stop running an experiment Reverse Scan Reverse potential scan direction CV only Zero Current Zero current Zero Time Zero time Run Status Set certain conditions for running an experiment Repetitive Runs Run an experiment multiple times Multiplexer Set options for
127. e is fully automatic and compatible w ith our model 600E and 700E series instruments primary channel only 4 Made of stainless steel and Teflon Not remote controllable Four glass cells are included 5 Not a replacement part for the CHI220 Cell Stand 2014 CH Instruments Inc
128. e limited to the feedback resistor of the i E converter This parameter will be ignored if automatic iR compensation is selected 2014 CH Instruments Inc Control Menu 135 5 13 Filter Setting command This command opens a Filter Selection dialog box 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 and can be used to filter out transient components The potential filter can be used for instance to convert a staircase ramp to a linear sweep A capacitor can be connected to the feedback resistor of the i E converter to form a low pass RC filter This can remove the high frequency noise at the first hand The signal filter is applied before the gain stage It is a second order Bessel low pass filter These filters are useful for reducing the amount of noise during measurements Click the Help button in the resulting dialog box for more information This command has a toolbar button ANT The Filter Setting command presents this dialog box Ix Filter Selection Potential Filter VE Conv Filter Signal Filter 2nd VE Filter 2nd Signal fi 50 Hz fi 50 Hz fi 50 Hz Cancel Selection Selection Selection Selection Selection Help d Automatic Automatic Automatic Automatic 32K Hz 150K Hz 3200 Hz 15K Hz 320 Hz 1500 Hz 32 Hz 150 Hz 3 2 Hz 15Hz 0 32 Hz 1 5Hz 0 032 Hz 0 15 Hz The 2nd
129. e peak height of the unknown species if available to allow calculation of its concentration X Axis Title Enter the desired X axis title e g Concentration to be plotted X Axis Unit Enter the X Axis unit or dimension e g ppm or M to be plotted Y Axis Title Enter the desired Y axis title e g Peak Current to be plotted Y Axis Unit Enter the signal unit or dimension such as A to be plotted Header 2014 CH Instruments Inc Analysis Menu 1 Enter the desired title header for the data To display the header on the top of the plot check the Header box using the Graph Option command Note Enter any comments about the plot The note will not be displayed on the plot but will be saved in the data file It allows you to put additional comments about the data and is well suited for a brief description of the purpose and conditions of the experiment Read Use this command to read data from file Save Use this command to save data to file XY titles units header and note will be saved along with the data Calculate Use this command to calculate the slope intercept and correlation coefficient of the calibration curve If the unknown peak height is given 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 2014 CH Instrument
130. e unnecessary 2014 CH Instruments Inc Setup Menu e 4 2 13 FT AC Voltammetry Parameters dialog box In Fourier Transform AC Voltammetry FTACV the DC potential is scanned from Init E to Final E in increments of 0 3 mV On top of this DC scan a sine waveform is superimposed applied continuously without interruption The resulting current is sampled and displayed directly at all times cf ACV Once the experiment is complete data analysis by Fourier transform yields the absolute AC current DC current first second third and fourth harmonic components as well as the complete response spectrum Hence a very rich set of information can be obtained from a single measurement Parameter Range Description Init E V 10 10 Initial potential Final E V 10 10 Final potential Frequency Hz 0 1 50 AC frequency Amplitude V 0 001 0 5 AC amplitude Total Data Point 8192 65536 Total number of data points sampled Data PointsPer 4 256 Number of data points per AC waveform period Sine Sweep Segments 1 2 Single or cyclic DC potential scan Quiet Time s O 100000 Quiescent time before potential scan Sensitivity A V 1e 12 0 1 Sensitivity scale Notes e Init E and Final E should be at least 0 01 V apart e For a given frequency the more data points per sine wave the faster the sampling rate will be Faster sampling will result in less noise more signal averaging but lower data density If the specified
131. each other as shown in Figure 2 1 The box with three DA 9 connectors a 4 pin round connector and a DA 15 connector on the front panel is the stepper motor and piezo controller Connect the stepper motors to the 15 pin DA connectors labeled Stepper labeled from left to right for the X Y and axes For the model 920D also plug connect the piezo to the 4 pin round connector labeled Piezo and the sensor to the 15 pin DA connector The other instrument box contains the bipotentiostat digital function generator and data acquisition circuitry You need to connect the two boxes together plugging the 3 ft DB 25 cable into the two connectors labeled Cell Control on their rear panels CH Instruments Scanning Electrochemical Microscope Connect with a DB 25 cable H CH Instruments Scanning Electrochemical Microscope Piezo ye Front View Rear View Figure 2 1 Front and rear view of the instrument chassis for the stepper motor piezo controller bottom and bipotentiostat top It is recommended to power the bipotentiostat on first Turn the motor controller off first when powering down the system It is recommended to keep the motor controller turned off when the piezo block is not going to be used in the next hour or longer model 920D The bipotentiostat can still be used when the motor controller is turned off and this will extend the lifetime of the piezo For model 920D please m
132. echanism list and let the program automatically assign their values If an overdetermined equilibrium constant involves a chemical reaction the backward rate constant will be determined by the program You should still enter the forward rate constant For charge transfer reactions the standard redox potential will be determined by the program You should still enter the heterogeneous rate constant and alpha 2014 CH Instruments Inc z6 CH Instruments Model 900D Series 9 1 3 Concentration and Diffusion Coefficients dialog box This dialog box allows you to specify the concentration and diffusion coefficients for CV simulations Concentration and Diffusion Coefficients Reactions Species Conc M De em2 s A e B A 0 001 fi e 005 Cancel C e D Ae fi e 005 Help B D De fi e 005 4 D C B ii El ial Ga All steps of the reaction mechanism are listed in the first column The second column lists all species in the system In the right two columns you can enter the concentration and diffusion coefficient for each species 2014 CH Instruments Inc Sim Menu 217 9 1 4 Surface Concentration dialog box This dialog box allows you to specify the surface concentration for CV simulations Surface Concentration All steps of the reaction mechanism are listed in the left column The middle column lists all species in the system In the right column you can enter the surface concentration for each speci
133. ect one of many electrochemical techniques Choose experimental parameters Start experiment m Pause experiment Stop experiment Reverse CV scan direction Zero current E Set and test iR compensation Set potential and current filters J Set purge stir cleaning and other cell conditions J Calibrate and control SECM probe J Plot current data graphically Increase zoom in graphics mode W Report results manually H Define peak or wave parameters Adjust graphics options lM Set color and legend in graphics Set caption font in graphics 2 Copy graphics to clipboard Data smoothing Compute derivative J Compute semi integral and semi derivative View current data as text LUView SECM probe status Krier context sensitive help mode Shift F1 2014 CH Instruments Inc CH Instruments Model 900D Series 10 6 Add or Remove Buttons command This command opens the Customize Toolbar dialog box It is available as a drop down arrow on the default toolbar There are several ways to add remove or reorder buttons on your toolbar For maximum convenience use method 1 to reorder or remove buttons method 2 to add buttons in specified locations and method 3 to add buttons to the right end of your toolbar Use the Reset button in the Customize dialog box to restore the default toolbar buttons and menus if applicable 1 In the main program window while holding down the Alt key you ca
134. ective product In order to obtain service under this warranty the customer must notify CH Instruments Inc before the expiration of the warranty period and make arrangements for service The customer shall be responsible for packing and shipping the defective product with prepaid shipping charges CH Instruments Inc will pay for return shipping of the repaired or replacement product to the customer within the United States The customer shall be responsible for all shipping charges duties taxes and other charges for products sent outside of the United States Warranty service does not cover failures caused by misuse accident modification unsuitable physical or operating environment improper maintenance or service of the product by unauthorized personnel In no event shall CH Instruments Inc be liable or in any way responsible for any lost profits lost savings incidental or other financial consequential damages This is true even if you advise CH Instruments Inc of the possibility of such damages 2014 CH Instruments Inc o CH Instruments Model 900D Series 12 6 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 a reasonable background knowledge of electrochemistry Any adjustments maintenance or repairs must be carried out as defined by this manual please refer to Appendix secti
135. ediately following the experiment Graphics can be copied to the clipboard during the run The experiment can be halted by invoking the Stop command This command has a toolbar button gt 2014 CH Instruments Inc Control Menu 113 5 2 Pause Resume command Use this command to pause and unpause your experiment This command is unavailable for time based techniques e g CA CC BE DPA DDPA TPA IMP IMP t CP PSA This command has a toolbar button DI 2014 CH Instruments Inc CH Instruments Model 900D Series 5 3 Stop Run command Use this command to stop running your experiment This command can also be used to stop repetitive runs or macro commands It has a toolbar button m 2014 CH Instruments Inc Control Menu 115 5 4 Reverse Scan command Use this command to reverse the potential scan direction during a cyclic voltammetry experiment Each time this command is invoked the sweep segment counter increments If this command is used during an experiment certain data analysis features will be unavailable e g peak search This command has no effect for other techniques It has a toolbar button EI 2014 CH Instruments Inc ne CH Instruments Model 900D Series 5 5 Zero Current command During an Amperometric i t Curve experiment the Zero Current command will manually bias the current to zero to facilitate current reading after the baseline has settled This is particul
136. eeeeeeeeeeeeeeeeeeeeeeeeeeseeeeeeeseeeeeeeseeeaeeeseseeeeeeeeeeeeeeeeanees 42 3 10 Rripnteommand Zgeededeet a aaa aa a a aa a a aa ae a a ta beuetecdvcceatebedueve 43 3 11 Print Multiple Files COMMANG cceeeeceeeeeeeeeeeee eee eeee ee eeeeee ee eeeeeeeeeeseeeeeeeseeeeeesseeseeesseeseeeses 44 3 12 Print Setup command sssaaa ernieren ara rian e aAa EUa AANEEN EEN Eeer 45 3 13 o aa EEEE ETET T 47 Chapter 4 Setup Menu 49 41 Technique command rsca AANA ANURA ANAA ENNAN ENEAN Era 50 4 2 Parameters COMMANG c122ccccccceeccnecccentscctavesseeecuerccceedioceteueseesacwdebectebssetaedcecesccudeieaeewccoeeess 4 2 1 Cyclic Voltam metry Parameters dialog DOX ccecscetessesseseeveevseeseeneeneesaesaesseeseesoeseesaesesessevaneanes 4 2 2 Linear Sweep Voltam metry Parameters dialog box 4 2 3 Staircase Voltam metry Parameters dialog DOX cccesessseseeveevseeseeseeneenesesseeseeseesnesaessesesenvaneanes 4 2 4 Tafel Plot Parameters dialog DOX isie raae aea aa enaa a a aa aaea aaia daaa aa daaa aooaa a 4 2 5 Chronoamperometry Parameters dialog DOX s s nsnsnsnnnnrnsnnnnnnrnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnennnnnnnnnnnnn nnna 2014 CH Instruments Inc i CH Instruments Model 900D Series 4 3 4 4 Chapter 5 1 5 2 5 3 5 4 5 5 5 6 5 7 5 8 5 9 5 10 5 11 5 12 5 13 4 2 6 Chronocoulometry Parameters dialog box sessersrrsersee 61 4 2 7 Differential Pulse Voltam metry Parameters dialog box 63
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138. elatively low high cutoff frequency You may be able to select the desired cutoff frequency by altering the sensitivity scale Signal Filter The grayed out box displays the actual signal filter setting Choose the signal filter cutoff frequency from the list The signal filter is a 2nd order Bessel filter The appropriate setting for this filter should take the type and time scale of the experiment into account 2014 CH Instruments Inc Control Menu 137 5 14 Cell command This command opens a Cell Control dialog box Use this command to control purge stir and electrochemical cleaning settings You can also set the signal level of the stir line mercury drop collection prerun drops and stabilizing capacitor Click the Help button of the resulting dialog box for more information This command has a toolbar button The Cell command presents this dialog box Cell Control 3 E Control Level of Stir Line Active High C Active Low Cancel Immediate Stir Help Sti Time sec fio Ste SMDE Drops Before Run SS p Immediate Purge Stabilizing Capacitor Purge Tine sec 240 IV Automatic Setting CoO CG Op e n rus I 4Electodes m Immediate Cel fe _ Mereury Drop Collection M Sp Between Run R Purge Between Run Number of Drop Ju E ep and Purge Soch D Time Intergal sec I Test with Internal Dummy Cell Collect I Cell On Between Runs Retum to Init E after Run
139. elected Experimental Parameters Parameter Rane Techniques Potential V Tu ag ET Current A 0 020 25 peak 0 35 Sensitivity AW Izeg o Sampling Rate 1 MHz at 16 bitresolution 2014 CH Instruments Inc 25 CH Instruments Model 900D Series 12 10 Model 700E Series Bipotentiostat Techniques O wv e e Po DEET KEE EECH SG EC HE EE WEE EE GE DEET E EE SE E EE ee ee ME E EE E E EE E 2 Corresponding polarographic mode can be performed S Corresponding stripping mode can be performed Phase selective data are available Dynamic Range of Selected Experimental Parameters Parameters LI Range JL Techniques Current A 0 to 20 25 one channelony Current A 0 to20125 dualchanne 102100 1 both channels Me O Frequency Hz 0 00001 to 1000000 IMP Dual channel measurements are available for CV LSV SCV CA DPV NPV SWV and i t 2014 CH Instruments Inc 12 11 Model 800D Series Electrochemical Detector Techniques CV EE gt E E EE a e e WEEN Eo a e a e e o BE CH CA 800D 802D 810D 812D_ 820D 822D_ 830D 832D 840D 842D_ 850D 852D RS owo o e o e o e T e T e fee CC DPV 8 es NPV 8 DNPV amp SWV eS ACV 8 SHACV s Ht BEE DPA le DDPA EE TPA IPAD BE SSF me STEP Eo y cP eee CPCR ISTEP PSA ECN OC ee hes S a ae ae a SES Galvanostat DE control 0 10V out Full CV Simulator Limited CV Simulator iR Compen
140. en Click the Zero button to re zero the relative position of the corresponding axis at any time Click the Move button of the corresponding axis to move the stepper motor to the specified position in absolute or relative coordinates If the requested move hits the zero or full range limit a warning will be issued You can also use the scroll bar to move the stepper motor Every click on the left or right arrow on the scroll bar will move 1 100 of the full scale If you click and hold down the left or right arrow after finishing the last move the system will move in the requested direction until you release the mouse button This is useful for moving the stage while watching the position Piezo Stage Calibration The Piezo block used in the Model CHI920D needs to calibrate its motor before the first measurement Calibration is performed using the stepper motor because its travel distance is known Before calibration place four plastic washers on top of four stainless steel columns and underneath the rectangular stainless steel plate of the cell sample holder Use four nylon screws to mount the rectangular plate to four stainless steel columns This is because during calibration a voltage will be applied to the metal plate through counter and reference electrode clips The rectangular plate must be totally isolated from the positioner base which is grounded Four plastic washers and four nylon screws are provided when the instrument is shipped A
141. en the original data and the fitted baseline When Baseline is selected the fitted baseline data will be saved View Baseline This button plots the original data and the fitted baseline together to evaluate the fitting results Use this command to preview the quality of the baseline fit The original data remains unchanged Use the Present Data Plot command under the Graphics menu to display the original data If peak defining lines obstruct your view you can turn off the Screen Baseline option by using the Graph Options command under the Graphics menu View Difference This button plots the difference between the original data and the fitted baseline This is helpful when evaluating the fitting results Use this command to preview the quality of the baseline fit The original data remains unchanged Use the Present Data Plot command under the Graphics menu to display the original data 2014 CH Instruments Inc 190 CH Instruments Model 900D Series 7 7 Linear Baseline Correction command This command opens the Baseline Correction dialog box Use this command to visually correct the baseline of the currently active data You can compensate a sloped baseline and shift the DC level of the curve The Linear Baseline Correction command presents this dialog box Baseline Correction E xi OK Cancel rel To perform baseline correction click the OK button first The mouse cursor will change to an up arr
142. enseesenees 166 6 13 X Plot COMMANG Eege cde cece dtececes KE i eaeedtee eden duue ev edecteedenaceceds dua svelecueevesucpaveesuvees 167 6 14 Peak Parameter Plot COMMANGA c ceeesceceeeeeeeeeeeeeeeeeeeseeeeneseeeeeeeseeeeeeseeeeeenseeseneeneenaeees 169 6 15 Semilog Plot COMMANG cccccceeeeeeeeeeeeeeeeeeeeeeeeeeeseeeeeeeseeeeeeeseeeeeeseeeeeeseeeeeeeseeseeeeseesanees 171 6 16 Special Plot Gommand Zuse VEKEEEEENEEREREVEEEEEENEEEEEEEEENEEEEENEEE EE nnmnnn nenna nennen nnmnnn nnmnnn nnn 172 6 17 Graph Options COMMANA ccceeeeeeeeeeeeeeeeeeeeeeeeeeeseeeeeeeseeeeeeeseeeeeeeseeeneseeeeneeseeeeeeeseeeaeees 173 6 18 Color and Legend COMMANGA cececeeeeeeeeeeeeeeeeeeeeeeeeneeseeeeeeeseeeeeeeseeaeeseeeeneeeeeeeeenseenanees 176 6 19 F n command iraner ae ERTA EENAA TRAIRA TEENETE ATERA E ATESA ANA 178 6 20 Copy to clipboard cCOoMmMand s ssssssssssnsunnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnn nn RREE EE EREE EE EREE EEN 179 Chapter 7 DataProc Menu 181 7 1 Smoothing COMMANGA cece cence cece ee ee ee eee ee ee ee EEEE ERR EEEE ERR eee ERR EEEE RRE nennu nnmnnn mennene 182 7 2 Derivatives COMMANG ccccceeeeeee cece ence eee eeeeeeee ee ERR EEEE eeeeeeeeeeseeeeeeeseeeeeeseeeseeesseeseeeseeeeeeeses 184 7 3 Integration COMMANG ceceeeeeee cece ee eeeeee eee ee seen RRE KEE eeeeaeeeeeeeaeeeeeseeaseeseeeseeesseeseeeseeeeeeees 185 7 4 Semiinteg and Semideriv COMMANA ccccceeeeeceeeeeeeeeeeeeeeeee
143. ensitivity A V E2 On i2 On Probe Stop No Abs Current A Mode Frequency Hz Amplitude V Bias DC Current AutoSens Scan Direction Const Current A Current Tolerance Max Z Incr um Travel Distance um 100 Constant Current I 1e 009 J i Incr Dist um eer 0 5 d Current Tolerance 5 1 be MaxZ Ines um zz nerimas eee 0 02 S irs Quiet Time lgl 2 Range Description 10 10 First probe potential 1e 12 0 1 Probe sensitivity scale 10 10 Probe pulse potential 0 10 Pulse duration 0 1 50 Delay time after pulse before sampling Check or Uncheck Probe pulse potential on off 10 10 Substrate potential 1e 12 0 1 Substrate sensitivity scale Check or Uncheck Substrate potential on off Check or Uncheck Substrate current measurement on off Select or Unselect Manually stop probe motion O 0 01 Probe will stop at the specified current threshold Select Amperometry potentiometry constant current or impedance 1 1000000 AC frequency 1e 5 0 7 AC amplitude Check or Uncheck Enable DC current bias during run Check or Uncheck Enable automatic sensitivity scale impedance only Select Scan X Y or Z direction 5e 12 1e8 Constant current control value 0 01 5 Allowed current tolerance for constant current control 0 0001 10 Maximum increment in Z direction 2014 CH Instruments Inc Setup Menu Motor Selection Select Auto stepper or piezo Travel Dist um 50000 5
144. ent oy DH A eck haest W CH Instruments inc Made in U S A Signals 1 Power switch On off switch of unit 2 Fuse State fuse value here 3 Power input socket IEC type connection socket for mains cable 4 Cooling fan Fuse rating 0 8 A for 110V AC input 0 4 A for 230V AC input Power cord rating 15 A for 110V AC input 10 A for 230V AC input All other features are clearly labeled on the rear panel itself 2014 CH Instruments Inc 250 CH Instruments Model 900D Series 2014 CH Instruments Inc Appendix 12 7 Abbreviations of Electrochemical Techniques ACV AC Voltammetry including phase selective BE Bulk Electrolysis with Coulometry CA Chronoamperometry CC Chronocoulometry CP Chronopotentiometry CPCR Chronopotentiometry with Current Ramp CV Cyclic Voltammetry DDPA Double Differential Pulse Amperometry DNPV Differential Normal Pulse Voltammetry DPA Differential Pulse Amperometry DPV Differential Pulse Voltammetry ECN Electrochemical Noise Measurement FTACV Fourier Transform AC Voltammetry HMV Hydrodynamic Modulation Voltammetry IMP Impedance Spectroscopy IMP t Impedance Time IMP E Impedance Potential IPAD Integrated Pulse Amperometric Detection ISTEP Multi Current Steps i t Amperometric i t Curve LSV Linear Sweep Voltammetry NPV Normal Pulse Voltammetry OCPT Open Circuit Potential Time PSA Potentiometric Stripping Analysis QCM Quartz Crystal Microbalance SCV Staircase Vo
145. ents Inc 134 CH Instruments Model 900D Series 7 2 Derivatives command This command opens the Derivative dialog box Use this command to compute the numerical derivative of the currently active data After performing a first order derivative the Y axis has dimensions of Y unit X unit A V for voltammetry A s for i t curves etc The new unit is not explicitly expressed but you should be aware of it This command has a toolbar button The Derivatives command presents this dialog box Derivative S Derivative Order OK 1st Order Derivative Cancel 1st Order Derivative 2nd Order Derivative 3rd Order Derivative 4th Order Derivative 5th Order Derivative Least Square Point E DI IV Override Present Data rel Help Derivative Order Up to fifth order derivatives can be taken Least Square Point Derivative computation requires an odd number of points between 5 and 49 More points will result in better smoothing but may also cause distortion Numerical differentiation will inherently amplify high frequency noise so a relatively large number of points should be considered More points will result in less noisy derivative data but may also cause distortion The program performs numerical differentiation using the algorithm of Savitzky and Golay For more details about the Savitzky and Golay algorithm please refer to Smoothing and Differentiation of Data by Simplified Least Squares Procedures Anal C
146. eqs 0O 100 Number of points per decade frequency Bias DC Current off range on Enable DC current bias during run Notes e Above 100 Hz both current and potential are measured in order to calculate impedance 12 frequency components per decade will be measured In the Fourier transform case each measurement covers a decade of frequency range Below 100 Hz only current is measured The applied potential is assumed to have no extra phase shift and be accurate e When DC current is high and AC current is low sensitivity cannot be increased because the DC current will overflow This problem is more serious when the frequency is relatively low The application of a DC current bias allows higher AC signal amplification A 16 bit DAC is used for this purpose On the other hand if the DC current is not expected to be large and the frequency is high a DC current bias may be unnecessary The power line frequency 50 or 60 Hz depending on your region can interfere with measurements Use a longer measurement time between 1 100Hz to improve data quality of this frequency range 2014 CH Instruments Inc Setup Menu e e Automatic sensitivity scale is used by default The sensitivity scale setting can also be manually overridden by clicking the Manual button top open the Manual Sensitivity Setting dialog box 2014 CH Instruments Inc CH Instruments Model 900D Series 4 2 24 Impedance Time Parameters dialog box In the Impe
147. er capacitance of the working electrode is large such as in bulk electrolysis or when a high degree of iR compensation is required When the Automatic Setting box is checked default the system will manage the stabilizing capacitor without user intervention uncheck this box to manage the stabilizing capacitor manually with the radio buttons in this section Mercury Drop Collection This useful option allows you to collect and weigh mercury drops Specify the number of drops you want to collect from 1 to 1000 and the time interval between drops from 0 5 to 10 and click the Collect button to activate the collection process 4 Electrodes Check this box to set the potentiostat in 4 electrode mode The 4th electrode is used for sensing the voltage drop due to the contact resistance of the electrode clip connector relay and circuit board traces The contact resistance can be about 0 2 0 3 ohm and can cause a 50 75 mV voltage drop if the current is 250 mA making low impedance cell measurements impossible e g battery With the addition of the 4th electrode the effect of contact resistance can be eliminated and low impedance cells can be readily measured The 4th electrode can also be used for liquid liquid interface measurements In the first liquid phase the red clip is connected to the counter electrode and the white clip is connected to the reference electrode In the second liquid phase the green clip is connected to the coun
148. erence electrodes and two auxiliary electrodes The modified potentiostat controls the potential difference between 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 user friendly Most electrochemical techniques can be used albeit without galvanostat or bipotentiostat functions This is a legacy accessory for the model 700A series Liquid liquid interface measurement capabilities using 4 electrode configuration are built into our model 400 A B 600A B C D 700B C D 800B C 900B C and 1100 A B series instruments with no need for the CHI682 Liquid Liquid Interface Adapter 2014 CH Instruments Inc CH Instruments Model 900D Series 12 19 Accessories Part No Description Unit Hectrode Hectrode 5 12 5 um dia Gold Microelectrode P 12 5 um dia Gold Microelectrode 5 um dia Gold Microelectrode 5 um dia Gold Microelectrode P 10 umdia Platinum Microelectrode P 25 um dia Platinum Microelectrode Ag AgCl Reference Electrode 3 pk Non Aqueous Ag Ag Reference 1 Hectrode 1 CHI112P Non Aqueous Ag Ag Reference 3 pk Hectrode 1 CHI115 Platinum Wire Counter Electrode CHH16 10 mmm dia Platinum SECM Tip CHI116P 10 mmm dia Platinum SECM Tip i ok 3 3 Q SI IS IL L als S t hg a x IS eR IS P CHI112 OO Q
149. ers dialog box In the AC Impedance technique IMP the base potential is held constant at Init E A sine waveform is superimposed onto the base potential and its frequency is scanned from high to low with 12 components per decade Current and potential are sampled and analyzed to obtain the real and imaginary parts of the impedance During the experiment you can switch between a Bode plot and a Nyquist plot by right clicking After the experiment impedance data can be presented in various forms The following diagram shows the potential waveform applied as a function of time Amplitude xX Init E Potential V High Freq Low Freq Time s Parameter Range Description Init E V 10 10 Initial potential High Freq Hz le 4 Zep High frequency limit Low Freq Hz te 5 1e5 Low frequency limit Amplitude V te 5 0 7 A C amplitude Quiet Time s O 100000 Quiescent time before potential scan Sensitivity Scale Select Automatic or Manual Meas Mode FT Single Galv Select measurement mode above 100 Hz Avrg 1K 1M Hz 0 1 4 Average factors Avrg 1 999 Hz 1 256 Average factors Cycles 0 1 1 Hz 1 25 Number of cycles at each frequency point Cycles 0 01 0 1 1 25 Number of cycles at each frequency point Cycles 1e 3 1e 2 1 25 Number of cycles at each frequency point Cycles 1e 4 1e 3 1 16 Number of cycles at each frequency point Cycles 1e 5 1e 4 1 4 Number of cycles at each frequency point Points all fr
150. ers x m Probe Electrode OK a Probe E1 MI E em Hold Time 1 el jo pEi Probe E2 V fo Help Hold Time 2 s 0 1 Sensitivity AZV 1 e 008 e Substrate Electrode Create New Pattern Substrate E1 V jo Substrate E2 V fo V Return to Origin after Run Sensitivity A V 1 e 008 e Boo m Motor Selection Ge Auto Stepper C Piezo Probe Travel x Distance um ft DU Long Travel Direction Y Distance um D ft 00 Ze X Axis as Long Direction Incr Dist um fi C Y Asis as Long Direction Parameter Range Description Probe E1 V 10 10 First probe potential Hold Time 1 s O 4000 Hold time at first probe potential Probe E2 V 10 10 Second probe potential Hold Time 2 s 0 4000 Hold time at first probe potential Sensitivity A V 1e 12 0 1 Probe sensitivity scale Substrate E1 V 10 10 First substrate potential Substrate E2 V 10 10 Second substrate potential Sensitivity A V 1e 12 0 1 Substrate sensitivity scale E On Check or Uncheck Substrate potential on off control X Distance um 50000 50000 Probe travel distance in X direction 2014 CH Instruments Inc CH Instruments Model 900D Series Y Distance um 50000 50000 Probe travel distance in Y direction Incr Dist um 0 0001 100 Probe increment distance during scan Create New Patt Button Click to create new pattern Return to Origin Che
151. es 2014 CH Instruments Inc zas CH Instruments Model 900D Series 9 1 5 Concentration at Equilibrium dialog box This informational dialog box allows you to view the equilibrium concentrations computed by the CV simulator Concentration at Equilibrium All steps of the reaction mechanism are listed on the left The equilibrium concentration of each species is displayed on the right 2014 CH Instruments Inc Sim Menu z9 9 1 6 Simulation Variables dialog box This dialog box allows you to specify selected CV simulation parameters x Simulation Yariables Temperature Deg C 25 Electrode Area cm2 1 Capacitance lut Temperature Enter the temperature in Celsius here Both thermodynamic and kinetic parameters depend on 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 and 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 2014 CH Instruments Inc 220 CH Instruments Model 900D Series 9 2 AC Impedance Simulator and Fitting Program An impedance simulator is integrated into the program To use the impedance simulator you need to set Technique to AC Impedance IMP and then use the Mechanism command to e
152. es open data files read directly from binary or plain text files save data file binary plain text formats for exporting data e g to spreadsheet list data file convert to text files for exporting multiple data files text file format print present data print multiple data files print setup Experimental Setup technique a large repertoire of electrochemical techniques experimental parameters extremely wide dynamic range system setup line frequency potential current axis polarities hardware test digital and analog circuitry diagnostic test Instrument Control e run experiment real time data display in most cases e pause resume during run e stop running experiment e reverse CV scan direction during run e repetitive runs automatic data save signal averaging delay or prompt e run Status stir purge smooth after run iR compensation RDE and SMDE control status e macro commands edit save read and execute any series of commands open circuit potential measurement e working electrode conditioning before running experiment e analog filter settings automatic or manual setting of UV converter potential and signal filters e stripping mode enable disable deposition potential and time stir and purge conditions e cell control purge stir cell on SMDE drop collection pre run drop knock and stabilizing capacitor e rotating disk electrode rotation speed on off control during deposition quiescent time run
153. evice 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 settings or connection cables might be needed 2014 CH Instruments Inc 2 CH Instruments Model 900D Series 12 2 Firmware Update Instructions The instrument is controlled using software on the PC side and updates will often be as straightforward as replacing chi exe with a newer version Occasionally however the instrument firmware will also need to be updated The instrument firmware is now stored in flash memory allowing it to be distributed electronically rather than through the inconvenient mailing of an EPROM chip Software and firmware are both available from info chinstruments com Software installation is described in Chapter 2 of this User Manual Firmware updates are distributed in the form of a hexadecimal file chi hex where is the model number To initiate a firmware update use the Update Instrument Program command under the File menu to bring up the following dialog box Update Flash Memory in the Instrument Ed Filename C CYGNAL chi660d hex Browse Update Click the Browse button to select the appropriate hex file or type its name and full path in the Filename field Click the Update button to upload the hex file to the instrument flash memory During the upload please be patient and wait Please do n
154. ezo positioner Otherwise the stepper motors will be used If the piezo positioner is selected but the X or Y distance exceeds the piezo range the stepper motors will be used instead A maximum of 512 x 512 pixels per image is allowed If the number of data point in a dimension exceeds 512 its increment distance will be automatically adjusted Xand Y distances cannot be zero At least two points are needed in each direction 2014 CH Instruments Inc Setup Menu 4 2 33 Probe Scan Curve Parameters dialog box In this technique the SECM probe is scanned in the X Y or Z direction and the resulting probe and or substrate current is measured Both the potential and sensitivity of the probe and substrate electrode can be controlled independently The probe electrode can also be subjected to a pulse of specified potential and duration for electrochemical cleaning prior to data sampling The substrate electrode can be turned on or off Scan increment distance and increment sampling time can also be specified Optionally a probe scan can be aborted if the measured current exceeds the specified thresholds for the purpose of probe protection Several measurement modes are available When performed in the Xor Y direction amperometry potentiometry and impedance modes maintain constant probe height Amperometry measure probe current as a function of position Potentiometry measure probe potential as a function of position Consta
155. f the calibration curve for each species to calculate the concentration of the compound A value must be specified for each species Peak Shape Select the peak shape that is most appropriate for your data The currently available choices are Gaussian diffusive and sigmoidal Data Type Choose between original data semi derivative and first derivative to report the concentration Number of Species Enter the number of species for the data file report Concentration Unit Enter the units dimension of concentration e g ppm or M Report Filename Enter the report filename if you want to save the report text file If a file with the specified name already exists an overwrite warning will be issued If no filename is specified the report will be shown but not saved Report Data Type Either concentration or peak current can be reported Header Enter the desired title header for the data To display the header on the top of the plot check the Header box using the Graph Option command Note Enter any comments about the plot The note will not be displayed on the plot but will be saved in the data file It allows you to put additional comments about the data and is well suited for a brief description of the purpose and conditions of the experiment Read Use this command to read data from file Save Use this command to save data to file XY titles units header and note will be saved along with the data Report
156. f the tip is over the insulating part of the surface current will drop as the tip approaches the surface If the tip is over the conducting part of the substrate current will increase as the tip gets approaches the surface Tip approach will stop when the specified threshold current ratio or level is reached The threshold current ratio should be less than 100 for insulators and greater than 100 for conductors if the current ratio is improperly specified approach will stop at a current ratio of 75 or 125 Once the tip is close to the surface you can use the Probe Scan Curve PSC technique to scan across the sample surface For a platinum substrate electrode it is useful to find the boundary between the insulator and the conductor A good test is to image this boundary If the tip is close to the leftmost boundary a standard SECM scan of 80 um x 80um using Xas the long axis should reveal a vertical boundary because your scan area is much smaller than the curvature of the disk electrode If you move the tip to the frontmost edge and image using Y as the long axis you should see a horizontal boundary line Check your PAC PSC and SECM images to verify the correct operation of your SECM instrument These are not very exciting images or curves but they constitute a good test of the instrument 2014 CH Instruments Inc Getting Started 27 2 4 Some Useful Tips If you are comfortable with Windows applications you may not have any p
157. fter the initial calibration please save them for future use in case calibration is needed again Insert the stainless steel pin with 10K ohm resistor also shipped with the instrument into the probe holder Then position the metal pin so that it is close to the base metal plate of the cell sample holder Please see the figure below for an illustration of the pin position The small circle indicates one of the small holes around the center round opening of the base metal plate For X and Y calibration the sharp pin end should be moved below the metal plate surface For X calibration the pin will move to the right and use the wall of the hole to make electrical contact For Y calibration the pin will move to the front and use the wall of the hole to make electrical contact For Z calibration the pin should be placed slightly above the base metal plate The pin will move down and use the base metal plate to make electrical contact 2014 CH Instruments Inc wa CH Instruments Model 900D Series O X Calib Y Calib Z Calib Relative position of metal pin and base metal plate for piezo calibration Connect the working electrode clip green to the resistor attached to the metal pin Connect the counter red and reference white clips to the metal base This configuration will allow current to flow when the pin contacts the base metal plate During calibration the motor will move in the negative direction first The positive direct
158. g spectroscopic signals simultaneously with the voltammogram maximum scan rate may be limited Use the 9 pin D connector on the rear panel for signal input Consult the User s Manual for the pin out and signal level requirements When the second electrode is in Scan mode it will have the same potential as the primary electrode throughout the experiment The potential of the second electrode is therefore not independent When the second electrode is enabled the maximum scan rate is reduced to 100 V s and the sampling interval will be doubled at high scan rates When the second electrode is enabled the auxiliary signal recording channel will be disabled 2014 CH Instruments Inc Setup Menu 55 4 2 2 Linear Sweep Voltammetry Parameters dialog box In Linear Sweep Voltammetry LSV the potential is scanned from Init E toward Final E The following diagram shows the potential waveform applied as a function of time Current is recorded as a function of potential Final E E 2 O A Scan Rate V s Time s Parameter Range Description Init E V 10 10 Initial potential Final E V 10 10 Final potential Scan Rate V s 1e 6 20000 Potential scan rate Sample Int V 0 001 0 064 Data sampling interval Quiet Time sec 0 100000 Quiescent time before potential scan Sensitivity A V 1e 12 0 1 Sensitivity scale Auto Sens Check or Uncheck Automatic sensitivity switching during run Aux Signal Rec Chec
159. he instrument and the Amp Booster It is generally good practice to turn the instrument on before the Amp Booster and to turn the Amp Booster off before the instrument The cell connector is a 6 pin connector with four cell leads The green white and red clips correspond to the working reference and counter electrodes respectively The black clip is for the sensing electrode of the 4 electrode configuration which can be turned on or off with the 4 Electrodes box using the Cell command under the Control menu When the 4 electrode option is on you should connect the sensing lead to the working electrode short the green and black leads together The 4 electrode configuration is useful for liquid liquid interface or high current measurements It helps eliminate the resistance about 0 2 0 3 ohms due to the connectors relays and printed circuit board traces If you think there might be something wrong with the hardware please conduct a hardware test with the Amp Booster disconnected If the instrument passes the test then connect the Amp Booster and test it with a standard resistor For instance conduct a CV experiment and verify that a straight line with a slope of voltage resistance is correctly obtained CHI682 Liquid Liquid Interface Adapter Liquid liquid interface studies are very important in applications involving charge transfer chemical sensing drug release and solvent extraction among others This typically involves two ref
160. hem 36 1627 1639 1964 Override Present Data Check this box to replace the currently active data with the resulting derivative data If this box is not checked the derivative data will only be displayed without overriding the currently active data and invoking the Present Data Plot command will display the original data 2014 CH Instruments Inc DataProc Menu 18 7 3 integration command This command opens the Integration dialog box Use this command to integrate the currently active data After performing integration the Y axis has dimensions of Y unit x X unit A V for voltammetry coulombs for i t curves etc The new unit is not explicitly expressed but you should be aware of it The Integration command presents this dialog box x OK M Qvernde Present Date Cancel Le e Override Present Data Check this box to replace the currently active data with the resulting integrated data If this box is not checked the integrated data will only be displayed without overriding the currently active data and invoking the Present Data Plot command will display the original data 2014 CH Instruments Inc 136 CH Instruments Model 900D Series 7 4 Semiinteg and Semideriv command This command opens the Semi derivative and Semi integral dialog box Semi derivatives and semi integrals can be used for a variety of purposes For instance the semi derivative can be used to convert a diffusive peak to
161. high scan rates When a large number of sweep segments is involved the data sampling interval will be automatically increased up to 0 02 V If the scan rate is higher than 0 5 V s or 3 V s using fast com port speed the number of sweep segments will be limited by the instrument memory size 64K points If the scan rate is lower than 0 5 V s or 3 V s using fast com port speed the maximum data length specified by the System command will take effect When the scan rate is low the specified sweep segments will be executed but only a limited number of segments will be stored Large sweep segments can be useful for say electrode conditioning When the scan rate is below 0 01 V s the sensitivity scale during the run can be automatically adjusted according to the current level When Auto Sens is enabled the value of the Sensitivity field will have no effect on the measurement However the smallest available automatic sensitivity will be 1e 6 A V instead of 1e 12 A V The Picoamp Booster will not work either In order to specify smaller sensitivities the automatic sensitivity switching option must be disabled The Enable Final E option will allow you to scan complete cycles when the number of Sweep Segments is odd and Initial E is different from High E and Low E Check the Enable Final E box and set Final E equal to Initial E and the last segment will stop at Initial E instead of High E or Low E It is possible to record external voltage signals e
162. his box is not checked the operated data will only be displayed without overriding the currently active data and invoking the Present Data Plot command will display the original data 2014 CH Instruments Inc 196 CH Instruments Model 900D Series 7 13 Fourier Spectrum command This command opens the Fourier Spectrum dialog box Use this command to obtain the Fourier spectrum of the currently active data The Fourier Spectrum command presents this dialog box Fourier Spectrum x x Scale Y Scale C nth R n a ies Cancel Bees Cer a e Hel Cary Logrithmic Help IV Override Present Data X Scale The X data array of the Fourier spectrum can have an nth component a 1 s scale or a 1 V scale depending on your choice An nth component scale is generally used It is available for all techniques Its physical meaning is derived 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 CV and LSV experiments are special cases both 1 s and 1 V scales can be used here Y Scale The Y data array contains the Fourier coefficients and can have either a linear or logarithmic scale Override Present Data Check this box to replace the currently active data with the Fourier spectrum data If this box is not
163. hn This is used in a For Next loop to select the channel according to the For Next loop counter The minimum number of channels for the CHI684 is 8 The channel increment is 8 The maximum number of channels is 64 2014 CH Instruments Inc 12 18 Amp Booster and Liquid Liquid Interface Adapter CHI680C Amp Booster With the CHI680C Amp Booster current can be measured up to 2 A The CHI680 is compatible with our Model 600 A B C D series instruments The CHI680C is compatible with our Model 600D E series of instruments You can stack the CHI600D E and the CHI680C together The CHI680C can also be connected to the model 700E series but it will only work for the primary channel When the Amp Booster is connected cell control signals such as purge knock and stir will be disabled The Amp Booster will also allow low current measurements You may need to use a Faraday cage to eliminate line frequency noise when the scan rate is above 50 mV s The frequency response of the Amp Booster is somewhat lower than that of the 600 A B C D E For high speed experiments the Amp Booster should be disconnected Before connecting the Amp Booster turn the instrument power off Connect the 6 pin connector of the Amp Booster to the Electrodes connector on the rear panel of the CHI6xxD Also connect the Cell Control ports of the Amp Booster and the instrument with a straight through DB 25 cable included You can then turn the power on for both t
164. hoose Rows and click Next The ChartWizard Step 3 of 4 dialog box will appear Enter descriptive labels and change graph options as desired Click Finish when done 10 A 3D surface plot will appear in the spreadsheet data area You can resize the plot by left clicking RON OO OO JO Om 2014 CH Instruments Inc File Menu and dragging on the edges of the plot 11 Copy and paste the graph into a word processor for further usage or printing Exporting the graph to a picture format like JPEG or PNG e g by pasting in Paint and inserting the resulting picture into a word processor document will generally reduces the final file s size but will also lower the resolution of the plot If the data density is so high that the lines between data points cannot be seen clearly set the data point interval to more than 1 as described above Nanoscope Header This option applies only to SECM image data CHI 900 series When this box is checked the output text data file will be directly readable by Nanoscope Veeco Instruments Inc Santa Barbara CA software to create a 3D image However as Veeco Instruments frequently updates their Nanoscope software your generated text file may not be readable if your version of Nanoscope is older than the CHI 900B series software 2014 CH Instruments Inc a2 CH Instruments Model 900D Series 3 9 Import Text File command This deprecated command opens the Import Text Fi
165. hould be reset to 0 after e4incr 1 1 increment e4 in for loop should be reset to 0 after e5incr 1 1 increment e5 in for loop should be reset to 0 after e6incr 1 41 increment e6 in for loop should be reset to 0 after e7incr 1 1 increment e7 in for loop should be reset to 0 after e8incr 1 1 increment e8 in for loop should be reset to 0 after sequential sequential measurements simultaneous simultaneous measurements indcell independent cell onecell single cell with common reference and counter For a complete list of technique specific macro commands please consult your chm or hlp help file 2014 CH Instruments Inc 132 CH Instruments Model 900D Series 5 11 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 is flowing through the cell This is an important parameter It gives you information about the initial conditions before you start the experiment You can then figure out if the compound under study is oxidizable or reducible After the measurement the program will display the open circuit potential value through the Open Circuit Potential dialog box Open Circuit Potential Measurement x Open Circuit Potential DM fi 210 2014 CH Instruments Inc Control Menu 133 5 12 iR Compensation command This command opens the iR Compensation dialog b
166. ht indicates that the tip has moved upward downward Before the measurement the Z piezo will be set to its middle position and the specified constant current level will be reached with a combination of stepper motor and piezo movements Once the scan starts only the Z piezo will be adjusted to keep the current constant Since the Z piezo has a maximum range of about 80 microns and its start position is at the middle its maximum adjustable range is 40 microns If a Z move exceeds 40 microns a warning will appear and the scan will be terminated At the end of a scan in Constant Current mode the Z piezo will be set back to the zero position Constant Current mode is not available for a Z probe scan cure 2014 CH Instruments Inc ER CH Instruments Model 900D Series 4 2 34 Probe Approach Curve Parameters dialog box This technique carefully moves the SECM probe towards the surface of the substrate and measures the resulting current response Probe current is always measured the substrate electrode can be optionally monitored Both the potential and sensitivity of the probe and substrate electrode can be controlled independently The probe electrode can also be subjected to a pulse of specified potential and duration for electrochemical cleaning prior to data sampling The substrate electrode can be turned on or off The maximum increment distance the increment sampling time and the probe current ratio or absolute current level fo
167. ialog box The Mechanism command presents this dialog box This section of course applies only when the A C Impedance technique is not active l Mechanism Edit Mechanism Select Square Scheme Cancel Help OK 2 Lei He a LC Ss Empan ie Se Entin Esc Read Save Exp Param Kinetics System under study Diffusive D Conc S Equilibrium Dimensionless current 3 Variables Iw Display concentration profile during run Cone Range H Dist Range 1 Time Delay Loop usec fo Before running a simulation use this dialog box to set the reaction mechanism species concentrations kinetic experimental and other parameters All settings can be saved to and read from file The equilibrium concentration can also be checked Mechanism Edit This edit box allows you to edit the reaction mechanism The Mechanism Select list contains several pre defined mechanisms which when clicked automatically fill out the Mechanism Edit box Type directly in the edit box to input a user defined mechanism select models only To write your own mechanism use a single letter A Z to represent each chemical species The letter e is reserved for electron transfer The program will treat uppercase and lowercase letters as identical and ignore any spaces The program can simulate any reasonable combination of electron transfer 1st order and 2nd order chemical reactions up to 11 reactions and 9 chemical species
168. ied out with a potentiostat frequency counter which is in turn controlled by a personal computer The 400C 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 440C only The QCM is integrated w ith the potentiostat and galvanostat to facilitate simple and convenient EQCM studies Instead of measuring the frequency directly the 400C series uses a time resolved mode as follows The observed frequency of the QCMis subtracted froma standard reference frequency and the resulting difference is measured by a reciprocal technique greatly reducing the required sampling time and yielding much better time resolution for the QCM signal With direct counting a QCM frequency resolution of 1 Hz requires 1 second of sampling time 0 1 Hz resolution requires 10 seconds etc In contrast our time resolved mode allow s the QCM signal to be measured in milliseconds w ith much better resolution QCM data can be recorded for a scan rate of 1 V s or lower The EQCM cell consists of three round Teflon pieces see Figure below The total height is 37 mm with a diameter of 35 mm The top piece is the cell top which holds the reference and counter electrodes There are also two 2 mmholes for manual purging The center piece is the solution cell and the bottom piece is for mounting purposes Four screws are used to tighten an
169. iental Windows When set to Oriental the program will use u instead of p Erase ADC Calibration Coefficients The analog to digital converter ADC calibration coefficients are stored in the instrument s non volatile memory ADC calibration is carried out in the factory before the instrument is shipped Use this command only if you want to recalibrate the ADC yourself To do so simply click this button and the program will automatically prompt you to calibrate the ADC during the next hardware test or experiment Data Length requires program restart The default data length is 128K It is recommended not to use longer data lengths unless necessary Longer data lengths will require more computer resources slow down your PC and may prevent other programs from running After changing this setting please exit and restart the program otherwise the program may crash If data are acquired and saved with a longer data length but read back with a shorter data length the program may also crash To prevent this if the data length has been increased it should not be decreased to a smaller value later Please take this into consideration before you decide to increase the data length Save retrieve data during run This option allows data to be saved on the PC hard drive during an experimental run In case your experiment does not run to completion e g due to external interference interruption or missed communication data can be recovered p
170. iew Difference r Baseline Fitting Algorithm and Orders Baseline Fitting Orders P Orthogonal L S C Least Square r Save to Override Original Data NoAction Difference Baseline The following options allow you to select fitting parameters and data file options Two sides of Peak Foot When fitting the baseline data points corresponding to peaks must not be included In a mountaineering analogy the user must mark off the feet data interval of each peak Adjusting peak foot values can 2014 CH Instruments Inc DataProc Menu 189 improve your baseline fit If there are multiple peaks feet need to be specified for each peak up to 5 or alternatively you can also specify a large potential or time range covering several peaks Baseline Fitting Algorithm and Orders Orthogonal Least Square and Least Square algorithms are available for fitting the baseline both utilizing polynomial fits The Baseline Fitting Orders field specifies the order of the polynomial fit first order stands for linear fitting aX b second order stands for aX bX c fitting and so on Save to Override Original Data This option determines what data are output upon clicking the OK button When No Action is selected the original data will be plotted with the fitted baseline and the original data remains unchanged When Difference is selected the original data will be replaced by the difference betwe
171. ile you want to save as When saving in the txt or csv formats a corresponding bin file will be generated unless a binary file is currently open The use of binary files is encouraged since they contain many system parameters that are not stored in other formats Extension Description bin Binary data files recommended txt Plain text files compatible with most other programs CSV Commaz separated value files useful for spreadsheet programs 2014 CH Instruments Inc File Menu 33 For a macro file the extension is mcr For a simulation file the extension is sim Other extensions are not allowed 2014 CH Instruments Inc 34 CH Instruments Model 900D Series 3 3 Delete command Use this deprecated command to delete files permanently via the File Delete dialog box The Delete command bypasses the Recycle Bin that has been available starting with Windows 95 and its use is discouraged for all but the audacious and the accustomed To send one or more files to the Recycle Bin unless it has been disabled in your Windows system settings in the CHI program environment select the desired file s in the say Open or Save As dialog box and press the Del key Windows will then prompt you for confirmation to send the file s to the Recycle Bin To delete files permanently in the same manner press Shift Del instead of Del The deprecated Delete command presents this dialog box File Deletion F 2 x Look
172. ill end normally Current Display during Quiet Time Specify whether the current during quiet time is displayed numerically graphically or not at all The sensitivity scale will be automatically adjusted in order to read the current properly If No is selected the current will not be displayed during quiet time and the sensitivity will be the same as that used in the experiment 2014 CH Instruments Inc Control Menu 121 5 8 Repetitive Runs command This command opens the Repetitive Run dialog box Use this command to run an experiment multiple times Before each run the program will first verify data link with the instrument aborting the series of runs if link fails The program will also verify the values of experimental parameters if illegal values have been entered the command will terminate and the program will issue an error message The Repetitive Runs command opens this dialog box Repetitive Run i x Number oh ME e fi Time Interval Between Runs sec fo Cancel m Prompt Before Each Run Help Ge None Manual External Trigger Base Filename _ C Achistest smpl Browse IT Data Averaging When Done Number of Runs Enter the number of runs the parameter range is 1 9999 Time Interval Between Runs Specify the time delay between two successive runs the parameter range is 0 32767 This parameter is ignored if Prompt Before Each Run is enabled Prompt Before Each Run If Manual i
173. iment instead of using the Retrieve command In order to enable the Retrieve command use the System command under the Setup menu and check the Save retrieve data during run option Data from the previous run must be retrieved before starting a new run Once a new run has started the saved data for the last run will be lost and cannot be recovered 2014 CH Instruments Inc s CH Instruments Model 900D Series 3 5 Update Instrument Program command This command opens the Firmware Update dialog box Control of the instrument control is accomplished by two interacting components the software that resides on the PC and the firmware that resides on the instrument This command available in all of our newer models with flash memory allows the user to install firmware updates which are issued occasionally by CH Instruments Inc For more information about software and firmware updates please consult the Appendix of this User Manual or contact info chinstruments com 2014 CH Instruments Inc 3 6 File Menu List Data File command This command opens the List Data File dialog box Use this command to display a saved data file in text mode Formatting options are available in the Text File Format command The current data remains unchanged when this command is executed To view the current data similarly use the Data Listing command under View menu The List Data File command presents this dialog box List Data File 2
174. ing laboratories The Model 1200B series allows 7 5 V compliance voltage which ensures its w orking potential range of 2 4 V for most electrochemical systems it also uses dual 16 bit DAC and 16 bit ADC for high resolution and accuracy The model 1200B series potentiostats 12x0B 1205B and 1207B and bipotentiostats 12x2B 1206B and 1208B are offered in several models tailored to meet a wide range of applications and budget levels Specifications Potentiostat bipotentiostat CV and LSV scan rate 0 000001 to 10 V s Potential range 2 4 to 2 4 V CA and CC pulse width 0 001 to 1000 sec Compliance voltage 7 5 V CA and CC Steps 1 320 Current range 2 mA DPV and NPV pulse width 0 001 to 10 sec SWV frequency 1 to 5000 Hz F 12 Ref l m nce 1 ohm eference electrode input impedance 10 ACV frequency 0 1 to 2000 Hz Sensitivity scale 10 0 001 A V in 7 ranges Low pass filter for current measurements Input bias current lt 100 pA Data length 128K 4096K selectable Current measurement resolution lt 1 pA Chassis dimensions 7 W x 4 5 D x 1 H Data acquisition 16 bit 1 MHz Techniques for Model 1200B Series 1202B 1206B 1208B 1212B 1222B 1232B 1242B Cyclic Voltammetry CV T f T f f gt l Linear Sweep Votammetry auf 1 o Soo defe tt Chronoamperometry CA o Joo To o T IL Te Il Chronocoulometry CO LI T T SeSe oe Differential Pulse Votammetry mu lo TT tT tT Noma Puse vota
175. instrument power on The DB 25 connector provides power and control lines see Cables and Connections in the Appendix When the DB 25 connector is disconnected you can still do experiments with the Faraday cage although the Picoamp Booster will be disabled To purge inert gas unscrew one of the screws on the back of the faraday cage to open a hole for inert gas tubing When the Picoamp Booster is not in use please disconnect the DB 25 cable CHI684 Multiplexer The CHI684 is a multi channel multiplexer for the model 400 A B 600A B C D E 700A B C D E 800B C 900B C D and 1100A B C series The multiplexer switches four lines working sensing reference and counter for single channel potentiostats working 2nd working reference and counter for bipotentiostats You can have up to 64 cells but only one cell can be connected at a time The multiplexer is controlled using the Multiplexer command under the Control menu You can select any channel s and run experiments in a sequence of selected channels Data will automatically be saved to file after each run You can also be prompted before each channel run Arbitrary channels can be set immediately An experiment can then be run for that particular channel 2014 CH Instruments Inc 268 CH Instruments Model 900D Series Two Macro commands are available for the multiplexer One is mch which allows the user to choose an individual channel The other macro command is mc
176. ints visually Data Point Modifying Modify data points visually Background Subtraction Subtract background data from present data Signal Averaging Average multiple data sets Mathematical Operation Perform mathematical operation on X or Y data Fourier Spectrum Compute Fourier spectrum of data 2014 CH Instruments Inc 182 CH Instruments Model 900D Series 7 1 Smoothing command This command opens the Smoothing dialog box Use this command to smooth the currently active data This command has a toolbar button The Smoothing command presents this dialog box Sengen x m Method Selection o fe Cancel C Fourier Transform Smoothing Help Least Square Point 7 DI I Smooth After Fun ET Cutoff 1 s or 1 E Je Override Present Data The following options allow you to specify the smoothing method and corresponding parameters Method Selection Least square and Fourier transform FT smoothing options are available Least Square Point Least square smoothing requires an odd number of points between 5 and 49 More points will result in better smoothing but may also cause distortion The program performs least square smoothing using the algorithm of Savitzky and Golay For more details about this algorithm please refer to 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 cu
177. ion and Data Acquisition e Fast waveform update 10 MHz 16 bit e Fast data acquisition dual channel 16 bit ADC 1 000 000 samples sec simultaneously e External signal recording channel at maximum 1 MHz sampling rate 2D and 3D Graphics e Interactive visualization of SECM surfaces Color mapping e Laplacian smoothing e Stereoscopic 3D anaglyph imaging e High compatibility Window s 98 256 colors and up Other Features e Automatic and manual iR compensation Current measurement bias full range w ith 16 bit resolution 0 003 accuracy e Potential measurement bias 10 V with 16 bit resolution 0 003 accuracy e External potential input e Potential and current analog output e Programmable potential filter cutoff 1 5 MHz 150 KHz 15 KHz 1 5 KHz 150 Hz 15 Hz 1 5 Hz 0 15 Hz e Programmable signal filter cutoff 1 5 MHz 150 KHz 15 KHz 1 5 KHz 150 Hz 15 Hz 1 5 Hz 0 15 Hz e RDE control output 0 10V corresponding to 0 10000 rpm 16 bit 0 003 accuracy e Digital input output lines programmable through macro command e Flash memory for quick softw are update e Serial port or USB port selectable for data communication Cell control purge stir knock e Maximum data length 256K 16384K selectable e Real Time Absolute and Relative Distance Display e Real Time Probe and Substrate Current Display e Dual channel measurements for CV LSV CA DPV NPV SWV i t e CV simulation and fitting program
178. ion files would be stored in the C CHI directory and if this directory was not found the configuration files would be annoyingly spread everywhere This behavior should not occur in the current software version and it should be safe to extract the program to any directory on any drive or partition for which you have write and execute permission 2014 CH Instruments Inc Getting Started 15 To uninstall the software simply delete all program files the executable exe help chm and hlp if present and configuration cfg and ini Since no settings are stored on the registry an uninstaller is unnecessary The software CD also contains a hyperlinked electronic copy of this User Manual and the USB Driver In addition you can find a Lab Manual from the 2003 SECM Summer School at the University of Texas at Austin Note that an older model 900 SECM was used in the Summer School nevertheless it contains quite a bit of information that you may find useful 2014 CH Instruments Inc 16 CH Instruments Model 900D Series 2 1 3 Hardware System hardware installation is also easy and simple After unpacking the instrument you should check your power lines The AC voltage of the instrument was preset in the factory and is indicated on the serial number label on the back panel If the AC voltage is correct connect the instrument to the power with the power cord There are two instrument boxes you can stack them on top of
179. ion of nanometers and allows a maximum traveling distance of several centimeters The potential control range of the bipotentiostat is 10 V and the current range is 250 mA The instrument is capable of measuring current in the picoampere range Stepper and Piezo reference Bipotentiostat amp Positioner amp Controller Data Acquisition solution with mediator The model 900D 920D is designed for scanning electrochemical microscopy but is also capable of many conventional electrochemical techniques for convenience Model 900D uses a stepper motor positioner that can travel 50 mm with 8 nm resolution The Model 920D combines the stepper motor positioner with a three dimensional closed loop piezo positioner Model 900D 920D is an upgrade to the 900B 910B SECM The stepper positioner has better linearity and resolution 8 nm versus 100 nm and longer travel distance 50 mm versus 25 mm Also waveform generation and data acquisition are significantly faster The waveform update rate can be 10 MHz and 2014 CH Instruments Inc General Information 3 the sampling rate can be 1 MHz at 16 bit resolution while maintaining low noise levels AC measurement techniques including electrochemical impedance spectroscopy have also been added Improvements also include very stable and accurate potential and current control and dual channel data acquisition at high speed The instrument can be controlled by any PC running Windows 98
180. ions for X Y and Z are right front and down respectively The piezo is fully extended The stepper motor then moves in the positive direction until the pin touches the base metal plate allowing a current to flow This stepper motor position is saved as point 1 The piezo is then fully retracted The stepper motor moves further in the positive direction until the tip touches the base metal plate again This stepper motor position is saved as point 2 The distance between point 1 and point 2 is the full scale distance the piezo can travel Typically there might be a few percent deviation in calibration It is recommend to calibrate several times to verify that the results are reasonably repeatable Any observed error is probably due to variations in the metal contact position caused by the roughness of the base metal plate and the metal pin Please save the metal pin plastic washers and nylon screws for future calibration use You may want to check if the piezo behavior changes over time say months or years later Piezo Stage Position The probe position is continuously updated while this dialog box is open Click the Zero button to re zero the relative position of the corresponding axis at any time Click the Move button of the corresponding axis to move the piezo to the specified position in absolute or relative coordinates If the requested move hits the zero or full range limit a warning will be issued The tip will stop at zero or full range
181. irection the cursor will move along the data curve This is particularly useful for identifying data points When Free is selected the cursor will move freely in the XY plane 2014 CH Instruments Inc Graphics Menu 175 This option is not available for the SECM technique Current Density Check this box to display current density Electrode Area This value is used to calculate the current density E vs Reference Electrode Specify the name of the reference electrode used in the experiment in the Ref Electrode field e g Ag AgCI The default potential axis title is Potential V Check the E vs Reference Electrode to append the Ref Electrode field to the potential axis title e g Potential V vs Ag AgCl Header Enter your header in this field To display this header at the top of your plot check the Header box under Screen and or Printer options in this dialog box Note Enter your notes in this field Notes will not be displayed on the screen or printed but will be saved in the data file allowing you to add comments about the experiment and remind yourself later about the purpose and the conditions of the experiment 2014 CH Instruments Inc CH Instruments Model 900D Series 6 18 Color and Legend command This command opens the Color Selection dialog box Use this command to specify color and legend options for your graphical plots You can change the color of the background axes grid and da
182. ive 3 d plots rotate zoom etc are available from the Graph Options menu once the experiment has completed The program presents the following dialog box 2014 CH Instruments Inc Probe Electrode Probe E Quiet Time s Sensitivity IA Substrate Electrode Substrate E V Sensitivity IA l EOn Probe Travel x Distance um Y Distance um Incr Time s Incr Dist um 1 e 006 z 1 e 006 DI M i20n 80 Long Travel Direction mo Amplitude fo 005 SECM Mode Amperometry Potentiometry C Constant Current Impedance Constant Current Mode Constant Current L f e 009 Current Tolerance i Max Z Incr um i Motor Selection Iw Returm to Origin after Run Auto Stepper C Piezo Impedance mode Frequency Hz f 00000 ddi Setup Menu 13 Scanning Electrochemical Microscope Parameters gt gt l Ki Tere OK Cancel Help X Axis as Long Direction Bias DC Current C Y Axis as Long Direction 7 AutcSens Parameter Probe E V Quiet Time s Sensitivity A V Substrate E V Sensitivity A V E On i2 On X Distance um Y Distance um Incr Dist um Incr Time s SECM Mode Const Current A Current Tolerance Max Z Incr um Impedance Mode Frequency Hz Amplitude V Bias DC Current AutoSens Motor Selection X Y Axis
183. k in S itstst sCS rh PS OCPT1 PSAO gt Filename IMPE3 BIN CET BIV CVO BIN CV1 BIN Files of type Data Files bin DI Cancel 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 The box abowe lists files with the extension you select in the Files of type box To select multiple files hold down the Ctrl key and left click on the desired files You don t have to type the extension the system will automatically attach a bin extension to the filename Other extensions are not allowed Files of type Select the type of file you want to print Only bin files binary data are available 2014 CH Instruments Inc File Menu 3 12 Print Setup command This command opens the Print Setup dialog box Use this command to select a printer and a printer connection This command presents a Print Setup dialog box where you specify the printer and its connection e Print Setup i Printer Name Ms File PS D Properties Status Ready Type MS Publisher Color Printer Where FILE Comment Paper Orientation Size Letter D Portrait e Landscape Cancel Printer Name Specifies the printer you want to use Use the default printer or select one of the currently installed printers shown in the box You can install printer
184. k or Uncheck Record external signal when scan rate lt 0 1 V s Electrode 2 Potential V 10 10 Second working electrode potential Differential E V 0 2 0 2 Potential difference with 1st channel if Diff Scan is enabled Sensitivity A V 1e 12 0 1 Sensitivity scale for second electrode Off Select or deselect Second working electrode turned off Constant E Select or deselect Hold second electrode at constant potential Scan Select or deselect Scan 2nd channel with 1st channel Diff Scan Select or deselect Scan 2nd channel at constant potential difference with 1st channel Notes e Init E and Final E should be at least 0 01 V apart e The maximum potential scan range is 13 1 V e When the scan rate is high the data sampling interval will be automatically increased e When the scan rate is below 0 01 V s the sensitivity scale during the run can be automatically adjusted according to the current level When Auto Sens is enabled the value of the Sensitivity field will have no effect on the measurement However the smallest available automatic sensitivity will be 2014 CH Instruments Inc ER CH Instruments Model 900D Series 1e 6 A V instead of 1e 12 A V The Picoamp Booster will not work either In order to specify smaller sensitivities the automatic sensitivity switching option must be disabled Linear polarization resistance plots can be generated using the Special Plots command under the Graphics menu The potential inc
185. l will be ignored 3 The steps are applied in the sequence of Step E1 Step E2 Step E1 Step E2 Thus the final potential will be Step E1 for an odd number of segments and Step E2 for an even number Run Click the Run button to activate the step function generator No data will be collected and displayed A status box will be displayed showing the number of steps completed the remaining steps and the remaining time Cancel this function by pressing the Stop pushbutton 2014 CH Instruments Inc Control Menu 141 2014 CH Instruments Inc 42 CH Instruments Model 900D Series 5 16 Preconditioning command This dialog box opens the Preconditioning before Run dialog box Use this command to condition the working electrode before running an experiment This can be useful for cleaning the electrode among other purposes Preconditioning occurs before the deposition or quiet time The Precondition command presents this dialog box Preconditioning before Run A xj First step Cancel Potential D fo Help Lire E Seccccescseecs fo TE Second step Potential V fo Time fei fo m Third step I Electrode 2 Potential VJ fo IT Stir On Time s fo T Purge On The working electrode will be conditioned with up to three potential steps Enable Preconditioning Uncheck this box to disable proconditioning which occurs before the deposition or quiet time Poten
186. le Menu 29 Chapter 3 File Menu The File menu offers the following commands New Creates a new document Open Opens an existing document or text file Close Closes an opened document Save As Save current document can convert to plain text csv Delete Delete existing data files permanently legacy command Retrieve Retrieve lost experimental data Update Instrument Prog Update instrument firmware List Data File Display an existing data file in text format Convert to Text Convert multiple existing data files to text files Text File Format Choose text file formatting options Import Text File Import text file legacy command superseded by Open Print Prints a document Print Multiple Files Print multiple documents Print Preview Displays the document on the screen as it would appear printed Print Setup Selects a printer and printer connection Send Sends the active document through electronic mail Most Recently Used Open the most recently used documents quickly Exit Exits the program 2014 CH Instruments Inc so CH Instruments Model 900D Series 3 1 Open command This command opens the File Open dialog box Use this command to open one or more existing documents each in a new window You can open multiple documents at once The program displays the File Open dialog box so you can select the files you want to convert Binary data files and text files saved from the program can both be read directly
187. le dialog box Use the Import Text File command to import text files CHI and BAS text file formats are both supported For CHI text files this command will only succeed if Memo and Parameter fields are present For BAS text files parameters will be converted to be CHI format This command can only import one text file at a time to import multiple files use the Open command instead The Import Text File command presents this dialog box EE Files of type Data Files P bi DI Cancel b A 2014 CH Instruments Inc File Menu 3 10 Print command Use this command to print a document The printer output is identical to what is displayed on the screen What You See Is What You Get Use the Graph Option command in the Graphics menu to customize the print output The paper orientation must be set to landscape If a warning pops up use the Print Setup command to set the paper orientation to landscape This command has a toolbar button 2014 CH Instruments Inc a CH Instruments Model 900D Series 3 11 Print Multiple Files command This command opens the Multiple File Print dialog box Printer output is identical to what is displayed on the screen What You See Is What You Get Use the Graph Option command under the Graphics menu to customize the print output Use this command to print multiple data files The Print Multiple Files command presents this dialog box Multiple File Print 2j x Loo
188. le the axis This provides a convenient way to zoom out further than the default scale and can be particularly useful for overlay plots when some data files go off the charts Double clicking on an axis opens the Axis Options dialog box Double clicking elsewhere in the plot area opens the Insert Text dialog box Other settings are available under the Graph Option Color and Legend and Font commands When data is saved to file the display format is also saved and is recovered when the file is loaded This is also true for Overlay Plots Parallel Plots and Print Multiple Files This command is disabled if there is no currently active data Its toolbar button is 1 Double clicking on a graph axis will open this dialog box i x Grid and Iny Pg Vv Grid I Curent Density Cancel T Invert Electrode Area fi ma Aus Label Expression Dep 1 Scientific IT E vs Reference Electrode Engineering Ref Electrode Ag AgCl Long Auto DI Short Auto DI Freeze fo To 3 6e 006 P Title Unit Grid change Point Color Thickness x Axis CJ Change ho x Y axis Title Rotation on Printer 270 degree e Axis Label E egular fir Change Arial Narrow Axis Title Times New Roman Bold 16 a Change 2014 CH Instruments Inc Graphics Menu 153 Many settings listed here can also be set using the Graph Options Color and Legend and Font commands The options unique to this dial
189. lectrode for insulator substrate with O ring 1 _ Teflon cell with Pt wire counter electrode for conducting substrate 1 CHI303 Jr disk electrode as conducting substrate with O ring 1 2 CHI16 10 mmm Pt disk orbe A Tools wrenches ll User manual electronic oo ll l e 6 USB A B cable for communications oa _ 3 25F 25M cable for connections between bipotentiostat and motor controller 1 _ Electrode leads WS L Software CD oi Please examine the contents of your shipment carefully and immediately report any missing parts to CH Instruments Inc i h leck lach 2014 CH Instruments Inc CH Instruments Model 900D Series 2 1 2 Software The instrument can be controlled by any PC running Windows 98 NT Me 2000 XP Vista 7 8 A free USB port or serial port is required for communication between the instrument and the PC Refer to your Windows system documentation to gain familiarity with Windows operation Windows Vista can control the instrument properly but will sometimes can experience graphical glitches The program may paint single pixel dots incorrectly or leave entire areas of the screen blank Choose other legends such as circle square triangle or line to plot data correctly These glitches appear endemic to Vista and do not occur in versions of Windows older or newer than Vista The software in program documentation has been upgraded to compressed HTML chm files
190. les are displayed they will be 1 100 1 10 and 1 1 of full scale 2014 CH Instruments Inc CH Instruments Model 900D Series 4 2 18 Integrated Pulsed Amperometric Detection Parameters dialog box In Integrated Pulse Amperometric Detection IPAD six segments of potential sweeps or steps are applied Current is sampled and integrated during the first four segments Electrode conditioning or cleaning occurs during the last two steps The integrated current is averaged and recorded as a function of time The following diagram shows the potential waveform applied as a function of time and the current sampling scheme EE E Oxd E Potential V gt Integration Time k Cycle 1 Cycle 2 Parameter Step 1 Start Start E V Hold Time s Step 2 For Scan Peak E V Scan Time s Step 3 Rev Scan Return E V Scan Time s Step 4 Hold Hold E V Hold Time s Step 5 Oxidation Oxd E V Oxd Time s Step 6 Reduction Red E V Red Time s Number of Cycles Quiet Time s Sensitivity A V Range 3 276 3 276 0 05 1 3 276 3 276 0 15 1 3 276 3 276 0 15 1 3 276 3 276 0 05 1 3 276 3 276 0 05 1 3 276 3 276 0 05 1 5 65535 O 100000 1e 12 0 1 Time s Description Start potential constant Start potential duration current integration for last 10 ms Potential is scanned Start E to Peak E Potential scan time current integration continues Po
191. low you to edit your data and enter plot options X Y Data Array Editor Enter your own X Y data points Use comma or space to separate Xand Y values one pair per line x1 y1 x2 y2 x3 y3 Overlay Plot Click this button to plot multiple sets of data in a single graph To display both data markers and lines 2014 CH Instruments Inc 168 CH Instruments Model 900D Series save your data with two different names and select proper legends with the Color and Legend command To freeze the axes use the Graph Option command The program will display the Overlay Data Display dialog box so you can select the data files you want to plot along with the data in the X Y Data Array Editor Multiple files can be selected The plot will be automatically scaled to fit the data in the X Y Data Array Editor If both X and Y values fall into the plot scale the data point will be plotted Parallel Plot Click this button to plot multiple sets of data side by side The program will display the Parallel Data Display dialog box so you can select the data files you want to plot along with the data in the X Y Data Array Editor Multiple files can be selected Each plot will be automatically scaled to fit its individual data unless the scale is frozen using the Graph Option command In this case all plots will have the same frozen scale Plot Use this command to plot the data entered in the X Y Data Array Editor The plot will be automatical
192. ltammetry SHACV Second Harmonic AC Voltammetry including phase selective SSF Sweep Step Functions SWV Square Wave Voltammetry TAFEL Tafel Plot TPA Triple Pulse Amperometry 2014 CH Instruments Inc 252 CH Instruments Model 900D Series 12 8 Model 400C Series Time Resolved Electrochemical Quartz Crystal Microbalance The quartz crystal microbalance QCM is a variant of acoustic w ave microsensors that are capable of ultrasensitive mass measurements For example using our crystal which has a fundamental frequency of 7 995 MHz a net change of 1 Hz in oscillation frequency corresponds to 1 34 ng of mass adsorbed desorbed onto from a crystal surface of area of 0 196 cm QCM in conjuction w ith electrochemistry EQCM has been widely employed for the determination of deposited metals studies of ion transport processes in polymer films biosensor development and investigations of the adsorption desorption kinetics of adsorbate molecules In EQCM experiments measurements of various electrochemical parameters such as potential current and charge at the working electrode are conducted simultaneously with the acquisition of the corresponding frequency and resistance changes using the experimental setup show n in the Figure below For any model in the 400C series application of a specific potential w aveform e g triangular potential w aveform for cyclic voltammetric experiments current measurement and frequency counting are carr
193. luding the date and time of the experiment data source and type of data processing You can also enter your own notes about the experiment The Data Information command presents this dialog box Data Information Smoothing Baseline Correction Data Point Removing Data Point Modifying Filename This non editable box displays the name of the file containing the currently active data If the data have not been stored the filename is Unsaved Data Source This box will read either Experiment or Simulated Model This box displays the instrument model with which the data were acquired Date This box displays the date that the data were acquired Time 2014 CH Instruments Inc View Menu 220 This box displays the time that the data were acquired Data Proc Performed This list box displays what types of data processing have been previously performed on the data if applicable If several types of data processing have been performed multiple items will be highlighted Header This box displays the optional data plot header title Note This box displays user defined notes and is best suited for a brief description of the purpose and conditions of the experiment simulation 2014 CH Instruments Inc 20 CH Instruments Model 900D Series 10 2 Data Listing command This command opens the Data List dialog box The format of the list can be altered by the Text File Format command under
194. ly scaled to fit the data range unless the scale is frozen using the Graph Option command X Y Axis Title Unit Specify titles and units dimensions for the X and Y axes Header Enter the desired title header for the data To display the header on the top of the plot check the Header box using the Graph Option command Note Enter any comments about the plot The note will not be displayed on the plot but will be saved in the data file It allows you to put additional comments about the data and is well suited for a brief description of the purpose and conditions of the experiment Read Use this command to read data from file Save Use this command to save data to file XY titles units header and note will be saved along with the data Linear Curve Fitting Toggle least squares fit if this box is checked a best fit straight line will also appear on the plot 2014 CH Instruments Inc Graphics Menu 16 6 14 Peak Parameter Plot command This command opens the Peak Parameter vs Scan Rate Plot dialog box Use this command to plot peak current or potential against the scan rate This command can also perform a linear fit to the data This command works only for cyclic voltammetric CV or linear sweep voltammetric LSV data For CV data the system only searches for the currently active data segment After specifying the peak potential window and selecting the proper files click OK to render the plot The resulti
195. ly used keyboard shortcuts press the Alt key to move focus to the menu bar then type underlined letters to enter menus and run commands 6 The internal noise of the instrument is quite low The most common and most serious source of noise is the line frequency 60 Hz or 50 Hz The instrument contains analog low pass filters to reduce this noise At a scan rate of 0 1 V s the automatic filter cutoff setting is 150 or 320 Hz which does not cover the line frequency but at a scan rate of 0 05 V s the cutoff frequency of the filter is 15 or 32 Hz and the line frequency noise can be effectively reduced Line frequency noise can also be reduced if the sampling interval is set to a multiple of the period of the power line For small signals or relatively fast experiments use of a Faraday cage is strongly recommended 7 Use the Graph Options command under the Graphics menu to adjust the way data is displayed see Chapter 6 for more information on the wide variety of options available 8 The latest version of the software includes interactive 3D graphics for visualizing SECM data You can also generate a 3D surface plot with the SECM image data in Microsoft Excel by converting the data to text format First use the Text File Format command under the File menu and check the Excel 3D Format box Consult the context sensitive Help in the Text File Format dialog box to read the procedures for making Excel 3D surface plot 2014 CH Instruments Inc Fi
196. mber software revision date and manufacturer s contact information About CHI 2014 CH Instruments Inc Appendix 241 Chapter 12 Appendix This chapter contains technical details safety information and an overview of our full line of electrochemical instrumentation More information about the latter is also available on our website at www chinstruments com Cables and Connections Firmware Update Instructions Troubleshooting Maintenance and Serice Limited Warranty Safety Abbreviations Model 400C Series Time Resolved Electrochemical Quartz Crystal Microbalance Model 600E Series Electrochemical Analyzer Model 700E Series Bipotentiostat Model 800D Series Electrochemical Detector Model 920D Scanning Electrochemical Microscope Model 1000C Series Multi Potentiostat Model 1100C Power Potentiostat Galvanostat Model 1200B Handheld Potentiostat Bipotentiostat Pico Liter Solution Dispenser Picoamp Booster Faraday Cage and Multiplexer Amp Booster and Liguid Liquid Interface Adapter Accessories 2014 CH Instruments Inc om CH Instruments Model 900D Series 12 1 Cables and Connections Electrode connection Video connector Pin Function Color if applicable 1 Working electrode Green 2 Sensing electrode Black 3 Second working electrode Yellow 4 Reference Electrode White 5 Counter electrode Red 6 Analog Ground This electrode is used for 4 electrode configuration which can be used fo
197. mmetry ev TT Tt OO Dtteemianev onv LL o TT i SqareWave Votammetry wv LI T T drede acvotammeryiacy d ST IL Se andHarmonicACVottammetry sHacyy LI To T T T T AmperometricitCurve t IL fT oo T T TT gt ___Diferential Pulse Amperometry DP Double DPA DOPA Triple Pulse Amperometry TPA Tt ft BEER EE Open Circuit Potential Time OCP 1 i O i asl Full version of CV simulation fitting Limited version of CV simulation fitting amp Corresponding stripping mode can be performed Second channel bipotentiostat mode can be performed Note 12x0B 1205B and 1207B are single potentiostat models 12x2B 1206B and 1208B are bipotentiostat models 2014 CH Instruments Inc 12 16 Model 1550A Pico Liter Solution Dispenser The CHI1550A solution dispenser is designed for making high density and high accuracy solution arrays which can be used in a wide variety of chemical biological and medical applications The solution dispenser consists of a high resolution three dimensional positioner a piezoelectric jetting device and a sample platform as shown in the Figure below i Te Slight A lt Jetting Device overpressure c Jetting Device solution solution spots j pe j Figure Diagram of the solution dispenser 3D Positioner Controller Piezo Jet Device Controller Sample Plate Support The three dimensional positioner can tr
198. mperes range The program presents the following dialog box Run Lime sec 400 OK er Oox Sample Interval sec 0 1 Sara High E Limit VJ D CR Low E Limit Mi D te Help Parameter Range Description Run Time s 1 500000 Experiment running time Sample Interval s 0 0025 50 Sampling interval High E Limit V 10 10 High potential limit Low E Limit V 10 10 Low potential limit Notes e If the high or low potential limit is reached a warning will be given e 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 2014 CH Instruments Inc ER CH Instruments Model 900D Series 4 2 31 Parameters for Electrochemical Noise Measurement dialog box In Electrochemical Noise measurements ECN no waveform is applied to the electrochemical cell The working electrode is at the zero resistance ammeter and its potential is at virtual ground very close to ground it cannot be connected to a true ground To measure electrochemical noise an electrode identical to the working electrode should be connected to the instrument ground the black banana jack on the rear panel labeled GND and both electrodes should be immersed in the same solution The electrochemical noise current passing through these two electrodes will be measured To measure potential noise add a reference electro
199. mputerized eight channel potentiostat The system contains a digital function generator and multiplexed data acquisition circuitry The multi potentiostat can work with eight independent cells or eight working electrodes in the same solution with common reference and counter electrodes The potential control range is 10 V for all channels and the current range is 10 mA The instrument is capable of measuring current down to picoamperes Each electrode can be individually controlled including on off control potential and sensitivity settings each can be set to an independent potential or the same potential as the primary channel so that they can sweep or step potentials together with the primary channel The model 1000C series is an upgrade to the model 1000 1000A 1000B series The instrument allows eight independent cells simultaneous or sequential measurements fast waveform generation and data acquisition speed 1 MHz 16 bit and easy software update using flash memory Many electrochemical techniques are available in this model series including cyclic voltammetry and amperometric i t measurements with all eight channels available except for open circuit potential measurements The parameters for all channels must be set before running an experiment you cannot alter parameter settings during experiments During a run you can toggle between single and multi data set display parallel or overlay plots After a run you can choose data from
200. multiplexer sold separately hardware support required Macro Command Execute a series of commands cf batch file or shell script Open Circuit Potential Measure the open circuit potential iR Compensation Set and test iR compensation select models only Filter Setting Set potential and current filters Cell Set and control the electrochemical cell Step Functions Generate square waveform for cleaning etc select models only Preconditioning Condition working electrode before experiment Rotating Disk Electrode Set rotating disk electrode control parameters select models only Other Set miscellaneous options select models only Stripping Mode Set stripping mode and conditions SECM Probe Calibrate and control the SECM probe 900 series only 2014 CH Instruments Inc 112 CH Instruments Model 900D Series 5 1 Run Experiment command Use this command to start running your experiment This command can also be used to skip Quiet Time Deposition Time or Preconditioning and go to the next step Before each run the program will first verify data link with the instrument before proceeding The program will also verify the values of experimental parameters if illegal values have been entered the command will terminate and the program will issue an error message During most experiments data can be displayed in real time When the data acquisition speed exceeds the data transmission rate the results will be displayed imm
201. n click on any button and drag it to a new position or even drag it off the toolbar altogether to remove it To add buttons simply drag them from the Customize Toolbar dialog box onto the toolbar direct drag and drop and user customizable menus require Windows XP or higher and the corresponding edition of our software 2 In the Customize Toolbar dialog box drag and drop buttons to conveniently add remove or reorder them That is click on an item in the list of Current toolbar buttons and drag it around in the Current list to change its position or drag it into the list of Available toolbar buttons to remove it from your toolbar Similarly buttons can be added from the Available list by dragging them into the Current list 3 In the Customize Toolbar dialog box double click on a button in the list of Available toolbar buttons to add it to the toolbar However this will add it to the bottom of the list and to change its position you must either drag it vertically or click the Move Up Down button Similarly double click on a button in the list of Current toolbar buttons to remove it from your toolbar it will be automatically sorted into the Available list 4 In the Customize Toolbar dialog box click on the corresponding buttons to perform the desired operations The Reset button will restore the default toolbar Caveats e f your toolbar displays improperly please restart your application e This command is currently
202. n double layer capacitance or surface reactions A charge to voltage converter true integrator is a better choice H the current to voltage converter is employed due to high total charge a shorter sampling interval will increase data density but also reduce the signal to noise ratio If earlier transient data are important a shorter sampling interval is recommended If later data points are of interest a longer sampling interval is recommended However a minimum of 1000 points per step is required unless the sampling rate 2014 CH Instruments Inc e CH Instruments Model 900D Series does not allow it If the sampling interval is shorter than 0 002s or 0 0005s with fast com port speed data will not be transferred in real time but rather after the experiment is completed The cell is turned off during data transfer unless the Cell On between Run option has been enabled using the Cell command The total number of data points will be limited by the instrument memory size 64K points The sampling interval may be automatically adjusted to fit the data points in a reasonable range If the sampling interval is longer than 0 002s or 0 0005s with fast com port speed data will be transferred in real time during the experiment The number of data points for each step will be limited by the instrument memory size 64K points The sampling interval may be automatically adjusted to fit the data points in a reasonable range If the current to vol
203. n the CP210x USB to UART Bridge Controller item in Device Manager to display various status information driver version number whether the driver is functioning correctly etc If you have a free serial port available on your PC we recommend its use over a USB port This is because we implement USB connectivity using a USB to serial chip on the instrument allowing serial 2014 CH Instruments Inc 2 CH Instruments Model 900D Series communication to occur through the USB port using drivers provided by the chip vendor USB therefore provides no specific advantages over the serial port besides the difference in physical connectivity and both the instrument and the PC will interact as if connected by a serial connection The reason we include USB support is that most computers sold today do not include a serial port and it may be impractical or even impossible to add a serial port card However the supplied third party USB serial port drivers may not be perfect We have tested them on several computers in our office and they all seem to work but if problems occur since the Windows drivers are closed source we have no way to modify let alone debug them Our only recourse in that scenario would be to file a support ticket with the chip vendor and it may prove more expedient to buy a USB to Serial Adapter cable and a DB 25 male to DB 9 female cable each 10 USD at the time of this writing Depending on your instrument model you ma
204. n which you can get help About Displays the version number of this application 2014 CH Instruments Inc 28 CH Instruments Model 900D Series 11 1 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 for using the program and various types of reference information Once you open help you can click the Home button whenever you want to return to the opening screen 2 CHI Mod m e 4 Hide Back Forward Contents Search Favorites 2 Menus a of Print Options 1000A Series Help Commands File menu Setup menu Control menu Graphics menu DataProc menu Analysis menu Sim menu View menu Window menu Help menu Context sensitive help is available for the pull down menus and the buttons on the toolbar Press Shift F1 to activate context sensitive help the mouse pointer will change to an arrow and question mark and click on a menu command toolbar button or other part of the application window to learn more about it 2014 CH Instruments Inc Help Menu ER 11 2 Old Help command Check this item to enable legacy hlp file context sensitive help if available Please note that such hlp files are no longer kept up to date 2014 CH Instruments Inc o CH Instruments Model 900D Series 11 3 About command Use this command to display the copyright notice version nu
205. nc CH Instruments Model 900D Series rates 2014 CH Instruments Inc Graphics Menu 171 6 15 Semilog Plot command This command opens the Current Potential Semilog Plot dialog box Use this command to display a current potential semilog plot This 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 sigmoidal 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 deviation from this expected slope indicates slow kinetics or complexity of the electrode reaction This command can also perform a linear fit to the data After specifying the peak potential window and selecting the proper files click OK to render the plot The resulting plot is temporary and will disappear if other data display commands are invoked You can use the Graph Option Color and Legend and Font commands to customize your plot The Semilog Plot command presents this dialog box Current Potential Semilog Plot x m Potential Window E From VJ j 0 39 Cancel ETME 0 45 Hel nep MV Linear Curve Fitting Potential Window Enter the range of potential values to be plotted The potential window should be near the half wave potential and within 0 059 n V Data points outside the specified potential window will be ignored Linear Curv
206. nction of time for sweep segments it can also be presented as a function of potential Segments 1 l2 3l4 sl 6 Izlslol10 11 12 Se Step E D Final E C g O A Init E Scan Rate V s Time s Parameter Range Description Seq 1 3 5 7 9 11 Sweep Init E V 10 10 Initial potential Final E V 10 10 Final potential Scan Rate V s 1e 4 50 Potential scan rate Seq 2 4 6 8 10 12 Step Step E V 10 10 Step potential Step Time s O 10000 Step duration Init E V 10 10 Initial potential Sweep S I V 0 001 0 05 Sweep function sampling interval Step S I s 0 0001 1 Step function sampling interval Quiet Time s O 100000 Quiescent time before potential scan Sensitivity A V 1e 12 0 1 Sensitivity scale Notes e A Sweep sequence will be ignored if the difference between its Init E and Final E is less than 0 01 V e A Step sequence will be ignored if its step time is less than 0 001 sec or its number of points is less than 3 To remedy the latter case either increase its step time or decrease its sampling interval e Ifthe scan rate for a Sweep sequence is less than 0 5 V s data will be transferred and displayed in real time e Ifthe sampling interval for a Step sequence is larger than 0 002 sec data will be transferred and displayed in real time e The potential differences between Init E Final E and Step E should be less than 13 1 V 2014 CH Instruments Inc Setup Menu
207. ng Some Useful Tips USB Driver Installation 2014 CH Instruments Inc 12 CH Instruments Model 900D Series 2 1 Installation Important Note After you unpack the instrument please check the contents of the shipment carefully You should find the instrument USB cable electrode leads software CD and a printed copy of this User Manual optional Electrodes and other accessories are sold separately if you ordered electrodes and accessories please thoroughly check the shipment and compare its contents with the packing list If anything is missing please search thoroughly inside the container since the missing items may have been mixed with the packing material over the course of shipping Please report any missing or damaged items immediately and do not throw away the shipping materials as these may be used for return shipping 2014 CH Instruments Inc Getting Started 13 2 1 1 Parts List The CHI900D series SECM comes with the following parts Part tem O Stepper motors with translation stages Cd Po Stan o O Piezo Positioner CHI920D only S O Mounting Piece for Z stage or Piezo positioner Black T shaped Bee Sample holder o O Probe holder Teflon O o o O Mounting piece for probe holder O Z O Z o S O Nylonscrews for piezo calibration O O C i LS CY Nylonwashers for piezo calibration CC Cd Brass pin with 10K ohm resistor for piezo calibration 1 Teflon cell with Pt wire counter e
208. ng Data Points Specify the number of data points to be removed from the beginning of the data set If this number is zero no points will be removed from the beginning Remove Ending Data Points Specify the number of data points to be removed from the end of the data set If this number is zero no points will be removed from the end Override Present Data Check this box to replace the currently active data with the new data after data point removal If this box is not checked the new data will only be displayed without overriding the currently active data and invoking the Present Data Plot command will display the original data 2014 CH Instruments Inc 192 CH Instruments Model 900D Series 7 9 Data Point Modifying command This command opens the Data Point Modifying dialog box Use this command to visually modify the data points of the currently active data e g to correct data points due to a bad mercury drop The Data Point Modifying command presents this dialog box Data Point Modifying WS xj Segment il Cancel IV Override Present Data Help To modify data points click the OK button first The mouse cursor will change to an up arrow When you move the mouse cursor in the data display region crosshairs 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 crosshairs appear at the selected
209. ng plot is temporary and will disappear if other data display commands are invoked You can use the Graph Option Color and Legend and Font commands to customize your plot The Peak Parameter Plot command opens this dialog box Peak Parameters vs Scan Rate Plot F xj m Peak Potential Window Ep From Lo Cancel ERTEM cece Los Help OK Ea m Type of Plot C ip vs Scan Rate Ge ip vs Sot Scan Rate Ep vs log Scan Rate IV Linear Curve Fitting Peak Potential Window Specify the potential range in which the program will search for peaks The first peak in this potential range will be used for plotting Type of Plot Plot peak current versus the scan rate peak current versus the 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 of the scan rate for a reversible reaction A change in peak potential with scan rate indicates either slow kinetics or chemical complexity Linear Curve Fitting Checking this box will generate a linear least squares best fit line on the plot Select Files Select data files to be plotted CV or LSV only Select at least three data files obtained at different scan 2014 CH Instruments I
210. nge Measured potential range 0 025 V 0 1 V 0 25 V 1 V 2 5 V 10 V Measured potential resolution 0 0015 of measured range Electrometer Reference electrode input impedance 1e12 ohm Scanning Probe Techniques SECM Imaging SECM constant height constant current potentiometric and impedance modes Probe Approach Curves PAC Probe Scan Curve PSC constant height constant current potentiometric impedance and constant impedance modes Surface Patterned Conditioning SPC Surface Interrogation SECM SISECM Z Probe Constant Current Control Sweep Techniques Cyclic Voltammetry CV Linear Sw eep Voltammetry LSV Tafel Plot TAFEL Step and Pulse Techniques Staircase Voltammetry SCV Chronoamperometry CA Chronocoulometry CC Differential Pulse Voltammetry DPV Normal Pulse Voltammetry NPV Differential Normal Pulse Voltammetry DNPV Square Wave Voltammetry SWV AC Techniques AC Voltammetry ACV Second Harmonic AC Voltammetry SHACV Fourier Transform AC Voltammetry FTACV AC Impedance IMP Impedance versus Potential IMPE Impedance versus Time IMPT Galvanostatic Techniques Chronopotentiometry CP Chronopotentiometry w ith Current Ramp CPCR Multi Current Steps ISTEP Potentiometric Stripping Analysis PSA 2014 CH Instruments Inc e Reference electrode input bandw idth 10 MHz e Reference electrode input bias current lt 10 pA 25 Waveform Generat
211. nnnnnn ennen 4 2 33 Probe Scan Curve Parameters dialog bOX ssssssssssenesseeseesseeeeensseeeseeeseesseeeseesenesseesenenenesenseenenenenns 4 2 34 Probe Approach Curve Parameters dialog DOX s s nnnnnnusnnnnsnnnnnnnnrnnnnrnnnnnunnnnnnnnnnnnnnnnnnnennnnnnnnnnnnnn nna 4 2 35 Surface Interrogation SECM Parameters dialog DOX s ssuseusuurensunrnnnunnunnunnunnunennnnnnnnnnnennnnnenn ennenen 4 2 36 Scanning Electrochemical Microscope Parameters dialog box ei System commander saaken naana Na EEKE EENS ENEE EENEG Hardware Test coMmmMand ssssssssssrnnusnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnn EE ERER EE EREE nnmnnn 5 Control Menu Run Experiment command sssssssrr1u1snunnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnn ennum nnmnnn nnmnnn nennen 112 Pause Resume COMIMANG cccccceeeeceeeee eee eeee ee eeeeee ee eeeeee se eeeeee se eeeeeeseeeeaeseeeeeeeseeeeeeeneeeaeees 113 Stop Ruin command ive eiiiai eanne ENERE NATARE AEN ve deta veccctiatecgecians enettoves 114 Reverse Scan Commandes EegeEEEEEN ENEE EENEG ENEE EEGEN EEEEE ENEE 115 Zero Current COMMANG seisein cesses eicded eee cocdueetedeauvectacndesdetdesdeceensectecndseendeeeve 116 Zero TIME ul Ee DEE 117 Run Status COMMANG 2 2 25ceccccsceccecseceetectevescctseeedeceadeesencaveeueceaseescueveetecddeecsecasseedeaaieeetoans 118 Repetitive Runs COMMANGA ccccceeeeceeeeeeeeeeeeeeeeeeeeeeeeeeeeseeeeeeeseeeeeeeseeeeeeseeeeeeaseeeaeenseeeseees 121 Multiplexer CO
212. nnnnnnnnnnnennnna 78 4 2 20 Hydrodynamic Modulation Voltam metry Parameters dialog box ww 79 4 2 21 Sweep Step Function Parameters dialog bOX s s nsnsunnnnnnunnnnnnnnnnnnnnna 80 4 2 22 Multi Potential Steps Parameters dialog box 81 4 2 23 A C Impedance Parameters dialog DOX s s nnnsnsunnnrnsnnnnrurnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnennnnnnnnnnnnnnnnnnnnnnn aneneen 82 4 2 24 Impedance Time Parameters dialog bOX s nsnsunnnnusnnnnurnnnnnnnnnnnnnnnnnnrnnnnnnnnnnnnnnnnnnnnnnnnnennnnnnnnn nnen nna 84 4 2 25 Impedance Potential Parameters dialog DOX nsnnnnnnnnnusnnnnnnnnnnnnnnrnnnnrnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnenn nna 85 4 2 26 Chronopotentiometry Parameters dialog DOX s sns nnnnnsusnnnnnnnnnnnnnnnnnrnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnenn nna 86 4 2 27 Chronopotentiometry with Current Ramp Parameters dialog DOX s snnnnsnsnnnnnnnnnnnnnnnnnnnnnnnnnnnna 88 4 2 28 Multi Current Steps Parameters dialog DOX s nnsusnnnnusnnnnnnnnnennnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnennnnnnnnenn nna 89 4 2 29 Potentiometric Stripping Analysis Parameters dialog box 90 4 2 30 Parameters for Open Circuit Potential vs Time dialog DOX snsnnnnnnsnnnnnusnnnnnnrnnnnnnnnnnnnnnnnnnnnnnnennnna 91 4 2 31 Parameters for Electrochemical Noise Measurement dialog DOX ssscssceeeseseeenseeseeeseeeeeeenes 92 4 2 32 Surface Patterned Conditioning Parameters dialog DOX s sunsuseussunnnnnunennnnnuunnnnnnnnnnennennenn
213. nstruments Inc Sim Menu 215 9 1 2 Potentials and Rate Constants dialog box This dialog box allows you to enter the kinetic parameters for CV simulations Potentials and Rate Constants A x Reactions o Eo Lo alpha os Cancel A e B ule C e D ko 0 01093 Eo 0 49566 alpha 0 5 Help D I kf 7 78867 kb 0 3894 B D kf 7 788e 006 kb Determined A D C B MES kb Determined All steps of the reaction mechanism are listed on the left Depending on the type of reaction up to 3 parameters can be specified on the right For charge transfer reactions you should enter the heterogeneous rate constant ko the standard redox potential Eo and the charge transfer coefficient alpha For other chemical reactions forward and backward rate constants should be specified Certain kinetic parameters may be predetermined This is because the concentrations of n species can be determined by n 1 reactions plus the initial conditions It is often the case that there are more equations than the number of species and hence some of the equations must be linearly dependent In this case The equilibrium constants of the reactions are overdetermined and if they are all be assigned arbitrarily the system will never reach equilibrium The software will automatically detect this situation and properly assign the linearly dependent kinetic parameters You should put the reactions whose kinetic parameters are not well known on the bottom of the m
214. nt current measure probe height as a function of position e Height Z will be adjusted automatically to maintain current constant e Ifthe sample or substrate is an insulator the resulting plot yields topographic information e Current value and tolerance must be specified Impedance measure probe impedance as a function of position e AC frequency and amplitude must be specified e In aZdirection scan the impedance will increase sharply when approaching the surface thus allowing a close probe approach without a redox mediator in solution The program presents the following dialog box 2014 CH Instruments Inc ER CH Instruments Model 900D Series Probe Scan Curve Parameters Probe Electrode Probe E DW Sensitivity A V Pulse E MI Pulse Duration s Delay time sl EI Pulse On Substrate Electrode Substrate E WI Sensitivity A V T E20n Probe Stop at Current L e No lt C Absolute 4 gt Probe E Pulse before Sampling kl RSC Cancel Help Mode 1 e 006 e e Amperometry Potentiometry Constant Current Impedance GE Impedance mode Di o Frequency Hz 100000 Amplitude v 0 005 Bias DC Current M AutoSens ER 1e 006 Scan Direction Motor Selection M i20n x cy 2 Auto Stepper Piezo evel Constant Current Mode Parameter Probe E V Sensitivity A V Pulse E V Pulse Duration s Delay time s E1 Pulse On Substrate E V S
215. nter the equivalent circuitry Once the Mechanism command has been invoked the original toolbar will be replaced by a new one containing symbols for components and commands ie ec Imp0 bin ll x C Bile Setup Control Graphics DataProc Analysis Sim View Window Help x E A R p o dle ae om GN Ge Fit 3 Undo previous action Redo previous action fo Rearrange components Move components left right up or down Clear all components ZS Cut remove circuit element or connection aii Add resistor Ohms AFAdd capacitor Farads Add inductor Henries beJ Add Warburg impedance 2JAdd constant phase element f Add Cole Cole impedance Add Cole Davidson impedance Add Finite Length Diffusion impedance Add Open Finite Length Diffusion impedance Add Gerischer impedance El Change simulation parameters e g frequency range 2014 CH Instruments Inc Sim Menu 221 Open equivalent circuit file for simulation or fitting fel Save current equivalent circuit SimRun impedance simulator FitRun impedance fitting program W Stop fitting in progress Exit mechanism editor simulation environment Circuit Editor The equivalent circuit editor is fully graphical To add a circuit element click the appropriate symbol on the toolbar and click in the main window to place the component Double click the component to specify the name and value of the circuit element Connect two elements b
216. ntial step Low E V 10 10 Lower limit of potential step Init P N Pos or Neg Initial step direction Number of Steps 1 320 Number of potential steps Pulse Width s te 4 1000 Potential pulse width Sample Interval s 1e 6 10 Data sampling interval Quiet Time s O 100000 Quiescent time before potential step Sensitivity A V 1e 12 0 1 Sensitivity scale Aux Signal Rec Check or Uncheck Record external signal when sample interval gt 0 005s Electrode 2 Potential V 10 10 Second working electrode potential if not step Sensitivity A V 1e 12 0 1 Sensitivity scale for second electrode On Check or Uncheck Second working electrode at constant E Step Check or Uncheck Step the second electrode potential Notes e High E and Low E should be at least 0 001 V apart e f unreasonably values for High E or Low E are entered the system will automatically readjust them e Depending on the Init E High E and Low E values the system will automatically readjust the initial scan direction The maximum potential scan range is 13 1V A shorter sampling interval will increase data density but also reduce the signal noise ratio If earlier transient data points are important a shorter sampling interval is recommended If later data points are of interest a longer sampling interval is recommended However a minimum of 100 points per step is 2014 CH Instruments Inc ER CH Instruments Model 900D Series required If the sam
217. nto the bottom of the Teflon SECM cell You will need to insert a rubber O ring between the Teflon cell and the metal ring to avoid leakage Screw the Teflon cell to the stainless steel plate Usually the counter and reference electrodes will be on the right side when viewed from the front Pour the solution into the cell Insert the reference electrode into the hole on the Teflon cell wall Insert the tip into the tip holder You need to move the tip close to the substrate surface Initially you should use the SECM Probe command under the Control menu You will find the XYZ move command at the bottom left of the dialog box which moves the tip fairly fast Make sure sure it does not get too close to the surface If the tip touches the surface the surface will be damaged fortunately the 10 um tip will not be damaged so easily On the other hand you do not want the tip to be too far away from the surface because the following Probe Approach Curve experiment moves the tip rather slowly 2014 CH Instruments Inc CH Instruments Model 900D Series Once the tip is reasonably close to the surface you can use the Probe Approach Cune technique to bring the tip closer to the surface You can set experimental parameters using the file PACxx bin included on the software CD For ferrocenemethanol the tip is held at an oxidation potential around 0 5V vs Ag AgCl The substrate potential is held at a reduction potential around 0 V vs Ag AgCI I
218. og box are Axis Label Expression The format of axis values can be selected as Scientific e g 1e 6A or Engineering e g 1 uA Warning if you are using Oriental Windows such as Chinese Japanese Korean the micro symbol will not appear properly you need to adjust the Windows setting using System command under the Setup menu The micro symbol will then be expressed as u Long Short These options allow you to customize long major and short minor ticks You should freeze the axis scale when adjusing these settings manually Double clicking on a graph opens this dialog box a Text I Erase 0 x 0 35524 sy 1 99824e 00 Rotation O Cancel Font Style Size Color F egular fe Change Default E Arial Narrow Junk Je Text Display Enabled Monochrome The entered text will be saved with the data when you save the data file The following options allow you to type and format text in the data graphics field Text Enter the text to be displayed If you clear an existing Text field text will be removed from the plot upon exiting the dialog box Erase Clear the text field X and Y Change the position of the text X and Y give the precise coordinates of the upper left corner of the first letter The initial values indicate where you double clicked Rotation Rotate the text clockwise by an angle between 0 and 360 degrees Font 2014 CH Instruments Inc 154 CH Instruments Model
219. ommand before the simulation is run In order to do simulation make sure the instrument is correctly connected to your PC e g by running the Self Test command 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 You can copy the screen graphics to the clipboard during the simulation 2014 CH Instruments Inc Sim Menu 225 9 4 CV Fitting command Use this command to fit parameters to existing CV data leveraging our built in CV simulator to evaluate the fit select models only Before you run the fitting program make sure the instrument is correctly connected to your PC e g by running the Self Test command The program will verify that your instrument model is supported This check only needs to be performed once after the program is started After the first fit you do not need to have the instrument connected anymore First open the CV data file you want to fit This can be either experimental or simulated data Using the CV Fitting command will then open the CV reaction mechanism dialog box discussed in a previous section A judicious choice of mechanism is critical here the numerical fitting algorithm could find an excellent fit to an incorrect mechanism yielding unmeaningful and misleading results The system must be specified as diffusive or a surface reaction but kinetic parameters need
220. ons above by a qualified person aware of the hazards involved 2 a It is essential that operating personnel follow safe working procedures 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 vapours 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 switch it off immediately and contact the nearest dealer CH Instruments Inc contact details at the front of this manual 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 possible exposure to chemicals 2 c Despite the customer s 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 with sensitivity set to 1e 6 An Ohmic plot through the origin should be obtained with maximum current of 1 UA Working contacts green and black are connected to one side of the resistor and co
221. ot activate any other program and as when updating the firmware BIOS of any piece of electronics do not interrupt power to either the PC or the instrument Any of these actions could cause the upload to fail and corrupt the flash memory rendering the instrument unusable short of force programming back at the factory Please contact CH Instruments Inc at info chinstruments com if this event should occur If the upload does not succeed you will get an error message In this case turn the instrument off for 5 10 seconds then turn it back on You may need to exit and restart the PC program before trying again If the upload is successful you will get a confirmation message The updated instrument is now ready to use 2014 CH Instruments Inc 12 3 Troubleshooting Problem 1 Possible Caus Actin Le ales disconnect Connect the instrument to the computer Faulty cabe Check and changecable MR E settings using System command port in use under Setup menu te rrr network modem cards if present if problem persists try other computers Bisi discharge Reset instrument and computer s ss computation process Wait for computation to complete mouse Communication failed Reset instrument and computer error message to info chinstruments com broken Noisy data Unreliable data transfer If data reading exceeds 10 x sensitivity scale the problem could be related to the COM port remove network modem cards if present or tr
222. otential Notes e The experimental sequence consists of a cleaning step the first pulse and the second pulse This sequence is repeated until the total number of cycles is reached or the experiment is interrupted by the user There is no data acquisition during the 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 Data sampling occurs during the second half period of pulses 1 and 2 The longer the pulse width the longer the sample interval will be resulting in better signal averaging and less noise During an 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 unexpectedly long experiment When only 1 current scale is displayed during a run the data will be automatically scaled to fit When 2 current scales are displayed during a run they will be 1 100 and 1 10 of full scale When 3 current scales are displayed they will be 1 100 1 10 and 1 1 of full scale 2014 CH Instruments Inc CH Instruments Model 900D Series 4 2 16 Double Differential Pulse Amperometry dialog box Double Differential Pulse Amperometry DDPA alternates between two instances of differential pulse amperometry with two sets of data recorded and displayed In each instance a cleaning potential can be applied for electrode conditioning during which
223. otential range starts at 60 mV more negative than the equilibrium potential and has a default range of 100 mV You can manually override this default 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 has a default range of 100 mV You can manually change this potential range Calculate Once data segment equilibrium potential and anodic and cathodic potential ranges are properly set click this button to calculate the cathodic and anodic Tafel slope linear polarization resistance in 2014 CH Instruments Inc 208 CH Instruments Model 900D Series ohms and the corrosion current in amperes 2014 CH Instruments Inc Sim Menu 209 Chapter 9 Sim Menu The Setup menu offers the following commands Mechanism Set CV or IMP simulation parameters CV Simulate Run CV simulation CV Fitting Run CV data fitting 2014 CH Instruments Inc 210 CH Instruments Model 900D Series 9 1 Mechanism command Select instrument models include built in CV simulation impedance simulation and impedance data fitting software For most techniques this command opens the Digital Simulation dialog box However when the A C Impedance technique is selected under the Setup menu this command will instead launch the impedance simulator 2014 CH Instruments Inc Sim Menu 211 9 1 1 Digital Simulation d
224. ound current which are insensitive to changes in the kinetic parameters and difficult to fit accurately The potential subinterval near the peak currents tend to be more sensitive to the kinetic parameters 2014 CH Instruments Inc 226 CH Instruments Model 900D Series Since charging current can also make a significant contribution to CV data the double layer capacitance is also available as a variable or constant Our algorithm minimizes the absolute error defined as sqrt F E 2 N where the F are fitted data points E are your input data points and N is the total number of data points Absolute instead of relative error is used to avoid overweighting points for which the current nearly vanishes The Skip parameter allows you to to omit data points from the fitting procedure which can greatly reduce the fitting time The Error parameter is the desired error threshold below which the fitting procedure will end Click OK to start the fitting procedure F Pie iho Control Gracies Datarec Arem Ze Yem Window Dep a osaa Orgel lcldiel IG Alles tele A m wi FitError 0 0034145 S HAAN 014V i Time 00 01 399 4 oom C Mar 16 2011 11 19 05 L Tech CV 1 0 r E File ev1 bin i i Init E V 0 5 0 8 j i ies High E V 0 5 l d ee EE A E Low E V 0 1 lt 0 6 l i F It EIN e N _ a Scan Rate V s 0 1 D 044 d ememr F Segment 2 keng i f Smpl Interval V
225. ow Left click at the starting point and drag to define a sloped baseline When the mouse button is released this line is subtracted from your data X values not covered by the line will be unaffected To shift the DC level left click and drag to create a horizontal line which defines the new zero of the entire curve You don t have to draw a line to cover the entire X range If more than one segment of data is available such as CV data you can choose the segment to operate on with the Graph Option command under the Graphics menu This command is applied only once per invocation To compensate or shift the baseline more than once invoke this command repeatedly Override Present Data Check this box to replace the currently active data with the resulting baseline corrected data If this box is not checked the baseline corrected data will only be displayed without overriding the currently active data and invoking the Present Data Plot command will display the original data 2014 CH Instruments Inc DataProc Menu it 7 8 Data Point Removing command This command opens the Data Point Removing dialog box Use this command to remove unwanted data points from the beginning or end of the currently active data The Data Point Removing command presents this dialog box Data Point Removing Remove Beginning Points fo Remove Ending Points m Cancel IV Override Present Data Help Remove Beginni
226. ox Use this command to test the solution resistance and cell time constant as well as switch between automatic or manual iR compensation This command has a toolbar button avi The iR Compensation command presents this dialog box iR Compensation x iR Comp Test Results OK Resistance ohm ae Cancel RC Constant Iusecl eee Comp Level Ee Help Uncomp A ohnn ees d J D Compensation for Next Run H Comp Test iR Comp Enable Test EM tc Once Always Step Amplitude om D Comp Mode Comp Level 5 fico E Automatic Manual Overshoot SL 2 m Manual Compensation Iest Resistance ohm jo iR Comp Test Results Click the Test button to execute the solution resistance and cell time constant test The result will be reported here After that the program will test stability by gradually increasing the compensation level until the desired compensation level is reached or the system is no longer stable The allowed compensation level and 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 and compensation may be limited to the feedback resistor of the UE converter iR Comp Test Before starting the iR compensation test these test parameters must be specified correctly
227. ox to set the potential back to the Initial E value after a run otherwise the potential will remain at the final value of the previous run It only makes sense to enable this option if Cell On Between Runs is also checked 2014 CH Instruments Inc mo CH Instruments Model 900D Series 5 15 Step Functions command This command opens the Step Functions dialog box Use this command to generate a continuous square waveform for electrode conditioning cleaning or other purposes No data will be collected and displayed The Step Functions command presents this dialog box Step Functions x Stat EM cr OK Duration sl fo Cancel Step Ei Mi An 0 Help Step Time 1 ll for StepE2 V AG 0 Step Time 2 s for Step Segment 2 Run aadi I Galvanostatic Mode Parameter Range Description Start E V 10 10 Starting potential Duration s 0 100000 Duration at Start E Step E1 V i1 A 10 10 First step potential Step Time 1 s 0001 100000 Duration of each step Step E2 V i2 A 10 10 Second step potential Step Time 2 s 0001 100000 Duration of each step Step Segments 1 2000000000 Step segments each segment is a half cycle Galvanostatic Mode Check or Uncheck Galvanostatic or potentiostatic unchecked mode Notes 1 The potential range between Start E Step E1 and Step E2 should be less than 13 1 V 2 If Duration is less than 0 001 sec the Start E potentia
228. p if the SMDE occasionally traps little air bubbles in the capillary and loses contact This option can also be varied using the Cell command under the Control menu E2 off During Quiet Time if applicable Not applicable for your instrument series Abort Experiment at Level The experiment will terminate automatically if the current or charge level reaches the specified value or overflows This allows electrode over current protection If No is selected the experiment will end normally 2014 CH Instruments Inc 120 CH Instruments Model 900D Series If 10s Change lt is selected the experiment will terminate automatically if the signal change after 10 seconds is less than the specified value in Amperes for current and Volts for potential This option is applicable only for time based techniques such as CA IT DPA DDPA and TPA The program does not monitor the signal change during the first 10 seconds of the experiment After that the program checks every time it samples The response time is equal to the sampling interval After data is read the program compare with the data point sampled 10 seconds ago and the difference will be checked If the difference is less than the specified value the experiment will terminate Abort Quiet Time The quiet time before data acquisition will terminate automatically if the current or charge level reaches the specified value or overflows If No is selected the experiment w
229. pedance data and SECM results Laplacian smoothing Delaunay triangulation and stereoscopic 3D anaglyph imaging no special video card or display required Data Processing smoothing 5 49 point least square and Fourier transform derivatives 1st 5th order 5 49 point least square numerical integration convolution semi derivative and semi integral interpolation 2x 64x 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 data point removal data point modification visual data point modification background subtraction difference between two data sets signal averaging averaging multiple sets of data mathematical operations both X and Y data arrays 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 saved data files based on user defined peak potential range species and calibration information gener
230. pling interval is shorter than 0 002s or 0 0005s with fast com port speed data will not be transferred in real time but rather after the experiment is completed The cell is turned off during data transfer unless the Cell On between Run option has been enabled using the Cell command The total number of data points will be limited by the instrument memory size 64K points The sampling interval may be automatically adjusted to fit the data points in a reasonable range If the sampling interval is longer than 0 002s or 0 0005s with fast com port speed data will be transferred in real time during the experiment The number of data points for each step will be limited by the instrument memory size 64K points The sampling interval may be automatically adjusted to fit the data points in a reasonable range H the sampling interval is greater than 0 005s it is possible to record external voltage signals e g spectroscopic signals simultaneously with the voltammogram Use the 9 pin D connector on the rear panel for signal input Consult the User s Manual for the pin out and signal level requirements When the second electrode is set to Step its potential will be the same as the primary electrode it is not independent 2014 CH Instruments Inc Setup Menu st 4 2 6 Chronocoulometry Parameters dialog box In Chronocoulometry CC the potential is stepped from Init E to Final E and may then be stepped back The following diagram shows
231. plitude is applied The current at the end of each potential pulse is sampled and recorded as a function of the pulse potential The following diagram shows the potential waveform applied as a function of time and the current sampling scheme Pulse Width Final E J k B Incr E A x Pulse Period Sample Width Time s Parameter Range Description Init E V 10 10 Initial potential Final E V 10 10 Final potential Incr E V 0 001 0 05 Increment potential of each pulse Pulse Width s 1e 3 10 Potential pulse width Sampling Width s 1e 4 10 Data sampling width Pulse Period s 0 01 50 Potential pulse period or dropping time Quiet Time s O 100000 Quiescent time before potential pulses begin Sensitivity A V 1e 12 0 1 Sensitivity scale Electrode 2 Potential V 10 10 Second working electrode potential if not scan Sensitivity A V 1e 12 0 1 Sensitivity scale for second electrode On Check or Uncheck Second working electrode at constant E Scan Check or Uncheck Scan the second electrode potential Notes e Init E and Final E should be at least 0 01 V apart e Pulse Width should be no more than half of Pulse Period otherwise the system will automatically readjust Pulse Width Sample Width should be no more than half of Pulse Width otherwise the system will automatically readjust Sample Width e When the second electrode is set to Scan its potential will be the same as the primary electrode it is not in
232. point left click and drag vertically to move the data point and release the mouse button to finish The old data point will be erased and a new data point will appear at the new position Segment Choose the data set segment you want to modify The range of valid values will depend on the electrochemical technique used Override Present Data Check this box to replace the currently active data with the modified data If this box is not checked the modified data will only be displayed without overriding the currently active data and invoking the Present Data Plot command will display the original data 2014 CH Instruments Inc DataProc Menu 193 7 10 Background 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 the following dialog box Background Subtraction 2 x Lkn h S dend EK EJ MP1 feito EJ IMPE1 FJ svo EJ IMPE2 fd NPVO EJ IMPE3 EJocpTi EJIMPE4 EJ Psao A File name evo Files of type Data Files fb D Cancel This allows you to select the background data file th
233. ppendix of the user manual for pin assignments iR Comp for Next Run When this box is checked iR compensation will be enabled for the next run You may be unable to enable iR compensation if automatic compensation has been set but the iR compensation test has not been conducted or if the sensitivity scale has been altered iR compensation is not available for certain techniques such as TAFEL BE IMP CP and PSA This option can also be turned on or off from the iR Compensation command under the Control menu Smooth After Run When this box is checked automatic smoothing will be performed after the run Certain techniques such as TAFEL BE and IMP do not allow smoothing This option can also be turned on or off using the Smoothing command under the DataProc menu where the mode of smoothing can be set to least square or Fourier transform Purge Between Runs Check this box to enable purging between runs Stir Between Runs Check this box to enable stirring between runs SMDE Drops Before Run When using the static mercury drop electrode SMDE specify the number of mercury drops to be dispensed before the experiment Normally the system will issue a combined dispense and knock signal before running the experiment to allow a new drop to be formed This parameter should be between 0 20 default 1 if set to 0 the same drop used in the previous experiment will be used for the next experiment It may be useful to use more than one prerun dro
234. pping Voltammetry Second Harmonic A C Stripping Voltammetry Controlled Current Techniques e Chronopotentiometry e Chronopotentiometry with Current Ramp e Multi Current Steps e Potentiometric Stripping Analysis Amperometric Detection Techniques e Amperometric i t Curve e Differential Pulse Amperometry 2014 CH Instruments Inc General Information 5 e Double Differential Pulse Amperometry e Triple Pulse Amperometry e Integrated Pulse Amperometric Detection Other Techniques e Bulk Electrolysis with Coulometry e Hydrodynamic Modulation Voltammetry e Electrochemical Noise Measurement e Open Circuit Potential Time 2014 CH Instruments Inc 6 CH Instruments Model 900D Series 1 3 Software Features User Interface Unicode tabbed document application compatible with 32 and 64 bit Windows monolithic architecture minimal installation footprint and portable design bypasses the Windows registry multiple instances control multiple instruments by simply duplicating the program customizable toolbar quick access to your most frequently used commands complete intuitive environment run experiments analyze data and generate plots all in the same window dock able toolbar quick graphical access to the most commonly used commands status bar technique file status and command prompt WYSIWYG graphics comprehensive context sensitive help File Management Unicode support international file and folder nam
235. r Electrochemical Noise Measurement Parameters for Open Circuit Potential Time Parameters for Surface Patterned Conditioning Parameters for Probe Scan Curve Parameters for Probe Approach Curve Parameters for Surface Interrogation SECM Parameters for Scanning Electrochemical Microscope Parameters for Z Probe Constant Current Control Parameters for Sampling Scheme 2014 CH Instruments Inc Setup Menu 53 4 2 1 Cyclic Voltammetry Parameters dialog box In Cyclic Voltammetry CV the potential is linearly swept from Init E to High E or Low E depending on the Init P N polarity parameter The potential is then swept back in the reverse direction The following diagram shows the applied potential waveform as a function of time Current is recorded as a function of potential Potential V Init E High E Scan Rate V s Parameter Init E V High E V Low E V Final E V Init P N Scan Rate V s Sweep Segments Sample Int V Quiet Time sec Sensitivity A V Auto Sens Enable Final E Aux Signal Rec Electrode 2 Potential V Differential E V Sensitivity A V Off Constant E Scan Diff Scan Notes 2014 CH Instruments Inc Low E Segment 1 Segment 2 Segment 3 Time s Range Description 10 10 Initial potential 10 10 Upper limit of potential scan 10 10 Lower limit of potential scan 10 10 Final potential if enabled Pos or Neg Initial scan dire
236. r approach to stop can also be specified as listed below Please refer to the Notes below for more details The program presents the following dialog box Probe Approach Curve Parameters Probe Electrode Probe E WI Sensitivity A V eg sl Probe E Pulse before Sampling Pulse E MI Pulse Duration sl Delay time s EI Pulse On Substrate Electrode Substrate E V Sensitivity A V 1 e 006 lt E20n i20n Parameter Range Probe E V 10 10 Sensitivity A V 1e 12 0 1 Pulse E V 10 10 Pulse Duration s 0 10 Delay time s 0 1 50 E1 Pulse On Substrate E V 10 10 Sensitivity A V 1e 12 0 1 SC Cancel Help Motor Selection e Stepper Approach Speed e Normal C Fast Probe Stop at Current Level Ratio 0 C Absolute 4 Max Incr fum Withdraw Distance um 0 0166667 Incr Time s Quiet Time s Description First probe potential Probe sensitivity scale Probe pulse potential Pulse duration Delay time after pulse before sampling Check or Uncheck Probe pulse potential on off Substrate potential Substrate sensitivity scale E2 On Check or Uncheck Substrate potential on off i2 On Check or Uncheck Substrate current measurement on off Motor Selection Select Auto stepper or piezo 2014 CH Instruments Inc Setup Menu ER Approach Speed Select Normal or fast Ratio 1 1000 Current ratio threshold Absolute A O 0 01 Cur
237. r each species The program will warn the user if Conc Data Type is selected and a slope is zero Intercept Enter the intercept of the calibration curve for each species to calculate the concentration of the compound A value must be specified for each species Peak Shape Select the peak shape that is most appropriate for your data The currently available choices are Gaussian diffusive and sigmoidal 2014 CH Instruments Inc 206 CH Instruments Model 900D Series Data Type Choose between original data semi derivative and first derivative to report the concentration Y Axis Title Enter the desired Y axis title e g Concentration or Peak Current to be plotted Y Axis Unit Enter the units dimension of concentration e g ppm or M Report Name Enter the report filename if you want to save the report text file If a file with the specified name already exists an overwrite warning will be issued If no filename is specified the report will be shown but not saved Report Data Type Either concentration or peak current can be reported Header Enter the desired title header for the data To display the header on the top of the plot check the Header box using the Graph Option command Note Enter any comments about the plot The note will not be displayed on the plot but will be saved in the data file It allows you to put additional comments about the data and is well suited for a brief description of the p
238. r liquid liquid interface measurements In this case the red and white clips are respectively connected to the counter and reference electrodes in phase L and the green and black clips are respectively connected to the counter and reference electrodes of phase Il The 4 electrode configuration also helps to eliminate contact resistance due to clips connectors and switching relay and the resistance of circuitry traces which is very important for large current gt 100 mA measurements and low impedance cells lt 1 ohm However some instruments have a maximum current of 10 mA or lower It is therefore not necessary to employ 4 electrode configuration in non L L measurements in these instances To use 4 electrode configuration please check the 4 Electrode option using the Cell command under the Control menu If you are using the 4 electrode configuration to eliminate contact resistance you should connect the sensing electrode together with the working electrode When not using 4 electrode configuration please make sure that the 4 Electrode box in the Cell Control dialog box is unchecked Otherwise noise and other problems may occur When using 3 electrode configuration please leave the Sensing electrode unconnected RDE Control Connection Banana jacks Red Signal Black Analog Ground Signal Output on Rear Panel 9 pin D connector 1 Current 1 Output 2 Current 2 Output bipotentiostat 3 Potential Output 4 External Potential
239. rement is 0 1 mV when the scan rate is below 1000 V s 1 mV at 5000 V s and 4 mV at 20000 V s The sampling interval can be 1 mV when the scan rate is below 1000 V s 2 mV at 2000 V s 5 mV at 5000 V s and 20 mV at 20000 V s The data sampling interval will be automatically increased at high scan rates If the scan rate is below 0 1 V s it is possible to record external voltage signals e g spectroscopic signals simultaneously with the voltammogram The input full scale range is 10V Use the 9 pin D connector on the real panel for signal input Consult the User Manual for the pin out and signal level requirements When the second electrode is enabled the auxiliary signal recording channel will be disabled When the second electrode is in Scan mode it will have the same potential as the primary electrode throughout the experiment The potential of the second electrode is therefore not independent When the second electrode is enabled the maximum scan rate is reduced to 100 V s and the sampling interval will be doubled at high scan rates 2014 CH Instruments Inc Setup Menu 4 2 3 Staircase Voltammetry Parameters dialog box In Staircase Voltammetry SCV the potential is incremented from Init E toward Final E and it may be scanned back The following diagram shows the potential waveform applied as a function of time Current is sampled after every potential increment and recorded as a function of potential Final E Z
240. rent level threshold Max Incr um 0 0001 1 Maximum increment of probe when approaching surface With Dist um O 10000 Probe withdraw distance before surface approach Incr Time s 0 001 0 2 Increment or sampling time Quiet Time s O 100000 Quiescent time before probe approach Notes When E2 On is checked the substrate potential will be turned on but no current will be measured When i2 On is checked the substrate potential will be turned on and current will be measured The probe can be stopped either manually or at an absolute current level depending on the selection made in the Probe Stop at Current Level area H the Current Ratio parameter is lower than 100 but the current increases as the probe approaches the e g conducting surface a default value of 125 will be used instead If the Current Ratio parameter is higher than 100 but the current decreases as the probe approaches the e g insulating surface a default value of 75 will be used instead PID control Proportional Integral Derivative is used for the probe approach The tip moves faster i e moves with bigger increments when the tip is far away from the surface and slows down i e moves with smaller increments when the tip is closer to the surface and the system senses a change in the tip current PID control reduces the risk of tip overshoot collision with the sample and consequent sample and or tip damage The maximum increment should be set according
241. ring to use it as a conducting substrate electrode Alternatively you can use the round plate to hold other samples Use a rubber O ring to seal the sample and cell holder to prevent leakage The Teflon cell should be mounted on the rectangular or T shaped plate using screws You may want to change the line frequency program setting 60 Hz or 50 Hz using the System command under the Setup menu This will set the default sampling period to a multiple of the reciprocal line frequency when applicable which will help to reduce noise Connecting the stepper motors and XYZ piezo block Use 15M 15F extension cables to connect the stepper motors to the 15 pin DA connectors labeled Stepper on the front panel marked for the X Y and Z axes from left to right You should use the 3 ft 15M 15F extension cables included with the instrument Other cables may have too high resistance which can cause serious errors in motor control To connect the piezo block to the controller simply connect the 4 pin round plug to the 4 pin round connector labeled Piezo on the front panel of the motor controller Please be advised that there are high voltages in the round connector You also need to connect the sensor connector to the front panel Understanding the piezo block The piezo lifetime depends essentially on the amplitude of the voltage applied to the piezo and how long a high voltage is applied At highest voltage 150V for this piezo the lifetime is about
242. roblem using the instrument Most of the following tips are intended for users who do not have much experience with Windows but may still be useful even for experienced users 1 Familiarize yourself with with the toolbar the bar with many buttons under the main menu bar which provides quick access to the most commonly used commands Hover the mouse cursor over a button without clicking to display a descriptive comment in the lower left corner of the main window 2 To select multiple filenames for multiple file printing overlay plots parallel plots etc left click on the name of the first file you want to select and drag the mouse while holding the left button to select multiple files If the files you want are scattered in the directory i e non consecutive you can select them by holding down the Ctrl key and clicking on each filename 3 If the Y axis title is oriented in the wrong direction use the Font command under the Graphics menu to change the rotation angle of the Y axis for printing 4 To select a file or technique you can double click the item This is equivalent to clicking the item and then click OK 5 To change parameters in a dialog box you can use the Tab key to cycle through its fields Text in the edit box will become highlighted and you can type directly to replace the highlighted text This can sometimes be much more convenient and faster than using the mouse Advanced users should also consider memorizing frequent
243. s Inc Setup Menu 4 2 15 Differential Pulse Amperometry Parameters dialog box In Differential Pulse Amperometry DPA a cleaning potential can be applied for electrode conditioning during which current is not sampled Two potential pulses are applied after the cleaning step and the current at the end of each pulse is recorded as a function of time During the experiment only the difference between the two current samples is displayed After the experiment the current responses to the two potential pulses will also be available for display The following diagram shows the potential waveform applied as a function of time and the current sampling scheme Data Sampling ki ki E 1 Clean E Init E Potential V E2 Clean T T1 T2 Cycle 2 Cycle 3 0 Time s Parameter Range Description Init E V 10 10 Initial potential Cleaning E V 10 10 Electrode cleaning potential Cleaning Time s 0 32 Electrode cleaning time Pulse E1 V 10 10 First pulse potential Pulse T1 s 0 01 32 First pulse time Pulse E2 V 10 10 Second pulse potential Pulse T2 s 0 01 32 Second pulse time Number of Cycles 10 100000 Number of Repetitive Cycles Quiet Time s O 100000 Quiescent time before potential pulses begin Scales During Run 1 2 3 Number of current display scales Sensitivity A V 1e 12 0 1 Sensitivity scale Open Circ Clean Check or Uncheck Cleaning step held at constant or open circuit p
244. s Inc om CH Instruments Model 900D Series 8 2 Standard Addition command This command opens the Standard Addition dialog box Use this command to calculate the concentration of the unknown by standard addition Namely the unknown is measured first and its peak height is recorded Then the standard solutions are added repeatedly measuring the peak height of the unknown after each standard addition 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 Standard Addition command presents this dialog box Standard Addition WS xi Concentration Peak Height Unknown H 425e 007 Cancel Addition 1 E 629e 007 2 2851 e 009 ion 10 999933 Addition 3 hee E Read Addition 4 fo Save x Axis Title Concentration x Axis Unit ppb Etat Y Axis Title Peak Current Y Axis Unit ja Header Pb in water water Note 100 Addition 2 200 7 361e 007 Seier ii Help CEE Kn D The following options allow you to specify data calculating the concentration of the unknown species or plotting Unknown Enter the peak height of the unknown species to allow calculation of its concentration Addition Enter the concentration and peak height current after adding standard solutions X Axis Title Enter the desired X axis title e g Concentration to be plotte
245. s and configure ports using the Windows Control Panel Printer Properties Displays a dialog box where you can make additional choices about printing specific to the type of printer you have selected Orientation Specifies Portrait or Landscape The paper orientation should be set to landscape in the CHI program environment If you choose Portrait and try to print a warning may pop up and you will have to use the Print Setup command to set the paper orientation back to landscape Paper Size Specifies the size of paper that the document is to be printed on Paper Source Specifies the paper source because some printers offer multiple trays for different paper sources Network 2014 CH Instruments Inc CH Instruments Model 900D Series Click this button to connect to a network location assigning it a new drive letter 2014 CH Instruments Inc File Menu 3 13 Exit command Use this command to end your program session The program prompts you to save documents with unsaved changes Upon exiting settings including directory system setup control status macros data processing simulation and graphics options color and font will be saved 2014 CH Instruments Inc Setup Menu 49 Chapter 4 Setup Menu The Setup menu offers the following commands Technique Select one of many electrochemical techniques Parameters Choose experimental parameters System Set system defaults Hardware Test Test system hard
246. s have been included to undo or redo your actions remove all components and connection wires save your equivalent circuit drawing to file and read it back later and change the impedance simulation parameters such as frequency range and number of data points per decade of frequency Simulation and Fitting Please notice that the equivalent circuit you draw can be used for both simulation and fitting To perform a simulation click the Sim button the program will close the circuit editor in order to display the simulated data on the screen Warning unsaved data will be erased when a new simulation starts Save your existing data before starting a simulation Data fitting requires an equivalent circuit as well as a set of impedance data obtained from impedance measurements or even from a preceding simulation A poor fit may indicate an equivalent circuit that is a poor approximation to your physical system You may need to revise your proposed equivalent circuit to obtain a better fit 2014 CH Instruments Inc 222 CH Instruments Model 900D Series The fitting program has known limitations Sometimes a poor fit will be obtained even with a known simulated data set Results may also depend on the initial values of the components If you experience problems please send the data to info chinstruments com We will try to study and improve it but cannot guarantee better results Efficient fitting algorithms are difficult and complicated to
247. s in Windows or shell scripts in Unix Linux and is much more flexible than the Repetitive Runs command The Macro Command command presents this dialog box Macro Command Ea Macro Command Editor OK Cancel Help Read Save save cv001 vs UA run save cv002 0 3 run save cv003 vs b ha Run Macro A Read Load macro from file The program displays the Open dialog box so you can select your file Save Save macro to file for later use The program displays the Save As dialog box so you can name your file Test Test macro for syntax errors The program will automatically do this when the macro is run this button is included so that you can check your macro before you are finished writing it Run Macro Click this button to execute the macro The system will verify the commands and parameter ranges of your macro before proceeding Run on OK When this box is checked the macro will execute after you click the OK button When this box is unchecked the dialog box will close when you click OK saving your macro without running it the old default behavior of OK Macro Command Editor 2014 CH Instruments Inc 126 CH Instruments Model 900D Series Type in the desired series of 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 sep
248. s of the stepper stage are lost Before doing so ensure that no tip is present in the tip holder otherwise the motor move will cause the tip to be broken Clicking on the Reset button will move the stage to its home position which is stored in memory and then move it to the center position After clicking on the Reset button please wait for the operation to be completed The stage position will be remembered even after the motor controller is powered off Stepper Stage Moving Speed When this value is below 32 um sec setting resolution will be 1 nm As moving speed increases setting resolution and accuracy will worsen i e there is a tradeoff between speed and setting resolution When the Max Speed box is checked the motor will move at maximum rate with relatively low setting resolution Please keep in mind that the stage may vibrate slightly when the moving speed is high It is recommended to raise the tip at fast speeds to prevent the tip from touching the sample surface due to stage vibration 2014 CH Instruments Inc Control Menu 1 Stepper Stage Position Set and Relocate Up to four positions can be defined by the user for quickly changing the stage position Click the corresponding Set button to memorize the current position as one of these points click the Goto button to move the stepper stage to the preset point Stepper Stage Position The stepper motor position is continuously updated while this dialog box is op
249. s sec Y 1e 12 to 1e12 d vD 1e 6 to 1000 Open Finite Layer OFD Siemens sec Y 10 12 to 1612 Diffusion d vD 1e 6 to 1000 Siemens sec Y 1e 12 to 1612 k 1e 12 to 1e12 Gerischer Impedance G Circuit Element Properties Element Impedance Conductance Phase R resistor d e SR Yk 1 R 0 frequency independent C capacitor Ze j C Yo jad Q w2 L inductor Z joL Y Vol p w2 W Warburg Zy We k Yw 19 Y p w4 Q phase Za Gay Ya Wo Y p nW2 0 lt n lt 1 CC Cole Cole Zso Hiel Yoc 1 jor PH tan t sin an 2 1 wt cos an 2 CD Cole Zen R aalt Von aler PR tan g a t 2014 CH Instruments Inc Sim Menu 223 Davidson FD Finite Layer Z 1 Y Yep Y Sato tan ol arg ce Diffusion tanh sqrt ja D OFD Open Finite Zen 1 Y ofp Yorp Ya Sart ja tan Lol arg Den Layer Diffusion coth 5 sart jw D GI Gerischer Seegen Yo Y Sart k jo tan ol arg Yo Impedance For more information refer to J R Macdonald Ann Biomed Eng 20 289 305 1992 or Impedance Spectroscopy E Barsoukov and J R Macdonald Wiley Hoboken 1987 1st ed 2005 2nd ed 2014 CH Instruments Inc 24 CH Instruments Model 900D Series 9 3 CV Simulate command Use this command to generate simulated CV data The reaction mechanism concentrations kinetic parameters and experimental parameters must be first set with the Mechanism c
250. s selected you will have to click on a message box before each run except the 1st run The instrument will wait until you respond If External Trigger is selected the instrument will wait for an external trigger signal before each run The trigger signal is an active low signal and can be applied to Pin 13 of the Cell Control port on the rear panel When Manual or External Trigger is selected the Time Interval Between Runs parameter is ignored Base Filename Click Browse or type directly in this field to specify the filename prefix up to 5 characters Data will be saved after each run The run number will be attached to the base filename i e filenameN where N is the run number If a base filename is not specified a warning will be given If you continue the system will run the experiments without saving any data Data Averaging When Done 2014 CH Instruments Inc 122 CH Instruments Model 900D Series When this item is checked the data of the repetitive runs will be averaged and saved as filenameo0 2014 CH Instruments Inc Control Menu 123 5 9 Multiplexer command This command opens the Multiplexer dialog box Use this command to run a series of experiments using the CHI684 Multiplexer sold separately The multiplexer switches four lines working sensing reference and counter for a single potentiostat second working reference and counter for a bipotentiostat You can have up to 64 cells but only one cell
251. sation External Potential Input Auxiliary Channel k Corresponding polarographic mode can be performed S Corresponding stripping mode can be performed Dynamic Range of Selected Experimental Parameters Parameters Rane Techniques Potential V neo TI Current A fotooo TI Sensitivity Av 10 too 001 TI Single channel 8x0D or dual channel 8x2D electrochemical detection High sensitivity and low noise Fast 16 bit A D converter 1 MHz Bipotentiostat can also be used for RRDE 2014 CH Instruments Inc 258 CH Instruments Model 900D Series 12 12 Model 920D Scanning Electrochemical Microscope The scanning electrochemical microscope SECM was introduced in 1989 as an instrument that could examine chemistry at high resolution near interfaces By detecting reactions that occur at a small electrode the tip as it is scanned in close proximity to a surface the SECM can be employed to obtain chemical reactivity images of surfaces and to make 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 interfaces The trapping and electrochemical detection of single molecules by SECM has also been reported 1 A J Bard F R F Fan J Kwak and O
252. selected technique will become the new default when the program starts as well as for all new documents This will not take effect if you click Cancel or the close button Always confirm parameters When this option is checked a parameters dialog box will always be displayed after technique selection even if your selection has not changed Run prompt after params When this option is checked you will be asked whether to run the experiment immediately after confirming parameter values 2014 CH Instruments Inc Setup Menu 51 Polarographic Mode When this option is checked polarographic mode will be enabled allowing the mercury drop to grow and be dislodged for every data point Polarographic mode is available only for the following techniques e Differential Pulse Polarography DPP e Normal Pulse Polarography NPP Enabling polarographic mode will automatically disable stripping mode To re enable stripping mode the Polarographic Mode option must be unchecked View as tree When this option is checked the Technique Selection item will be displayed as a categorized list The categories can be expanded or collapsed by clicking the plus or minus boxes to their left The program will remember which categories you previously had expanded 2014 CH Instruments Inc 52 CH Instruments Model 900D Series 4 2 Parameters command This command opens a dialog box to set experimental parameters for the technique currently
253. seline will appear with corresponding numerical values reported at the right side of the plot Notice that half peak area is reported in this case For a sigmoidal wave two baselines are needed one at the foot and one at the plateau of the wave Left click and drag to draw each baseline A vertical line connecting the two baselines and crossing the middle of the wave will appear with corresponding numerical values reported at the right side of the plot 2014 CH Instruments Inc 166 CH Instruments Model 900D Series 6 12 Peak Definition command Use this command to define the peak shape as Gaussian diffusive or sigmoidal You can also choose to report peak or wave potential half peak or wave potential peak or wave currents and or peak area The selected peak definition is used by both automatic and manual result reporting This command opens a technique dependent dialog box ACV CV IT SWV other This command has a toolbar button The general Peak Definition dialog box is Peak Definition x Peak Shape Report Option o IV Peak or wave potential Gaussian Cancel SE Half peak potential Help rl IV Peak or wave current C Sygmoidal IV Peak area Peak or wave search potential range hl os General Peak Definition options are Peak Shape Define the peak shape as Gaussian diffusive or sigmoidal as appropriate to your data A default peak shape is assigned based on
254. serting a deposition step before the quiet time step preceding the experiment The deposition potential and time can be specified in this dialog box After the deposition period and before quiet time the potential will be set back to its initial value The potential scan during the stripping step will start from this value Purge During Deposition When this box is checked the system will purge the solution during the deposition period Stir During Deposition When this box is checked the system will stir the solution during the deposition period Deposition Potential Specify whether the initial potential or the value specified in the Deposition E field is applied during the deposition period 2014 CH Instruments Inc Control Menu 147 Quiet Potential Specify whether the initial potential or the value specified in the Quiet E field is applied during the quiescent period Deposition E Specify the value of the potential to be applied during the deposition period if the Deposition E option is selected under Deposition Potential this value is ignored if Initial E is selected instead Deposition Time Specify the deposition time from 0 to 100000 Quiet E Specify the value of the potential to be applied during the quiescent period if the Quiet E option is selected under Quiet Potential this value is ignored if Initial E is selected instead 2014 CH Instruments Inc ms CH Instruments Model 900D Series 5 20 SECM
255. set to unity by default and all concentrations during simulation are scaled relative to this value The unit distance is set to 6 sqrt Dt by default where D is the diffusion coefficient and t the total time involved in the given experiment To change the scales for concentration and distance from these default values see the two sections below 2014 CH Instruments Inc Sim Menu 213 Conc Range Enter the scale factor for displaying the concentration profile The range is 0 001 100000 and the default is 1 Dist Range Enter the scale factor for displaying distances The range is 0 001 10 and the default is 1 Time Delay Loop The execution time of the simulation depends on the problem you want to study and the type of computer used When the execution time is too short you may not be able to visualize changes in the concentration profile clearly The Time Delay Loop variable allows you to slow the simulation down for such visualization purposes by inserting a delay of this value between the computation of two points The range of this parameter is from 0 to 1e6 The appropriate value will depend on the problem you want to study and the speed of your PC Read Save You can read from save to sim files that contain all the parameters needed for simulation On clicking the Read Save button the program displays an Open Save As dialog box so you can select name your file Exp Param Click this button to set experimental p
256. t peak foot to potential BC 2nd peak foot from potential BC 2nd peak foot to potential BC 3rd peak foot from potential BC 3rd peak foot to potential BC 4th peak foot from potential BC 4th peak foot to potential BC 5th peak foot from potential BC 5th peak foot to potential BC polynomial order BC algorithm O orthogonal 1 least squares specify note field specify header field in plot terminate program use at your own risk Legal Commands bipotentiostat only Command e2on e2off i2on i2off e2 e2scan e2d e2dscan 2014 CH Instruments Inc Parameter 10 10 Explanation turn on 2nd working electrode no data recording turn off 2nd working electrode turn on 2nd working electrode and record data turn off 2nd working electrode initial potential for channel 2 2nd channel scan or step w primary channel constant potential difference between 2nd and primary channel during potential scan or step enable 2nd channel potential scan w primary channel but keep constant potential difference 130 CH Instruments Model 900D Series Legal Commands multipotentiostat only Command ei e2 e3 e4 e5 e6 e7 es sens sens2 sens3 sens4 sens5 sens6 sens7 sens8 elon e2on e3on e4on e5on e6on e7on e8on eloff e2off e3off e4off e5off e6off e7off e8off e2scan e3scan Parameter 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 1e 9
257. ta curves You can also change marker line options Legend for data curves and the grid Color and legend options will be saved when you exit the program and will be reloaded when you restart the program To change text color use the Font command instead This command has a toolbar button EI The Color and Legend command presents a dialog box Color Selection E xi x Color Legend Size Interval OK Curve 0 E SolidLine zl h d 1 E Cancel Curve 1 B Change SoidLine zl D d D d Help Curve 2 C Change SolidLine zl D sl D sl te Curve 3 E Change Led Une zl fi sl D d Dest Curve 4 Di Change SolidLine zl D sl D Monochrome Curve 5 C Change SolidLine zl h d fi sl Curve 6 F Change SoidLine zl D d D d Curve 7 BB change Solid Line DI D sl D sl Curve 8 EI change Solid Line DI D sl D sl Curve 9 EI change Solid Line E Dn d i i Grid change Point Color Color Thickness Bkgnd Change x Y Axis E Color Bar Two Color z lel GE D Ve bi 4 1 The following options allow you to specify the colors and the data marker line options of the plot Curve Curve 0 indicates the currently active data Curves 1 9 indicate Overlay Plots Color 2014 CH Instruments Inc Graphics Menu 177 You can specify the color of data curves the grid the background and the axes by clicking the corresponding Change button to open a system Color dialog box
258. tage Next stack the Z stand on the X stage plate Use four cap screws to secure the Z stand to the X stage The front edge of the Z stand should be aligned with the front edge of the X stage and not recessed in at all to ensure that when the Z stage does not collide with the X stage when it moves up and down Please note that the positive direction for the X axis is to the right The positive direction for the Y axis is to the front The positive direction for the Z axis is downward For the 920D once all three stages are mounted you need to mount the XYZ piezo block to the Z stage The piezo mounting piece piezo positioner and tip holder are shipped pre assembled Use two 5 mm cap screws to mount the T shaped mounting piece with the XYZ piezo block to the middle row of the Z stage The cell sample holder should be mounted on top of the bottom supporting stainless steel plate with a rectangular plate on top of the columns You can put the cell and sample on the plate for measurements If you want to adjust the tilt level of the cell and sample you can mount three fine adjustment screws on the rectangular plate and put the T shaped stainless steel plate on top of those fine adjustment screws Each turn of screw corresponds to 317 um The resolution is 1 um On both the rectangular and T shaped plates there is a hole for a round plate or a ring The round plate and ring are interchangeable Insert the platinum disk working electrode into the
259. tage converter is employed during the run an Overflow warning may appear This is caused by the current transient immediately following the potential step If the intercept which gives information about double layer capacitance and adsorption of the Anson plot Q t 1 2 plot is not your primary interest you need not worry about this However if data distortion can be observed visually you should lower the sensitivity scale In some cases you may want to use the 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 measurement accuracy it is recommended to use the highest sensitivity scale possible 2014 CH Instruments Inc Setup Menu s 4 2 7 Differential Pulse Voltammetry Parameters dialog box In Differential Pulse Voltammetry DPV the base potential is incremented from Init E toward Final E A potential pulse is applied Current is sampled before the potential pulse and at the end of the pulse The difference between these two current samples is recorded as a function of potential The following diagram shows the potential waveform applied as a function of time and the current sampling scheme o Pulse Width T J k 7 2 Amplitude Final E O A Init E J kk ARE Pulse Period SCHERGEN Time s Parameter Range Description Init E V 10 10 Initial potential Final E V
260. te a report for stored data files Options are available to specify peak potential windows slope intercept of calibration curves destination file name etc The Data File Report command presents this dialog box Data File Report a xj Species 1 Species 2 Species 3 Species 4 OK Species Cu Fb Cancel Ep From Mt Lo oz fo jo Ep To J EZ Los jo Slope 2 279e 9 2 285e 3 jo Intercept 1 652e8 3 8259 pooo Peak Shape Gausian Y Data Type Original DI Number of Species E Fispor Data Tus Concentration Unit ppb s Ze Conc C Current Report Filename ww Bn Header Waste Water Batch 16 Note The following options allow you to specify peak potential windows slope intercept of calibration curves and select the data files to be reported Compound Enter the names of the species to be analyzed Up to 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 Ranges should not overlap for different species Slope Enter the slope of the calibration curve for each species to calculate the concentration of the compound A value must be specified for each species The program will warn the user if Conc Data Type is selected and a slope is zero Intercept 2014 CH Instruments Inc Analysis Menu 203 Enter the intercept o
261. tential is scanned Peak E to Return E often Start E Potential scan time current integration continues Hold potential constant Hold potential duration current integration for first 10 ms Oxidation potential for electrode treatment Oxidation time duration Reduction potential for electrode treatment Reduction time duration Number of cycles through six steps Quiescent time before potential scan Sensitivity scale 2014 CH Instruments Inc Setup Menu Notes e The experimental sequence consists of a constant 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 is reached or interrupted by the user e 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 e During an 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 unexpectedly long experiment 2014 CH Instruments Inc CH Instruments Model 900D Series 4 2 19 Bulk Electrolysis with Coulometry Parameters dialog box In Bulk Electrolysis with Coulometry BE a constant potential is applied and the integrated charge is recorded as a function of time The following diagram shows the potential w
262. ter electrode and the black clip is connected to the reference electrode You should turn the 4th electrode off if you do not use a 4 electrode configuration Otherwise the potential will be out of control if the sensing electrode is left unconnected which could damage the electrodes Purge Between Runs 2014 CH Instruments Inc Control Menu 1 Check this box to enable purging between runs This option can also be turned on or off using the Run Status command under the Control menu Stir Between Runs Check this box to enable stirring between runs This option can also be turned on or off using the Run Status command under the Control menu Stir and Purge Simultaneously Check this box to stir and purge at the same time Test with Internal Dummy Cell Check this box to run the experiment with the instrument s internal dummy cell a built in 1K ohm resistor instead of an external cell which can be useful for testing the instrument Cell On Between Runs Normally the cell will be turned on only during an experiment and turned off after the experiment ends Check this box to keep the cell connected after a run Be careful when this option is enabled Connecting or disconnecting the cell in an improper sequence can damage the electrodes when the cell is on You should connect the reference and counter electrodes first When disconnecting disconnect the working electrode first Return to Initial E after Run Check this b
263. the potential waveform applied as a function of time The charge passing through the working electrode is recorded as a function of time Final E Final E Pulse Width Pulse Width Potential V Time s Parameter Range Description Init E V 10 10 Initial potential Final E V 10 10 Final potential Number of Steps 1 320 Number of potential steps Pulse Width s 1e 4 1000 Potential pulse width Sample Interval s 1e 6 10 Data sampling interval Quiet Time s O 100000 Quiescent time before potential step Sensitivity A V 1e 12 0 1 or Sensitivity scale q1e 9 1e 6 C V Notes e Init E and Final E should be at least 0 01 V apart e The maximum potential step range is 13 1 V e A true integrator charge to voltage converter can be employed in which case the sensitivity is 1e 9 to 1e 6 C V If charge exceeds 8e 6 coulombs the capacitor of the 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 may be discontinuities in the charge time curve due to this capacitor discharge These discontinuities should be negligible but if they turn out to have a significant effect on the measurement you can use the current to voltage converter instead and use the software integrator to convert current to charge A current to voltage converter is not ideal for chronocoulometry particularly if early transient data are important as i
264. the selected experimental technique However you can change this setting Report Option You can also choose to report peak or wave potential half peak or wave potential peak or wave currents and or peak area Peak or wave search potential range Depending on peak shape the peak search potential range can be adjusted For a broader peak or wave the search potential range should be larger The search potential range should include both sides of the peak or wave This parameter is only meaningful for automatic result reporting 2014 CH Instruments Inc Graphics Menu 167 6 13 X Y Plot command This command opens the X Y Plot dialog box Use this command to input data manually for plotting Linear curve fitting can also be performed After the data have been input click the OK button to generate the plot The resulting XY plot is temporary and will disappear if other data display commands are invoked You can use the Graph Option Color and Legend and Font commands to customize your plot You can also save your data overlay your data plots or make parallel plots The X Y Plot command presents this dialog box X Y Plot EN x Y Data Array Editor Cancel Help Read Save Overlay Plot Parallel Plot Plot ekibe 1 00 7 83 H I Linear Curve Fitting X Axis Title Potential Unit fv Y Axis Title Dropping Time Unit sec Header Electrocapillary Curve Note The following options al
265. tial The parameter range is from 10 to 10 Time The parameter range is from 0 to 6400 Set to 0 to skip a given step If a nonzero value less than 1 msec is specified the time control may not be accurate Stir On Check this box to enable stirring during preconditioning Purge On Check this box to enable purge during preconditioning 2014 CH Instruments Inc Control Menu 143 2014 CH Instruments Inc m CH Instruments Model 900D Series 5 17 Rotating Disk Electrode command This command available only in select models opens the Rotating Disk Electrode Control dialog box Use this command to specify the rotation rate of the rotating disk electrode You can also turn the rotator on and off in certain cases The Rotating Disk Electrode command presents this dialog box Rotating Disk Electrode Con Ed Rotation Speed rpm Gem oy V Rotate during DepositionTime Cancel Jh Rotate during Quiet Time Help Jh Rotate during Run Rotate between Run Rotation Speed rpm Specify the speed of the rotating disk electrode from 0 to 10000 rpm There are banana jacks on the rear panel of the instrument that will output 0 to 10 V corresponding to these speeds Rotate during Deposition Time Check this box to turn the rotator on during deposition time in stripping analysis This option can also be found in the Run Status command under the Control menu Rotate during Quiet Time Check this box to turn
266. tiple sets of data side by side This is particularly useful to view data obtained with different techniques and for data comparison To view a saved parallel plot use the Replot Parallel command This command presents the following dialog box Parallel Data Display j 2 x Look in acs s rh PS fs MP1 EJ IMPE1 EJ IMPE2 EJ IMPE3 EJocpTi EJ IMPE4 EJ Psao Cancel gt Filename SHACVO BIN CH BIN ONS BIN LSVO B Files of type Data Files bin DI E Select the data files you want to plot alongside 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 while holding the Ctrl key down to select files one at a time This command allows you select multiple files in the same directory In order to plot data files located in a different directory or drive use the Add Data to Parallel command Each plot will be automatically scaled to fit its individual data unless the scale is frozen using the Graph Option command In this case all plots will have the same frozen scale The Graph Option Color and Legend and Font commands allow you customize your overlay plot 2014 CH Instruments Inc Graphics Menu e 6 7 Add Data to Parallel command This command complements the Parallel Plots command allowing you to add more data to an existing parallel plot This allows
267. to the probe size the smaller the probe diameter the smaller the increment should be Before the probe moves toward the surface it will move backward for by Withdraw Distance The options in the Probe E Pulse before Sampling area can be used for electrode cleaning purposes during an experiment If E1 Pulse On is unchecked this feature will be ignored Normal approach speed should be used if the probe approach curve is to be recorded for data analysis purposes or if the probe is already close to the surface Fast approach speed can be used for a quicker probe approach without causing the probe to touch the surface This is useful when the probe is far away from the surface lf Automatic motor selection is selected the stepper motor will be used if the increment is greater than 0 1 micron Otherwise the piezo will be used If the piezo positioner is selected but the travel distance exceeds the piezo range a warning will appear and the approach will stop To reduce interference from the power line frequency the sampling period via Incr Time should be a multiple of the reciprocal of the line frequency For instance if the line frequency is 60 Hz an Incr Time of 0 01667 0 03333 0 05 0 06667 0 08333 0 1 etc is recommended If the line frequency is 50 Hz an Incr Time divisible by 0 02 is recommended 2014 CH Instruments Inc 10 CH Instruments Model 900D Series 4 2 35 Surface Interrogation SECM Parameters dialog box
268. toff frequency For a time based experiment e g CA CC TB the Fourier conjugate frequency has units of 1 s or Hz voltammetry it has units of 1 V In the latter case the physical meaning is how many signal cycles are allowed in one volt of potential range A lower cutoff will result in better smoothing but may also cause distortion The program performs Fourier transform smoothing using the algorithm of D E Smith et al For more details about this algorithm please refer to 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 Distortion may be minimal if the signal band is well separated from the noise band However this method is more time consuming than least square smoothing 2014 CH Instruments Inc DataProc Menu 183 Smooth After Run Check this box to enable automatic smoothing after each experimental run Certain techniques do not allow smoothing e g TAFEL BE IMP This option can also be turned on or off from the Run Status command under the Control menu Override Present Data Check this box to replace the currently active data with the resulting smoothed data If this box is not checked the smoothed data will only be displayed without overriding the currently active data and invoking the Present Data Plot command will display the original data 2014 CH Instrum
269. trol menu You should observe a straight line with current from 5e 6 A to 5e 6 A To test software performance open a data file using the Open command under the File menu to open the test data files included on the software CD These are the actual test results for this particular instrument To open the files select the files and click OK or double click the filename After reading them in you can display or process the data Try the commands under the Graphics and DataProc menus To revert to the original data and undo all unsaved changes simply close the file and reload the data with the Open command When you assemble the SECM as shown in Figure 2 3 above you need to calibrate the piezo first for model 920D Use the SECM Probe command under the Control menu see Chapter 5 To test the SECM it is suggested to use 1 mM ferrocenemethanol in 0 1M KNO Ferrocenemethanol can be purchased from Aldrich Chemical Co It is water soluble and its redox reaction is reversible It is better than ferricyanide or rutheniumhexamine and gives more reproducible data The curve is flatter in the diffusion limited region Moreover the electrode surface will not be contaminated whereas ferricyanide reaction products may adsorb to the surface of the electrode decreasing current flow over time First mount the platinum disk substrate electrode onto the SECM cell The substrate electrode can be inserted into the metal ring Insert the substrate electrode i
270. ulometry BE Hydrodynamic Modulation Voltammetry HMV AC Impedance IMP Chronopotentiometry CP Potentiometric Stripping Analysis PSA 2014 CH Instruments Inc 232 CH Instruments Model 900D Series 10 4 Clock command This command opens the Clock dialog box Use this command to view the current date and time which are refreshed constantly The Clock command presents this dialog box which displays the current system date and time 2014 CH Instruments Inc View Menu 233 10 5 Toolbar command Use this command to display and hide the toolbar which includes buttons for some of the most common commands in the program such as File Open A checkmark 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 as shown below d CHIG60A Electrochemical Workstation C 1 i z Oj x File Setup Control Graphics DataProc Analysis Sim View Window Help Gelle TE gt moll elalem gt aa wl DN For Help press F1 3 Electrode 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 click Toolbar from the View menu DilCreate a new document 2 Open an existing document using the Open dialog box Save the active document Print the active document m Sel
271. uments Inc File Menu 31 separated by spaces for example CVO CV1 Files of type Specifies the type of file you want to open by default all files are displayed Extension Description bin Binary data files txt Plain text files CSV Comma separated value files 2014 CH Instruments Inc 32 CH Instruments Model 900D Series 3 2 Save As command This command opens the File Save As dialog box Use this command to save and name the active document The program displays the Save As dialog box so you can name your document When a non binary file type is selected this command allows you to perform the Convert to Text operation on the currently active data file without having to navigate to the file This command has a toolbar button The Save As command presents this dialog box Em A Saeklc cht zs rh ES Flmp feito Ewe STE FJ IMPE2 EJ NPVO Ewe EJocpTi EJ IMPE4 EJ Psao gt Save as type Data Files bin DI Cancel A The following options allow you to specify the name and location of the file you re about to save File name Specifies a file name to save the current data and system variables with a different name You don t have to type the extension the program will automatically add the extension you specify in the Save as type box If an existing filename is used the system will display a confirmation prompt before proceeding Save as type Specifies the type of f
272. unter aux and reference red and white to the other Noticeable divergence from this behawor i e linearity through the origin may suggest faulty leads 2 d Erroneous data behavior in an actual electrochemical experiment may be due to factors such as faulty cell connections poor reference electrode contact or poor condition of the working electrode Reference and working electrodes are consumable items and are readily available from CH Instruments Inc or your local dealer see Appendix for a description of the range of accessories available When a customer uses his her own electrodes it is recommended that experimental data be compared against known standards from time to time 3 The cover of the instrument should only be removed by qualified personnel at the direction of CH Instruments Inc 4 Users should always refer 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 as applicable Hardware faults are usually diagnosed through the instrument s own self test procedure see Troubleshooting in the Appendix 6 As the instrument requires a data connection 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 a
273. urpose and conditions of the experiment Read Use this command to read data from file Save Use this command to save data to file 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 2014 CH Instruments Inc Analysis Menu 207 8 5 Special Analysis command Currently this command is only active for TAFEL measurements Use this command to calculate the corrosion rate from Tafel experiment results by opening the Corrosion Rate Calculation dialog box When TAFEL data are available invoking the Special Analysis command presents this dialog box Corrosion Rate Calculation BS xj Data Segment fi DI Equilibrium E 0 313 Cancel m Cathodic Tafel Slope Potential Range Help o1 53 to 0 253 m Anodic Tafel Slope Potential Range 0 373 to 0 473 Cathodic Tafel Slope Anodic Tafel Slope Linear Polarization R Corrosion Current Data Segment If you have more than one segment of data you need to specify which segment of data to use in the corrosion rate calculation Equilibrium E The program will automatically estimate the equilibrium potential by searching for the potential value where current is closest to zero You can manually override this default estimate Cathodic Tafel Slope Potential Range By default the cathodic Tafel slope p
274. urrent plot is not an overlay plot 2014 CH Instruments Inc 158 CH Instruments Model 900D Series 6 4 Replot Overlay command Use this command to display the most recent Overlay plot This is useful after clicking the Present Data Plot button or when loading plots from file 2014 CH Instruments Inc Graphics Menu 159 6 5 Manage Overlay command Use this command to open the Manage Files dialog box This will allow you to add reorder and remove files from a multi file plot The Manage Overlay or Manage Parallel command presents this dialog box This dialog box displays a list of all files being plotted with the current file As in older versions of the program the current file is always the first plot so it cannot be moved or removed Click OK to confirm all changes Add Clicking this button has the same effect as the Add Data to Overlay or Add Data to Parallel command Move Up Down Select multiple files by holding down Ctrl or Shift key and left clicking You can then to move your selection up or down in the list by clicking the appropriate Move button The current file is always the first plot so you will not be able to move your selection above it Remove Select file s as when using Move Up Down Once you click Remove these files will be removed from your plot 2014 CH Instruments Inc 160 CH Instruments Model 900D Series 6 6 Parallel Plots command Use this command to plot mul
275. ve context sensitive help to be available The program has been designed with ease of use in mind It is self contained and portable Double click chi exe to start the program The only file required to run the software and control the instrument is chi exe which can be placed in any directory for which you have write and execute permission This can be particularly useful in restricted user settings teaching labs portable installations on removable media etc simply copy the exe file and chm file to say the user s home directory The first time it is run the program will automatically generate a binary configuration file chi cfg containing virtually all user preferences and settings This configuration file will have the same name and location as the executable and multiple instruments can be controlled using multiple copies of the executable each with its own configuration file e g chi660d1 exe chi660d1 cfg and chi660d2 exe chi660d2 cfg Newer versions of the software will also generate chi ini which harkens back to a kinder gentler time when ini files ruled the electronic earth untrammeled by the unreliable tyranny of the registry Even now our software avoids the registry completely storing all settings in the cho and ini files streamlining the transfer of user settings between directories or computers to a simple file copy operation In previous versions of the software the auto generated configurat
276. vity scale automatic or manual Notes e When DC current is high and AC current is low sensitivity cannot be increased because the DC current will overflow This problem is more serious when the frequency is relatively low The application of a DC current bias allows higher AC signal amplification A 16 bit DAC is used for this purpose On the other hand if the DC current is not expected to be large and the frequency is high a DC current bias may be unnecessary Automatic sensitivity scale is used by default During the experiment the system tests the current size and determines the proper sensitivity scale This usually works pretty well The sensitivity scale setting can also be manually overridden which may yield better results in certain cases 2014 CH Instruments Inc ER CH Instruments Model 900D Series 4 2 26 Chronopotentiometry Parameters dialog box In Chronopotentiometry CP two current levels can be specified to pass through the working electrode with the switching between the two dictated by time or potential Potential is recorded as a function of time The following diagram shows the current waveform applied as a function of time Anodic Current Anodic Time Current A lt Cathodic Time Cathodic Time gt Cathodic Current Cathodic Current Segment 1 Segment 2 Segment 3 0 Time s Parameter Range Description Cathodic Curr A 2 2 Controlled cathodic current Anodic Current A 2 2
277. ware 2014 CH Instruments Inc so CH Instruments Model 900D Series 4 1 Technique command This command opens the Electrochemical Techniques dialog box Use this command to select an electrochemical technique This frequently used command is the fountainhead from whence all experiments spring forth This command has a toolbar button The Technique command presents this dialog box which lists all electrochemical techniques available on your instrument Technique Selection There are multiple ways to perform technique selection e Double click the desired technique e Single click the technique then click OK e Single click the technique then press Enter e Use the Up Down arrow keys then press Enter Tech Help Click this button to toggle technique specific help When this is enabled information about the selected technique will be displayed automatically Tech Help is not compatible with the Old Help option Also please note that the parameter value ranges and technical details shown here may not apply to your instrument model for model specific information click Help once a technique specific dialog box is shown Show on startup When this option is checked this dialog box will be presented each time the program starts Show for new documents When this option is checked this dialog box will be presented each time you create a new document Use current tech on startup When this option is checked the currently
278. x Lookin lc de Ee ES Pe IMPO Elwen Pd ito EJ IMPE1 PALsva ad IMPE2 fd NPVO EJ IMPE3 EJocpTi EJIMPE4 EJ Psao Files of type Data Files bin DI Cancel i h The following options allow you to specify the name and location of the file you re about to display in text mode File name Type or select the filename you want to display The box abowe lists files with the extension you select in the 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 Files of type Select the type of file you want to list Only bin files binary data are available 2014 CH Instruments Inc 3 CH Instruments Model 900D Series 3 7 Convert to Text command This command opens the File Conversion dialog box Use this command to convert one or more binary data files to text the format can be altered with the Text File Format command in the File menu The program displays the File Conversion dialog box so you can select the files you want to convert The resulting text file can be read by other software such as commercial spreadsheet or database handlers The Convert to Text command presents this dialog box Look in amp chi lo e ES Pe IMPO fs MP1 feito Ewe PALsvo ad IMPE2 fd NPVO EJ IMPE3 EJocpTi EJIMPE4 EJ pPsao 2 Filename Files of type Data Files
279. y also need to set the USB serial selection switch inside the instrument see Figure 2 2 above to the appropriate setting For more information please visit lt www chinstruments com downloads shtml gt 2014 CH Instruments Inc Getting Started 25 2 3 Testing The instrument was thorougnly tested by our quality assurance team before it was shipped The bin files included on the software CD are the data actually acquired with the particular instrument you received To test communication between the computer and the instrument start the software and turn the instrument on Use the Hardware Test command under the Setup menu If a Link Failed error appears should check the connection and port settings Use the System command under the program Setup menu to see if the port setting matches the port in use If hardware test results appear on the screen the PC instrument communication is working properly The hardware test results will provide further details regarding the status of your instrument To test hardware performance you can use say 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 to be 0 5 V to 0 5 V using the Parameters command under the Setup menu The sensitivity can be set to 1e 6 A V Run the experiment using the Run command under the Con
280. y moving the cursor to the left or to the right of an element When the mouse cursor is close to the left or right side of an element a black dot will appear Left click and drag the mouse cursor to the left or right of the other element releasing the left mouse button when a black dot appears on beside the other component The two elements will now be connected To remove a circuit element or connection wire left click to select it The color of the element or wire will change to red Click the Cut button on the toolbar to remove the element or wire When an element is deleted all of its connections are deleted with it You can also remove a component by left clicking it and dragging it out of the window To move elements and wires left click and drag releasing the left mouse button at the desired location in the window Alternatively use the Move button on the toolbar to move all components left right up or down To rearrange components and connection wires automatically click the Rearrange button on the toolbar 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 to the two big dots on the left and the right sides of the window If you do not connect these two dots the program will be unable to determine the two terminals of your circuit and to start the simulation Other potentially useful toolbar button
281. y other computers Reference electrode impedance too Check for trapped air bubble at reference high electrode tip use reference electrode with Vycor tip GE Faraday cage see Useful Tips section in Chapter 2 double layer capacitance manually turn on stabilizing capacitor Computer problem Remove network modem cards if present or try other computers ata out of range menu to test hardware during experiment incorrect toggle Y axis title rotation Unreasonable Incompatible configuration cfg or default conditions In file generated automaticall Simulation program lInstrument not found does not run this instrument model 2014 CH Instruments Inc 26 CH Instruments Model 900D Series 12 4 Maintenance and Service The recommended operating temperature is 15 28 C Since the instrument is a sophisticated piece of equipment you should not try to service it yourself If it is not working properly please run the hardware test and contact the factory for service 2014 CH Instruments Inc 12 5 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 shown on the purchase receipt CH Instruments Inc will at its option either repair the defective product without charge for parts and labor or provide a replacement in exchange for the def
282. you to plot data files from multiple directories or drives as well as control the sequence of the data in the plots This command presents the following dialog box Add Data to Parallel Plots gll Look in IO tst sS ri Fe IMP1 ITO scvo cv4 IMPE1 Lsvo SHACVO Dog IMPE2 Sep E3 cv500 2d IMPE3 23 ocPT1 EJ swvo DPVO IMPE4 PSAD TAFEL1 _ 2 File name NPVO BIN IMPO BIN Files of type Data Files bin DI Cancel h 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 while holding the Ctrl key down to select files one at a time Each plot will be automatically scaled to fit its individual data unless the scale is frozen using the Graph Option command In this case all plots will have the same frozen scale The Graph Option Color and Legend and Font commands allow you customize your overlay plot This command is disabled if there is no currently active data or if the current plot is not a parallel plot 2014 CH Instruments Inc 162 CH Instruments Model 900D Series 6 8 Replot Parallel command Use this command to display the most recent Parallel plot This is useful after clicking the Present Data Plot button or when loading plots from file 2014 CH Instruments Inc Graphics Menu e 6 9 Manage Parallel command Use this command to open the Manage Files dialog box This will

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