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Manual 2010 color - Ivium Technologies

1. Digout1 Digout2 Digout3 JR ee Digital input M Digin1 Diging Read ExtACin 10 X Read analog inputs The Direct control sheet e Top panel DC AC normally DC is active and DC signals are measured pressing the AC setting will enable the ac tabsheet below that allows the application of ac signals and AC signals are measured and shown in the measurement panel IRcorr turns on the online IR correction by current feedback The settings are controlled from the IR comp sheet below HiSens turns on the 4 lower current ranges As these rely on the postgain amplifier this option cannot be used simultaneously with IRcorr or in galvanostatic mode Zstat for using the instrument as constant load constant Z This option is not available e Measurement panel displays E and in idle mode or Rs and Cs when impedance measurements are running When no potential current is controlled E and display open cell values within specified accuracy In idle mode when the instrument is connected the actual current and potential are updated regularly once second e Current range radiogroup allows setting of the current range manually Please note that in Galvanostatic mode the current range is selected automatically depending on the applied current 32 Connect group this controls the connections to the electrode internal dummy cells Bipotentiostat and potentiostatic galvanostaticoperation
2. Verify device Manual contrat SN B03117 Powermode usb power Bens Firmware running idle mode Reboot device CompactStat BiStat LinS can Coul HiS ens FRA Check device Synchronize device Verify firmware Upgrade firmware 133 Method 1 Synchronized Method 2 Config upgrade M Set configuratio Code innit Apply Upload file Caibaim Method 1 Calibrate measurement offset Disable idle sampling Calibrate applied offset Calibrate Frequency Response Analyser The right middle panel Upgrade firmware gives access the firmware upgrade functions Press Method 1 Uploading Firmware Press Start to begin Uploading Firmware or Close to Cancel After pressing Start the firmware is transferred to the instrument When no error messages occur press close and in the Device Maintenance panel press Reboot Device top right under Manual control Now close and re start the pc software The new firmware will be activated after re connecting If during this process an error message is shown try to upload again If Method 1 remains ineffective after several attempts try to apply Method 2 Here in the pop up use the right top button indicated with Start If the instrument becomes unresponsive after a failed upgrade see the restore instrument paragraph 91 8 4 Resto
3. Manual peak addition tool Peaks can be added manually by first marking left mouse click the desired locations in the graph and thereafter pressing the Add marked peak button Peaks can be added either from 2 marks or from 3 marks When 3 markers are set these are taken as the beginpoint toppoint and the endpoint of the peak When 2 markers are set these are taken as the beginpoint and the endpoint of the peak while the top is determined automatically When Cyclic Voltammograms are edited the checkbox must be checked before markers on the reverse scan can be set Note that manual addition works independent of the peak search parameters and always whole peaks are added Baseline subtraction Sometimes it is convenient to remove the baseline before the peak analysis is executed To activate the baseline subtraction tool select the Baseline subtract tabsheet 52 Search Peaks Baseline subtract Peak search Rescale Copy araph A Potential Set markers with Left Mouse button and press subtract baseline when ready Baseline type Marked baseline properties order Bi D ws exponential marked 5 g g CY reversescan V automatic calculate subtract baseline C automatic C3 B C 9 clear markers undo subtraction Example of baseline subtraction with a 6th order polynomial polynomial marked 77 The operator should use left mouse clicks to set anchor points markers to which the baseline
4. Note should be taken that the IviumSoft software has many conditions and safeties incorporated When using Labview to control an lvium device the programmer her himself will be responsible for supplying valid input parameters 3 Example Ivium Driver 1 0 As an example how Labview may be used to control an Ivium device a Labview VI is build using Labview 8 2 In this example all functions that can be controlled through Labview are included This example has been set up in such a way that the user interface resembles the user interface of the IviumSoft itis tir iG m Eile Edit View Project Operate Tools Window Help DJA g uj 13pt Application Font x Tar ee Disconnect Connect Read device serial number Device serial number p Direct Control Method control Get device status Device Status indicator c STOP VI C a Current range Configuration pa Set Mux channel off toma Bistat4EL jo Set Filter cell potential Get current 10kHz joo w o Set Stability cell current Get potential Standard 10 000 A SE O 10 000 10 000 AC Extern Bstat reu son Analog output Digital output C Dig out 1 0 00000 LI Dig out 2 C Dig out 3 DODA 0 00000 0 00000 0 00000 Digital input 1 Digini 1 Digin2 0 00000 0 00000 0 00000 Read Read analog inputs Amplitude Start stop writing Y Scale Range Minimum data to spreads
5. Options menu is 0 4sec while this parameter in the EIS method is set to 2sec default when Noise reduction is activated AutoCR Automatic current ranging The instrument will automatically select the appropriate current range Automated current range switching is possible for sampling rates below 100 datapoints second In case the DualCR option is checked for impedance measurements the active current range depends on the applied frequency AutoCR Max range Maximum allowed current range AutoCR Min range Minimum allowed current range DualCR This option may be checked for potentiostatic frequency scans that use automatic current ranging It will override the automatic current range selection and set the current range depending on a user specified frequency e at frequencies gt SwitchFreq the AutoCR Max range is selected e at frequencies lt SwitchFreq the AutoCR Min range is selected Note that this option is only active if the AutoCR option is checked DualCR SwitchFreq Frequency at which current range is switched Potential range Maximum potential range for potentiometric galvanostatic measurements More sensitive ranges give higher accuracy but lower the range of measurable potentials Frequency Frequency of the superimposed sinewave Because of data speed limitations the range is limited to 10Hz to 2 MHz and no oversampling is carried out Amplitude Amplitude 0 05 mV to 1 V Frequencies Number of frequenci
6. Find levels allows operator to identify and analyse levels SolarcellReport will automatically create a solar cell report of the available data in memory Curve fit will allow curve fit analysis Electrolysisreport will automatically create an electrolysis report of the available data in memory 70 7 6 1 Equivalent circuit analysis The equivalent circuit fit module can be started from the Analysis dropdown menu on the Graphic tool Ivium Equivalent Circuit Evaluator File bar After selecting Equivalent circuit the module is opened in a new window Edit Options Pafi R1 r1 1 050E 02 4 05E 02 Ohm r Fit progress Par 2 R2 O Q 996E 02 8 97E 02 Ohm eee iterations 0 Par 3 C1 O 1 007E 06 1 70E 10 WF Graph Data Equivalent circuit fitting E S pnta Mode R1 R2 C1 N 20 coe R R2CU x Apply E o 22 Calc Startvalues chisquare 0 m Fit range start 0 end 10log frequency Hz Accept Cancel e Simulate Execute Stop Rescale 2D 3D Option Data if ELPhi Rs Cs zz v v errors phase degrees On top a menu appears File e Edit e load fitresult loads a previously saved model including the parameter values save fitresult saves current model including the fitted parametervalues if available load Zplot data imports a datafile produced with the Zplot pro
7. Measurement bar indicates the actual current range and overload status EovI will turn red if the voltage compliance limit is exceeded on CE If this occurs the data obtained will not be reliable Usually it is caused by a bad connection to RE lovi will turn red if the WE current exceed 3 X the current range In some cases data could still be reliable but it is recommended to select a larger current range Ext will turn red if the voltage on the analog input channel 1 exceeds the defined value The operator may set this value Current range will show the actual current range If automatic current ranging is activated this value will be updated during the scan Operational mode Basic Advanced sets the access level for the operator In Basic mode only the essential method parameters are shown In Advanced mode more specialized parameters are accessible Also in Advanced mode the automatic selection of filters and stability settings can be overridden etc Sigview opens a window that shows voltage and current signal trace during a measurement Can be used to verify the quality of the signal and to check for i e overload oscillation situations BatchMode opens the batch programming window This can be used for automating measurements 4 Measurement results When a measurement is started the data are shown real time in the result graph A right mouse click on the graph will give the user a number of options including chang
8. e Copy copies plot into clipboard WMF format Olay panel overlays data from previous measurements e Overlay list overlays can be made in visible by un checking the corresponding box e Load loads a datafile idf that will be overlaid Multiple files can be overlayed at the same same by keeping the CTLR or Shift buttons pressed while selecting the files Overlay Dataset loads a complete Dataset file ids as overlay Delete deletes the selected overlay data Delete all deletes all listed overlays clears the list Data appearance manipulate data appearance of the overlay data lines symbols colors styles etc NB in all 3 panels all in visible checkboxes can be checked at once by pressing show all and unchecked by pressing hide all 4 8 Data appearance A right mouse click on the graph or a click on the button at the bottom of the legend panel will make the data appearance available This will allow the user to choose the colors for the lines and the colors size appearance of symbols in the graph lines symbols size mm gt E v indexed colors style 7 none C filled circle C circle C filled square C square C filled triangle C triangle C filled diamond diamond C indexed C cross 42 4 9 Graphic toolbars Above and to the left of the Result graph two graphic toolbars are shown These contains a number of tool buttons that are visible depending on th
9. Data reduction min I delta Adaptive sampling only values differing more than this value from the previously stored data point will be stored Automatic save When activated that data will be saved automatically Automatic save filename Filename at which the automatic backup wil be saved If a file with this name already exists an index number will be added to the filename Automatic save save every Every x seconds the data will be saved to disk This is intended for measurements that take a long time to complete Note that when short periods of time x for saving are chosen during long term experiments the data saving action may take longer than the chosen period and there will be a conflict which may result in non responsive PC software Automatic save on completion When checked the data will be saved automatically at the end of the measurement 131 AUX The IviumStat CompactStat has been prepared for controlling external equipment via the peripheral port external trigger that signal begin amp start of a measurement purge control stirrer control RDE control new drop control DME SMDE etc will execute a selectable number of knock dispense cycles at the start of the measurement The trigger stirrer and purging is controlled via digital outputs TTL compatible active low The rotation speed of the RDE is controlled from an analog output with 16 bits resolution The new drops are controlled via the Analog
10. Disconnect Connect Read device serial number Device serial number gt von 3 iad STOP VI Read method Start method gt Parameter name ii Set method parameter New value C Plot 0 File path method files Method name Save method XY Graph n Read available datapoints Available datapoints C jo o e 2 2 E E Save data to File path data files File name Ivium data file _ 0 Furthermore separate parameters of method can be changed D and this new method can be saved E Care should be taken that the entered method parameters to be changed are spelled exactly as in the IviumSoft otherwise it will not register During running of a method the number of available data points can be requested F In Labview there is no possibility to abort a method once started Finally upon completion of executing a method the then in the IviumSoft available data can be stored as a lvium data file idf G 143
11. For connections to external cells also the checkbox must be enabled Available configurations Off default cell is switch off and instrument is placed in idle configuration open cell Cell Estat4 potentiostatic operation with 4 electrodes Cell Estat2 potentiostatic operation with 2 electrodes WE and CE 1 kOhm Estat potentiostatic operation with internal 1 kOhm resistor 100 kOhm Estat potentiostatic operation with internal 100 kOhm resistor 10 MOhm Estat potentiostatic operation with internal 10 MOhm resistor R RC Estat potentiostatic operation with internal 250 ohm resistor IviumStat or 100 ohm resistor CompactStat in series with a 1kohm resistor placed in parallel with a 1 uF capacitor Cell Istat4 galvanostatic operation with 4 electrodes Cell Istat2 galvanostatic operation with 2 electrodes WE and CE Dummy Istat galvanostatic operation with internal dummy cell Cell Bistat4 potentiostatic operation with 4 primary electrodes and the bipotentiostat WE2 Cell Bistat2 potentiostatic operation with primary electrodes WE and CE and the bipotentiostat WE2 Stability set bandwidth of the applied signal hispeed standard high stability Filter set filter of measured signals 1MHz 100kHz 10kHz 1kHz 10Hz These filters are applied to all measured signals current potential and bipotentiostat current Apply set the potential in potentiostatic mode or current in galvanostatic mode enter
12. Phi Z model will display the modelled numerical phase impedance data Z Z model will display the modelled numerical complex impedance data Copy data will copy the currently displayed data into the clipboard 7 6 2 Corrosion analysis The corrosion rate analysis can be applied on data from a Linear Sweep experiment The analysis can be started from the Analysis dropdown menu on the Graphic toolbar Corrosion anatysis anix Defined constants meo Linear j Log ivsE E vsi Copy plot Rescale ES Sem Surface area Equivalent weight 18 ot Corrosion rate analysis Density 1 0 gav cm 3 ic ery 0 007 0 1843 i cor 6 125E 6 8 545E 6 8 167E 8 1139E7 ep Rp Ohm 6052 7882 6039 0 171 0 385 z 0 317 0 378 O 00002672 0 0003728 Ei v Automatic analysis Slope Analysis Tafel Analysis Model Analysis minimize logarithmic errors Clear results Copy results Exit Tafel Analysis Potential V Potential range markers Eat Ea2 Ecl Ec2 0 358 V 026801 V 0127 V foo V Clear The corrosion analysis window contains a data panel on the left where input data is supplied and analysis results are shown 3 types of analysis are available e Slope analysis the corrosion potential and Rp are calculated at the zero current intersection point e Tafel analysis the corrosion parameters are calculated from the 2
13. The Edoubler requires an external 5 Volt powersupply included in shipment that must be connected When the Edoubler module is connected the configuration in the software should be updated In the Options menu the Edoubler checkbox should be checked Note that when Edoubler is connected the internal dummy cells the 2 Electrode mode and the BiStat module should not be used 1 7 Install HiMux The HiMUX XR multiplexer is connected to the IlviumStat CompactStat via de 15 pins cell cable connector Each multiplexer comes with 8 standard cell cables 1 for each of its 8 channels Each 12 channel cell cable can then be connected to an electrochemical cell in the same way that the IviumStat CompactStat would be connected directly The HiMux requires an external 5 VDC powersupply included in shipment that must be connected before operation In case multiple HiMux modules are used a cell cable connection assembly should be used This consists of a flexible cell cable extender and a connection box This box has 1 input F and 3 outputs M and can connect to 3 HiMux modules Assemblies may be cascaded to connect more units HiMux clamp kit The HiMux clamp kit is intended to enable easy mounting of the 8 channel HiMux into a 19 inch rack The HiMUX Clamp Kit consists of an aluminium front with 2 brackets on the rear side for clamping the multiplexer unit in place When mounted on the front side all 8 channels are available
14. and the measurement has been terminated When a new measurement starts the IviumBoost is automatically reset and the indicator will switch off When a unforeseen situation occurs where it is desired to protect the test subject substrate from the reigning electrical conditions an emergency manual override is possible The cell WE CE will be instantly isolated from the lviumBoost by pressing the red Disconnect switch located at the bottom right on the front of the IviumBoost A representation for the same indicators that are on the front of the IviumBoost can be found in the IviumSoft window under and to the right of the menu bar These will change color in the same manner when an overload is detected When after a method these indicators are still lit to indicate the latest condition they can be reset manually before the next measurement by clicking on the Reset button to the right Alternatively they will be reset when the next method measurement is started Connecting the IviumBoost to the IviumStat To connect the IviumBoost to the IlviumStat 1 Take the 40 cm M F HD15 cable Insert the M side into the Cell connector of the IviumStat Insert the F side into the IviumStat connector 2 Connect the RE S cable to the RE S connector 3 Connect the heavy WE CE cable by inserting the plug so that the notch and the slid line up Then turn the plug clockwise until it clicks in place To unfasten pull the silver button and turn the pl
15. tabsheet is added that will list important measurement and instrument data 135 z Scan Report 2 0 x Remarks Process report This scan was performed by Jan Janssen 3 electrode cell was used with AgCl ref electrode and PT CE WE was 0 023 cm2 glassy carbon Conditions during the scan gas bubbles evolced at WE etc z Scan Report PRISES Remarks Process report instrument B03117 Ichannel software vs 1803 lfirmware vs 193 Ihw config CompactStat BiStat LinScan Coul HiS ens FRA start time 26 02 2010 17 16 22 lend time 26 02 2010 17 16 31 lendcondition normal The process report is added automatically after measurement completion It is not editable by user 136 Appendix 1 Labview Interfacing Product note for lvium Labview Driver 1 0 1 Order of communication hierarchy For optimum results when using Labview to control an Ivium device it is very important to realise the order of hierarchy for communication between the various software and hardware In this case Labview the VI communicates with the lvium remdriver which in turn communicates with the IviumSoft software Only the lviumSoft communicates directly with the lvium device IviumStat CompactStat This implicates that the IviumSoft software should always be running in the background when using a Labview VI to operate the device The lviumSoft can be minimised when operating Labview 2 Dire
16. 04ms 120 If the Alpha parameter remains unchecked the value reverts to 1 default Alpha Value Fraction of the step at which sampling occurs Values of 0 125 to 0 625 can be entered Interval time Time between 2 consecutive samples The sample rate equals 1 interval time or scanrate E_step Max 60s Run time For the transient technique Electrochemical Noise and for the electroanalysis method AC detection duration of the experiment Levels Number of potential or current levels to be applied 0 to 255 A pop up window allows each level to be specified individually In the pop up window the interval time is only shown it can be changed in the method parameters the time base can be adjusted The number of levels can be changed by pressing the up down arrows In each level the potential current and time duration of that level can be changed by entering the desired value in the appropriate cell In ChronoPotentiometry also the current range can be selected from the drop down menu Levels index time Time duration of level index from 1 to 4E9 times the interval time in Standard mode In HiSpeed mode the total number of datapoints must be lower than 8192 Levels separate When applying the Transient methods ChronoAmperometry Chronopotentiometry or Mixed Mode each level can be viewed and stored separately Each level is plotted as an independent scan i e the time coordinate starts at 0 sec at the start of eac
17. 119 119 119 119 120 120 120 120 120 120 120 120 120 120 Alpha Value Interval time Run time Levels Levels index time Levels separate Stages Cycles Cycles separate N samples Thresholds Thresholds E max Thresholds E min Pulse time Pulse amplitude SQRWV frequency Phase sensitive Phase sensitive phase 2nd Harmonic Deposition time Current stripping Current Stripping Stripping current Equilibration time Current range Noise reduction Noise reduction Acquisition period AutoCR AutoCR Max range AutoCR Min range DualCR DualCR SwitchFreq Potential range Frequency Amplitude Frequencies Frequencies Single sine Frequencies Multi sine Frequencies Start Frequencies End Frequencies Frequencies each decade Frequencies Amplitude Frequencies manual override Filter Stability Connect to Analog inputs Anout2 Anout2 Level Anout2 Pulse period Apply wrt OCP Apply wrt OCP monitor time Apply wrt OCP monitor interval Apply wrt OCP Estart wrt OCP Apply wrt OCP Vtx End wrt OCP Apply wrt OCP Estandby wrt OCP Apply wrt OCP Record real E Remove DC initial IR feedback IR feedback Compensation BiStat BiStat E offset 128 BiStat Current range 128 BiStat CR min 128 BiStat CR max 128 BiStat mode 128 Cell after measurement 129 Cell after measurement E standby 129 Pretreatment 129 Data Options 129 Data reduction 130 Data reduction average every 131 Data reduction no averaging 131 Data reductio
18. 2 points on either side to decide whether a datapoint is a spike FFTsmooth On the FFTsmooth tab sheet smoothing based on Fourier frequency analysis is executed When this sheet is activated 2 graphs appear the original data and the Fourier transform The original data is recalculated to the corresponding time transient to calculate the proper frequencies For example Linear PotentialSweep data is recalculated to current vs time from current vs E In the frequency plot the most abundant frequencies are visible Usuallly a peak is visible at the 50 60 Hz line frequency and possibly its multiples This can be removed by either using the Low pass filter or the Band reject filter For the Low pass set the cutoff frequency and press apply Set the cutoff frequency low enough to remove the noise but not too low that data is deformed For the Bandreject set the cutoff frequency the Bandwidth and press apply It is also possible to remove the higher harmonics by checking that option this will repeat the bandfilter at all multiples of the cutoff frequency Change point In the Change point tab sheet it is possible to change individual data points Activate the mouse editor left click on the data point to be changed and drag it to its desired vertical position 7 5 2 Smooth all data From the Edit menu select Smooth all and all presently loaded scans will automatically be smoothed and spikes are removed This is done by Savitzky
19. 20mV 1mV 10mV 200mV 100mV pe OV VOY a 2 Envronmnt NEHMEN RN Specifications subject to change Ivium Technologies 2010 9 3 Ivium n Stat Specifications Ivium n Stat main frame 5 11Bkg with8 modules s Module System Performance J a as Measured current resolution Doo ee Potentiostat 103 Galvanostat 0 033 of applied current range 0 2 10mV 100mV 1V 10V 0 038 of potential range minimum uV Po Impedance Analyser fF 0 03 to 100 of currentrange oe n o pT Electrometer o ee E Peripheral connections O o ci x RR NN Environment 1 Specifications subject to change lvium Technologies 2010 9 4 IviumStat System Performance Current compliance Maximum output Voltage 10V below 1A and 8V up to 5A signals Potentiostat Galvanostat ee Oa Potentiostat PT 1pA 10pA 100pA 1nA Current feedback ohmic drop n ohm current range 65 536 with n 0 to compensation 65 535 OOo O Galvanostat pT 104 Applied current accuracy 0 2 Potential ranges timV 10mV 100mV 1V 10V Applied current resolution 0 033 of applied current range 02 o Measured potential resolution 0 003 of potential range minimum 40nV a MONEMUS Impedance Analyser a Frequency range Amplitude po 0 0 03 to 100 OF currentrange DC offset 16 bit dc offset subt
20. 5 channel 6 E Id 7 channel 7 C ld 8 channel 8 Set default Apply to selected data Apply to all data In the Ecorrections tab an offset potential may be entered and or reference electrode potentials may be converted see graphic toolbar 129 3 Data ptionForm E nl x Analoginputs Ecorrections Electrode Offset potential 0 000 V Convert Reference Electrode potentials actual RE base RE Calculate Set default Apply to selected data Apply to all data In the Electrode tab the electrode surface area and reference capacity may be entered in order to be able to plot current density see graphic toolbar Data reduction When data is captured over extended periods and or at high sample rates the large data files produced can become slow and cumbersome to manage For ChronoAmperometry and ChronoPotentiometry in standard mode and in MixedMode the data can be reduced in real time Skipping or Averaging datapoints Reduce the number of datapoints by entering a number of points to use in computing an average This is stored as a single value By ticking the box No Averaging every n th value is stored without averaging the intermediate values The averaging is done inside the instrument and only the average values are sent to the pc Thus less points are transferred and stored For example at an interval time of 0 002 sec and an average count of 50
21. 7 Frequency sca i Manual override Start 10000 Hz End 1000 Hz Ampiitudel O01 y Close em e freq 10000 10 00 It is recommended to always start with the highest frequency because real systems have usually lower impedance at higher frequencies Starting at the lowest impedance is favorable because the probability for overloads is less and the system will find the optimal set of internal gains more quickly MultiSine For EIS measurements MultiSine applies multiple sine wave frequencies simultaneously and the corresponding impedances are collected in a single measurement For measurements at lower frequencies this can decrease measurement time considerably and minimize artefacts caused by to time variable impedances In Multi sine mode 5 frequencies within a single decade are combined By using the odd harmonics 1 3 5 7 9 Hz etc and carefully controlling the relative phase of these frequencies it is possible to minimise the total combined amplitude for a given effect Thus the maximum amplitude from the combination of 5 frequencies is less than 2 5 times the individual amplitudes This minimises the signal degradation which is traditionally inherent in the multi sine technique whilst still producing fast results Compared to SingleSine there are some constraints e Start and End frequency must be at decade boundaries e Manual override of individual frequencies amplitudes is no
22. Abort Cycles separate For multi cycle experiments each cycle will appear as a separate scan as is done in cyclic voltammetry Turning on this option will keep subsequent scans separated and will appear as different scans on top of each other Thus the first level wil always start with time 0 seconds Turning off this option will combine all cycles in a single scan Subsequent scans are appended to the datafile and the time will appear continuous See both examples for ChronoPotentiometry for a comparison N samples Number of samples to be acquired Thresholds Activate dynamic level switching in ChronoPotentiometry Standard mode If during a level with a positive current charge cycle the potential exceeds E max this level is ended and the next level is applied If during a level with a negative current discharge cycle the potential falls below E min this level is ended and the next level is applied If the interupted level was the last level the scan is ended or proceeds to level 1 for multi cycle experiments Please note that the potential is sampled each interval time In this case the interval time coincides with the reaction time Thresholds E max Set maximum potential threshold for dynamic levelswitching Thresholds E min Set minimum potential threshold for dynamic levelswitching Pulse time Time DPV Technique that pulse is applied 0 1 ms to 400 ms must be less than half of the interval ti
23. Advanced mode the methodparameter Anout2 can optionally be selected When checked 2 parameters appear e Level the voltage to be applied to Analog output 2 e Pulse period the duration of the pulse 0 05 to 500 ms or 0 If a Pulse period of 0 ms is set the level will be applied continuous The value will be applied during the whole measurement and thereafter In such case the analog output retains its setting and must be reset in manual control or by the next executed scan Anout2 Level Potential level of the pulse The pulse level can be defined at 16bits resolution Anout2 Pulse period Period of the pulse The pulse duration can be programmed from 0 05ms to 500 ms at 10us resolution The pulse is applied just before measurement sampling starts In the HiSpeed techniques the first recorded measurement sample follows within 0 05ms after the pulse level change If a Pulse period of 0 ms is set the level will be applied continuous The value will be applied during the whole measurement and thereafter In such case the analog output remains its setting and must be reset in manual control or by the next executed scan Apply wrt OCP Potentials are referred to the Open Cell Potential Before the measurement starts the instrument determines the OCP by monitoring the potential with CE disconnected no current passes The determined OCP is added to E start and the other scan potentials before the measurement starts Results are v
24. Golay smoothing using a sliding polynomial of default 11 points This number may be modified in the Edit data screen Every time the Smooth all function is activated the data will be smoothed again this can be applied repeatedly 7 5 3 Subtract ohmic drop The potential loss due to the effects of ohmic resistance on Linear scans and Cyclic Voltammograms can be corrected by calculation If the resistance is known the ohmic drop can be calculated from the product with measured current The real applied potential can thus be calculated First select the scan to be processed and from the Edit menu select Subtract ohmic drop A window will popup at which the resistance should be entered Pressing Apply will process the selected scan 7 5 4 Average scans The operator can average scans In the graphic toolbar select the Edit menu Average scans Clicking this option will automatically average all scans in Scan panel 69 7 5 5 Subtract overlay With this function the operator can subtract the scan in the Overlay panel from the scans in the Scan panel Note that this function can be applied repeatedly each time it is activated the overlay will be subtracted from the scans The scan to be subtracted should be saved as a normal datafile idf and loaded as the first overlay After recording the new scan you can select Subtract Overlay 1 from the Edit menu The overlay will be subtracted from all scans However it only works for datafil
25. Note AC voltammetry is similar to the impedance potentialscan technique but with a few differences Only 1 frequency is used and the results are obtained as currents instead of impedances Because AC voltammetry must obey the time constraints of the potentialscan no re measurements are done and automatic gaining is not used Therefore the dynamic range for accurate measurement is less and on occasion flyers might be observed during automatic current range selection 57 5 18 ElectroAnalysis Potentiometric Stripping A potentiometric stripping experiment contains 2 stages first a product will be deposited on the electrode at potentiostatic conditions during a longer period thereafter the product will be stripped in a relatively short time while recording the potential under galvanostatic conditions For the second stage 2 variants are possible e chemical stripping occurs spontaneous at Open Cell Potential no external current is applied Current stripping option Off e electrochemical stripping the galvanostat applies a constant current that removes the reactant electrochemically Current stripping option On According to convention the recorded potentials are transformed to the inverse differential w r t time dt dE This will yield a pattern of peaks that can be used to determine concentrations 5 19 ElectroAnalysis AC detection The technique AC Detection can be used to record the ac impedance with time at a fixed frequen
26. Tafel lines e Model analysis the corrosion parameters are calculated with a numerical analysis of the available data 73 Manual and automatic analysis can be used For manual the operator has to set the potential markers by mouse click while in automatic mode the software will set the markers The 3 analysis types can be run by pressing the corresponding buttons the results are shown in the grid above Because the result fields are independent the various results can be compared Note that the Tafel analysis is based on simplifications that do not always apply For instance one must have data over a very wide potential range on either side of the corrosion potential which is often not available The Model analysis usually gives the most reliable result 7 6 3 Peakfinding and baseline correction The lviumSoft program contains an integrated peak finding tool It is accessible from the Analysis menu via the options Peakfind automatic and Peakfind advanced The automatic option will execute the peak search automatically with a single click The advanced option will allow the operator to manipulate the automatic peak search parameters or manually add remove peaks subtract baselines and process the results The advanced tool also contains a baseline corection option as wel as the option to manually add remove peaks 7 6 4 Peakfind automatic This will automatically find and draw the peaks Note that the peakfind parameters can be mo
27. as well as two connectors for connecting the multiplexer to the Ivium potentiostat and for connecting an optional next multiplexer unit for additional channels For detailed instructions on how to assemble the HiMux and clamp kit refer to the Installation notes for HiMux clamp kit There two models of the HiMux available Both models are connected and controlled in the same way e The older models of the HiMux have a blue and white plastic housing and the 8 channels have 4 BNC connectors each for WE CE RE S The compliance of this model is 10V 5A e The later model HiMUX has a blue and grey metal housing and the 8 channels have the lvium standard 15 pins HD cell connector for WE CE RE S WE2 GND The compliance of this model is 20V 5A Operation After the HiMux has been installed the sequential use of all channels is available either by choosing the channel in the Direct mode and then executing the desired technique 1 or automated via the Batchmode 2 1 In the Direct control tab sheet select the channel number next to the Set MUX channel button by entering the channel number manually or using the up down arrows Then mouse click on the Set MUX channel button to activate this channel The red LED of the chosen channel on the HiMUX XR will now light up 2 In the Batch mode use the Direct Command to set a channel number directly SetMuxChannel or use the Loop command to set the channel number to the loop index Set
28. cable to the CompactStat device and a free USB socket of the pc e Startthe lviumSoft program From the top left corner of the screen in the drop down menu select the serial number of the CompactStat that you will be using This can be verified with the serial number written on the underside of the CompactStat e Wait 10 seconds and press the connect button at the left top corner The IviumSoft program will turn on the CompactStat and the green LED at the front of the CompactStat should now be lit 2 2 Starting the lviumStat IviumStat e Attach the powercord to the instrument and mains and press the power button e Connect the USB cable to the IviumStat device and a free USB socket of the pc e Startthe IviumSoft program From the top left corner of the screen in the drop down menu select the serial number of the IviumStat that you will be using This can be verified with the serial number written at the rear of the instrument e Wait 10 seconds and press the connect button at the left top corner The IviumSoft program will activate the IviumStat and the instrument should indicate the connection e Before starting measurements be sure that the red disconnect button is depressed and is un lit 2 3 Starting the lvium n Stat Ivium n Stat e Connect the USB cable to the IviumStat device and a free USB socket of the pc e Attach the powercord to the instrument and mains and press the power button e Start the IviumSoft program e Execute
29. currents for all 32 working electrodes are recorded Each scan will therefore produce 32 curves Individual curves can be stored with save data while all 32 scans can be stored in a single file with save dataset 16 1 10 Install Plus module The Plus module as a separate unit is available in 2 models maximum 250mA and 20V maximum 800mA and 10V The Plus module is to be connected to the CompactStat via de 15 pins cell cable connector The original cell cable is connected to the output cell connector of the Plus module The Plus requires an external 12 Volt powersupply included in shipment that must be connected When the Plus module is connected the configuration in the software should be updated In the Options menu the relevant Plus checkbox should be checked 1 only CompactStatPlus for the 250mA and 20V model both CompactStatPlus and type II for the 800mA and 10V model 2 When the relevant box is checked close the Options window and in the software Disconnect the instrument and Connect again to switch on the Plus module Note that when Plus is connected and activated the internal dummy cells the 2 Electrode mode and the BiStat module can not be used 17 2 Getting started 2 1 Starting the CompactStat CompactStat e f operating on adapter power first connect the acdc adapter to a mains socket and to the round dc plug at the rear of the instrument e Connect the USB
30. desired component on the element toolbar and drop it on the desired location in the grid Components can be removed with the del element Vertical conductors are placed automatically between upper and lower neighbors Where this is not wanted maintain an empty row between elements Horizontal conductors are placed after selecting the element When editing is finished press Accept and the components are named and the CDC expression is evaluated When Apply is pressed the model will be implemented in the fitting engine the fit able parameters are shown in the parameter grid below Instead of entering the circuit manually predefined circuits might be loaded load fitresult or be selected from the dropdownlist in the CDC field In the parametergrid e Par name of the parameter the symbol R C etc en the sequence number corresponding to the componenigrid and the CDC expression e Fixed when checked this parameter will not be changed by the fitting engine not fitted e Value start value at which the fitting starts will be updated during fitting and contains end value after fitting is complete a start fixed value may be entered manually by selecting the field and entering the desired value e Error calculates the error of the fitted parameter is only calculated after fitting is completed e Unit unit in which the parameter is listed Ohm F etc Calc Startvalues It is important to supply start values that are close to the actual va
31. duration e Setdefault will reset all FRA setting to default values 2 10 Tools menu Device maintenance the device maintenance window will allow the user to diagnose the instrument calibrate and upgrade instrument firmware Also in this window the idle sampling of the instrument may be disabled Restore device this option is only available when the instrument is not connected in the software When not connected this option may be used to return the instrument to factory settings factory firmware or previous firmware Performance test opens a window to run a performance test of the instrument Pulse generator opens a window that allows operation of the pulse generator CurrentInterrupt opens the window to operate the CIM Current Interrupt Module Define channels to define sModules as channel only available with an Ivium n Stat 2 11 Help menu Contents lists the topics on which help is available Topic search search for help on specific topics Help on help how to use the online help tool 27 2 12 About This opens a window that shows the release version of the IviumSoft that is running 2 13 Internal dummy cells The instrument has 4 internal testcells dummy 1 1 kOhm resistor dummy 2 100 kOhm resistor dummy 3 10 MOhm resistor dummy 4 250 ohm resistor IviumStat or 100 ohm resistor CompactStat in series with 1 kOhm resistor parallel over 1 uF capacitor An internal dummy cell can be selected in Direct as w
32. during a previous driver installation the re installation may not start automatically when the USB cable is plugged in again The process can be started from the Windows device manager 1 Go to Start gt Control panel select System properties gt Hardware mouse click on device manager 2 Expand Universal Serial Bus controllers and right click Ivium Device 3 Select update driver and follow instructions as stated above under Driver installation Hardware Installation Depending on your location and environment as well as whether you have additional Ivium modules or instruments connected the Ivium instrument hardware configuration may need to be correctly set in the Options menu 1 After installation of the IviumSoft software and lvium driver start the IviumSoft 2 Inthe left top of the IviumSoft window mouse click on the Connect button 3 In the menu go to Options Options 4 Under Environment check the relevant boxes 5 Close the window The new settings are now implemented in the Ivium instrument To make sure these new settings are activated in the left top of the IviumSoft click the Connect button once to disconnect the device and again to reconnect the device The instrument is now ready for use 1 6 Install Edoubler The Edoubler module is to be connected to the IviumStat20V via de 15 pins cell cable connector The original cell cable is connected to the output cell connector of the Edoubler module
33. end of each interval unless the Alpha parameter is activated Standard mode allows for interval times down to 0 002 s for shorter intervals use HiSpeed mode 5 5 Cyclic voltammetry Generic features of all cyclic voltammetry techniques are 1 When a CV scan is running standard speed the datapoints appear real time on the screen It is possible for a user to react directly on the result and change a vertex by mouse click During a CV scan the operator can reverse the scan direction immediately by pressing the ReverseScan button at the bottom of the Result graph sheet Clicking the button is only effective when the scan is moving away from E start thus the scan range can be constricted but not extended The new vertex is applied to the ongoing cycle only Also an ongoing scan can be paused with the Pause button during a pause the applied potential current will be kept constant and the instrument will suspend measurements A paused scan can be continued by pressing the Resume button 2 Cyclic Voltammograms are usually displayed as Current vs Potential but also the Current vs time and Potential vs time plots can be shown Note that the interval time between 2 consecutive datapoints equals Estep Scanrate To show the CV time plots move the mouse on the resultplot right click and select CV plots 3 For plots with Cyclic Voltammograms the scan direction can immediately be recognized the scan in positive direction is plotted
34. expands the peak Smoothing Apply smoothing on the data from which the peaks are to be determined Use higher levels more points on noisy data Note that the underlying data will not be changed Search Peaks Baseline subtract Peak search ReScale Copy graph Copy peaks amp ece Search parameters automatic peakfind pA Fe in KNO3 Construct from front flank Find method 2nd derivative Height mode proportional Minimum height 0 025 Width mode absolute Minimum width 0 025 Sensitivity Smoothing 5 points Manual peak addition Add marked peak mark CV reverse scan 1 Eft 0 0 0 2 Clear markers Pote ntial Peak results 44081077E 05 0 220 3 2464822E 08 1 8492964E 06 3 4642724E 06 0 134 7 4435075E 10 1 4887015E 08 Clear all peaks Remove peak 1 a Done Automatic peakfind example with front flank and 2nd derivative selected 76 Peaksearch parameters are stored When peak search parameters are changed by the operator these become the default values which are applied to all subsequent peak finding actions When a datafile that contains peakresults is stored also the used peak search parameters are included in that datafile When such a datafile is loaded at a later time it may thus contain peak search parameters that could be different from the active default values However if all peaks are cleared in this dataset the default search parameters will be applied on subsequent search actions
35. for each WE all techniques e WE32 allchannels whether to record all channels simultaneously only available for LSV Standard CV Standard and CA Standard Of course the MultiWE32 is also integrated in the Batch mode The MultiWE32 can be operated in 2 modes 1 Sequential mode All available potentiostatic methods can be run in this mode Before a method is started the user can select the channel number on the Direct Control tabsheet The MultiWE32 operation is similar to the HiMUX multiplexer select the channel number next to the Set WE32 channel button by entering the channel number manually or using the up down arrows Then mouse click on the Set WE32 channel button to activate this channel The red LED of the chosen channel on the front of the MultiW E32 will now light up The selected channel will be measured however note that the potential is applied to all channels simultaneously Channel selection can be automated in the Batchmode similar to the HiMUX The Loop command has a property SetW E32TolIndex that will set the channel number to the loop counter Alternatively the channel number can be set directly with the DirectCommand property SetW E32channel 2 Simultaneous mode To acquire measurement from all 32 channels simultaneously It is available for the following techniques LSV standard CV standard and CA standard This is activated with the WE32 allchannels method property in Advanced mode When checked the
36. from the graphic toolbar The selected data to be manipulated will be shown in a different smoothing dialog window After smoothing is completed and accepted by the operator the original data is replaced Edit data Smooth FFTsmooth Change point Low pass filler Cut off 50 Hz Fourier spectrum 7 Apply c o 8 Band reject filter 31 v D Cut off 50 Hz 9 9 Bandwidth 0 56 He remove harmonics Apply Log treq Hz ij Cancel and close 68 On the left of the smoothing dialog window 3 tabsheets are shown from which the data editing process is controlled Smooth FFTsmooth Change point Generally with smoothing data if the noise is non frequency specific the general smoothing gives better results However when noise is concentrated in specific fequency bands such as 50 60Hz the Fourier variant works better Smooth The Smooth tab sheet gives access to Savitzky Golay smoothing and spike rejection Savitzky Golay smoothing will process the data by using a moving window that interpolates each point using the position of neighboring datapoints The algorithm calculates a quadratic fit and shifts the center point to the modeled position The smoothing effect is stronger when more points are used 5 11 25 Spike rejection uses an algorithm that detects spikes and when detected interpolates these The algorithm uses
37. in standby mode green LED is off In standby mode the instrument will lower power consumption to about 50 mA Note 1 In the serial number read out window the lower case b before the serial number indicates that this CompactStat is using usb power while a capital B indicates mains adapter power This can be verified in Device maintenance under Tools by selecting Check device Note 2 No features are disabled in USB powered mode The operator should be aware that formal USB limits may be exceeded if he she applies the features listed above Note 3 Some USB hubs are not compliant to 500 mA and cannot be used to power the CompactStat In this case connect the CompactStat directly to the USB port of the pc or use the external power adapter 1 4 Ivium n Stat instrument Rearpanel e Power connector fits the standard power cable which should be connected to the main power e Fuseholder contains 2 fuses Replacement should be done by a qualified person e USB connector fits to the supplied USB A B cable which should be connected between instrument and PC e EMO connector Red 4mm socket banana e GND connector Green 4mm socket banana Frontpanel e On Off button when pressed the instrument powers up and the button lights up blue when ready Please allow several seconds for the startup sequence to be completed sModule channel e Peripheral port 15p subD connector that provides access to a range of analog dig
38. in 2 different plots by ticking the relevant box when ticked the corresponding channel will be displayed in plot 2 Each of the 3 plots can have its own transformation 4 When the rest of the method is defined as desired click Start to start the measurement 5 Click Ain in the graphic toolbar to the left of the graph window to make the extra graph visible containing the signals of the analog inputs When any of the signals is plotted in plot 2 there will be 2 plot windows Plot 1 and Plot 2 otherwise only one extra plot will be visible 99 Result graph Result data Scale v areas v Edt Ecor idend Nes Peripheral Port E 3 Peripheral Port Scan Chan Olay 3D enone SPRL o P EEL EC US Ru Der LEME LTO LO Hide all Di 0 03 eee T 8J Show all p E E vi i 4 channel 2 zm 0 02 v channel 3 Cor 4 M channel 4 Michannel 5 oo M channel 6 e o 2 M channel 7 Ain 2 2 al channel 8 124 000 g jp EN To 02 04 B 08 0n 02 04 6 08 b Potential v s Potential v Rs Cs pA Fe in KNO3 800 600 400 E o 200 o 0 Option 0 0 0 2 0 4 0 6 0 8 n Data appear Potential M Cony 6 Inthe legend panel to the right of the graph click on the Chan tab to select individual traces to be plotted display 7 All analog signal data are stored in the same data fil
39. in a thicker line that the negative direction 49 5 6 CyclicVoltammetry Standard HA 2 Fe in KNO3 20 10 t o 5 10 O 20 0 6 0 4 0 2 0 0 0 2 Potential v Each scan consists of 3 linear segments E begin to Vertex 1 Vertext 1 to Vertex2 and Vertext 2 back to E begin The segments are created by increasing the potential with E step at each interval so that a staircase scan is applied to the cell with a defined scanrate The interval is defined by E step scanrate The recorded currents are measured at the end of each interval unless the Alpha parameter is activated Standard mode allows for interval times down to 0 002 s for shorter intervals use HiSpeed mode In standard mode the number of datapoints is unlimited in HiSpeed mode a maximum of 32 000 datapoints applies 5 7 CyclicVoltammetry CurrentAveraging Linear potentialsweeps are applied identical to the standard variant However instead of recording the current at the end of each interval the current is integrated during the whole interval and divided by the interval time This results in the average current over each potentialstep In some situations this technique yields the same results as when using a True Linear Scan technique This particular technique can be used when the standard staircase method does not give the desired results such as experiments involving time dependent phenomena such as film formation or electrochemical nu
40. individual scans Note that the scan that is highlighted blue is the scan in active memory This is the one that is evaluated in Analysis or has the numerical data shown in Result data etc Clicking on a different scan will select that one highlight it making it available for analysis saving etc Save data will save data only of the selected scan as data file idf Save dataset will save all scans as data set ids Delete will delete the selected scan Delete all will delete all scans Data appear will allow user to change the appearance of the data lines colours symbols 2 Olay will allow the user to load data from file to overlay it so that it can be compared to the scan data that was just recorded Several scans can be loaded at the same time All the same options apply as in the scan tab 3 The Chan tab shows when analog inputs are sampled advanced method parameter it allows the user to show hide analog channels in the second graph 6 Status bar Start Abort ReverseScan Pause E 400 00 mV I 3 665 u 40 pnts cycle 2 scantime 18 95 Measurement in progress At the bottom of the user interface the Status bar is located Depending on the status of the instrument idle running a method kind of method etc a series of parameters is shown In the case of a CV scan see figure above it shows actual E actual number of acquired data points so far cycle number runtime of th
41. is fitted The software will recalculate the baseline automatically after the addition of each anchor point unless this is disabled with the indicated checkbox There is no limit to the number of anchor points When the projected baseline is satisfactory press lt subtract baseline gt and the data correction will be applied Please note that this procedure will change the underlying data and prior calculated peakdata will be cleared Two baseline types are available e Polynomial 1st order corresponds to linear 2nd to parabolic etc e Exponential the sum of exponents of increasing order up to the indicated value The baseline order can be set from 1 to 6 However the order will always be lower than the number of data points for example on 3 anchor points the baseline order is limited to 2 For Cyclic Voltammograms forward and reverse scan baselines have to be subtracted separately Use the mark CV reverse scan checkbox to select each branch Search Peaks Baseline subtract Peak search Rescale Copy araph E Fe in KNO3 0 2 0 0 Potential Set markers with Left Mouse button and press subtract baseline when ready Baseline type Marked baseline properties polynomial marked order ENT NA exponential marked gt g g T CVreversescan JV automatic calculate subtract baseline C automatic C3C6 B C 9 clear markers late undo subtraction Figure a baseline determination of CV for
42. of Apply wtOCP of IR feedback at BiStat V On E offset Current Range 10u4 CR min 10u4 CR max 10u4 Mode Scanning Delete Cell after meas aot Delete all Pretreatment 0 _ levels i i 05 Save data WE2 Current Save dataset Data ptions Data appear Bia Potential Automatic save 201 pnts Note that the bipotentiostat result here plotted in blue is referenced to the right axis In some cases automatic scaling will cause both curves to be drawn exactly over each other To identify the separate curves use the Show Left Right axis option 3 Direct control 3 1 Direct control The instrument can be controlled directly from the Direct control sheet and simple measurements can be performed This is intended for very simple measurements diagnostics or trouble shooting Normal measurements are controlled from the Method sheet It is important to note that the method settings are not related to the direct control settings 31 Direct Method IReor HiSens stat E 0 00 mV 618 605 nA Current range C 10m Connect 1m standard stability C 10004 fi D kHz filter C 10uA Apply o o00 V C 1uA Set MUX channel o C 100A Set WE32 channel 0 v Automatic E rangin C 100 BiStat Ac Extem IR comp PDA value V Analog outpu chi 0000 V che 0000 V Digital output
43. output 2 Connections Purging control line is Digital Output 1 pin 21 from 37pins peripheral port Stirrer control line is Digital Output 2 pin 3 from 37pins peripheral port Trigger output line is Digital Output 3 pin 22 from 37pins peripheral port RDE control line is Analog Output 1 pin 7 from 37pins peripheral port New drop output line is Analog Output 2 pin 26 from 37pins peripheral port Digital ground is pin 24 analog ground is pin 25 In the lviumSoft program the auxiliary equipment can be activated with the AUX methodparameter When enabled new options appear Purging period Stirrer pretreatment RDE speed The trigger output is activated automatically with the AUX parameter When auxiliary equipment is activated by the AUX parameter the corresponding output ports are set cleared depending on the progress of the measurement Sequence of events 1 2 3 ONO RDE is turned on and set to selected rotation speed Purging is turned on for the indicated Purging period If this parameter is set to 0 no purging will occur Selected number of new drops will be dispensed at 1 sec interval If New drops at start is set to 0 no knock dispense cycles will be exceuted If Stirrer pretreatment is checked the stirrer is turned on for the duration of the complete pretreatment NB OCP determination and equilibration time are not part of pretreatment Trigger line goes to LO active low logic The actu
44. potential at the end of each step Transients TR o ChronoAmperometry applies up to 255 voltage steps and records current o ChronoPotentiometry applies up to 255 current steps and records potential o MixedMode applies up to 255 definable steps records current amp potential amp impedance o Electrochemical Noise corrosion measurement records current amp potential at 2 separate working electrodes ElectroAnalysis Amperometric detection Differential Pulse Square Wave AC Voltammetry Potentiometric Stripping Analysis AC detection Normal Pulse Voltammetry Oo0oo0o00000 Impedance EIS o Controlled E voltammetric frequency scan at a fixed DC potential o Controlled galvanostatic frequency scan at a fixed DC current o PotentialScan voltammetric frequency scans for a range of DC potentials o CurrentScan galvanostatic frequency scans for a range of DC currents 47 5 1 LinearSweep Standard LSV sensor B os Current Potential A linear potentialsweep is created by updating the potential with E_step at each interval so that a staircase scan is applied to the cell with a defined scanrate The interval is defined by E_step scanrate The recorded currents are measured at the end of each interval unless the Alpha parameter is activated Standard mode allows for interval times down to 0 002 s for shorter intervals use HiSpeed mode 5 2 LinearSweep CurrentAveraging A linear potent
45. progress can be monitored with the IV Ndatapoints function e When reading datapoints with the IV readdata command during an ongoing scan be sure to check whether data is available with the IV Ndatapoints function before attempting to access the data e The IV_setmethodparameter pchar1 pchar2 function will change method parameters of the currently loaded procedure If subsequently a scan is started the new values will be used It requires 2 arguments the parameter name and the parameterv alue o Parametername this must correspond exactly to the spelling on the method tabsheet o Parametervalue textual expression of the parameter value The format of the supplied value must correspond with the type of the selected parameter name If the selected parameter is a checkbox a value of true will correspond to the checked condition anything else will uncheck the box Numerical text strings must be of the correct format o When the technique should be modified first set the Method thereafter the Technique For example when selecting Standard Cyclic Voltammetry setmethodparameter Method CyclicVoltammetry setmethodparameter Technique Standard o If wrong or unavailable Parameter names are selected or when unavailable parameter values are entered the commands are ignored without an error message When a parameter value with improper format is supplied the command is ignored and an error message is shown Please note that the p
46. terminated This is controlled from inside the instrument independent from the software that is running on the PC e atexternal signal Ext1 gt when this box is checked the Analoginput1 of the peripheral port is measured When this signal exceeds the voltage that is entered in the adjacent box the measurement will be terminated 26 e at temperature unavailabele for change by user when the instrument s inside reaches a temperature exceeding 80 degC the measurement will be terminated This is an automatic safety feature to protect the instrument e at Eovl CE electrode when this option is checked in galvanostatic mode the instrument will terminate the measurement when an E overload is reached The potential range can be set by user in the advanced method parameters e atcurrent OVL WE electrode when this box is checked in potentiostatic mode the instrument will terminate when a current of 3 072 x the set current range is exceeded This option may also be used in combination with Automatic Current Ranging AutoCR When a method is aborted by the automatic disconnect feature a message is shown on the bottom Statusbar Also the condition is logged in the process report Note that Automatic disconnect is intended as a safety feature It is directly hardwired in the electronics therefore it works instantaneous and does not depend on whatever the software is doing at that time Even in the event the software has crashed the electrode
47. the potential and current noise are calculated by statistical analysis Also derived parameters such as Corrosion resistance and Pitting index are evaluated Moreover with the software tool one can monitor the changes of the parameters vs time by segmenting the datastream 80 The Frequency domain analysis offers 2 methods to calculate frequency spectra e Fast Fourier Transformation FFT straightforward transformation e Maximum Entropy Method MEM alternative method to calculate the frequency spectra using a finite number of coefficients MEM yields more smooth spectra if less coefficients are used If the number is increased the MEM result converges to the FFT curve Zi Electrochemical Noise Analysis Time domain analysis Frequency domain analysis Baseline remove mm Elgraphs CopyFFT CopyMEMS Noise power spectra SN i 7 D 8 5 9 S 10 B B I 2 4 5 2 3 89 4 5 5 6 3 2 4 D 10log frequency Hz Noise impedance g 06 is e a go D 2 e DA 0 2 1 Olog frequency IHz Analysis type C FFT C MEMS FFT MEMS MEMS coefficients gt 5 gt Window function 7 C square C Bartlett Welch C Hann Hamming C Blackman w Subract baseline Evaluation of noise data with FFT black and MEM red Data was recorded by TNO Den Helder The Netherlands Because FFT and MEM are affected by the so called leakage effect i
48. the result can be converted to another value The following sub properties can be defined factor resultvalue is multiplied by a definable constant deault 1 time On Off when checked the result is multiplied by time charge On Off when checked the result is multiplied by charge unit text textual value that is written behind the result value e Smoothing none 5 11 25 integrated Savitzky Golay smoothing that is applied before each find option to be used for noisy data Selecting more smoothing points will result in stronger smoothing When parameters are changed these are automatically stored in the configuration file IviumSoft ict thus these are always copied from a previous session Results can be copied to for example to WORD EXCEL with the Copy results button numerical data or the Copy graph button graph When a datafile is saved after an analysis is executed the analysis results are stored in the file idf 84 7 6 9 Solar cell report The lvium instruments and lviumSoft are equiped to carry out experiments to characterize solar cells for example in combination with a light source such as the Ivium ModuLight When the relevant measurements are carried out a Solar cell report can be created by selecting in the graphic toolbar Analysis SolarcellReport This will open a pop up window where by choice a basic basic model or more elaborate including Rs Rp model can be executed After entering the
49. this graph to be copied printed 39 Show Cyclic Voltammogram 3 E Dy xj pA Fe in KNO3 C E vs time 4 7 Legend panels To the right of the Result graph sheet the legend panels are shown These panels allow the selection of particular scans that can be manipulated saved analysed etc Clicking on a particular scan will make that scan available for manipulation etc it will be highlighted blue independent of whether the box next to it is un checked 40 Scan char Olay no labels m Hide all Show all All extradata Save data Save dataset Delete Delete all Data appear Scan panel recently measured data will be shown here e Datalabel selector optionally shows the numerical values of the datapoints in the plot It is possible to show only every nth datalabel e Scanlist displays a checklistbox of all available scans Scans can be made in visible by un checking the corresponding box Scans can be selected by clicking them with the mouse these will appear blue e Save data saves the selected data to disk as idf If none is selected the most recent is taken at the bottom of the list Save dataset saves all listed data to disk in a single file as ids Delete deletes the selected data Delete all deletes all listed data clears the list Data appearance manipulate data appearance of the data lines symbols colors styles etc When multip
50. upgrade may be re tried After the relevant option has been selected click on it remove power and USB cable CompactStat or switch instrument off IviumStat Ivium n Stat Then re connect or switch instrument on again and retry to connect in the IviumSoft Please note that these recovery functions can only be used directly after power on before the Connect button in the IviumSoft was pressed For the CompactStat it means that the usb cable and power cable must have been removed 92 8 5 Performance test To verify proper operation and to diagnose possible problems the instrument can be instructed to perform a self test To execute the test e Connect the cellcable and Testcell 1 e Select Performance test from the Tools menu e Click the Run test button Each individual test result is compared to preset limits and a Pass or Fail status will be assigned A testreport is generated that can be saved or printed directly Also it can be copied to the Windows clipboard and transferred to the application of choice The report is generated in ASCII format and can be read by any text editor e All status reports should read Pass If one reads Fail re run the test If after repeatedly running the test a fail continues to show up the instrument may need recalibration Note that the report is stored automatically in the IviumStat main directory with the serial number as filename and ipt as extension for example B07003 ip
51. will be kept until re assigned by the operator After a fresh software install the actual serial numbers can be read from the modules by opening and closing the assignment screen 5 After assigning the connection selectionbox will display the channel numbers instead of the serial numbers File Options Tools Help About _Connect m z Chan 1 Direct Method Chan 2 E 0 001 Chan 6 The assignment has to be done only once after installation The settings are kept when the software restarts Connecting the instrument e Inthe channel selection box select the channel that you wish to connect e Press the Connect button at the left top corner The IlviumSoft program will activate the selected channel and the instrument will indicate the connection see status LED In a way the lvium n Stat can be regarded as a number of separate lvium instruments in one single box each channel sModule can be operated as a separate instrument and is identified with a unique serial number In the current IviumSoft the operator can connect to the channel sModule of choice and a new instance of the IviumSoft needs to be opened to connect to the next channel 19 For ease of use the operator can identify the channel that is currently connected in the IviumSoft instance In the Direct mode tab there is an Identify button When this button is clicked the channel that is connected will flash its LED for two seconds 2 4 M
52. 0 only 1 point per second will be produced This feature is convenient for very long measurements that otherwise would produce too many datapoints At very long interval times for example at 1 sec interval and an average count of 600 only 1 point per 10 minutes is recorded Data reduction by averaging has the beneficial effect that noise is suppressed and curves will become more smooth Because less data needs to be communicated the speed limit for standard mode is increased The minimum interval time is reduced from 2ms to 0 5ms at sufficient average counts 500 Hz 2 kHz This feature has some consequences for other functions If AutoCR is active the average values are used to decide to change a current range Also when averaging is activated and analog inputs are recorded simultaneously with the measurement only channels 1 amp 2 can be used To use this feature check the Data reduction option and set the average parameter to the desired number Adaptive sampling enables the user to set a minimum change in the measured parameter E I which will be stored in the data file Thus all relevant trends are captured with a minimum of datapoints The user can define a minimum potential and or current difference which he considers relevant Datapoints that differ less than the defined delta from the last recorded point will not be stored Only datapoints 130 that differ more than the minimum defined delta will be displayed The excepti
53. 00 600 4 2 Potential ECN data after baseline subtraction 7 6 8 Find levels The IviumSoft program contains an integrated level finding tool for chronopotentiometric data It is accessible from the Analysis menu via the option Level Find This will open a window where the operator can execute the tool manipulate level search parameters and process the results 83 2 Find Levels replot copy graph Search for plateau Vv E 0 005 ChronoPotentiometry level find Minimum separatior 500 s Value reference absolute Convert result IY On factor 1 000 time off charge IY On unit C Smoothing 5 points E o o oO 7 84E 01 2 97E 02 2 97E 02 _Copy rests 1 54E400 1 54E 01 1 54E 01 Close Pressing the Find button will execute the search The results are shown in the graph and written to the table below the graph On the left parameters can be altered before a find is done e Search for plateau only option for now enhancements possible upon request e Threshold slope set detectionpoint for a level e Minimum separation minimum distance between 2 results e Value reference absolute differential for absolute all results are referenced to time O for differential relative subsequent result values are referenced from the preceeding found result e Convert result On Off normally Off the timevalue is taken as the result alternatively this option can be checked On at which
54. 13 Ac Extem PDA Ac signal Frequency 2 Hz Amplitude V ME Note When controlling the ModuLight from the direct mode it should be taken into account that communication between PC and lvium device only takes place once per second This means that there may be a delay of up to one second before a change takes effect Running a single method A single method can be run by first setting the desired parameters of the ModuLight such as wavelength and intensity in the Direct mode tab Then in the Method mode tab a method can be run l e to measure an E I curve of a solar cell the desired wavelenght and intensity can be set and then the E I curve can be measured using the linear sweep method To run an impedance measurement first the ModuLight parameters need to be set in the Direct mode tab Then in the Method mode tab the desired impedance technique is selected for example Constant E Then the Advanced parameters need to be activated In the method parameters now MeasConfig is available This parameter determines how and which signals are recorded and shown in the graph Running automated methods In the BatchMode it is possible to run several methods successively In between running the successive methods it is possible to change the wavelength and intensity of the ModuLight To do this add a DirectCommand line in the appropriate place in the batch program When this line is selected in the Line p
55. After connecting all functions can be operated This includes the reading of the device serial number If the IviumSoft is not running a pop up window will show mentioning this Upon clicking the OK button the Ivium Driver 1 0 VI will stop running Prompt User for Input Please start IviumSoft before running this VI 141 When connected the lvium device can be simply operated by using the controls on the various tab pages Direct Mode In the direct mode tab page the device and cell status can be called and all parameters of the Ilvium device can be controlled directly For some of these parameters a property node is called to enable disable the controls when relevant This has been done to eliminate the possibility of sending illegal or conflicting commands that might result in an error and subsequent ceasing of Labview oium driver 1 0 vi Front Panel Ele Edi view Project Operate Tools Window Help 2 a GL tpt Application Font x tar EAEN Disconnect Connect Read device serial number Device serial number 1 Direct Control Methbd control Device Status indicator 3 m STOP VI Get cell status Current range Configuration Apply Set Mux channel AASA i i er oL L fin mA IBistat4EL off Yo Get current Set Filter cell potential 10 kHz 10 00 v A 10 000 A cell current Get potential 19 000 A 0 000 Y current range Set Bi Stat mode Ji m Stand
56. Electrical Compliance DECLARATION OF CONFORMITY We lvium Technologies De Zaale 11 5612 AJ Eindhoven The Netherlands Certify that the products IviumStat CompactStat and lIvium n Stat are in conformity with EC Standard IEC 61326 Standard Electrical equipment for measurement control and laboratory use referring to the following norms IEC 61000 4 2 IEC 61000 4 3 IEC 61000 4 4 IEC 61000 4 5 IEC 61000 4 6 IEC 61000 4 11 CISPR 22 Eindhoven September 2010 Dr A Baars director Conformity applies to configuration and cabling as delivered by Ivium Technologies Ivium Technologies Eindhoven The Netherlands will not accept any liability for damages caused directly or indirectly by connecting this instrument to devices which do not meet the relevant safety standards Ivium Technologies cannot under any circumstance be held responsible for the outcome or interpretation of data measured with these instruments 1 Introduction 2 Getting started 3 Direct control 4 Method control 5 Techniques h h h ee ee ee ee lA OMWNDORWD eo Index IviumSoft IviumStat instrument s CompactStat instrument Ivium n Stat instrument Installation and setup Install Edoubler Install HiMux Install lviumBoost Install MultiWE32 Install Plus module Starting the CompactStat Starting the IviumStat Starting the Ivium n Stat Multiple Ivium instruments on 1 PC Measurement Connecting the electrodes Scree
57. MuxTolndex 1 8 Install lviumBoost The lviumBoost is a current booster for the IviumStat that will increase the maximum current of the IviumStat Two models are available 13 maximum 20A at 20V maximum 40A at 10V The 20A amp 20V version can be used at its full range in combination with the IviumStat XR The 40A 10V can be used optimally with either the IviumStat or the IviumStat XR Safeties and Alarms The lviumBoost is a very powerful device which is capable of high power outputs In order to protect the user and the test subject as well as the device itself the booster is equipped with a variety of electronic safeties some of which have LED alarm indicators Located at the front of the IviumBoost is an indicator window that contains 8 LED indicators in two columns of 4 Indicator Shows when E ovl orange potential range positive maximum is reached E ovl orange potential range negative maximum is reached ovl orange current range maximum is reached Cell on green cell is electrically connected E max red positive power supply overload E min red negative power supply overload Temp red temperature maximum inside IviumBoost is exceeded Osc red an oscillation of the electrical signal in the electrometer occurs The orange LEDs show a warning that a range maximum has been reached The red LEDs show that a terminal condition has occurred and subsequently automatically the cell has been disconnected
58. Sample Auto H black left blue right 4 38 B uw Potential Period 20 ms 24 3563 0 07 E 24 3655 0 16 Top panel Rescale clicking will rescale the graph Options shows graph options Copy copy graph to clipboard Freq shows frequency based signal Sample when clicked will give a signal sample Auto shows continuous signal trace Hide hides the window Graph Black plot corresponds to left axis Blue plot corresponds to right axis Left axis Current of full current range as selected Right axis Potential of full range as selected by automatic E ranging or maximum range Lower panel Period enter period of measurement actual value with accuracy interval E actual E value with accuracy interval 34 2 During an impedance measurement Method control the perturbing and resulting sine waves are shown with the actual filter and amplifier settings This will give a good idea about the quality of the result and may be useful for experimental optimizations Signal Monitor P x Rescale Options Copy Freq Hide black left blue right 1 0 1 0 0 5 05 3 00 o0 S 3 05 45 5 O tL 40 4 0 Freq 1000000 Hz Igain 1 Filter 0 CR 1m Egain 1 Coupling 1 Top panel Rescale clicking will rescale the graph Options shows graph options Copy copy graph to clipboard Freq sho
59. Ssettingsheet parameters that control impedance measurements Environment e 60Hz check this box in countries that have 60Hz mains frequency A correct setting will strongly improve noise suppression because the measurement period will be synchronised with the line frequency e XR 20V mode check this box to enable the 20 V potential range of the IviumStat XR note that the increased potential range decreases the potential resolution e Edoubler check this box if the Edoubler is connected only for IviumStat20V e CompactStat 8V check this box when you are using an 8V conversion CompactStat e CompactStatPlus check this box if the Plus module 20V 250mA is connected to the CompactStat e type Il also check this box if the Plus2 module 10V 800mA is connected to the CompactStat e viumBoost check this box when the lviumBoost is Connected to the IviumStat the radio buttons allow the correct setting for your IviumBoost e MultiWE32 check this box when you are using the MultiWE32 module e Audio off checking this option will disable the instrument s internal speaker e AC input check this box when the AC input of the peripheral port is used in method mode Automatic disconnect The automatic disconnect functions can be activated for extra protection of a testobject When checked and the cut off criterium is reached during a method run experiment the instrument will automatically disconnect the cellcable and the measurement is
60. Switching between Potentiostatic Galvanostatic and OCP mode lt 5ms Minimum measurement interval time 2ms When AC measurements are required the minimum interval time is 0 2s Dynamic level parameters parameter available E applied E vs Eprev CT previous level If the previous stage was dynamically ended _ from threshold criteria the actual last applied measured potefilisused O 1 Estep scanrate intervaltime lappied Istat Appledcurent LLstep scanrate interval time PCT frequency and amplitude 54 Lo e 0 0 00 O o vale 0000000000000 Lo value 8bitconversin 0 all digouts off fedigouttondigoutand3off etc During the dc measurements the ac amplitude is removed The analog input threshold criteria are only active if the analog inputs are measured in the analog 2 channel mode The dynamic threshold tests will ignore the 1st measured point after a new level was applied Levels 4 m Properties for Level 1 control 120 050 A for 100 s or until E 3 500 V applied Open cell for5s Duration control 0 050 A for 100 s or until E 0 100 V Record ac Open cell for5s Until E gt lt I I Sa i 23 3 value Until E lt Until dE dt Until dE dt Until amp n1 Until An1 Until d n dt gt Until d n dt lt Be eee Example stages e Apply 50mA constant cu
61. TI Scale Analysis Edt LinearSweep Scan Olay mA Standard TEST2 no labels Current4veraging TrueLinear l viscan 1 CyclicVoltammetry Standard Title E start 0 0000 V i E end 10000 V E step 5 my i Scanrate 0 05 V s Current Range 1m Save data AutoCR ot Save dataset Cell after meas ot Pretreatment 0 _ levels AUX ot Delete Delete all Data appear T 0 6 Potential 201 pnts Scan completed 2 17 Test 3 standard testcell amp BiStat The cell cable must be connected to the instrument and the testcell as described this test is not available for the Ivium n Stat Start the instrument as described go to Method mode and load the measurement procedure TEST3 imf that was supplied by the manufacturer Measurement procedures can be loaded with the Load method function from the File Menu Press Start and the instrument starts the measurement When completed the result should look like the plot below 30 32 viumStat Control tex File Options Tools Help About i Connect l BOSI A IE ov lov Ext 1mA l Advanced Sigview Direct Method Result graph Result data D iviumstat manual TEST3 X Scale l Analysis v Edit E LinearSweep UA Sean Dlay Standard no labels x Current veraging TrueLinear m scan Vf ad scan 2 CyclicVoltammetry scan 3 Transients M Sang Analog inputs none AutoCR
62. al measurement is executed RDE is turned off Trigger line goes to HI AUX purging period Specify the purging duration in seconds AUX Stirrer pretreatment Switch stirrer on off during pretreatment AUX RDE speed Specify rotationspeed from 0 to 100 Standard 100 corresponds to 4 096 V optionally this can be increased to 10 V To increase to 0 to 10V or to 10 to 10 V a PLT is needed AUX New drops at start Specify the number of knock dispense cycles If this value is non zero the new drops will be dispensed directly after purging before pretreatment starts The new drops are dispensed at 1 second intervals If applied to Static Mercury Electrodes usually this value is set to 3 5 to eliminate memory effects 132 The Analog output 2 will go LO for 1 millisecond to dislodge the previous drop and suspend the new drop It will remain HI after the last drop has been dispersed LO 0 Volt HI 4 Volt AUX InvertDig polarity When this box is ticked the polarity of the digital output is reversed Modules Check this if special modules are to be activated Modules PDA Check this if external PDA modules should be used If multiple PDA units are used gt 8 channels this will activate the selection of the extra PDA modules MeasConfig For impedance measurements the applied and measured signals can be redefined This is especially useful when using external equipment in combination with the potentiostat galvanostat One
63. al time At interval times larger than 2 ms the standard mode can be applied Here the number of datapoints is unlimited For interval times shorter than 2 ms the HiSpeed mode must be applied In HiSpeed mode the maximum number of datapoints is 8192 In standard mode the multicycling option and dynamic level switching can be applied 52 52 lviumStat Control File Options Tools Help About Eovilovi Ext tus Direct Method D iviumstat manual cp1 LinearSweep CyclicVoltammetry Transients Electro amp nalysis Impedance Standard Multicycle CP Cycles Cycles separate Interval time Current Range Potential range mi levels _ levels el Result graph Result data Scale Analysis gt Edit Potential Multicycle CP Send method Scan Olay no labels scan 1 cycle 1 Save data Save dataset Delete Delete all Data appear 2857 pnts cycle 1 Scan completed Example of ChronoPotentiometry with 2 levels and 4 cycles and dynamic level switching at 0 9 Volt and 0 2 Volt 2 IviumStat Control File Options Tools Help About Frese Direct Method D iviumstat manual cp1 LinearSweep CyclicVoltammetry Transients Electro amp nalysis Impedance Standard Multicycle CP Interval time Current Range Potential range IP
64. alchronoAmpPlaatie T Scale Analysis Edit l Chrono amp mperometry D mA Scan Olay ChronoPotentiometry nolabes gt Electro amp nalysis 3D skh Amperometric Detection vl scan 1 chronaar Differential Pulse Square Wave v Value Unit Mode HiSpeed Title Scan 1 Levels 5 _ levels Interval time 0 00001 s Equilibration time 0s Current Range 1m amp Filter automatic EGER Stability automatic Sane Connect to Cell 4EL 1 Analog inputs none Delete Apply wtOCP D of dus l l l i Delete all IR feedback ot BiStat Off Cell after meas nt Ee During chronoamperometry a single or a series of potential pulses max 255 is applied and the current is recorded The timebase of the experiment is set by the interval time it defines the 51 measurement speed and the pulse duration The minimum interval time is 10 us and the maximum level duration is 4E9 times the interval time At interval times larger than 2 ms the standard mode can be applied Here the number of datapoints is unlimited For interval times shorter than 2 ms the HiSpeed mode must be applied In HiSpeed mode the maximum number of datapoints is 8192 In standard mode the multicycling option can be applied During ChronoAmperometry the user can change the applied potential manually without stopping the experiment The operator may specify potentials that deviate from the fixed potential levels
65. am is the possibility of connecting with the Ivium device 1 Upon connecting a flat sequence is carried out 2 connecting the device and subsequently setting the current range again to ensure that the shown value is the actual one NETTE TA F F while loop timer Direct Control Default Reset device status indicator E Direct Mode E E device stat Reset cell status indicators The rest of the while loop is reserved for a tab controlled case structure 3 This case structure operates depending on the choice of direct or method mode The direct case includes all operating parameters as well as the tab controlled case structure for the AC Extern BiStat controls It also includes the writing data to file operation and the simple chart The method case includes all the operating parameters for reading starting changing and saving experimental methods Operating the Ivium Driver 1 0 Operating the Ivium Driver 1 0 mostly resembles the IviumSoft software First start the VI from Labview Clicking the Disconnect Connect button at the top of the user interface above the tab control connects the lvium device i View Project Operate Tot Rar 13pt opica E E Tau me ae ee ee ee FR Rura If the device is not connected none of the direct operating controls or the method controls work
66. ame char1 char2 IV Ndatapoints int Returns actual available number of datapoints IV readmethod char Loads method procedure from disk with char as filename procedure is used else the procedure is loaded from disk 96 Po indicates progress during a run IV_readdata int d1 d2 d3 Read datapoint with index int returns 3 doubles d1 d2 d3 that p represent measured values depending on the used technique for S example LSV CV methods return E I 0 Transient methods xo return time I E 0 Impedance methods return Z1 Z2 freq etc Programming considerations e All imported functions return an integer as result 32 bits signed number O successfully executed 1 no device 1 illegal command 2 argument out of range Note that IV getdevicestatus return codes are different Arguments are passed by reference Pchar zero terminated string int 32 bit signed integer double 8 byte floating point number Current is expressed in Ampere potential in Volt time in s and frequency in Hz The driver must be opened with the IV open function before the control functions can be used When the driver is opened it automatically connects the first connected device For single device users nothing needs to be done to select it For multi device configurations use the IV selectdevice command to select each different device e After starting a method IV getdevicestatus will indicate whether a scan is ready During a scan
67. an be started form the Tools menu Please note that the settings for Current range and Stability are copied from the Direct tabsheet These settings should be set before the Pulse generator form is opened After pressing lt Apply gt the pulse will be applied and repeated continuously until Stop is pressed The period and Voltage Ampere values will be retained until the IviumSoft program is ended 8 7 Current Interrupt The current interrupt technique can be used for measuring the IR drop of an electrochemical system This application is designed to operate in combination with the Ivium Technologies CIM As the name of the technique suggests the current of a running experiment is interrupted instantly and the response of the cell potential is measured in high speed mode The momentary drop of the cell potential representing the IR drop of the electrochemical system is then shown in a graph of the potential vs time Operation In the IviumSoft the current interrupt technique is integrated as a diagnostic tool To operate the current interrupt technique in the Direct Mode set the desired potential in either the potentiostatic 4 electrode or 2 electrode configuration and then apply so that the potential is applied to the test object and the current flows Then in the menu bar choose Tools CurrentInterrupt and then press apply The current is momentarily interrupted and a graph is produced showing the potential vs time From this resu
68. arameter availability depends on the chosen Method and Technique 8 9 Galvanostatic generation icw Amperometric detection with BiStat The techniques Chronopotentiometry galvanostatic CV and galvanostatic LSV can be combined with the bipotentiostat module Several applications that normally require 2 potentiostats galvanostats can be performed with a single instrument The primary WE and CE will control the applied current in galvanostatic mode while the BiStat module is operating in potentiostatic mode applying a potential and measuring a current The bipotentiostat will use the RE standard mode or S scanning mode electrode as reference Its offset potential can be set in the 2V range When the Bistat option is activated the measurement plot will show both working electrode currents The WE CE electrode pair may be located in a different cell compartment than the WE2 RE S pair For a typical application the WE CE pair would generate a product that is detected by measurement with the WE2 97 8 10 Labview interfacing LabView drivers are bundled with the IviumSoft These will facilitate the control of the Ivium instruments from a LabView development environment More information is given in the lvium Labview driver product note in Appendix1 of this user manual 8 11 lvium data file registration It is possible to register Ivium datafiles idf and Ivium datasets ids This action will make it possible to double mouse cli
69. ard offset potential 0 000 y Start stop writing Y Scale Range Minimum data to spreadsheet file start Chart glo 2 lt Scale Range Maximum In the direct mode as an example an operation for writing data to spread sheet file 1 and a simple chart 2 have been incorporated The chart plots data from the data file and thus only operates when the data is being written to file The name of the data file is automatically genrated as test date time This filename can be altered in the Block Diagram The direct mode also shows an extra number of tab pages AC Extern BiStat 3 e The AC page allows to control a simple AC experiment e The Extern page allows to read and control all external ports e The BiStat page only shows when the configuration BiStat4EL or BiStat2EL has been chosen It then allows BiStat control 142 Method mode In the method mode tab page a method can be selected A This method can then be read into the Ivium software and the device B Then the method can be started C When start method is clicked and no method was read into the IviumSoft the method currently selected in the IviumSoft is started 3 ium driver I US Front Panel x File Edit Yiew Project Operate Tools Window Help m gt JA D pE 13pt Application Font Soy Tar hie 5 D A
70. art button and aborted with Abort button e Results can be saved with the File menu item Save data 20 2 6 Connecting the electrodes The standard lviumStat CompactStat electrode cable has 6 leads with 4 mm plugs e CE black counter electrode e WE red working electrode e WE2 red working electrode for bipotentiostat inactive if not ordered potential sensor for sModule Ivium n Stat e RE blue reference electrode e S white sense electrode e GND green ground connection Usually an experiment does not require all these electrodes separately In that case tie multiple leads together The GND lead is normally not connected to an electrode but to a grounding point like a Faraday cage to reduce noise Configurations For a 2 electrode Electrochemical experiment e connect WE and S together to the electrode to be studied e connect CE and RE together to the other electrode NB it is possible to let the instrument make the WE S and the CE RE shortcuts internally by setting the 2 EL mode thus you only need to connect WE and CE However it is recommended to use the 4 EL mode because that configuration gives better performance in some cases see below For a 3 electrode Electrochemical experiment using a reference electrode e connect WE and S together to the electrode to be studied e connect CE to the counter electrode e connect RE to the reference electrode For a 4 electrode Electrochemical experiment us
71. as E standby Pretreatment Data Options Automatic save Report Current4yveraging Galvanostatic E CyclicVoltammetry Standard TEST 1 M of Iv On Im automatic automatic dummy 1 none M On 104 10n4 M oft off Standard M On 0 Off Off Off Off ogad Ic IviumStat datafiles TEST1 T 0 0000 1 0000 5 mV 0 05 V s 0 400 os 0 000 V _ levels E 37 4 4 Result graph sheet Here the results are shown in graphical form Result data Analysis Edit Scan Olay 2D nA xi DPV ps sensor nobe v scan l demo dp 0 5 Save data Current Save dataset Delete Delete all D 4 0 2 0 0 0 2 0 4 Data appear dt Potential On top the graphic toolbar is shown On the right the legend panels are shown In the center the data plots are shown The results of the primary measurements are always shown and optional 1 or 2 additional graphs are shown Extra graphs are accessible through the buttons to the left of the graph X show primary data Ain Analog peripheral inputs up to 8 channels can be displayed in 1 or 2 extra graphs These values can be shown as measured in Volt Or they can be transformed with user defined functions thus showing physical parameters as temperature pressure etc If 2 types of transformations are required 2 groups of analog inputs can be assigned to different graphic windows Data options are available fr
72. at hinder the interpretation of the result 61 5 23 Impedance PotentialScan The implementation is analog to the Constant E variant but it is repeated at a range of dc potentials The results can be stored as single potential files idf or all together as dataset ids In the primary data graph results for each potential are plotted in the usual manner Z1Z2 Y1Y2 etc On the Escan sheet results may be plotted vs potential e CsvsE Z vsE Z vsE Y vs E Y vsE Mott Schottky 1 Cs 2 vs E Z1vsE C Z2vsE C YlvsE C Y2vsE Mott Schottky from 5 000 v to 1 000 All Specific frequencies can be shown or hidden by clicking these in the Select frequencies checklist Also a specific potential range can be selected by setting the from and to in the Select potentials group 5 24 Impedance CurrentScan Galvanostatic impedance scans can be performed in combination with a dc Current scan in much the same way as the PotentialScan variant Select the Currentscan method and set the dc scan parameters Istart Istep and lend The frequency scan will now be repeated at every dc step value of the ramp The results can be stored as single potential files idf or all together as dataset ids 62 6 BatchMode Using BatchMode the operator can automate complex measurement sequences and interface to external equipment for process automation It is possible to automatic loading and execution of method fil
73. cable as shielding for the RE but they are not carried out to a banana plug RE RE shield WE1 brown blue WE2 WES WE4 WEB WE6 gey 1 1 6 WET WES WE9 WE10 violet 1 8 0 WEI2 greypnk 9 y Peripheral port connector DB37 female Pin Function Signalrange Remarks 1 Jesv max 100mA not to be used in usb powered mode digin Oto 5V PO 3 digout2 0to 33V 1 0 0 0 O 4 busy j0to 5V reserved for Ivium pe 6 dgn po 0 to 4 096V 0 0 0 0 0 0 0 0 0 0 0 0 5 to 405V 20 9 Q 0 Atoy ep ees pgain X 4to 4vV PO 117 HH ipgasine lt atom AW 55 5 5 5 20 digin2 Oto 5V PO j21 digouti 0to 33V 22 digout3 0to 33V 24 dgnd PP 25 lagd o o oo e 26 an out 2 0to 4 096V 0 0 0 0 0 OE 2 teas lagd 5 0 0 0 0 0 E out IviumStat signal range 10 to 10V i e for IviumStat XR in 20V mode E out E 2 CompactStat signal range 4 to 4V i e for CompactStatPlus E out E 5 33 for CompactStatPlus2 E out E 2 66 Peripheral connector Ivium n Stat DB15 female The peripheral connector of the sModule has 15 pins instead of 37 pins The sModule has fewer signals than the lviumStat CompactStat Also note that the analog input range is different Note in floating mode the peripheral sig
74. can use the ACout Xin and Yin connectors on the peripheral port for this purpose Some possible applications configurations e Interfacing a Solar cell to modulate a light source and measure the photocurrent potential Modulight module Interfacing with an electronic load Interfacing with an RDE to modulate rotation rate Hydrodynamic impedance Using the lvium FRA in combination with an external analog potentiostat etc In standard setting the impedance is defined as Y X which is normally the measured E I from the electrochemical cell When other external signals are used for X Y the meaning of the plotted impedance might be different from the classical definition The plot is always displayed as if Y X were E I and the user is responsible for any conversions To change the configuration of the signals in the method parameters the advanced parameter MeasConfig gives the user the possibility to adjust this configuration A list of possibilities is given in the table below _ MeasConfig x Y remarks 1 0 standard Iwe E si Internal DSG not applied 2 INTacE j lwe Jacintem 6 pO pO EXT acE _ s iwe Yperiph EXL IINTE Xperph acinem gt 0 7 EXT EINTI Jacinem Yperph gt 8 Directe Iwe E CEasreference instead of RE S 9 DirectE INT acintem E CE as reference instead of RE S 10 jDi
75. cation and height of peaks manually and to subtract baseline Clear peaks to remove peaks from the screen that were created with Peakfind analysis Electrochemical noise to analyse chemical noise results with FFT and or MEM Find levels level finding tool for chronopotentiometric data Solar cell report complete analysis of a solar cell from FRA experiments Curve fit to fit arbitrary polynomials Electrolysisreport will analyse and display the passed charge and current Edit see also Edit chapter Edit data data smoothing functions based on Savitzky Golay or Fourier transformation and change data point Smooth all data automatically smooths all data according to the prevailing smoothing settings Note once pressed the raw data is replaced by the smoothed data so save data before using Subtract ohmic drop to correct by calculation the potential loss due to the effects of ohmic resistance on Linear scans and Cyclic Voltammograms Average scans automatically averages scans in a dataset Subtract overlay 1 subtracts overlay graph from scan graph Add overlay 1 adds overlay graph to scan graph Impedance plot selection set graphical presentation of impedance data Z Phi Bode plot the absolute impedance is plotted with the left and the phase angle is plotted with the right axis Rs Cs the Rs is plotted with the left and the Cs is plotted with the right axis Z Z Nyquist plot impedances Z
76. cell area and light intensity clicking the Calculate button will result in all the relevant parameters of the solar cell given in the Analysis results window EE Solar cell analysis a E E x r Select model C basic model pA Solar Cell Modelling include Rs Ap Parameters Cell area 1 0 ma Light intensity 10 wum 2 Copy result Analysis results Isc 2 250E 04 A c o Jsc 2 250E 04 A m 2 5 Oo Eoc 8 3709 V E Pmax 6 3732 V Pmax 1 243E 03 W AA 4 260E 08 A BB 1 0240 V 1 FF 06631 Dhu CE 0 0012 Fis 462 8613 Ohm Rp 951995 7452 Ohm Power cise Potential v Solar cell fitting equations 1 I Isc AA exp BB V 1 V Rp with 2 V E I Rs total current E total potential V internal potential across solar cell 2 excluding potentialdrop over Rs Isc shortcut photocurrent V 0 AA saturation current BB exponential constant related to ideality factor Note that equation 1 and 2 cannot be solved by simple calculation IviumSoft uses the Leven Marquard method of nonlinear fitting by iterative minimizing the sum of quadratic deviations from the experimental E I data with the model 85 7 6 10 Curve fit A tool to fit arbitrary polynomials can be accessed from the Analysis menu in the graphic toolbar Choosing this option will open a pop up window where a curve analysis can be carri
77. ck on an Ivium data file set to load it in the scan panel of the IviumSoft To activate this option in the Options menu click on Register idf ids files Each time when double clicking on an Ivium datafile set the file set will be opened in the scan panel of a new lviumSoft instance Only opening a data file from the File menu will allow data to be opened in the same lviumSoft instance 8 12 Measurements using the peripheral port 8 12 1 Peripheral analog inputs Ivium Instruments are equiped with a peripheral I O port list of signals and connections see chapter 9 20 Connectors The peripheral port interfaces via a DB37 connector CompactStat IviumStat or a DB15 connector Ivium n Stat sModule For the DB37 connector a break out box is available the PPE peripheral port expander see chapter 9 9 that outputs all signals to 4mm banana connectors Alternatively the desired signals can be taken directly from the corresponding pins in the DB37 connector The peripheral port includes 8 analog inputs 0 to 4V for the CompactStat Iviumstat 2 analog inputs 0 to 10V for the Ivium n Stat Signals from these inputs can be recorded in pairs simultaneously with the primary signals In the 2 channel configuration ch1 amp ch2 are sampled at the same speed as the primary channel When 4 channels are sampled ch1 amp ch2 and ch3 amp ch4 are sampled alternately at half the sampling speed of the primary signals Likewise when 4 channels ar
78. cleation 50 The CurrentAveraging method is more sensitive to capacitive currents When that is undesirable the standard variant is more appropriate 5 8 CyclicVoltammetry TrueLinear Continuous linear analog potentialsweeps are applied instead of the standard staircase The E_step variable defines the interval time The interval is defined by E_step scanrate The recorded currents are measured at the end of each interval Standard mode allows for interval times down to 0 002 s for shorter intervals use HiSpeed mode 5 9 CyclicVoltammetry Galvanostatic This is similar to the Standard potentiostatic sweep but now galvanostatic Each scan consists of 3 linear segments start to Vertex 1 Vertext 1 to Vertex2 and Vertext 2 back to start The segments are created by increasing the current with step at each interval so that a staircase scan is applied to the cell with a defined scanrate The interval is defined by step scanrate The recorded potentials are measured at the end of each interval unless the Alpha parameter is activated Standard mode allows for interval times down to 0 002 s for shorter intervals use HiSpeed mode In standard mode the number of datapoints is unlimited in HiSpeed mode a maximum of 32 000 datapoints applies 5 10 Transients ChronoAmperometry 32 lviumStat Control File Options Tools Help About Connect m Advanced Se Siin Direct Method Result graph Result data D iviumstat manu
79. connections e Calibration values can be reset by pressing the Reset button 9 12 PLT Functionality enhance the potential range of the analog inputs and outputs at the peripheral port to 10V Specifications pre e To instrument peripheral port Powered from peripheral port wxdxh 7 5x53x1 5cm Weight 108 Application The standard input output range of the IviumStat CompactStat analog peripheral port is 0 to 4V The PLT transforms the range of the analog inputs 1 amp 2 to 10V and the analog outputs to O to 10V or 10V see note 1 When the PLT is connected the externally measured applied potential E can be calculated from E_PLT e analog inputs 1 and 2 E PLT 0 185 E 1 96 range 10V to 10V where E_PLT reading on screen E actual input on peripheral port e analog outputs 1 and 2 E 5 E_PLT range OV to 10V where E_PLT setting on screen E actual output of peripheral port Note 1 The analog inputs 3 8 remain unchanged Note 2 On request the analog output range can be adjusted to 10V In such case the potential transformation will be E 5 E PLT 2 048V Note 3 For CompactStat when using PLT make sure that CompactStat is fed from adapter power Installation The male side of PLT module can be placed directly on the peripheral port connector of the IviumStat CompactStat Any external equipment can be connected to the female side as before It is thus connected between the instrument and th
80. ctions for use Developed in Labview 8 2 Labview VI Ivium remdriver IviumSoft Order of hierarchy To install copy the Labview directory into the IviumStat directory of your computer The lvium remdriver dll was imported into Labview to create a Labview library Ivlib In this library a vi is present for all the functions that can be used to control the Ivium device These vi s can be found in the Ivium_remdriver directory A list of functions that can be controlled is given below a detailed description for each of these functions is given in the IviumSoft development driver which can be found in the Software Development Driver directory Imported function description GENERAL IV open Opens the driver IV close Closes the driver IV getdevicestatus Returns status of device IV readSN char Returns serial number of selected device IV connect int Connect to selected device DIRECT MODE IV getcellstatus int Returns cell status IV setconnectionmodev int Select configuration off EStat4EL EStat2EL EstatDummy1 EStatDummy2 EstatDummy3 EstatDummy4 Istat4EL Istat2EL Istatbummy BiStat4EL BiStat2EL IV setpotential double Set cell potential IV setpotentialW E2 double Set BiStat offset potential IV setcurrent double Set cell current galvanostatic mode IV getpotential double Returns measured potential IV setcurrentran
81. cy This application is comparable to AC Voltammetry but at a constant dc potential The results are plotted as Rs and Cs at left and right axis Rs amp Cs are determined from a circuit with a resistor and capacitor in series Rs Z1 Cs 1 2PI frequency Z2 Specifications e Frequency range 10Hz to 2MHz e Interval time 0 2s to 2 5s 5 20 ElectroAnalysis Normal Pulse Voltammetry With Normal Pulse Voltammetry a repetitive potential pulse is applied at increasing amplitude Starting at a base potential E start a pulse with a definable pulse time is applied at each interval time Estep Scanrate Each subsequent pulse is increased with Estep until E end is reached 5 21 Impedance Constant E A range of frequencies is applied at a constant dc potential Frequencies and amplitudes can be defined by pressing the Frequencies button in the method grid This will open a pop up window where a choice can be made to apply a SingleSine or MultiSine method SingleSine In SingleSine mode the operator can supply the amplitude a start and end frequency and the number of frequencies each decade When pressing Apply the software will calculate automatically a logarithmic spread of frequencies The operator may choose to override specific frequencies and amplitudes and enter these manually check Manual override box and enter values 58 Edit frequencies E ani xl Single sine Multi sine Frequencies each decade Frequencies 8
82. d record current and potential during the acquisition period determine theoretical optimal current range dc bias and gainsettings if actual settings are not optimal adjust settings and repeat measurement send result to pc and continue with next frequency Note that for each following frequency the settings are copied from the previous frequency If the frequency spacing is not too large the settings are usually almost the same and 1 or 2 attempts will probably give an optimal result Therefore the first frequency will often take a longer time than the rest Although in Advanced mode it is possible to override automatic Filter and Stability settings this is usually not recommended 60 kohm Scan 1 0 8 0 6 0 4 SF da 0 2 0 0 0 0 0 2 0 4 0 6 0 8 1 0 Z kohm The results are recorded and stored in the format Z1 Z2 frequency However these maybe visualized in a number of formats e Impedance plot selection set graphical presentation of impedance data with the buttons above the graph 5 22 Impedance Constant A range of frequencies is applied at a constant dc current The implementation is analog to the Constant E variant except e dc amp ac currents should be supplied instead of potentials e automatic current range selection is not possible Special care should be taken with the choice of the amplitude If the resulting ac potential gets too large non linearity effects might occur th
83. d by the user 5 Manual control Reboot device is needed after a firmware upgrade 89 6 Upgrade firmware methods for upgrading the firmware 7 Upload file to upload a specific file to the instrument internal PC This is not meant to be used without proper specific instructions from the manufacturer 8 Disable idle sampling clicking this button will disable the idle sampling when no method is running or in direct mode every second a sample taken to update the status bar and the values shown in direct control panel 8 2 Calibration Full calibration of any instrument is done by the manufacturer or the official distributor for your geographic region Only the offset calibration for the IviumBoost and the PDA calibration can be done on site by the operator If for some reason the instrument does not function properly or a performance test turns up a fail repeatedly please apply the Restore procedure described elsewhere Use Restore factory options 8 3 Upgrading firmware After upgrading the pc based software to a newer release it is necessary to also upgrade the internal software of the instrument the so called firmware No tools or files are necessary The required firmware is packed inside the pc software and the upgrade can be performed with the standard usb cable After the instrument is connected in the main menu press Tools Device Maintenance 90 Device maintenance Ol x
84. d to use the automatic setting The automatically selected filter depends upon sample rate It is subject to change in future revisions without notice but is currently as follows Filter e SR gt 500kHz 1MHz SR gt 50kHz 100kHz SR gt 5kHz 10kHz SR gt 50Hz 1kHz when AUTOCR and SR gt 8Hz 1kHz else 10Hz Stability Bandwidth that signals are applied on the sample highspeed standard high stability or automatic In Basic mode automatic is applied High speeds allow for faster pulses scanrates and higher frequencies but increase noise levels and worsen stability In automatic mode the system determines the most appropriate setting from the applied samplerate DC or applied frequency impedance method Overriding the automatic setting should be done with care because it may result in signal deformation and instability Especially for the impedance methods it is recommended to use the automatic setting In automatic setting the Stability is as follows e SR gt 1kHz hispeed e SR gt 20Hz standard e else histability Subject to change without noticfication Connect to Select electrode cable configuration or internal dummy cell Cell 2El only CE and WE need to be connected Cell 4El CE WE RE and S need to be connected Dummy 1 1kOhm Dummy 2 100kOhm Dummy 3 10Mohm Dummy 4 1kohm parallel over 1uF in series with 1000hm CompactStat or 250ohm IviumStat Analog inputs Measurement configuration of external analog i
85. data C al sequentially C extended dataset C OCP values Current units E C n E m C p C uA C A Potential units 6v C mC uw time units Cs C ms C us Impedance e 24 ne gp e Eo C ELphi C Y1 Y2 C Rs Cs Format scientific notation r The top toolbar contains 2 buttons Refresh and Export Refresh updates the displayed data and Export opens dropdown list with options for data export e Copy all to clipboard places all numerical data from the grid into the clipboard e Copy selected to clipboard places the selected numerical data from the grid into the clipboard e Save all to disk saves all the numerical data from the grid into the clipboard e Save selected to disk saves selected numerical data from the grid into the clipboard The data is formatted as shown in the grid thus as characters Note that non visual digits are lost and it is advisable to set the appropriate units first Show data defines which data is shown e selected data shows only data that is selected in the Scan Legend Usually this is the most recent scan e all data shows all data that is listed in the Scan Legend when the sequentially box is ticked the data will be shown sequentially in one column e extended dataset shows the selected scan together with the data from the external analog inputs e OCP values when an OCP measurement is selected this will show
86. dified in the advanced tool Scan 1 Current Potential V 74 7 6 5 Peakfind advanced Pressing the Peakfind advanced will open an extra window that contains e Automatic peak find tool and its editable parameters e Manual peak addition tool e Peak results list and peak removal functions e Baseline subtraction options Search Peaks Baseline subtract Automatic peak find ReScale Copy graph Copy peaks Search parameters automatic peakfind Sc an 1 Construct from whole peak Find method 1st derivative Height mode proportional Minimum height 0 015 Width mode absolute Minimum width 0 025 Sensitivity 5 pnts Smoothing 5 points r Manual peak addition Add marked peak mark CV reverse scan j i 0 4 Clear markers Potential m Peak results 4 0055819E 01 0 105 1 7272627E 02 6 9090509E 01 0 495 2 0729050E 00 0 175 1 2444864E 01 4 3779458E 00 0 230 6 5146951E 00 0 335 8 0533173E 01 3 2237263E 01 Clear all peaks Remove peak 1 Done Graphical presentation of the data with found added peaks drawn in Automatic peakfind example with whole peak and 1st derivative selected The automatic peak find tool is located on the top left panel It has an execute search button Automatic peak find and below that a list of parameters that will be applied during automatic search actions Construct from whole peak front flank rear flank Selecting whole peak w
87. e as the primary signal Measurement in Direct mode The analog input signals can be measured from the direct mode tab Connect the analog inputs as desired analog inputs are measured vs analog ground Select the Direct tab Below select the Extern tab Click on Read analog inputs A single signal sample will be measured on all analog inputs and displayed in the value array 8 12 3 Analog inputs via PLT The analog input measuring capability of the CompactStat Ivium Stat is standard 0 to 4 V This can be extended to 0 to 10 V or 10 to 10 V by using a PLT peripheral level transformer To measure via the PLT connect the PLT directly to the Ivium instrument and connect the external signal to the PLT Then the same procedure for measuring as described above can be used When using the PLT it is the operators responsibility to calculate the correct signal value based on the formula given for the PLT see chapter 9 11 100 8 12 4 Analog inputs via PDA The PDA module see chapter 9 10 is an interface box almost the same as the PPE see chapter 9 9 that outputs all signals to 4mm banana connectors The exceptions are e Normally the peripheral port analog inputs are measured vs the common analog ground resulting in an absolute measurement In the PDA the analog inputs are differential i e each signal is measured with a differential measurement range of 2V and a maximum common mode voltage 15V e PDA module
88. e data that is present Result graph Result data E scan Scale Analysis Edit ZLPhi nx IE rese Purse eripheral port m EB perip p 3D zm Cor x Ain ocp 0 10 20 ES X axis Result an val ay et To the left a vertical toolbar is displayed 2D 3D 3Di selects 2 or 3 dimensional presentation The assignment of the 3rd axis depends on the result type l e for scan techniques the 3rd axis equals the scan sequence number while for nyquist plots the 3rd axis equals the frequency In the latter case the 3rd axis can be forced to show the sequence number by selecting 3Di Zm Cor set Zoom or Correction mode Standard the Zoom mode is selected in which you can expand parts of the plot by left click and drag the mouse cursor In Correction mode you can correct erroneous data points select the point to be edited with a left mouse click while keeping the left mouse button pressed drag the point up or down to the desired location in the graph release the mouse button and the data point will be updated Note that the correction tool will change the measured datapoint and should be used with care when the point to be edited is right mouse clicked the option to delete the data point appears Note that deletion is irreversible Be sure to save the data before performing this action L R 2nd Left Right twin axis selector If the double vertical axis presentation is active i e for im
89. e periphery All signals are passed through this module and except level change of the analog inputs and outputs it is fully compatible with the situation without PLT For CompactStat when using PLT make sure that CompactStat is fed from adapter power 9 13 BiStat BiStat bipotentiostat module WE2 E 2 configurations o G WE2 at a fixed potential w r t RE scanning WE2 at a fixed offset potential w r t the primary WE Current compliance 30mA 1mA in USB powered mode CompactStat po lower 4 ranges use amplifier pf and 0 0000023 using gain amplifier simultanously with primary WE1 Oooo fOOkHzsamplrae O Note Configuration standard scanning is controlled by software and is determined by the method procedure parameter BiStat 109 9 14 LinScan Applies a smooth analog ramp instead of the standard staircase ramp LinScan True Linear Scan module pT 1 uV s 10 000 V s Software implementation LSV and CV 9 15 MultiWE32 The MultiW E32 module will accomodate cells with 32 Working Electrodes that share a single CE and RE The potential is applied to all channels simultaneously thus applied E is not multiplexed System Performance Current compliance 1mA for each WE 32 mA for CE Maximum offset Voltage t 2V Applied potential max 20 V depends on controlling potentiostat Potentiostat Bandwidth 2100 kHz Stability settings High Speed Standard and High Stabili
90. e sampled the peripheral channels are sampled at a quarter of the sampling speed of the primary signals Results are visualized in the Extra plot accessible via the graphic toolbars by clicking Ain 8 12 2 Analog inputs direct or via PPE Measurement in Method mode To use analog inputs in method mode 1 Connect the analog inputs as desired analog inputs are measured vs analog ground In the method parameters advanced at the Analog inputs parameter choose the number of channels to be measured keeping within the capability of your hardware 2 4 8 channels standard 3 In the method parameters advanced at the Data Options parameter select the Analog Inputs tab 98 DataOptionForm Analoglnputs Ecorrections Electrode Plot 1 Plot title Peripheral Port Avis tite Vot Transform none z Plot 2 Plot title Peripheral Port Avis tite Vot Transform none z M Transform parameters Transform parameter al o cf o0 al o0 channel 1 Id 2 channel 2 Id 3 channel 3 Id 4 channel 4 Id 5 channel 5 Id B channel 6 Id 7 channel 7 Id 8 channel 8 DOLO Set default Apply to selected data Apply to all data In this form it is possible to select how the inputs are displayed including plot title and a number of transformations that will be executed before the signal is plotted It is also possible to plot different channels
91. e scan and the notification that a measurement is in progress In case an OCP measurement is carried out the OCP value can also be found in the Status bar Note the values shown in the information bar may be lagging behind when high sampling rates are used Note that Scans and data are by default NOT automatically saved unless the option is activated in the advanced parameters of the method User action is necessary to save data When different electrochemical methods are used the data cannot always be represented in the same graph i e running a FRA scan after a CV scan without clearing the graph window will lead to unreadable graphs Running a CV scan will automatically clear the graph when the next experiment is started Save data before running the next experiment 2 8 File menu Load data load a datafile idf from a previously stored measurement This action will clear any data that might be present already Save data save the selected scan data to disk as idf If none is selected the most recent is taken Load dataset load a previously saved set of scans ids Save dataset save all data in the Scan panel to disk in a single file as ids file Save visible dataset save all data in the Scan panel that is made visible in the graph to disk in a single file as ids file 25 Load method load a previously saved measurement protocol imf Save method save the current measurement protocol as imf Ex
92. e the software e About information about the software To start e At the left top of the screen the serial channel number read out window is located In the drop down menu to the right side of that select the device by serial channel number e To operate this instrument click Connect Connect button connect or disconnect the instrument displayed in the indicated serial number box You must be connected before you can communicate with a device When the IviumSoft program is terminated the device will automatically disconnect A device can only be connected to one lviumSoft application at a time 2 Operating parameters Direct mode for direct control of the instrument e Intended for diagnostic purposes e Actual potential and current are displayed These values are updated every second 23 e When no potential current is applied the open cell potential S RE is displayed within specified accuracy Method mode for executing electrochemical methods The operator can define a technique or measurement protocol on the Method sheet When the Start button at the bottom of the tab sheet is pressed this measurement protocol is executed In this state the software takes control over the instrument Method control This will last until the measurement is completed or aborted by the user During Method control the Direct control functions are not available neither are some filing and analysis functions 3 Advanced parameters
93. ector fits the supplied 5V power adapter In usb powered mode this plug should be removed e USB connector fits to the supplied USB A B cable which should be connected between instrument and PC e Peripheral port 37p connector that provides access to a range of analog digital input output signals Frontpanel e OnLED when the instrument is turned on from the PC this LED will light up green e Cell LED when the cell is on CE this LED will light up red e Cell connector 15p connector that fits the supplied electrode cable The CompactStat instrument can be powered via the external adapter or from the USB cable The instrument selects its power supply automatically based on the presence absence of the dc connector plug This should be placed or removed before the usb cable is connected When powered via the external adapter the instrument can access full power and no restrictions apply When powered via the USB cable the instrument draws its power from the pc USB powered devices may formally draw a maximum of 500 mA and some restrictions apply to the CompactStat to remain below this formal limit e 10 mA current range should not be used e internal dummy cells should not be used e automatic 2 electrode mode should not be used However most pc s will have no problem if the 500 mA limit is exceeded slightly for short periods of time If the IviumSoft program is not running or the instrument is disconnected the CompactStat is put
94. ed out First select the curve to be analysed in the scan panel and press Analysis Curve fit On the left the projection can be chosen based on the available variables potential current time Z1 Z2 frequency etc Also both axis can be transformed linear log exp sqrt power etc If desirable the range that should be fitted can be constricted by clicking the Mouse on the start and end points On the right the order of the polynomial can be selected max 9 E Curve analysis E 10 x Projection Polynome PE ReScale Graph options Copy graph Copy results Zoom fitrange urrent vs time TAM order e zi Potential vs time Scan 1 Current vs Potential swap axis A 0 1 875E 02 A 1 1 573E 05 Mrs Potential 2 3 002 07 linear 3 1 350E 08 A 4 2 952E 12 i 0 0 A 5 3 536E 15 A B 2 357E 18 muligi 1 0 A 7 8 297E 22 A 8 1 185E 25 Horizontal time Cor Coef 0 9233 linear E k 0 0 T multiplier 1 0 S o tL i Subtract fit time ks Restore v Click mouse to set fitrange to 86 7 6 11 Electrolysis report From the Analysis menu in the graphic toolbar an Electrolysis report can be generated It will display the passed charge and current Also it will report the numerical values for Total Charge and Netto Charge The Netto Charge is defined as the Total Charge corrected for the Ba
95. ell as in Method mode All internal dummies are measured in the 2 Electrode configuration The external cell is disconnected while internal dummies are measured Therefore the cell cable does not need to be connected The internal dummy cells are used for calibration of the instrument or for performance tests see Test 1 Internal dummy cells are not available for the Ivium n Stat 2 14 Testcell1 module The instrument is delivered with a standard testcell TestCell1 It has six 4 mm sockets that correspond with the cell cable leads Each lead should be plugged in before measurement The testcell contains a number of resistors e 1 kOhm between CE and WE S is connected to WE RE is connected via 100 ohm to CE WE2 is connected via 100 kOhm to CE GND is connected to the internal shielding of the testcell box The TestCell1 is used for testing the instrument in combination with the cell cable see Test 2 28 2 15 Test 1 internal dummy 1 The cell cable does not need to be connected for this test this test is not available for the Ivium n Stat Start the instrument as described go to Method mode and load the measurement procedure TEST 1 imf that was supplied by the manufacturer standard C lviumStat datafiles Measurement procedures can be loaded with the Load method function from the File Menu Press Start and the instrument starts the measurement When completed the result should look like the plot below 3 IviumStat Contr
96. ertex 2 and back to start N scans Number of cycles to be executed 1 to 65535 for Standard mode At HiSpeed mode the maximum is limited by 32678 datapoints Scanrate Slope of the potential scan in Volts second The sample rate equals scanrate E step Iscanrate Slope of the current scan in Ampere second The sample rate equals Iscanrate l step Alpha During digitally produced sweeps e g in LSV and CV the potential current ramp is generated in step increments in a staircase shape This compares with the smooth analog shape of a True Linear sweep The standard practice for staircase sweeps is to sample the measured variable current for chrono amperometry potential for chrono potentiometry at the end of each step increment However in some cases a different sampling point is required for the measurement Hence the parameter alpha is used to indicate the fraction of the step at which sampling occurs For example alpha 1 the default setting means sampling at the end of each step whereas alpha 0 5 is halfway along and so on In practice the effect of alpha depends on the object under test For a pure resistor alpha variations have no effect but for systems with a capacitive component strong variations can be observed For the staircase techniques of LSV and CV in Advanced mode at Standard speed the parameter Alpha can be activated When checked a value from 0 125 to 0 625 can be entered The resolution for alpha is 0
97. es automatic saving of results create loops for repetitive tasks switch the multiplexer or MultiW E32 to fixed channels or to the loop index variable set the digital and analog outputs wait for a HI or LO level on the digital input set delays and program a schedule etc ee Ivium Batch language has a number of commands that may contain parameters to be manipulated the operator LoadMethod M A M Load method file from isk method file from disk Methodfile Filename of parameter file to be loaded ExecuteMethod Executeloaded method OverwritelfExists If left unchecked a unique filename will be generated by appending _ where is an increasing number If executed within a Loop the loopindex will be appended to the filename as L ClearGraph Clear plot before scan starts This is useful when different data are plotted i e CV and impedance Create a repetitive loop The number of loops is unlimited Nesting is allowed up to 32 levels deep Number of repetitions to the loop index to the loop index LoopEnd Set the end of the loop Each Loop command must be matched with a LoopEnd command method Textual expression of the parameter name 63 ValueText Textual expression of the parametervalue The format of the supplied value must correspond with the type of the selected parametername If the selected parameter is a checkbox a value of
98. es used in the frequency scan max 255 Actual frequencies will be calculated from a logarithmic spread between start and end frequency A pop up window allows frequencies to be configured 124 Frequency range min 10uHz max depends on instrument Before 2010 2 MHz After 2010 CompactStat 3MHz IviumStat 8MHz Ivium n Stat 250kHz Specifications subject to change The applied frequencies are derived from the main 8 MHz oscillator 8 MHz n An advanced software algorithm is developed for high resolution The applied frequency resolution is finer than 0 05 for the whole applicable frequency range The resolution is defined as the smallest possible separation between 2 applicable frequencies Note that the frequency resolution is not the same as the applied frequency accuracy Frequency resolution is defined as the smallest possible separation between 2 applied frequencies whereas frequency accuracy is the accuracy of each frequency point For all software versions with IviumStat CompactStat the frequency accuracy is better than 100ppm 0 01 for 10degC to 70degC Frequencies Single sine Single sine application of one frequency sine wave at a time Frequencies Multi sine MultiSine applies multiple sine wave frequencies simultaneously and the corresponding impedances are collected in a single measurement For measurements at lower frequencies this can decrease measurement time considerably and minimize artefacts caused by to t
99. es with identical structure same Estart Estep Vtx1 Vtx2 The Subtract overlay function also works with identical datafiles loaded from memory into the scan and overlay panels 7 5 6 Add overlay With this function the operator can add the scan in the Overlay panel to the scans in the Scan panel Note that this function can be applied repeatedly each time it is activated the overlay will be added to the scans The scan to be added should be saved as a normal datafile idf and loaded as the first overlay After recording the new scan you can select Add Overlay 1 from the Edit menu The overlay will be added to all scans However it only works for datafiles with identical structure same Estart Estep Vtx1 Vtx2 The Add overlay function also works with identical datafiles loaded from memory into the scan and overlay panels 7 6 Analysis The graphic toolbar Analysis will open a dropdown menu that allows the operator to execute a number of analysis options These analysis options are available when relevant to the data in memory Equivalent circuit equivalent circuit analysis for impedance measurements Corrosion rate analysis of corrosion rate for LSV Peakfind automatic will automatically draw peaks Peakfind advanced will allow operator to identify and analyse peaks Clear peaks will clear peaks that were drawn earlier from peakfind Electrochemical noise will allow analysis of electrochemical noise data
100. esult graph sheet depending on the electrochemical method running some commands may be available i e to pause the ongoing scan Note that when the IviumSoft is closed the method parameters of the last method that was used are in active memory and will show when the IviumSoft is started again 36 4 2 Sequence of a measurement After the Start button has been pressed a sequence of events is started e first the pretreatment stages are executed if the number of pretreatment levels gt 0 e thereafter the OCP is determined if that option was activated e thereafter the equilibrium stage is applied if the equilibration time gt 0 The equilibrium potential is equal to E_ start e thereafter the actual measurement technique is applied LSV CV etc 4 3 Method sheet The Method sheet contains all parameters to set up an automated measurement This is the normal way measurements are conducted Please note that the settings on this sheet are not related to the direct control settings From the top Method history list quickly select a predefined measurement protocol that was stored before Method tree select the measurement technique from a structured list You can expand nodes by clicking on the boxes Method parameter grid set the values of each method parameter e The first column lists the parameter name If a parameter contains subparameters a symbol will be displayed in front of it When such a parame
101. example a linear distribution is applied from 1V to 1V Suppose the basepotential is scanned from 0 to 1V the WE 1 will sweep from 1V to 2V and WE 32 will sweep from 1V to OV 134 WE32_offsets E imi xj Select offsets Single value offset 3j 0 0000 y 32 offset values wy Linear distribution offset 1 10y oftset 32 10 y no offsets To show the scans for all WE s in the graph tick the box WE32_allchannels in the method parameters Note that when a MultiW E32 is used there is no primary base electrode For most applications the offset potentials would remain at OV because potential manipulations are more conveniently done by setting the base potential WE32 allchannels To acquire measurement data from all 32 channels of the MultiWE32 simultaneously It is available for the following techniques LSV standard CV standard and CA standard When checked the currents for all 32 working electrodes are recorded Each scan will therefore produce 32 curves Individual curves can be stored with save data while all 32 scans can be stored in a single file with save dataset Report Data report add notes to datafiles The operator can include notes and extra information about the experiment in the datafile When pressing the Report button a window opens where notes can be typed in the Remarks tabsheet Additionally a Process Report
102. from the Ivlib onto the Block Diagram of the VI that you are building e Mum driver 1 0 vi Block Diagram j 8 IVIUM remdriver dll IV Ndatapoints vi IV close vi Iv connect vi IV getadc vi IV getcellstatus vi IV getcurrent vi IV getcurrent WE2 vi IV getdata vi IV getdevicestatus vi IV getdigin vi C o IV getpotential vi e IV open vi IV read SN vi m File Edit View Project Operate Tools Window aln e eike before terminating this VI eae DEPPA Close Ivium Driver When a VI is build to control an Ivium device make sure that the driver is opened before operating the device and closed again before the VI is stopped Boundary conditions Some of the settings of the Ivium device that can be controlled via Labview change an actual setting in the lvium device like for example the current range When one or some of these settings are changed outside Labview i e in the IviumSoft or by the device itself when for example using the AutoCR setting in a method this change of setting is NOT read back into Labview That implicates that the value in the User Interface in the Front Panel may not be the actual setting anymore 138 When using the method mode a number of strings file names and locations are communicated to the IviumSoft software These can only be communicated when the device is CONNECTED If the device is not connected it will result in an error
103. ge int Set current range 0 10A 1 14 etc IV setcurrentrangeW E2 int Set current range for BiStat 0210mA 1 1mA etc IV getcurrent double Returns measured current IV getcurrentW E2 double Returns measured current from WE2 bipotentiostat IV setfilter int Set filter IV setstability int Set stability 137 IV_bistat_mode int Select mode for BiStat IV_setdac int double Set dac on external port IV_getadc int double Returns measured voltage on external ADC port IV setmuxchannel int Set channel of multiplexer IV setdigout int Set digital lines on external port IV getdigin int Returns status of digital inputs from external port IV setfrequency double Set ac frequency IV setamplitude double Set ac amplitude METHOD MODE IV readmethod char Loads method procedure from disk IV savemethod char Saves method procedure to disk IV startmethod char Start method procedure IV savedata char Saves actual result data to disk IV setmethodparameter char1 char2 Modify method parameter IV Ndatapoints int Returns actual available number of datapoints indicates progress during a run To use the functions in Labview open the IVIUM remariver lvlib in the Labview directory in the getting started window of Labview Then drag the desired function
104. gram save as Zplot file exports a datafile so this can be read by the Zplot program Copy graph copy current graph to clipboard Copy fit parameters copy fit parameters to clipboard Swap Z for Y changes Z into Y in plot Copy simulated copies simulated data to measurement result Subtract as parallel components subtract the entered equivalent circuit off the data as parallel components to analyse remaining data Subtract as series components subtract the entered equivalent circuit off the data as series components to analyse remaining data Options Fitting options Optimize select which measured parameter should be used to fit best on the theoretical model ZlandZ2 Zabs Z1 Z2 phase Error weight equal for each point to minimize the absolute errors proportional to absolute impedance to minimize the errors relative to measurement accuracy proportional to value to minimize the relative errors allow negative values whether components R C etc can have negative values 71 On the left middle the graphical equivalent circuit editor is shown It contains a toolbar with the selectable electrical components e R resistor e C capacitor e W Warburg diffusion impedance e Q Constant Phase Element CPE e L inductance e T hyperbolic tangent e O hyperbolic cotangent e G Gerisher impedance e horizontal conductor e del delete element to remove components from the circuit To place a new element click the
105. h level The curves are listed in the Legends pane as level 1 level 2 etc and can therefore be selected saved and analysed separately To activate level separation check Levels separate in advanced mode This feature cannot be used in combination with Cycles separate Stages Indicate how many stages levels are sequenced in MixedMode 0 to 255 A pop up window allows each level to be specified individually In the pop up window the number of levels can be changed by pressing the up down arrows For each level E control I control Open cell can be selected from the drop down menu When a level is selected the parameters for that level can be entered in the Properties for Level window Cycles Number of times that the whole sequence of levels is repeated range 1 655535 only available in Standard mode This option will allow multi cycle experiments such a multiple charging and discharging of batteries supercaps Please see the Cycles separate option to select how cycles are displayed Also see the Thresholds option to select dynamic cycling limits 121 Continuous cycling For ChronoAmperometry and ChronoPotentiometry in standard mode and in MixedMode the scans may be repeated continuously When the parameter Cycles that normally is used to define a finite number of scans is assigned the value 0 it is translated to infinite Thus the cycling will never stop Note that the only way to stop cycling is to press
106. has a very high reliability This button can be used as an EMO or panic button to avoid dangerous situations During normal operation this button should not be used and the red light should be off Of course measurements are not possible while this button is pressed lvium n Stat At the back plane of the Ivium n Stat two 4mm sockets are available EMO red and GND green The EMO bus is a 0 to 5V compliant input and unconnected it pulls up to 5V which means EMO not activated When the EMO is pulled to GND i e via a wire bride it will actively disconnect the sModules of all channels in the frame and generate a shutoff event that will stop all running methods The EMO function operates independently from the software firmware The cells cannot be activated until the signal on the EMO bus is removed For both the IviumStat and Ivium n Stat the EMO function is also used for instrument restoration i e to recover from a firmware upgrade mishap 9 21 Connectors Cell connector Type 1 DB9 female S shield 4 5 WE2 S shield 7 TS E S RE shield Cell connector Type 2 HD15 female Pin Function Colour shield WE WE2 oo red 3 Reservedgnd 6 y 5V 8 9 5V 0 Reservedsel Reserved data out_ Reserved data in 13 S sheld Fs 14 REsheld 116 MultiWE32 cable assignment Note both RE shield leads are present in the
107. he Testcell1 e Connect the electrode cable to the HD15 connector at the front of the instrument e Connect the 4mm bananaplugs to the TestCell1 included in shipment o Gnd ground green o WE1 WE2 Working Electrode red WE2 refers to the Bipotentiostat o CE Counter Electrode black o RE Reference Electrode blue o S Sense white e Onthe Method sheet a measurement technique can be selected from the method tree and configured on the parameter grid e Measurements can be started with the Start button and aborted with Abort button e Results can be saved with the File menu item Save data Measurements with electrochemical cells e Electrode connections can be made similar to the TestCell1 described above o Gnd may be connected to a shielding body such a Faraday cage If possible connect gnd to a low impedance grounding point to avoid noise o WE1 WE2 should be connected to the electrode under test 0 CE to be connected to the electrode that delivers the counter current o RE to be connected to the electrode that maintains a fixed potential In 2 electrode configurations this is connected at the same point as CE o S allows for a secondary RE in a 4 electrode configuration in 2 or 3 electrode configurations this is connected at the same point as WE1 e Onthe Method sheet a measurement technique can be selected from the method tree and configured on the parameter grid e Measurements can be started with the St
108. heet file Start Chart Jo Y Scale Range Maximum cns Fo y 139 Set up of Ivium Driver 1 0 The lvium Driver 1 0 has been set up using a flat sequence to ensure that the order of events is correct Ivium Driver 1 0 set up e The first operation is to open the Ivium remdriver dll so the IviumSoft and device can be operated e Next a check is performed to see whether the IviumSoft is running If not the VI is stopped If IviumSoft is running a check is performed to see if the device is connect and if so it will be disconnected e Third sequence is the actual operation of the Ivium device either in direct mode or in method mode e Finally upon closing the VI the Ivium device is disconnected and the lvium remdriver dll is closed Operating sequence of lvium Driver 1 0 Block Diagram set u To ensure the continuance of operating the Ivium device the actual running sequence of the VI is incorporated in a while loop However before the while loop commences an initiation of the default values is executed for all the controls for the direct mode operation This has been done to ensure that the values shown in the user interface or Front Panel are the actual values After this has been done the while loop starts E Reset Connect button Disconnect Connect H 2 m 78 Direct control ethod control Device Status indicator 22 mm 78 fo pvalue 140 First in the while loop refer to Block Diagr
109. ialsweep is applied identical to LinearSweep Standard However instead of recording the current at the end of each interval the current is integrated during the whole interval and divided by the interval time This results in the average current during each potentialstep In some situations this technique yields the same results as when using a True Linear Scan technique This particular technique can be used when the standard staircase method does not give the desired results such as experiments involving time dependent phenomena such as film formation or electrochemical nucleation The CurrentAveraging method is more sensitive to capacitive currents When that is undesirable the standard variant is more appropriate 48 5 3 LinearSweep TrueLinear A continuous linear analog potentialsweep is applied instead of the standard staircase The E_step variable defines the interval time The interval is defined by E_step scanrate The recorded currents are measured at the end of each interval Standard mode allows for interval times down to 0 002 s for shorter intervals use HiSpeed mode 5 4 LinearSweep Galvanostatic This is similar to the Standard potentiostatic sweep but now galvanostatic A linear currentsweep is created by updating the current with step at each interval so that a staircase scan is applied to the cell with a defined scanrate The interval is defined by step scanrate The recorded potentials are measured at the
110. ignal is used as X which is the light intensity here instead of the cell current Note that the galvanostat current may be set to OCP conditions 120 but it may also be operated at other currents such as maximum power point WE32 offsets Applying a potential with the MultiWE32 By default the electrodes of the MultiWE32 act similar to a Bipotentiostat in Scanning mode This means that the potential that is selected by the user is applied to all working electrodes at the same time For example when a CV is run all 32 working electrodes will be sweeping at the same speed As an advanced parameter feature it is possible to give each working electrode an individual offset This offset is subtracted from the base potential Offsets are intended to apply fixed potential differences between the 32 working electrodes which remain constant during a scan Note that the value for the real time potential in the software measurement window and the graph axis will only show the base potential the potential potential range selected by user thus this potential does not include the offset part The offset potentials for each WE are stored in the datafile method parameters The offset potentials can be defined in the Method parameters selecting We32 offset will open a dialog screen that will allow the operator to set independent offsets for each electrode either manually or with a distribution function within a range of 2 V to 2 V In this
111. ill construct a full peak while front flank will only use the rising part of the peak and rear flank only the descending flank Whole peak is best suited for peaks with clearly defined flanks and horizontal baselines Front peak is appropriate when the tail of the peak is smeared out or has a steep baseline or is close to the scan boundaries as is often the case in Cyclic Voltammetry 75 Find Method 1st derivative 2nd derivative Selects the control variable for the method that is used by the algorithm that determines where peaks start and end The 1st derivative method is more sensitive to small peaks but only works well when the baseline is nearly horizontal The 2nd derivative technique can cope with sloped baselines as is often the case for fast scan techniques as Linear Sweep or Cyclic Voltammetry Height mode proportional absolute Refers to the minimum height Minimum height in absolute height mode it defines the absolute minimum height for a peak while in proportional mode it defines the minimum fraction from the maximum value in the whole scan Width mode proportional absolute Refers to the minimum width Minimum width in absolute width mode it defines the absolute minimum width for a peak while in proportional mode it defines the minimum fraction from the range of the scan Sensitivity number of consecutive points that must fulfill the begin amp end criteria for a peak to be accepted A higher number usually
112. ime variable impedances In this setting 5 frequencies within a single decade are combined By using the odd harmonics 1 3 5 7 9 Hz etc and carefully controlling the relative phase of these frequencies it is possible to minimise the total combined amplitude for a given effect Frequencies Start Start frequency Frequencies End End frequency Frequencies Frequencies each decade Can be used to automatically apply an evenly distributed number of frequencies per decade Frequencies Amplitude Amplitude of the applied ac signal Standard 0 0001V 1V Galvanostatic 0 001mA 1A Frequencies manual override Allow manual editing of frequencies and amplitudes If override is disabled standard the amplitudes are fixed and the frequencies are automatically calculated from the Start and End frequencies If manual override is activated the operator can change any frequency and amplitude value independently 125 Filter Signal measurement filter setting 1MHz 100kHz 10kHz 1kHz 10Hz or automatic In Basic mode automatic is applied This filter is applied to the signals to be measured current potential bipotentiostat or external X Y inputs In automatic mode the system determines the most appropriate setting from the applied samplerate DC or applied frequency impedance method Overriding the automatic setting should be done with care because it may result in signal deformation Especially for the impedance methods it is recommende
113. ing 2 reference electrodes e connect WE er to the electrode to be studied e connect CE to the counter electrode e connect RE to the reference electrode near the counter electrode e connect S to the reference electrode near the working electrode For an experiment with the bipotentiostat e connect WE S RE CE as described above e connect WE2 to the secundary working electrode Only for the Ivium n Stat WE2 lead e connect WE S RE CE as described above e the sModule is not equipped with a bipotentiostat Its WE2 lead can instead be used to measure potentials relative to the S electrode for example from the CE or an additional reference electrode e in Direct mode the WE2 voltage sensor can be activated with a checkbox on the Extern tabsheet E at WE2 e inthe Method mode for techniques that measure potentials the WE2 sensor can be chosen instead of the electrode potential by checking the E at WE2 parameter 21 Special techniques Special techniques may require an alternative way of connecting the electrodes such as electrochemical noise measurements A standard noise measurement uses 3 electrodes 1 reference electrode and 2 identical working electrodes Connect these is the following manner e RE to reference electrode e WE S to working electrode 1 e Gnd to working electrode 2 Theory of operation The WE and CE leads carry the current while the RE and S measure the potential The instrument has a control loop that wil
114. ing of E and I up to 500 samples second simultaneously e Minimum current resolution 0 15 fA e Minimum potential resolution 40nV IviumStat 16nV CompactStat A standard noise measurement uses 3 electrodes 1 reference electrode and 2 identical working electrodes Connect these is the following manner e RE to reference electrode e WE S to working electrode 1 e Gnd to working electrode 2 56 The software can evaluate the recorded results automatically It is possible to perform the analysis in Time domain or in the Frequency domain Before an ElectroChemical Noise scan the voltage bias can be removed If the checkbox Remove DC initial is checked method parameters the initial voltage is measured and subsequently electronically subtracted from the cell potential before measurement This option can improve the sensitivity of ECN measurements because it will allow for a more narrow Potential range setting with a higher resolution 5 14 ElectroAnalysis Amperometric Detection During amperometric detection a potential is applied and the current is recorded The timebase of the experiment is set by the interval time 5 15 ElectroAnalysis Differential Pulse During differential pulse voltammetry a staircase scan is applied with a superimposed pulse at the end of each interval The current is measured before and at the end of each pulse from which the difference is displayed The operator can choose pulse time and height The
115. ing the graph colour and background as well as copying the graph to clipboard The buttons to the left allow additional data to be displayed Graphic toolbar Data is by default displayed 2D 3D and SDi display may also be chosen Clicking the Cor button after the measurement has finished will start the correction mode allowing the user to change individual data points X shows the primary data Ain ocp pre Q Rs Cs will all open a second graph that shows the corresponding data when available optional analog inputs ocp measurement before scan pre treatment data etc The Scale button allows the scale of the graph to be adjusted via the drop down menu clicking on the button itself will auto scale the graph Analysis will make a number of analysis methods available to the data in memory Edit will allow smoothing of the scan data The buttons on the top right of the graph activate different representations of impedance data The tabs Result graph and Result data on top enable switching between graphical and numerical representation of the scan data The E scan tab will show the data for analysis when an impedance scan method has been carried out 24 5 Legend panel 1 Scan shows the scans that have just been measured or loaded as data from memory Hide all Show all will respectively hide and show all scans In the list of scans below that checking unchecking the box next to the scan will show hide
116. ipheral port will be superimposed on the DC signal that is set in the Direct mode In method mode For using the AC input during a method go to the Options menu Settings In the Environment area check the box for AC input Now the analog or ac signal connected to pin 9 of the peripheral port will be superimposed on the DC signal that is set in the method parameters 101 9 Instrumental specifications 9 1 CompactStat lvium CompactStat specifications System Performance SSC Poeniostat CSCS Current feedback ohmic drop compensation n ohm current range 65 536 with n 0 to 65 535 Galvanstat J 3 O Potential ranges 1mV 4mV 10mV 40mV 0 1V 0 4V 1V 4V Impedance Analyser Ci Amplitude 0 015mV to 1 0V or 0 03 to 100 of current range 16 bit dc offset subtraction 2 dc decoupling filters Electrometer O Z O Z A O Peripheral connections ae ee AC out 0 5V sinewave 10uHz 2MHz variable attenuation Environment power requirements in USB powered mode USB port capable of 5V 500mA standard pc spec Specifications subject to change Ivium Technologies 2010 102 9 2 CompactStatPlus Same specifications as CompactStat except System Performance Pls Pua pones mI Potentiostat eee a Applied potential range 20 V 0 666mV res 10 V 0 333mV res a CCCII Galvanostat a ee Potential ranges 2mV
117. ircuit analysis 7 6 2 Corrosion analysis 7 6 3 Peakfinding and baseline correction 7 6 4 Peakfind automatic 7 6 5 Peakfind advanced 7 6 6 Clear peaks 7 6 7 Electrochemical noise analysis 7 6 8 Find levels 7 6 9 Solar cell report 7 6 10 Curve fit 7 6 11 Electrolysis report 7 6 12 Mott Schottky analysis Device maintenance Calibration Upgrading firmware Restore instrument Performance test 8 6 Pulse Generator 8 7 Current Interrupt 8 8 Software development driver DLL 8 9 Galvanostatic generation icw Amperometric detection with BiStat 8 10 Labview interfacing 8 11 lvium data file registration 8 12 Measurements using the peripheral port 8 12 1 Peripheral analog inputs 8 12 2 Analog inputs direct or via PPE 8 12 3 Analog inputs via PLT 8 12 4 Analog inputs via PDA 8 12 5 Using AC input 9 Instrumental specifications 10 Method parameters 9 1 CompactStat 9 2 CompactStatPlus 9 3 lvium n Stat 9 4 IviumStat 9 5 IviumStat20V 9 6 lviumStat XR 9 7 lviumStat XRi 9 8 viumStat XRe 9 9 viumBoost 9 10 PPE 9 11 PDA 9 12 PLT 9 13 BiStat 9 14 LinScan 9 15 MultiWE32 9 16 HiMux 9 17 Edoubler 9 18 CIM 9 19 ModuLight 9 20 EMO Emergency Off 9 24 Connectors Mode Title E start start E end end E step step DynamicVertexes DynamicVertexes max DynamicVertexes min Vertex 1 vertex 1 Vertex 2 vertex 2 N scans Scanrate Iscanrate Alpha 119 119 119 119 119 119
118. is plotted vs Z In 3D the frequency is on the depth axis Y Y Admittances Y is plotted vs Y In 3D the frequency is on the depth axis Z freq the Z is plotted with the left and the Z is plotted with the right axis Y freq the Y is plotted with the left and the Y is plotted with the right axis epsilon the 10log e is plotted with the left and the 10log e is plotted with the right axis the complex permittivity The permittivity is defined as Epsilon j Addmittance 2 pi freq CapO with j the complex variable freq the frequency and Cap0 the reference capacity This reference capacity equals the capacity of an empty cell and it should be defined by the user It can be changed in the Data Options method parameter on the Electrode tabsheet Tan d the Tan delta is plotted with the left and the Cs CO is plotted with the right axis the so called Loss Tangent The Loss Tangent is defined as the ratio of real and imaginary impedance Cole Cole plot the Y w is plotted vs Y w E I value correction when in the method parameter Data options an offset potential or an electrode surface area are entered the graph data can be updated for these values Ecor updata graph for E corrections Idens updata graph for electrode area current density 44 4 10 Result data sheet Here the results are shown in numerical form Result graph Result data Refresh Export r Show data selected
119. isualized in the Extra plot accessible via the graphic toolbars The measured OCP is also shown in the bottom status bar Apply wrt OCP monitor time Time s that OCP is monitored The potential that is reached at the end of this period is assumed to be the OCP Apply wrt OCP monitor interval Sampling interval s during OCP monitoring Apply wrt OCP Estart wrt OCP When checked the startpotential is defined relative to OCP When unchecked the E start is applied as a real potential Apply wrt OCP Vtx End wrt OCP When checked the Vertex and End potentials are defined relative to OCP When unchecked these are applied as real potentials 127 Apply wrt OCP Estandby wrt OCP Determines whether the stand by potential needs to be applied with respect to OCP When checked the stand by potential is defined relative to OCP When unchecked it is applied as real potential Apply wrt OCP Record real E When checked the real potentials are displayed and stored When unchecked potentials relative to OCP are displayed and stored To improve clarity the OCP value is shown on screen in the bottom status panel Remove DC initial Before an ElectroChemical Noise scan the voltage bias can be removed If the checkbox Remove DC initial is checked the initial voltage is measured and subsequently electronically subtracted from the cell potential before measurement This option can improve the sensitivity of ECN measurements because it will allow fo
120. ital input output signals e Cell connector 15p HD connector that fits the supplied electrode cable e Multi color LED status LED between both connectors Status LED blue blinking white idle with no pc client connected green blinking white pc client connected Direct mode cell off red blinking white pc client connected Direct mode cell on red continuous pc client connected Method mode Notes on the Ivium n Stat The lvium n Stat multi channel potentiostat galvanostat is operated in much the same way as the lvium single channel instruments However there are some subtle differences e The lvium n Stat uses USB drivers that are standard included in MS Windows Just plug the system in a USB port and it is ready to go e Ina way the lvium n Stat can be regarded as a number of separate lvium instruments in one single box each channel sModule can be operated as a separate instrument see Starting the Ivium n Stat e The peripheral connector of the sModule has 15 pins instead of 37 pins The sModule has fewer signals than the lviumStat Also note that the analog input range is different e As opposed to the lviumStat and CompactStat instruments the Ivium n Stat sModules are not equipped with internal dummy cells Also the 2 electrode mode is not available If only a WE and CE are present simply connect the RE blue to the CE and the S white to the WE 10 e The sModule is not equipped with a bipoten
121. ive If this datapoint was obtained in an overload situation the status would indicate this Furthermore the original date and time of acquisition are shown mm dd yyyy hh mm ss Note that the display in Recall mode is different from the AC signal monitor shown during the EIS scan Lower panel Freq actual applied frequency CR actual current range Zabs value for Z abs Status status of overload situation for this datapoint Phase actual phase angle Date time of actual data point 4 Method control 4 1 Method control From the Method control panel the operator can define a technique or measurement protocol on the Method sheet When the Start button on the taskbar is pressed this measurement protocol is executed In this state the software takes control over the instrument Method control This will last until the measurement is completed or aborted by the user During Method control the Direct control functions are not available neither are some filing and analysis functions When during Method control the Abort button is pressed the measurement is halted immediately However in some cases there maybe a quantity of data pending in the buffers which has to be processed and it may take a while up to a few seconds before the software appears to return from method control During method control while the method is running the number of commands that can still be accessed is limited However at the bottom of the r
122. l codes are given in table 1 above Note that these codes are according to the electronic standards i e counting from right to left The digital outputs can be accessed in the lviumSoft from the Direct control tab in the Extern tab below As an example to choose the color white the digital code is IIO This means that Dig out 3 and Dig out 2 need to be checked and Dig out 1 is unchecked r Analog output chi 1000 V che 000g V Digital output I Dig out 1 v Dig out 2 Dig out 3 peni iesu Intensity The intensity of the light is controlled via the Analog output This output has a range of 0 4V which corresponds to a light output of 0 100926 For example enter 1 V into the ch1 field see above and press ch1 to apply this voltage This will effectuate a light output of 2596 of the chosen color Modulation The modulation of the light is controlled via the AC output of the peripheral port The AC output can be accessed in the IviumSoft from the Direct tab in the AC tab below The AC voltage has an amplitude of 0 1V which corresponds to a modulation of 0 100 The speed of modulation is controlled by the frequency For example if the analog output ch1 is set to 2V and when 2 is entered in the field for Frequency and 0 5 in the Amplitude field upon pressing Apply the light will start modulating between 100 intensity and 0 intensity with a frequency of 2 cycles per second 1
123. l keep the potential of WE near the gnd potential while applying a signal to CE In galvanostatic mode the instrument will apply a defined current through CE and thus WE In potententiostatic mode the instrument will force a current through CE amp WE so that the potentialdifference S RE is a defined value There are distinct advantages of using 4 electrodes instead of 2 because the separate current less measurement of potential eliminates losses over the cable e any cable has an ohmic resistance that causes a voltage drop at higher currents A good standard cable may add approximately 0 2 ohm that amounts to 200 mV loss at 1 A In such cases a 4 electrode configuration is recommended e anycable also adds inductance and parasidic capacitances These may become dominant at higher frequencies Therefore also for high fequencies the 4 electrode configuration is recommended 22 2 7 Screen layout Anabis Edt gt mw As Cel z z v v Ziea Yea epston Tantai Cole F CyckcVokammetry a Transients 4 Electroanalysis 4 Impedance CEACE op Current A 1 Device amp Software control On top the mainmenu is shown see also later in this chapter e File to load save method and datafiles e Options setting the device and module options incl FRA options e Tools tools for device maintenance upgrades calibrations and special functions e Help information how to us
124. l on all 8 analog inputs will be measured when the button Read analog inputs is pressed analog output set the potential of the 2 analog output ports enter the value in the box and click chi or ch2 to activate the value for that channel digital output set the levels of the 3 digital output ports by checking un checking the adjacent box digital input read the levels of the 2 digital input ports click the Read button Ext ACin 1 0 X when checked the analog or ac signal connected to pin 9 of the peripheral port will be superimposed on the DC signal that is set in the Direct mode multiplied by 1 IR comp to configure the online IR correction by current feedback Clicking Calculate will give the maximum compensation possible in the selected current range Entering the desired value in the box and clicking Apply will apply the IR compensation PDA when one or more PDA modules are used in this tab page the values of the analog inputs can be read 33 3 2 SigView The Signal Monitor window is accessible by clicking on SigView in the top function bar advanced parameters see Screen layout 1 In Direct control mode the signal can be observed in an oscilloscope type of screen current and potential vs time This can help to diagnose connection problems and find sources of noise The operator can manipulate the timebase in direct mode Signal Monitor EE xd ide Rescale Options Copy Freq
125. le scans are displayed it is possible that each was measured at different conditions The method parameters of each individual scan can be viewed by a right click of the mouse button while the mousepointer is on the scan in question in the Legend panel A form with the corresponding data will pop up In this form it is also possible to edit the Title of this single scan retype and press the Change button Additionally the specific parameters of the selected plot will be copied into the Method parameter panel when the CTRL key is pressed while the scan was selected keep the CTRL key pressed and click on the scan name in the Legendpanel Note that this will change the active Method parameters If thereafter Start were pressed it would start a scan using the parameters of the selected scan However the use of the CTRL key should avoid unintentional modification of the active parameters The latter function can also be used after reading a previously recorded Dataset 41 Chan panel when recorded shows the results of the analog input channels of the peripheral port when no analog inputs are entered in the method parameters this tab will be invisible e Channel list displays a checklistbox of all available channels Channels can be made in visible by un checking the corresponding box e Option manipulate plot appearance titles oackground colors etc e Data appearance manipulate appearance of the data lines symbols colors styles etc
126. lick over the graph will allow the graph options to be selected resulting in the 2 windows shown below 3D parameters only show when 3D graph is selected display Title Scan 1 X text Potential Y text Current v Axis arid Axis Color Text Color Background Color aradientfill Data Bckg Color IV draw databg loado poris savEeoptorns 4 6 Graph popup menu When the mouse is moved across a particular graph and the right mouse button is pressed a pop up menu appears Autoscale performs autoscale on all axis Graph options manipulates plot appearance titles background colors etc Data appearance manipulate appearance of the data lines symbols colors styles etc Scale X axis scale the horizontal axis manually or automatically Scale Y axis scale the left vertical axis manually or automatically Scale Z axis in 3D plots scale the depth axis manually or automatically in twin axis plots scale only the right vertical axis manually or automatically Copy graph copies graph to clipboard e Print graph send graph directly to printer The standard Windows printer dialog will appear at which the printer amp properties can be selected e Set phase opens a window to change the phase for phase sensitive AC voltammetry e CV plots opens a separate graph where data for cyclic voltammograms can be represented by users choice vs E vs time E vs time a right mouse click will allow
127. lt the IR drop is calculated see graph below 94 Rescale Options Copy plot Copy result v Current interrupt Current interrupt Rr Oj x interpolation C linear 10 esee exponential data IGS TRE 0 8 all v pnts e tau E D13E 04 s S E o 0 4 tL 0 2 D 200 400 600 800 time us Period 1 0 ms Close 8 8 Software development driver DLL You can develop your own software to control the IviumStat and CompactStat instruments Developing programs is easy because lviumSoft will do all the hard work The supplied driver will allow you to integrate the functionality in your own program You can still use the convenience of the IviumSoft software and program your specific tasks with a few program lines in the desired language VB Delphi C Labview etc Advantages e Faster development of applications than programming from scratch IviumSoft takes care of most overhead communication error handling graphic plotting datastorage etc You may mix modes for example first set the device in a desired state with IviumSoft and let your own program take control from that point e More flexible than using a scripting language You can use all the programming power of the higher programming language of your choice It is possible to customize data processing or react on specific results and events e Control multiple lvium devices at the same time and simultaneousl
128. lues or convergence might not be reached For some predefined circuits the software will calculate such values for you when the Calc Startvalue is pressed before the Fit is executed The Fit range the frequency range may be limited by selecting the start and end index of the included frequencies Simulate will draw the impedance curve using the present equivalent circuit and the parameter values in the parameter grid Execute will start the fitting engine that optimizes the parameters in the parameter grid on the present equivalent circuit Stop will stop an ongoing fitting process Accept closes the equivalent circuit fit module The present model and parametervalues will be included in this data If this data is stored later it will include the impedance analysis When the equivalent circuit fit module is started again with this data the same results will be shown Cancel closes the equivalent circuit fit module without saving the results The present model and parameter values will not be included in this data 72 Data The calculated parameters for the equivalent circuit can be exported from the Equivalent circuit calculator From the Edit menu choose Copy fit parameters This will place the results in the clipboard to be exported to other applications On the Data tabsheet of the Equivalent circuit calculator the numerical data can be accessed Phi Z phase impedance data Z Z complex impedance data
129. mask IV getdigin int Returns status of digital inputs from external port int is bitmask IV setfrequency double Set ac frequency double in Hz IV setamplitude double Set ac amplitude double in Volt ae ee NEA EMEN UR IT IV getcurrenttrace Returns a sequence of measured currents at defined samplingrate int double double npoints interval array of double npoints lt 256 interval 10us to 20ms IV getcurrentW E2trace Returns a sequence of measured WE2 currents at defined samplingrate int double double npoints interval array of double npoints lt 256 interval 10us to 20ms IV getpotentialtrace Returns a sequence of measured potentials at defined samplingrate 7 int double double npoints interval array of double npoints lt 256 interval 10us to 20ms IV_setmuxchannel int Set channel of multiplexer int channelnr starting from O default Select active WE32 channel chan Set WE32 offset chan value value 2 to 42V Usechan Otoapplythesameoffsettoallchannels with Nchan the number of channels 1 32 fhataremeasurdsimultaneousy O o i O METHOD MODE O IV savemethod char Saves method procedure to disk with char as filename IV startmethod char Start method procedure If char is empty then presently loaded IV savedata char Saves actual result data to disk with char as filename IV setmethodparameter Modify method parameter with char1 parameter n
130. me Pulse amplitude Pulse height 1 mV to 1000 mV Sign of pulse is defined by scan direction SQRWYV frequency Frequency of the square wave signal 2 Hz to 1kHz in Standard mode Up to 50 kHz in Hispeed mode 122 Phase sensitive Apply Y N phase sensitive current detection with AC Voltammetry If not activated the displayed result equals the RMS value of the current When Phase selective is turned on the result will show the current component detected at that phase angle for example at 0 degrees the ohmic component will be displayed Note that in AC Voltammetry both RMS and phase angle are collected and stored It is thus always possible to change the detection angle of existing measurements afterwards Phase sensitive phase Phase angle for Phase sensitive AC Voltammetry 2nd Harmonic Detects the AC current at double the excitation frequency This is useful to investigate non linear phenomena Please note the special relation with the excitation amplitude Deposition time Time duration deposition stage during which E_start is applied Current stripping Y N when current stripping is off the cell is turned off during the stripping stage i e no electrical current flows This is sometimes called Chemical stripping When current stripping is turned on the instrument is configured as galvanostat and the electrode is stripped at a constant applied current Current Stripping Stripping current Constant applied current during electr
131. n layout File menu Options menu Tools menu Help menu About Internal dummy cells Testcell1 module Test 1 internal dummy 1 Test 2 standard testcell Test 3 standard testcell amp BiStat Direct control SigView Method control Sequence of a measurement Method sheet Result graph sheet Graph options Graph popup menu Legend panels Data appearance Graphic toolbars Result data sheet E scan sheet LinearSweep Standard LinearSweep CurrentAveraging LinearSweep TrueLinear LinearSweep Galvanostatic 6 BatchMode 7 Data analysis and reporting 8 Special functions 7 6 Cyclic voltammetry CyclicVoltammetry Standard CyclicVoltammetry CurrentAveraging CyclicVoltammetry TrueLinear CyclicVoltammetry Galvanostatic Transients ChronoAmperometry Transients ChronoPotentiometry Transients MixedMode Transients Electrochemical Noise ElectroAnalysis Amperometric Detection ElectroAnalysis Differential Pulse ElectroAnalysis Square Wave ElectroAnalysis AC Voltammetry ElectroAnalysis Potentiometric Stripping ElectroAnalysis AC detection ElectroAnalysis Normal Pulse Voltammetry Impedance Constant E Impedance Constant Impedance PotentialScan Impedance CurrentScan Current density graphs Reference potential graphs Scaling and zooming Clipboard functions Edit 7 5 1 Edit data 7 5 2 Smooth all data 7 5 3 Subtract ohmic drop 7 5 4 Average scans 7 5 5 Subtract overlay 7 5 6 Add overlay Analysis 7 6 1 Equivalent c
132. n min E delta 131 Data reduction min delta 131 Automatic save 131 Automatic save filename 131 Automatic save save every 131 Automatic save on completion 131 AUX 132 AUX purging period 132 AUX Stirrer pretreatment 132 AUX RDE speed 132 AUX New drops at start 132 AUX InvertDig polarity 133 Modules 133 Modules PDA 133 MeasConfig 133 WE32 offsets 134 WE32 allchannels 135 Report 135 Appendix 1 Labview Interfacing 137 1 Order of communication hierarchy 137 2 Directions for use 137 3 Example lvium Driver 1 0 139 1 Introduction 1 1 IviumSoft The lviumSoft software can be used to control one or multiple CompactStat IviumStat or Ivium n Stat instruments by means of a Personal Computer The PC is used to specify the parameters of the measurement to display the measured curves and calculate the results of the measurements Each instrument contains a microprocessor and a potentiostat galvanostat which controls the potential or current applied to the electrodes and measures the current or potential response To ensure that the instrument s internal microprocessor gets enough time to run its start up procedure there should be at least 10 seconds delay between powering up the instrument and connecting it in the IviumSoft An instrument can be used with electrochemical sensors or electrochemical cells with 4 electrodes working electrode sens electrode reference electrode and auxiliary or counter electrode In the so called two elec
133. nals are referred to the local sModule gnd In floating mode the peripheral port should only be used with floating equipment 3 Range 4V 5 Function Remarks aN o e e A eee Ranges 4AV 7 GND o Ac output 10 11 O yi 12 13 14 Eat 0 00 00 000 0 o Frame GND f ConnectedtonStatcommon GND CompactStat power connector 5 5mm bus female 2 1mm inner 5 5mm outer diameter recommended shaftlength 12mm e center pin should be 5V 0 2V max 1A Plus module power connector 5 5mm bus female 6 8mm diameter e center pin should be 12V 0 2V max 1A 118 10 Method parameters Mode Standard HiSpeed mode Standard mode allows sample rates up to 500 samples s during Standard mode sampes are directly communicated to the pc Standard mode allows application of more features automatic current ranging etc HiSpeed mode allows sample rates up to 100 000 samples s during a HiSpeed expertiment the data is stored inside the instrument and communicated after experiment completion Maximum available datapoints 8192 32768 for CV methods Note that in HiSpeed some features are unavailable such as AutoCR Title Title that will appear above the result plot E start Start potential of the scan start Start current of the galvanostatic scan E end End potential of the scan lend End current of the galvanostatic scan E step Potential step size I step Current step size DynamicVertexe
134. nced and press Next c Atthe next screen select Search for the best river in these locations check Include this location in the search press the Browse button and locate the driver standard CAIVIUMSTATNVIUMDRIVERS and press Next d You will get a message that the this driver is not Signed Press Continue Anyway e Press Finish Driver installation Windows Vista and 7 Windows Vista or 7 may not successfully automatically install the driver Windows will give a notification when this occurs In this case the driver needs to be installed manually 1 For CompactStat first connect the power adapter to the CompactStat device The adapter should be connected to the mains Wait 2 seconds and connect the USB cable 2 For lviumStat connect the powercable to the mains switch the instrument on and connect the USB cable 3 Go to Start Control panel Select Hardware and sound Choose Device manager under Devices and Printers Expand USB controllers Find the Ivium Instrument USB right mouse click on it and select Update Driver Software f Choose Browse my computer and navigate to locate the driver standard CAIVIUMSTAT IVIUMDRIVERS g Click next to install the driver Dapo Note that the Ivium n Stat uses USB drivers that are standard included in MS Windows Just plug the system into a USB port and it is ready to go 11 Resuming from a failed driver installation In case an error occurred
135. nd where the generated data should be stored The small buttons at the right will open dialog screens to find folders Before running your script make sure all required methodfiles are in the Methodfolder and that the Datafolder exists To edit a batch script first select the commands in the top grid BatchCommand grid Clicking on a Line field will open a selection list with the available commands When a line in the Command grid is selected its parameters can be edited in the bottom grid the BatchParameter grid Above the BatchCommand grid there are several buttons AddLine add a new line at the bottom of the script DeleteLine delete currently selected line InsertLine insert a new line above the currently selected line Test test the script for illegal Loop constructions or non existing Methodfiles 65 Start execute the batchscript If the script contains errors it will not be executed AbortLine abort the action on the currently executing line and proceed to the next line AbortBatch abort the action on currently executing line and stop the batch Direct fBaich LoadBatch SaveB atch Batch file D iviumstat B atchFiles batchmus ibf Methad folder D iviumstat B atchFiles g Datafolder D iviumstat B atchFiles E Add line Delete in Insert ine Test de e 7 Line 1 LoadMethod Methodfile testmux1 Line 2 Loop LoopCycles 2 Line 3 ExecuteMethod Savedatafile tmux Line 4 LoopEnd Line 5 Em
136. nnected using the crocodile clips that are included in the lviumBoost shipment 1 9 Install MultiWE32 The lvium Technologies MultiWE32 works with CompactStat or IviumStat to provide simultaneous electrochemical potentiostatic control of 32 working electrodes versus one counter electrode and one reference electrode 32 channel impedance can also be measured sequentially 15 Connection to lvium potentiostat To connect the MultiW E32 to an IviumStat or CompactStat 1 Take the 40 cm M F HD15 cable Insert the M side into the Cell connector of the IviumStat or CompactStat Insert the F side into the HD 15 connector at the front of the MultiWE32 2 Insert the multi electrode cable to the HD 37 connector at the back of the MultiW E32 3 Connect the 5Vdc power adapter to the MultiWE32 at the back The green power LED at the front will now light up 4 Switch on the lviumStat or connect the CompactStat 5 n the Options menu check the option for the MultiWE32 6 Now in the various parameters to control the MultiWE32 are available in the Direct and Method modes The MultiW E32 is now ready for use Operation When the MultiWE32 option is activated the instrument can be controlled sequentially via the Direct mode or simultaneous via the Method mode In the Method mode in the method parameters of the various Techniques one or two extra parameters will become available depending on the technique e WE32 offsets to set the offset
137. not to be used in usb powered mode 2 j digini Oto 5V O 3 X digout2 0to 33V O E pugnd S 9 a ceo d 7 anout 1 0to 4096V 8 jJacout fto tV PO 9 Jani 4to 4V PO 10 pgain X 4to 4V PO 11 pgainY 4to 4V S 107 20 digin2 Oto 5V PT 21 digouti 0to 33V 22 digout3 0to 33V 24 dgnd X pT 25 agnd 000 o 0 26 anout2 0to 4096V 27085 agnd o 0000000000000 9 11 PDA Same specifications as for PPE except for analog inputs System Performance m No of channels 8 analog inputs for each unit Maximum no of channels 64 8 units Each Channel Differential measurement range Maximum common mode voltage Input impedance gt 100 Gohm 8pF lt 10pA oo O Input bias current lt 10pA Signal bandwidth 3 3 kHz ieee T y O Environment pec power requirements with external adapter 100 240V 45 65Hz 6VA wxdxh 12x26x2 5cm Weight 0 6 kg excluding cabling Calibration The PDA differential analog inputs can be calibrated in the Direct mode e Connect the PDA to the P G instrument e Inthe Direct mode select the PDA tab e Connect chi ch2 to E out i e use a banana lead e Connect ch1 ch2 to Agnd i e use a banana lead e Press the Calibrate button e Press the Save cal button e Remove the
138. nputs of the peripheral port The 8 channels from the peripheral port are recorded in pairs simultaneously with the primary signals In the 2 channel configuration ch1 amp ch2 are sampled at the same speed as the primary channel When 4 channels are sampled ch1 amp ch2 and ch3 amp ch4 are sampled alternatingly at half of the sampling speed of the primary signals Likewise when 4 channels are sampled the peripheral channels are sampled at a quarter of the sampling speed of the primary signals Results are visualized in the Extra plot accessible via the graphic toolbars Anout2 This is a facility to generate an external output pulse or variable voltage level just before the measurement starts With this option another measurement device can be triggered to start simultaneously or a generator can be controlled to perform at the selected analog level For example the intensity of a light source can be varied to study photoelectric phenomena It is both possible to 126 apply a pulse of defined duration before the measurement starts or apply a continuous voltage level at Analog Output 2 of the peripheral port The pulse level can be defined at 16bits resolution The pulse duration can be programmed from 0 05ms to 500 ms at 10us resolution The pulse is applied just before measurement sampling starts In the HiSpeed techniques the first recorded measurement sample follows within 0 05ms after the pulse level change For all techniques in
139. ochemical strippping potentiometry Please note that the current must be compliant with applied current range Equilibration time E start will be applied for indicated time before an experiment starts and at each new DC setting when relevant Current range Current sensitivity during the experiment When automatic current ranging is applied this parameter sets the initial current range CR The maximum current that can be measured is 3 the current range higher currents will trigger the current overload indicator Overload currents that are higher than 3 but lower than 4 the current range may still be correct but the reliability is not guaranteed In case the DualCR option is checked for impedance measurements the active current range depends on the applied frequency AutoCR is not available for galvanostatic techniques Noise reduction This parameter can be used to reduce the impact of noise in impedance measurements This can be convenient in cases that suffer from excessive noise When activated it will apply stronger automatic filtering with built in analog filters Also it will give easy access to the Acquisition period of the FRA settings which is the total period that is sampled averaged 123 Noise reduction Acquisition period Easy access to the acquisition period FRA settings a longer period will give better noise reduction Note that this will override the value in the Options menu The default value in the
140. oft program the actual method parameters are saved When lviumSoft is restarted these are reloaded In this manner new sessions can continue where the previous ended IviumSoft Help The IviumSoft software is equiped with a help function The help function can be accessed from the menu bar under Help to execute a topic or word search Alternatively positioning the cursor mouse anywhere on the lviumSoft and then pressing F1 will automatically pop up a window with a decription relevant to the indicated parameter area The help function is supported by the Windows Help Windows Help WinHIp32 exe is a Help program that has been included with Microsoft Windows versions however starting with the release of Windows Vista the Windows Help program does not ship as a feature of Windows IviumSoft uses the Windows Help program for the software help If you want to use or view the lviumSoft 32 bit hlp files when running under Windows Vista you must download and install the program WinHIp32 exe from the Microsoft Download Center The download file and a guide on how to install it can be found at the Microsoft Download centre 1 2 lviumStat instrument s ELECTROCHEMICAL INTERFACE Rearpanel Power connector fits the standard power cable which should be connected to the main power Fuseholder contains 2 fuses Replacement should be done by a qualified person USB connector fits to the supplied USB A B cable which should be connected bet
141. ol DA File Options Tools Help About li Connect IE B05001 z Eovi lovi Ext m inen l sigviewl Direct Method Result graph Result data D iviumstat manualchronpulsen Scale Analysis Edit LinearSweep Ry Standard E Scan Dlay TEST 1 3D no labels X CurrentAveraging TrueLinear 2m viscan 1 CyclicVoltammetry Standard Standard S Title E start 0 0000 V E end 1 0000 V E step 5 mv Scanrate 0 05 V s Equilibration time os Save data Current Range 1m amp Filter automatic Seve caue Stability automatic Delete Connect to dummy 1 Delete all Analog inputs none i i 0 6 i ii AutoCR ot Data appear Apply wit OCP Tone Pote nti al 201 pnts Scan completed 29 2 16 Test 2 standard testcell The cell cable must be connected to the instrument and the testcell as described Start the instrument as described go to the Methode mode and load the measurement procedure TEST2 imf that was supplied by the manufacturer Measurement procedures can be loaded with the Load method function from the File Menu Press Start and the instrument starts the measurement When completed the result should look like the plot below 2 lviumStat Control File Options Tools Help About Connect z EoviloviEw tm Basic Sigviewl Direct Method Result graph Result data D Niviumstal manua TES
142. oltage Potentiostat Bandwidth 2100 kHz Stability settings High Speed Standard and High Stability Potentiostat Galvanostat Programmable response filter 1MHz 100kHz 10kHz 1kHz 10Hz dual channel 16 bit ADC 100 000 samples sec Potentiostat lt 50us o lt 50 us ee Galvanostat 0 003 of potential range minimum 40nV PO y O l Impedance Analyser o Oooo DC offset 16 bit dc offset subtraction 2 dc decoupling filters 12nV to 10V 12nV to 20V Po and 0 05fA to 40A and 0 05fA to 20A eee Electrometer PT 106 Special functions p Ohmic drop compensation 2 V current range 16 bits resolution Safety features automatic disconnect on intern ext exceptions Peripheral connections 8 Analog in 0 to 4V 16 bits resolution 2 Analog out 0 to 4V 16 bits resolution 2 Digital inputs and 3 Digital outputs 0 to 45V l out and E out analog monitor for cell current and potential AC out 0 5V sinewave 10pHz 100kHz var attenuation Channel X and Channel Y inputs 4V to record impedance from peripheral devices eooo NO o Environment PT wx d xh 47 x 36 x 14 cm Specifications subject to change Ivium Technologies 2010 9 10 PPE Peripheral Port Expander Break out box for peripheral port Specifications O Z O DB87te32x4mmbananasockets 0 5 kg excluding cabling Peripheral connections 1 e5v maxx 100mA
143. om the Method sheet advanced parameters Data options ocp if the wrt OCP option was selected this window will show the results of the measured Open Cell Potential vs time pre Pretreatment data if pretreatment stages are applied this window will show the results of the data obtained during these stages Q will show the charge passed only if applicable Rs will show the Rs value only if applicable Cs will show the Cs value only if applicable 38 At the bottom of the graph sheet depending on the method used some extra method commands may show For example e In cyclic voltammetry the Reverse scan and Pause Resume buttons are shown These can be used during a scan to temporarily pause the scan or to reverse the scan direction e During a ChronoAmperometry scan in standard mode a button appears with a potential input field Any valid potential can be typed After pressing the Apply direct button the new potential will be applied to the cell immediately after the next measured point This potential will be applied for the remainder of the presently executing level e Anongoing chronamperometric scan in standard speed sample interval gt 2ms can be paused by pressing the Pause button at which it will maintain the momentary potential applied Pressing the Resume button will continue the scan sequence as defined by the method During a Pause period the data is not recorded 4 5 Graph options A right mouse c
144. on is the 1st datapoint after each new applied level change which will always be stored For ChronoAmperometry the instrument will use the min delta and for ChronoPotentiometry the min delta parameter For Mixed mode both parameters will be used either an E delta or an l delta will trigger a sample recording In this case a single parameter can be effectively disabled by entering a very high value In principle the averaging approach could be combined with the minimum delta method However this is not recommended because of the increasing complexity Therefore if using the minimum delta method keep the average every on 1 point And for the averaging approach keep both min deltas to 0 Data reduction average every Number of points to be averaged For example at 1 sec interval and an average count of 600 only 1 point per 10 minutes is recorded Data reduction no averaging In the existing data reduction option transient techniques the number of datapoints can be reduced by setting an averaging number In this manner the instrument will reduce the number of datapoints by a selectable fraction The intermediate datapoints are averaged to a single stored value However When no averaging is checked every n th value is stored without averaging the intermediate values Data reduction min E delta Adaptive sampling only E values differing more than this value from the previously stored data point will be stored
145. ored on the clipboard to be transferred to other applications such as WORD or EXCEL The graphic data is stored as WMF windows meta file which is vector based and can be resized without losses To place a graph in the clipboard move the mouse above the plot right click and select Copy Or use the Copy function on the graphic toolbar above the plot when available 67 Numerical data can also be stored on the clipboard to be copied to other applications The data is stored as textcharacters in columns separated by TAB delimiters and rows are separate by CR delimiters This is the basic format for applications as WORD or EXCEL and transfer goes 1 1 To place numerical data in the clipboard use the toolbar above the numerical grid for example see the Result data sheet 7 5 Edit In the graphic toolbar Edit will open a dropdown menu that allows the operator to execute a number of data manipulations Edit data will allow the operator to smooth data or change an individual datapoint Smooth all data will automatically smooth data Subtract ohmic drop will allow ohmic drop compensation when resistance is known Average scans will automatically average scans in the Scan panel Subtract overlay will subtract overlay scan from the one Scan panel Add overlay will add overlay scan to the one in Scan panel 7 5 1 Edit data Edit data allows the operator to smooth data or edit change a data point This can be activated
146. ow impedance objects 9 19 ModuLight Functionality The ModuLight module is a programmable light source designed to investigate photo electrical devices Its light intensity can be modulated with the IviumStat CompactStat The wavelength can be set programmatically from 465 635 nm in 7 steps with a maximum light intensity of 60 Im Table 1 Mode Color Wavelength Luminous Flux_ Radiant Flux Digital code _ 1 White 425 600nm_ 57Im NA I Royal Blue 465nm i0lmm 255mW lO O 3 Bue 475nm 19Im 278mw OO Green 535nm 52Im 91mW OI Amber 595nm _ 42Im 82mW TOO Red 635nm 40lm 260mW OCO Light intensity can be modulated with the FRAoutput of the build in sinewave generator of the lviumStat CompactStat from 10uHz to 2 MHz 3 4 Cyan 510nm 45lm 78mW Ol 6 7 112 Table 2 Specifications O pC O ee Interfacing connectivit Po penphrapot atDC conectot5b VIA Installation Connect The ModuLight module directly to the DB37 peripheral port via the 37 pin Male connector Then insert the 5V DC plug into the back of the ModuLight Plug the adapter into the mains power The ModuLight is now ready for use It is controlled via the lviumSoft software Operation Color Selection The color LED can be selected by using the 3 digital outputs of the peripheral port The digita
147. p to 5 potential or current levels may be applied before the experiment starts Each level is defined by a potential or current value and a time duration The pretreatment stage preceeds all operations also the OCP monitoring if that is activated Results are visualized in the Extra plot accessible via the graphic toolbar Data Options Transform the visualized result The peripheral port signals may be transformed with user defined functions the potential axis may be automatically corrected for various reference electrodes or the electrode surface area may be entered to plot current density Note that the transformations are on the visual graphs only the underlying data is always stored in original form Apply to selected data will apply the transformation only to the scan in memory Apply to all data will apply the transformation to all data in the graph sheet In the Analoginputs tab the 8 available analog inputs may be plotted in 2 separate graphs according to 2 different transformations see graphic toolbar Zi DataOptionForm E ni x Analoglnputs Ecorrections Electrode Plot 1 Plot 2 Plot title Peripheral Port Plot title Peripheral Port Axis title Vot Axis ttle Vot Transform none zl Transform none z Transform parameters Transform parameters al g a0 al oO cf o channel 1 ld 2 channel 2 ld 3 channel 3 E ld 4 channel 4 ld 5 channel 5 at ld
148. pactStat BiStat LinScan Coul HiSens F RA Synchronize device Check device Verify firmware Upgrade firmware 193 Method 1 Synchronized Method 2 Config upgrade Set configuration Code isnt Apply r Upload file gt m Calibration Method 1 Calibrate measurement offset Calibrate applied offset Disable idle sampling Calibrate Frequency Response Analyser Booster offset Close In the device maintenance window 8 area s can be distinguished 1 Verify device clicking the Check device button will show the power status and configuration of the instrument This will also show whether the instrument is USB or self powered 2 Verify firmware clicking the Check firmware button will display the firmware version that is running A new instrument will always have installed the firmware belonging to the software that is delivered When a software upgrade is carried out the firmware also needs to be upgraded After upgrading the firmware the Check firmware will show whether the firmware has been upgraded a higher version number will be shown 3 Set configuration when a LinScan or BiStat upgrade is purchased after the the instrument has been deliverd the upgrade code can be applied here When necessary special instructions will be sent 4 Calibration calibration is done by the manufacturer Only the Booster offset can be calibrate
149. pedance measurements you can select to hide either the left or the right axis by depressing L R Or you can split the graph into 2 separate plots by pressing 2nd N F B scanned pulse visualization at Differential pulse or Square wave voltammetry also forward and backward current can be shown N normal difference forward backward is shown F forward forward current is shown B backward backward current is shown 43 X Ain ocp pre Q display a 2nd graph above the primary data graph Ain analog inputs ocp OCP data pre pretreatment data Q integrated current charge while X will hide the secundary data graph On top a horizontal toolbaar is displayed Scale clicking Scale will autoscale the current graph on all axis The drop down menu will allow Autoscale performs autoscale on all axis Scale X axis scale only the horizontal axis manually or automatically Scale Y axis scale only the left vertical axis manually or automatically Scale Z axis in 3D plots scale only the depth axis manually or automatically in twin axis plots scale only the right vertical axis manually or automatically Analysis see also Analysis chapter Equivalent circuit to fit measured impedances with an equivalent circuit Corrosion rate to analyze and calculate corrosionrate from linear polarisation scans Peakfind automatic to determine location and height of peaks automatically Peakfind advanced to determine lo
150. port data as ASCII save the selected data to disk as textfile without method information Export dataset as ASCII the different scans from the actual dataset will be saved as ASCII in separate files with the addition of x to the filename with x the sequence number of the scan Import data as ASCII imports a textfile as measurement data The actual method protocol will be assumed to apply on this data This action will clear any data that might be present already Exit exits the IviumSoft program 2 9 Options menu In this menu 2 selections are possible 1 Options change instrument and FRA options see below 2 Register idf ids files clicking this option will register Ivium data files idf and Ivium data sets ids on your computer This action will make it possible to double mouse click on an lvium data file set to load it in the scan panel of the IviumSoft Note that each double click on a datafile will open a new instance of IviumSoft The Options Options menu is only available when an instrument is connected because some of these settings are changed inside the instrument When the window is closed the instrument should sound a beep to acknowledge that the changed settings are excepted The options menu will allow manipulation of o Device configuration settings parameters that control the instrument and module configuration o Safety settings parameters to terminate measurement for protection of the test object o FRA
151. pty Y Set Line 3 properties Savedatafile tmux OverwritelfExist off ClearGraph ot Start Abart line Abort batch Example of a batchscript measurement on 2 multiplexer channels Line 1 Load method with filename testmux1 Line 2 Loop with 2 repetitions set the multiplexer channel to loopindex Line 3 Execute method and save data as tmux Line 4 Close loop 66 7 Data analysis and reporting 7 1 Current density graphs All plots that show current can be plotted as current density When the Idens button on the top toolbar is pressed the data will be divided by the specified surface area The plot axis text will change to Current density and the recalculated data is shown The surface area can be specified by selecting the Data Options method parameter and the Electrode tab sheet The specified area will be saved in the method file and in the datafile Usually the area is specified before the measurement is executed However it is possible to change the area afterwards first select the scan and in Data Options press apply to selected data re save when necessary Note that the original data is not changed Releasing the Idens button will show the total current again 7 2 Reference potential graphs All plots that show potential can be automatically corrected to refer to an offset potential or various reference electrodes When the Ecor button on the top toolbar is p
152. pulse time must be shorter than half of the interval time Normally only the current difference is displayed Optionally the original measured currents can be viewed In analytical experiments the result usually appears as a peak which height is proportional to the concentration 5 16 ElectroAnalysis Square Wave During square wave voltammetry a staircase scan is applied with a superimposed square wave The interval time equals 1 frequency The current is measured at the end of the 1st flank forward and at end of the 2nd flank backward from which the current difference is displayed forward backward The sign of forward backward pulses is defined by the scan direction The operator can choose amplitude and frequency Normally only the current difference is displayed Optionally the original measured currents can be viewed forward and backward In analytical experiments the result usually appears as a peak which height is proportional to the concentration 5 17 ElectroAnalysis AC Voltammetry During AC voltammetry a staircase scan is applied with a superimposed sine wave The resulting ac current is measured and displayed The operator may set the amplitude and the frequency of the applied ac signal If Phase sensitive is turned off then the rms value is shown If Phase is turned on the user may choose the phase which will be used for detection Optionally the second harmonic current might be recorded advanced parameter
153. r a more narrow Potential range setting with a higher resolution IR feedback Compensates for ohmic drop in the sample via the direct feedback method The instrument will increase the cell potential by the amount that is defined by the product of current and Compensation resistance Care should be exercised because overcompensation will result in instabilities IR feedback Compensation The ohmic value to be compensated This value may range from 0 to 2V current range for example at 1mA current range at most 2 kohm can be compensated BiStat Use bipotentiostat When active WE2 will be connected and its current recorded BiStat E offset Potential offset for WE2 range 2V BiStat Current range Similar to the primary current range setting but for WE2 If CR min lt gt CR max then automatic current ranging is applied BiStat CR min Minimum allowed current range BiStat CR max Maximum allowed current range BiStat mode Select Standard or Scanning mode In Standard mode the WE2 potential is set to a constant offset with respect to RE In Scanning mode WE2 is kept at a constant offset potential with respect to the primary WE thus WE2 will scan at the same speed as WE1 128 Cell after measurement If activated the cell will remain connected after completion of the measurement the E standby will be applied between measurements Cell after measurement E standby Potential applied after measurement s Pretreatment U
154. raction 2 dc decoupling filters Dynamic range 12nV to 10V and 0 05fA to 5A LL Electrometer lin foe LC Input impedance gt 1000 Gohm 8pF lt 100A O Input bias current lt 10pA Bandwidth gt 16 MHz O T O Peripheral connections 8 Analog in 0 to 4 000V 16 bits resolution bandwidth 40kHz 2 Analog out 0 to 4 096V 16 bits resolution 2 Digital inputs and 3 Digital outputs 0 to 45V l out and E out analog monitor for cell current and potential AC out 0 5V sinewave 10pHz 1MHZz variable attenuation Channel X and Channel Y inputs 4V to record impedance from peripheral devices NEED GNMDENMMMMMZEsessye e Specifications subject to change Ivium Technologies 2010 9 5 IviumStat20V Same specifications as for lviumStat except System Performance Current compliance 2 5A Maximum output Voltage 20V 9 6 lviumStat XR Same specifications as for IviumStat except System Performance Current compliance 5A Maximum output Voltage 20V 105 9 7 IviumStat XRi Same specifications as for lviumStat except System Performance Current compliance 10A Maximum output Voltage 10V 9 8 IviumStat XRe Same specifications as for lviumStat except System Performance Current compliance 2A Maximum output Voltage 50V 9 9 IviumBoost 40A 10 V 20 A 20 V System Performance poU Maximum output V
155. re instrument If the connection process takes exceptionally long or the instrument fails to respond at all possibly its internal firmware is corrupt Please note that the recovery procedure is slightly different for different instruments For CompactStat e remove power cable and USB cable e start the pc software and re connect the usb cable do not press connect For IviumStat e switch instrument off with power button on the front of the instrument e press the CELL OFF button before switching the instrument on e start the pc software do not press connect For Ivium n Stat e switch instrument off with power button on the front of the instrument e connect EMO to GND make a wire connection between the EMO and GND sockets for example using a banana lead e switch on instrument the status LEDs will light up a faint red From the main menu press Tools and Restore Device E Restore device TTE Restore factory settings Restore factory firmware Restore previous firmware 3 options are shown Restore factory settings reverts back to the original settings and calibration values Restore factory firmware sets the firmware back to the original release Restore previous firmware go back to the version before the last upgrade The last option is useful when recovering from a failed upgrade If also the previous version was corrupt the factory version can be used When a firmware version is running again the
156. ressed the potential axis will be automatically corrected for the selected offset or reference electrode The plot x axis text will change to Potential and the recalculated data is shown The potential correction can be specified by selecting the Data Options method parameter and the Ecorrections tab sheet The values will be saved in the method file and in the datafile Usually the correction is specified before the measurement is executed However it is possible to change it afterwards first select the scan and in Data Options press apply to selected data re save when necessary Note that the original data is not changed Releasing the Ecor button will show the total current again 7 3 Scaling and zooming Standard plots are autoscaled When a new datapoint is recorded that is outside the present graphical range the scaling is adjusted to include the new point It is possible to override this behaviour e manually scale X Y Z axis over the graph press the right mouse button and choose the axis or use the scale option from the graphic toolbar e zooming left click the mouse on the graph keep button pressed and move over de area to be expanded When the leftmouse button is released the enclosed area is expanded to full scale It is always possible to restore automatic scaling either with the right mouse button popupmenu or pressing the scale button on the graphic toolbar 7 4 Clipboard functions Graphs can be st
157. retE EXT Xperph Ef 0 0 0 0 i BiStat lwe twee 12 EXT JBiStat Xperph lwe2 In the Direct configs the potential control loop is bypassed This means that the potential is the directly applied potential on the CE terminal w r t the gnd This can be useful when controlling other equipment such as loads The differential electrometer can be used independently for other purposes 133 Example 1 Solarcell IMPS The lviumStat CompactStat AC OUT port is used to drive the intensity of a light source and the ac photocurrent from the solar cell is to be recorded with reference to the incident light impedance Light photo Current The instrument is set to Impedance Constant E and the MeasConfig parameter to INT ac E With this parameter setting the internal applied ac signal is used as Y which is the light intensity here instead of the cell potential Note that the potentiostat potential may be set to shortcut conditions E20 but it may also be operated at other potentials such as maximum power point Example 2 Solarcell IMVS The lviumStat CompactStat AC OUT port is used to drive the intensity of a light source and the ac photopotential from the solar cell is to be recorded with reference to the incident light impedance photopotential Light The instrument is set to Impedance Constant I and the MeasConfig parameter to INT ac I With this parameter setting the internal applied ac s
158. retreatment AUX _ levels 1 4 cls ess S Il Seven oak Result graph Result data Scale FE Edt gt Multicycle CP Potential Scan Dlay no labels Y M scan 1 cycle 1 scan 2 cycle 2 scan 3 cycle 3 v scan 4 cycle 4 Save data Save dataset Delete Delete all 1708 pnts cycle 4 Scan completed Same experiment as above with CyclesSeparate option activated and plotted in 3D with cycles index as depth axis 53 5 12 Transients MixedMode The MixedMode technique provides maximum flexibility You can alternate between Potentiostatic Galvanostatic and Open cell mode Moreover it allows the combination of DC with Impedance measurements and potential current sweeps in a single experiment e Programmable switching between Potentiostatic and Galvanostatic and Open cell mode OCP while recording dc current and potential simultaneously e Potential and Current Sweep capability the Estat and Istat stages can optionally be defined as Sweep stages Sweeps can be activated by checking the SweepE Sweepl option When activated values for Eend lend and scanrate can be entered Note that the values for Estep Istep are defined by scanrate interval time e Up to 255 levels may be sequenced Each level can be set to Potentiostatic Galvanostatic Open cell mode Programmed sequences can be repeated up to 65535 time
159. roperties below the wavelength can be chosen by ticking the SetDigOut box The boxes for the individual digital outputs become available and by ticking the relevant boxes the wavelength can be chosen In the same way ticking the SetDAC box will make the analog outputs available Inserting the desired value in the DAC 1 field will set the intensity of the light Mixed mode In the transient technique MixedMode a sequence of operations can be programmed in the window of Stages method parameter In the Properties for Level at the bottom of the list the following parameters allow operation of the ModuLight e AnOut1 when ticked a value can be entered from 1 4 V which determines the intensity of the light 1 100 in the same way as in the direct mode operation see above e Digouts when ticket an integer value can be entered to select the color This integer corresponds to an 8 bit conversion for the digital outputs i e 0 all digouts off 1 digout1 on digout2and3 off etc The modulation of the light can be controlled by ticking the Record ac box In the method parameters the frequency and amplitude can be set 114 Photometry Luminous Flux The applied Led serie iz adapted to the so called luminous efficiency function This function describes the average sensitivity of the human eye to light at different wavelengths This meare that to obtain a relatively equal light output at different colors the radiant power will
160. rrent for 100s or until E gt 3 5V record impedance e Switch to open cell for 5 seconds e Apply 50mA constant current for 100s or until E lt 0 1V record impedance e Switch to open cell for 5 seconds 55 2 lviumStat Control File Options Tools Help About Connect zi E Ext 1mA Basic X SigView BatchMode Direct Method Result graph Result data D iviumstat datafiles g2_mixmade Scale l Analysis 7 Edit l Ecor Idens Transients op ohm Rs Scan olsy Chrono amp mperometry no labels Y ChronoPotentiometry 3D Mixed Mode i Hide all Electrochemical Noise Show all Electro nalysis l Title Stages _ levels Cycles 2 cls Resistance Cycles separate Off Interval time 02 s Amplitude 100 0 mV Frequency 1000 Hz Current Range Potential range Data Options i AUX lt Current Potential Example of Mixed mode 2 cycles with a 1F supercap using stage protocol above bottom plot in 2nd mode 2 separate graphs 0 top measured current o bottom measured potential top plot Rs activated o blue dots resistance measured at 1kHz Note that capacitance can be shown by pressing the Cs button on the toolbar at the left 5 13 Transients Electrochemical Noise This allows for noise measurements with a standard lvium instrument no hardware modifications are required Usually this technique is applied in corrosion research Specifications e Data sampl
161. s It is possible to define the scan boundaries depending on the measured currents The operator can set parameters for Maximum and Minimum current limits inside which the scan will remain If the current exceeds the defined I max or gets below I min the scan is stopped This feature is only available in Standard mode It is possible to use Dynamic Vertexes in combination with AutoCR However when AutoCR is activated the dynamic vertexes will only be active in the defined AutoCR Max range This means that the Absolute values of I max and I min should be larger than 0 25 the selected Max range In practice usually the Max range parameter will be chosen according to the desired vertexes 119 DynamicVertexes max Maximum current allowed when exceeded the sweep is terminated or the scan direction is reversed DynamicVertexes l min Minimum current allowed when exceeded the sweep is terminated or the scan direction is reversed Vertex 1 First vertex potential potential is scanned from E start to Vertex 1 subsequently to Vertex 2 and back to E start vertex 1 First vertex current current is scanned from start to vertex 1 subsequently to vertex 2 and back to start Vertex 2 Second vertex potential potential is scanned from E start to Vertex 1 subsequently to Vertex 2 and back to E start vertex 2 Second vertex current current is scanned from start to vertex 1 subsequently to v
162. s e Each level can be set to a fixed time duration Also levels can be ended dynamically when predefined criteria are met see table below e Simultaneously the ac impedance can be measured in both Potentiostatic and Galvanostatic mode e Automatic Current ranging can be used in the usual manner Only applicable for Estat stages In Istat and OCP stages the initial current range is reset a the beginning of the stage If an Estat stage is preceded by another Estat stage the starting current range is the same as the last current range of the previous stage If AutoCR is activated the dynamic threshold options I lt I gt dldt dldt Ifraction lt Q gt are not available AutoCR will only decide to change current ranges based on dc values If the simultaneous ac measurement is active the impedance is measured at the same current range as the dc signal e The analog output port from the Peripheral port can be set at the start of each level In this manner it is possible to generate complex waveforms to control external equipment RDE rotationrate intensity of light sources positioning of SECM temperature of thermostats etc Also this feature may be used to synchronize external events at defined point s inside the measurement sequence Unlike the AUX trigger function this may be different at each level from the start of the sequence e Specifications Switching between Potentiostatic and Galvanostatic mode lt 1us
163. s can be stacked up to 8 units resulting in a maximum of 64 differential analog inputs Measurement in Method mode 1 Connect the analog inputs as desired each analog input connected differentially 2 Inthe method parameters advanced at the Modules parameter tick the box and then tick the box next to PDA to activate the PDA module 3 Then in the method parameters at the Analog inputs parameter choose the number of channels to be measured keeping within the capability of your hardware up to 64 channels for 8 PDA modules 4 Proceed in the same manner as described above at Analog inputs direct or via PPE Measurement in Direct mode The differential analog input signals can be measured from the direct mode tab Connect the analog inputs as desired each analog input connected differentially Select the Direct tab Below select the PDA tab Using the arrow buttons select the number of PDA modules connected Click on Read units A single signal sample will be measured on all analog inputs on all modules and displayed in the value array 8 12 5 Using AC input The peripheral port of the CompactStat and lviumStat instruments is equiped with an AC input The AC input can be used to superimpose the analog or ac input signal on the DC signal of the instrument In direct mode In theDirect mode on the Extern tab check the box for Ext ACin When checked the analog or ac signal connected to pin 9 of the per
164. s will still be disconnected on the alarm conditions The automated disconnect at temperature overload will always be active and cannot be disabled FRA settingssheet e Stabilisation period time delay after an ac signal is applied before acquisition is started This allows the cell and instrument to reach a steady state after a new frequency or amplitude is applied It can be specified as an absolute time seconds or as a multiple fraction of the applied signal period cycles Both criteria must be true before the measurement starts thus the longest of the 2 is taken e Acquisition period time period that the ac signals are measured It can be specified as an absolute time seconds or as a multiple fraction of the applied signal period cycles Both criteria must be true before the measurement ends thus the longest of the 2 is taken Increasing the measurement time will let the instrument acquire more datapoints cycles that are used to calculate the average impedance and thus give more accurate results Range 2s 60s e Result optimalization set maximum number of re measurements for each impedance point In case of an overload or underload the instrument will attempt to change its settings current range and or gain settings and measure again at the new settings This process continues until optimum settings are reached or the maximum number of retries has occurred Increasing these numbers will improve accuracy but extend measurement
165. seline Current which is taken to be equal to the End current Note that this analysis can be used in combination with the Mixed Mode technique where in Potentiostatic mode the Until fraction parameter can be used to complete electrolysis Electrolysis Report EE as E E x Start current 5 012E 02 A Charge and Current End current 5 023E 05 A Total Charge 6 231E 03C Netto Charge 2 542bE 03 C 87 7 6 12 Mott Schottky analysis Mott Schottky After an impedance scan technique on the Escan tabsheet Mott Schottky can be selected Automatically the slope and intercept are calculated using Linear regression The results appear in a table below the graph If the selected potential range is decreased the non selected potentials are excluded from the calculation The results may be copied with the Copy button Excel format Result graph Result data E scan Fees e ran 2 154E 18 to oosv x 2 098E 18 from 1 499 V z 2 154E 18 Ea Example of Mott Schottky plots at various frequencies from measurements on a diode 88 8 Special functions 8 1 Device maintenance The Device maintenance panel can be accessed from the Tools menu It will open a pop up window where the instrument can be maintained E Device maintenance NE iol xj Verify device Manual contrat SN B03117 Powermode usb power slat dove Firmware running idle mode Reboot device Com
166. t subsequent reports with the same instrument will overwrite older reports The test report starts with recording time date and the instrument software configuration and is followed by the test results Each individual test result is compared to preset limits and a Pass or Fail status will be assigned lal xl 3 Test performance connect Testcell 1 to celle Report Testdate 26 02 2010 17 06 50 D0008 V 0 0030 0 0030 Pass E_applied 1 0011 V 0 9970 1 0030 Pass 10m 1 01 m 0 380 110 Pass 1m 1 001 m 0 397 1 003 Pass 100u8 100 7 pA 98 0 1020 Pass _10u4 10 02 pA 997 1003 Pass 1u amp 1 007 pA 0 980 1 020 Pass _100n4 1001 n 99 0 101 0 Pass 1 n amp 9 99 n 950 1050 Pass cable 1 008 m 0 330 1 010 Pass E cable 10011 V 0 9970 1 0030 Pass AC test R1 1068 Ohm 90 0 300 0 Pass AC test R2 994 9 Ohm 980 0 1020 0 93 8 6 Pulse Generator A continuously repeating pulse can be applied to the cell with variable period and duty cycle It is intended as a tool to treat the electrode without data being measured It can be applied in potentiostatic Estat or in galvanostatic mode Istat both in 4 electrode mode The duration of a pulse level can be defined from 10us to 0 6 seconds 0 01 to 650 ms Each level Hi period and Lo period can be set independently Pulse generator Estat Hi period 100 ms HL Voltage 10 y Lo period 1 00 ins La Vokaal 1 0 y The pulse generator c
167. t available The amplitudes are the same for all frequencies e Fixed number of frequencies per decade 5 The MultiSine method is applicable for frequencies below 100Hz However it is possible to combine the SingleSine method and the MultiSine method in a single frequency scan In the MultiSine tab simply select the frequency range required and the software will automatically determine which method to use over the frequency range In the screenshot below note that the frequencies above 100Hz will use the SingleSine method while below 100Hz the MultiSine method is applied Also note the logarithmic frequency distribution for SingleSine and the odd harmonic distribution for MultiSine 59 z Edit frequencies I ini xj Single sine j Multi sine Frequency scan Start 10 kHz ne End 1 kHz focal 001 y Close em ew The measurement data format will be the same as for SingleSine each frequency will be stored individually Also the data analysis is conducted in the same manner Note that MultiSine offers faster measurement however this is at the expense of measurement accuracy If measurement duration is not an overriding issue it is strongly recommended to use the standard SingleSine method Sequence The measurement sequence during a frequency scan e prepare the frequency set filters stabilization dc coupling etc apply the frequency and allow the system to settle stabilization perio
168. t is advisable to use a Windowing function A choice of 5 different Windows is provided If the data contains a dc drift it can be removed by checking the Subtract baseline box This will construct a baseline between 1st and last point which is subtracted from the dataset before transformation 81 A more extensive option to remove a baseline or trends from the data is available in the Baseline remove tab The order of the polynomial baseline is selectable from 1st linear to 9th order Pressing the Apply button will subtract the baseline from both the Potential and Current data Subsequent time domain and Frequency domain analysis will use the corrected data After the ECN Analysis tool is closed the original data is also changed and corrected curves can be saved thereafter For details about the mathematical background contact Ivium Technologies Electrochemical Noise Analysis Time domain analysis Frequency domain analysis Baseline remove A r Subtract baseline n Gold 07 06 1 fih order 20 Calculate Apply 10 D Restore o E Oo 10 my D 200 400 600 4 2 D Potential ECN data before baseline subtraction 82 Electrochemical Noise Analysis E E l ce ni x Time domain analysis Frequency domain analysis Baseline remove A r Subtract baseline n Gold 07 06 1 7thoder v Calculate 10 N E Restore J o SSS 10 Oo mM D 200 4
169. tem waits 64 until a HI level is applied If unchecked it waits for a LO level WaitForDigIn1 TimeOut Maximum period that is waited for the selected level on diginput 1 The batch script is kept in a simple text file and may be edited by any ASCII editor However it is strongly recommended to use the BatchEditor that is included in the lviumSoft Making scripts is fast and easy with the graphical interface The BatchEditor is activated by pressing the BatchMode button This will open the Batch tabsheet 2 IviumStat Control File Options Tools Help About Connect Mess m4 Advanced ov jJ Sidview BatchMode Direct Batch Result graph Result data LoadBatch SaveBatch Scale Analysis Edit Ecor Idens Batch file D iviumstat B atchFiles batch4 ibf 20 mA Scan Olay nm Gold 07 06 1 no labels v Method folder D Siviumstat BatchFiles B Datafolder D iviumstat B atchFiles E gea vl scan 1 Addline Delete line Insert line Test Line Properties LoadMethod Methodfile testl Loop LoopCycles 8 ExecuteMethod Savedatafile default LoopEnd Set Line 5 properties Value Potential Save data Save dataset Delete Data appear Abort line Abort batch ms On top of the Batch tabsheet are the batchfile options to load and save batchfiles Below are the Methodfolder and Datafolder fields that specify where the parameterfiles are located a
170. ter is activated the subparameter names will appear below it indented e The second column allows you to edit the parameter values text parameters can be entered by typing any string of characters value parameters can be entered by typing numerical characters non numerical characters are ignored On leaving the field the value is tested against its allowed limits boolean on off parameters can be set by un checking the checkbox enumerated list values can be set by selecting the desired item from the dropdown list The dropdown arrow will appear when the field is selected dialog variables are displayed with a square button in the grid When this button is pressed a dialog screen appears with the group of variables e The third column will indicate the unit of the parameter if applicable Note that pressing F1 will provide an explanation of the currently selected parameter When exiting the Iviumsoft program the actual method parameters are saved When lviumSoft is restarted these are reloaded In this manner new sessions can continue where the previous ended Direct Method El LinearS weep Standard TrueLinear Mode Title E start E end DynamicVertexes E step Scanrate Equilibration time Current Range Filter Stability Connect to Analog inputs 4utoCR Max range Min range Apply wrt OCP IR feedback BiStat E offset Current Range CR max CR min Mode Cell after me
171. that were pre defined in the procedure method This feature gives the user the possibility to react directly on an observed event It can be especially useful for long duration experiments During a ChronoAmperometry scan in standard mode a button appears below the Result graph with a potential input field Any valid potential can be typed After pressing the Apply direct button the new potential will be applied to the cell immediately after the next measured point This potential will be applied for the remainder of the presently executing level Note that if this feature is used the sequence of applied potentials will no longer be completely defined by the methodfile and user intervention is not recorded This may hinder the repeatability of experiments An ongoing chronamperometric scan in standard speed sample interval gt 2ms can be paused by pressing the Pause button below the graph at which it will maintain the momentary potential applied Pressing the Resume button will continue the scan sequence as defined by the method During a Pause period the data is not recorded 5 11 Transients ChronoPotentiometry During chronopotentiometry a single or a series of current pulses max 255 is applied and the voltage is recorded The timebase of the experiment is set by the interval time it defines the measurement speed and the pulse duration The minimum interval time is 10 us and the maximum level duration is 4E9 time the interv
172. the IviumStat window as well as in the software Direct mode tab page may be different from the calibrated value Nevertheless in all measurements the calibrated value is used Cell cable connections The lviumBoost is capable of outputting high currents and high powers In order to guarantee the best measurement results the current carrying cables of the WE and CE have been separated from the potential measurement cables RE and S It should be noted here however that the IviumBoost can only be operated in the 4 electrode mode The RE and S leads need to be connected The WE and CE electrode cables end in an o ring for fastening to the testsubject The shipment of the IviumBoost includes several appendages for connecting the cell cables to the test subject The gold plated bananas can be attached to the o ring of the WE or CE cables by unscrewing the back of the banana and re fasten it through the o ring Do not use other banana s because these gold plated banana s have been manufactured and tested for 50A capability To attach the battery clips to the WE or CE electrode cables remove the handle insulation of the battery clip Fasten the electrode cable o ring at the bolt in the handle and re attach the handle insulation The RE S cable includes the ground cable All end in a banana plug The RE and S should be connected to the appropriate contacts of the test subject or the WE and CE leads These cables do not carry any current and can be co
173. the channel management Channel management Each s module has a unique serial number assigned at the factory This number will never change For multi channel operation it is useful to assign sequential channel numbers instead of working with factory serial numbers When starting up after a fresh installation the software will show the factory serial numbers such as S09001 S09007 etc To convert these to channel numbers 1 After starting IviumSoft do not press the connect button but select select in the menu bar Tools Define Channels 18 2 A form will be opened with a list of connected devices Ex factory the Channel numbers are predefined according to the slot positions in the lvium n Stat Frame To accept this assignment simply press Close 38 slotassignForm SeriaNo ChanneNo Fws so9033 4 191 identi sos 5 H 191 identity soga 2 a 191 Identify sosoze 1 H 191 Identity so32 3 H 191 identi s09024 6 H 191 Identity Write Close 3 To change the channel assignment use the up down thumbs A ChannelNo of 0 means unassigned To identify specific modules pressing the Identify button will flash its LED for 2 seconds Pressing the Write button will apply the new channel assignments b x EE E E E E Eu EN 4 Note that the serialnumbers amp channelnumbers are stored in each datafile for your reference The ChannelNo is stored inside the sModule and
174. the numerical OCP data these can be subsequently copied and exported Current units set the format of the displayed current values Potential units set the format of the displayed potential values 45 Time units set the format of the displayed time values Impedance select the parameters of impedance data to be shown Format when the box is ticked the values are shown in scientific notation with a 2 digit exponent this is especially useful when small values are shown since by default only 4 digits are displayed 4 11 E scan sheet When an impedance scan is carried out the E scan tab will show next to the Result graph and Result data sheet This will allow impedance data to be plotted and evaluated Also Mott Schottky analysis done here see Analysis chapter 46 5 Techniques Available Methods LinearSweep LSV o Standard staircase voltammetry records current at the end of each step o CurrentAveraging records average currents integrated over each step o TrueLinear applies true linear voltage ramp requires optional LinScan module o Galvanostatic staircase potentiometry records potential at the end of each step CyclicVoltammetry CV o Standard cyclic voltammetry records current at the end of each step o CurrentAveraging records average currents integrated over each step o TrueLinear applies true linear voltage ramp requires optional LinScan module o Galvanostatic cyclic potentiometry records
175. the value in the box and click Apply to apply the signal Set Mux channel for manually choosing the channel to be measured of the multiplexer Enter a channel number in the adjacent box directly or use the arrows to increase decrease channel number After setting the desired channel click on Set Mux channel to activate this channel Set WE32 channel for manually choosing the WE32 channel to be measured of the Multi WE32 module only available when MultiW E32 module is active Enter a channel number in the adjacent box directly or use the arrows to increase decrease channel number After setting the desired channel click on Set WE32 channel to activate this channel Automatic E ranging when unchecked the potential measurements are done on the widest range Therefore the resolution for measured potential is limited 0 125mV for CompactStat 0 333mV for IviumStat etc When checked default the instrument will automatically choose a more sensitive range if possible This will increase resolution to below 1uV At the bottom of the Direct sheet some tabbed pages are located Some of these tabs are only visible if the configuration allows this BiStat to configure the bipotentiostat this page is only visible when the Cell BiStat is activated in the connect group AC to apply directly a sine wave of chosen indicated frequency and amplitude Extern to read and set signals of the peripheral port analog input the potentia
176. tiostat Its WE2 lead can instead be used to measure potentials relative to the S electrode for example from the CE or an additional reference electrode In Direct mode the WE2 voltage sensor can be activated with a checkbox on the Extern tabsheet E at WE2 In the Method mode for techniques that measure potentials the WE2 sensor can be chosen instead of the electrode potential by checking the E at WE2 parameter Specifications a Range 10V b Input resistance gt 12Mohm c Bandwidth gt 100kHz e No high sensitivity current ranges The lvium n Stat has a minimum current range for the sModule of 10nA full scale with a minimum current resolution of 1 2pA 1 5 Installation and setup Install software before connecting the USB cable Refer also to Quick reference guide Software installation 1 Insert CDROM with IviumSoft Installation program 2 From the CDROM root directory run setup exe and follow instructions Driver installation Windows XP 1 For CompactStat first connect the power adapter to the CompactStat device The adapter should be connected to the mains Wait 2 seconds and connect the USB cable 2 For lviumStat connect the powercable to the mains switch the instrument on and connect the USB cable 3 Now you will see a sequence of dialog screens a Welcome to the Found New Hardware select No not this time and press Next b At next screen select Install from a list or specific location adva
177. trode configuration the counter amp reference electrode and the working amp sens electrode can be combined to a single electrode In case the bipotentiostat is available a 5th electrode WE2 is present PC requirements e Windows XP Vista or 7 e free USB port Multiple Iviumstats CompactStats and lvium n Stat channels can be controlled with 1 pc When the IviumSoft software is started the operator can select the serial channel number of the desired device Pressing the arrow of the selectionbox at the rightside of the Connect button will dropdown a list of available devices Pressing the Connect button will assign this software instance to the device indicated by the selectionbox Multiple instances of IviumSoft can be started that can each be assigned to another device Once a device is assigned to a particular IviumSoft instance it is no longer available for other instances of course When multiple instances are running and assigned these can be recognized on the Windows taskbar by corresponding buttons When an lviumSoft instance is connected to a device the text on the taskbar button changes from IviumSoft to Ivium X with X the serial number or assigned channel number for an Ivium n Stat of that particular instrument It is thus possible to control different experiments on several instruments simultaneously from one pc These instruments will operate completely independent of each other When exiting the lviums
178. true will correspond to the checked condition anything else will uncheck the box Numerical text strings must be of the correct format Incremental If unchecked default the new value will replace the existing one If checked the new value will be added to the existing parametervalue This option is only valid for parameters that accept numerical data DirectCommand sd Execute adirectcommand Scheduler Events can be scheduled the Repeat time timer keeps track of total time lapsed since the Batch was started Events can be scheduled at a fixed time independent of the durations of previous executed scans Thus measurements can be repeated exactly every minute hour etc Note the difference with the DirectCommand Wait function that adds a delay To activate check Scheduler and set Repeat time variable Scheduler will take precedence over other DirectCommands in the same Batchline they will be set only after the Repeat timer period has passed Repeat period can be set 1 sec to 1E7 s 3 months switched SetMuxChannel channel Channel nost to be set SetW E32Channel If checked the channel is switched SetW E32Channel channel Channel no to be set SetDAC If checked the analog outputs are set If checked the DigOuts are set On if checked WaitForDigIn1 If checked the execution is halted until the digital input 1 reaches the desired level or timeout is exceeded WaitForDigIn1 WaitForHi If checked the sys
179. ty Potentiostat Galvanostat Programmable response filter 1MHz 100kHz 10kHz 1kHz 10Hz Signal acquisition dual channel 16 bit ADC 100 000 samples sec o ee Applied potential range determined by controlling Ivium potentiostat CompactStat max 4V IviumStat max 10V lviumStat XR max 20V Measured current resolution Current feedback ohmic drop compensationn ohm current range 65 536 with n 0 to 65 535 peu Impedance Analyser PC O Frequency range 10uHz to 2MHz Amplitude 0 015mV to 1 0V or 0 03 to 100 of current range DC offset 16 bit dc offset subtraction 2 dc decoupling filters 4nV to 4V a Electrometer Se Input impedance gt 1000 Gohm lt 8pF Input bias current lt 10pA Bandwidth gt 16 MHz Sa Environment external adapter 100 240V 47 63Hz 400mA Voltage input 5V 10 2Vdc max 2W 110 Interfacing USB 1 1 or 2 0 compliant wxdxh 12x 26 x 2 5 cm MOG 2 os Weight 0 6 kg PC requirements Windows XP Vista 7 with free USB port Specifications subject to change Ivium Technologies 2010 9 16 HiMux Ivium HiMux specifications System Performance ces S No of channels 8 for each unit with each 4 electrodes WE CE RE S Maximum no of channels 64 8 units C ai ee o Each Channel a NIME Environment power requirements with external adapter 100 240V 45 65Hz 6VA wxdxh 12x 26x 2 5 cm 0 9 kg excluding cabling Specifications subject to change Ivi
180. ug counter clockwise 4 Connect the power cable 5 Switch on the lviumBoost 6 Switch in the lviumStat Note that the lviumBoost can only be operated in the 4 electrode mode The RE and S leads need to be connected By default the lviumStat is configured to operate stand alone In order to operate the IviumStat with the IviumBoost the configuration needs to be changed in the Options menu see also Installation and setup 14 Calibration of the IviumBoost To calibrate the combination IviumStat IviumBoost for optimal accuracy at the given current range of 10A of the IviumBoost proceed as follows e IMPORTANT Press the red Disconnect button on the front of the IviumBoost so that it lights up red e In the lviumSoftware go to Tools in the menu bar and select Device maintenance e Atthe bottom left in the pop up window click on Booster offset This will induce a number of clicks in the devices followed by a beep in the lviumStat indicating that the devices have been calibrated e De press the red Disconnect button on the front of the IviumBoost so that the lights extinguishes e Close the pop up window and commence working Note that the calibration of the IviumBoost is done with all the cell relais closed hence the clicking noise during the calibration procedure After measurements all cell relais will be opened to return the IviumBoost to default mode This means that the value for the current that is displayed in
181. ultiple lvium instruments on 1 PC Multiple Iviumstats CompactStats and lvium n Stat channels can be controlled with 1 pc When the IviumSoft software is started the operator can select the serial number of the desired device Pressing the Connect button will assign this software instance to the device indicated by the selectionbox at the right side of the Connect button Pressing the arrow of the selectionbox will dropdown a list of available devices Multiple instances of IviumSoft can be started that can each be assigned to a specific device Once a device is assigned to a particular IviumSoft instance it is no longer available for other instances of course When multiple instances are running and assigned these can be recognized on the Windows taskbar by corresponding buttons When an lviumSoft instance is connected to a device the text on the taskbar button changes from IviumSoft to Ivium X with X the serial number of that particular instrument It is thus possible to control different experiments on several instruments simultaneously from one pc These instruments will operate completely independent from each other 2 5 Measurement Measurements can be done with the internal dummy the external TestCell1 see chapter TestCell1 module or electrochemical cells Execute the supplied test procedures 1 2 3 for an introduction to operations Also study the following section on electrode connections Measurements with t
182. um Technologies 2010 onfiguration WE and CE elected channel connected to primary instrument Ivium HiMux XR specifications System Performance O J Po with each 6 leads WE CE RE S WE2 GND Configuration RE amp S continuously connected to dedicated electrometers n ES Each Channel 20V limited by instrument En Environment ee power requirements with external adapter 100 240V 45 65Hz 6VA wxdxh 12x 26x 2 5cm Weight 1 kg excluding cabling Specifications subject to change Ivium Technologies 2010 111 9 17 Edoubler Specifications Applied Edoubler in combination with IviumStat20V Potentiostat Applied potential range 20 V at 0 66mV resolution Applied potential accuracy 0 2 or 4mV 9 18 CIM Current interrupt module Functionality Enable the current interrupt technique for measuring the IR drop of the electrochemical system Specifications y lt 25 o y Interrupt time lt 2us Oooo y Note When not using the current interrupt technique all signals are passed through this module and it is fully compatible with the situation without CIM However the CIM adds ca 130 mOhm impedance to the cell cable This should be taken into account when measuring in the 2 electrode mode and it will slightly lower the compliance voltage of the potentiostat The latter will only have a significant effect when measuring very l
183. ward scan 78 2 Search Peaks Baseline subtract l Peak search _escale Copy rach G Fe in KNO3 0 2 0 0 Potential v Set markers with Left Mouse button and press subtract baseline when ready Baseline typ Marked baseline propertie polynomial marked C exponential marked i v automatic calculate Subtract baseline automatic calculate baseline undo subtraction Figure b baseline determination of CV reverse scan 79 2 Search Peaks Baseline subtract Peak search Fe in KNO3 0 2 0 0 Potential Set markers with Left Mouse button and press subtract baseline when ready Baseline type Marked baseline properties polynomial marked Io FIM IL C exponential marked 2 C 5 C g M CV reverse scan V automatic calculate automatic 3 6 9 clear makers ilate baselir undo subtraction Figure c CV after baseline subtraction 7 6 6 Clear peaks In the graphic toolbar selecting the menu item Analysis gt Clear peaks will allow the operator to remove peaks from the graph that have previously been drawn by the Peakfind automatic or Peakfind advanced options 7 6 7 Electrochemical noise analysis The software can evaluate the recorded results of an electrochemical noise experiment automatically It is possible to perform the analysis in Time domain or in the Frequency domain and to subtract the baseline In Time domain
184. wary The relationship between luminous and radiant intensity can be described az lp 683 IxFuy I Luminous Interne ity in me I W Radiant Intensity in ar fu Luminous F unction ST Steradium Aim nu Lun irous ezciemoy funo tion Luminous Intensity The 100 intensity of the applied led s are specified at 350mA 350mA is applied when DC i setto BY and or AC E setto 1V The current to relative intensity cures can be found in the next tio graphs Eu E g E Bag ele etu a d a E EC Ha E E 8 amp o Ee E Ea 200 420 can gon Forward Current mA Ferward Current mA White Rayal Blue Blue Cyan Green Red Amber Sean oe A measurement atG25nm setto lm and z lm As can be found in the led s specifications the red led has an output of 40 lumens at 350m ede In the graph aboe 50 20m ean be set by applying a current of 150m A 1 7 ed F635 683x Fi 683 x 0 225 115 9 20 EMO Emergency Off Next to the software options for automatic disconnection of the cell the IviumStat and Ivium n Stat instruments are equiped with an external EMO emergency off function lviumStat All lviumStat instruments including XR s have a red push button for the EMO function on the front panel When pressed all electrode cables are disconnected and the button lights up red Its circuitry is independent of the pc software setting or the instruments microprocessor and its operation
185. ween instrument and PC Cooling element with fan Please make sure that air can flow freely Frontpanel On Off button when pressed the instrument powers up and the button lights up blue when ready Please allow several seconds for the startup sequence to be completed Disconnect button when pressed all electrode cables are disconnected LCD screen a graphical screen that displays the status of the instrument Peripheral port 37p connector that provides access to a range of analog digital input output signals Cell connector 15p connector that fits the supplied electrode cable The IviumStat20V and the lviumStat XR are connected identical to the IviumStat The LCD screen displays a number of user relevant information In the Left top an arrow gt shows the status of the instrument when changing between and gt the instrument is idle when fixed in position the instrument is busy Below the arrow it shows what method is running and the actual value of E and l Note that these are updated at an interval with low priority i e when the instrument is busy updates of E and may not show At the left bottom in the blue bar it is shown whether the instrument is operating in Estat or Istat mode Below that the actual current range is shown In the right bottom corner in the blue bar the version of firmware that is running is displayed 1 3 CompactStat instrument AGT C D Mica INTE Rearpanel e Power conn
186. ws frequency spectrum Hide hides the window Graph Black plot corresponds with left axis Blue plot corresponds with right axis Left axis Current of full current range as selected Right axis Potential of full range as selected by automatic E ranging or maximum range Lower panel Freq actual applied frequency CR actual current range lgain gain value for current measurement Egain gain value for potential measurement Filter filter number Coupling internal signal coupling code 3 During an impedance measurement the signal traces for each data point are stored in the datafile and can be recalled to be investigated analyzed later Not only the data is stored but also the measurement settings Current range overload flags etc for each individual frequency To display the specifics of a datapoint first open the Signal monitor and point the mouse at the datapoint in question on the graph of an opened impedance measurement The Signal view will show the data in Recall mode 35 Signal Monitor B x Rescale Options Copy Freq eiae black left blue right m un uei e e Current Potential 0 0 0 2 0 4 time 0 6 1 0 Freg 749894 2093H2 Zabs 1 096E 030hm Phase 15 62 deg CR 1m status OK 0 0 0 22 12 2003 15 39 In the example above the E I traces are displayed in recall mode It also shows the current range which is useful if AutoCR was act
187. y control read other types of devices pumps valves thermostats motors sensors etc Method 1 Import the provided dll in your program IVIUM remdriver dll 2 Embed the control functions in your software 3 Start IviumSoft and your own program The dll allows you to import and execute most basic functions of the Ivium device Imported function Description GENERAL Ooo NNI Opens the driver Closes the driver 95 Returns status of device 1 no lviumSoft 0 not connected P t available_idle 2 available busy O 1 Returns serial number of selected device empty string if not connected DIRECTMODE O Returns cell status bit 2 1 ovl bit 4 Anin1_ovl bit 5 E ovl bit7 Oellff butonpresed O Select configuration O off 1 EStat4EL default 2 EStat2EL Ss Estatbummyt 4 EStatDummy2 5 Estatbummy3 6 EstatDummy4 P Z2lstatdEL 8 Istat2EL 9 IstatDummy 10 BiStat4EL 11 BiStat2EL Returns measured current from WE bipotentiostat Set filter for int 0 1MHz 1 100kHz 2 10kHz 3 1kHz 4 10Hz ili HighSpe g i IV bistat mode int Select mode for BiStat for int O standard 1 scanning IV setdac int double Set dac on external port int 0 for dac1 int 1 for dac2 IV getadc int double Returns measured voltage on external ADC port int channelnr 0 7 int i int IV setdigout int Set digital lines on external port int is bit

Manual 2010 color - Ivium Technologies

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