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1. OK N Auto Cancel Figure 20 The settings for the external devices are defined in the hardware setup Depending on the type of instrument the control of the external device can be done through the connections provided by the DAC164 module on the front panel of the instrument or through a dedicated output for the pAutolab Il and Ill and for the PGSTAT101 M101 and PGSTAT204 The settings for each external device can be saved Each setting is identified by a unique name Saved settings can be selected from a drop down list see Figure 21 Wout Signal name External 1 y m l l Autolab LED Driver ran Autolab RDE Tkusul PL2Z1 E re CE Conversion slope plee M Conversion offset 0 M Upper limit 0 y Lower limit 0 M Figure 21 The settings are defined and saved in the hardware setup The device defined in the hardware setup can then be controlled manually in NOVA see Figure 22 15 Page Autolab display Ea a Autolab manual control UZAUT 0530 status cell manually off current range SSS LSS A External device control Autolab RDE RPM NAM Figure 22 The External device defined in the hardware setup can be controlled manually 16 Page NOVA 1 10 2 Release notes Released 24 07 2013 Introduction The 1 10 2 NOVA release adds the following improvements e Support for Metrohm devices in 64 Bit versions of Windows Dosino and Stirrers e Support for Avantes spectrometers in 6
2. Measured Manual 25 aera posits pH E V Add pH calibration buffer 4 000 v 4 000 f Remove 7 000 Measurement 9 000 Remove All Measured pH pH 7 833 dpH dt s 0 000 Regression 05 Voltage E V 0 049 dE dt V s 0 000 S o Temperature T C 24 66 dT dt C s 0 5 0 5 10 15 pH Slope 0 059 V pH Offset 0 000 V Accept Correlation coefficient 1 000 Print Report Cancel Figure 138 The redesigned pH Calibration interface The pH calibration tool requires the pX or the pX1000 module to be installed in the instrument Please refer to the pX tutorial available from the Help menu in NOVA for more information Redesign of the Edit Cutoff user interface The Edit Cutoff user interface integrated in the Edit Options menu has been redesigned in order to present the cutoff definition in a clearer way with respect to the previous versions see Figure 139 105 Page oI Edit Options Automatic Current Ranging Cutott Autolab control Automatic Integration Time tems E utat on WE 1 j i E UFFE nt B AS a ro a B rt i BS Signal WEH Current Action when gt Value 1 Action stop complete procedure Advanced properties Mr of detections 4 Additional cutoffs Mo Cutoff JK Cancel Figure 139 The Cutoff user interface has been redesigned for clarity Please refer to the Cutoff tutorial available from the Help menu in NOVA for more i
3. External devices Measurement general Measurement cyclic and linear sweep voltammetry Measurement voltammetric analysis Measurement chrono methods Adeasurement impedance Data handling Analysis general Analysis baseline correction Analysis corrosion Analysis impedance Plots general Plots impedance My commands H Ady command Figure 120 Right click a command to remove it from the Favorite commands group Manually removing a command from the list automatically forces the software to upgrade the 11 most used command to the favorite commands group Basic Undo Redo functionality The undo and redo functions have been added to Nova The following actions can be undone or redone e Delete command e Link or unlink command parameter e Insert or move command Note command parameters have to be edited again in order to reset them to an earlier value Two buttons have been added to the toolbar see Figure 121 Bete Sikes a PE Nae smi Se E E a Oe 2 Figure 121 The undo and redo buttons have been added to the toolbar It is possible to undo an action by clicking the 2 button in the toolbar if available or by right clicking anywhere in the procedure editor setup view or the data explorer frame analysis view and select the Undo option from the context 92 Page menu In Figure 122 this tool is used to undo the delete action performed on the CV staircase command of the Cyclic Voltammetry p
4. X Delete iR drop correction X Remove all from View Uncompensated resistance Q 208 coe Figure 91 The iR drop correction analysis tool allows to correct the data for iR drop after the measurement The Corrected potential signal is added to the original data after the calculation After the calculation the corrected data can be plotted see Figure 92 VS E 6E 5 jvs E Corrected eae ZE 5 SE 5 0 0 1 0 2 ee 0 4 0 5 0 6 0 7 0 8 0 9 Corrected potential W Figure 92 The R drop correction command can be used to correct the measured data for ohmic drop 72 Page File extension identification in Import GPES data command The mport GPES data command has been modified in order to recognize the extension of the file and assign the suitable signal names to the imported data Depending on the file extension of the specified file NOVA will import the data as detailed in Table 2 Extension Type of data Signals Plots OCW Cyclic voltammetry Linear sweep voltammetry i E i vs E OXW Chrono methods i t i vS t oew Voltammetric analysis i E i vs E Opw Potential stripping analysis E dt dE dt dE vs E onw Electrochemical noise E i t E vs t odw Multimode electrochemical detection i t i vS t Table 2 Overview of the identifiable GPES file extensions Avantes spectrometers support USB 2 0 controlled Avantes AvaSpec spectrophotometers are now directly Supported in NOVA The Avant
5. 8 More information on DIO triggers can be find in the External devices tutorial 162 Page Autolab display current Ay mA L nA IPSTAT 100 pA T owl I owl 10 pA ovl iA Ei GEE too mA 100nA 10 mA 10 n CELL ON OSC T m current range Waiting for DIO trigger OOOUO000 Figure 221 The DIO status is displayed in the lower right corner when waiting for a trigger Note the DIO connector status is verified with an interval time of 100 ms Changes to the Autolab procedures The following default procedures have been added to the Autolab group in the setup view e Linear sweep voltammetry potentiostatic e Linear sweep voltammetry galvanostatic e Differential pulse voltammetry e Square wave voltammetry e Sampled DC polarography e Chrono amperometry high speed e Chrono potentiometry high speed The following Autolab procedures have been renamed for clarity purpose e Cyclic voltammetry linear scan previously called Linear scan e Cyclic voltammetry linear scan high speed previously called High speed linear scan e Chrono amperometry At gt 1 ms previously called Chrono amperometry e Chrono potentiometry At gt 1 ms previously called Chrono potentiometry 163 Page The following Autolab procedures have been removed from the list e Cyclic voltammetry with EQCM e Cyclic voltammetry with BA e Cyclic voltammetry with ECD Specific instructions on how to use these three modules are provi
6. Add Plot to MeasurementPlot2 ivsE Add Plot to Measurement Flot3 Ivst N Add Plot to Measurement Plot4 Logi vs E Log i vs Log t E wsi Evst E vs Logi E vs Log t Figure 127 Adding a plot to the CV staircase command Note the list of plots available in the right click menu depends on the signals measured by the command These signals are specified in the signal sampler Modification of the plot options in real time It is now possible to change the plot options while the procedure is running All the plots generated by a given command are now listed in the procedure progress frame Right clicking a plot displays a menu through which the plot options can be edited see Figure 128 File View Profile Run Tools Help De S M Sa a Cyclic voltammetry potentiastatic Tired procedure Autolab control Wait time 5 e Optimize current range C staircase Set cell Plot Options X A Delete 96 Page Figure 128 It is possible to change the plot options while the measurement is running by right clicking a plot in the measurement progress frame Note the same menu can be used to delete the plot see Figure 128 Create Windower from X axis A new way of using the Windower tool has been added to the analysis view It is possible to zoom in on the data shown in a plot to focus on a specific part of the plot see Figure 129 a S000 T000 B000 S000 4000 S000 2000 1000
7. Commands Farameters Links New procedure Remarks aaa End status Autolab E oignal sampler Time WWE 1 Current m Options Mo Options m Instrument Instrument description Import GPES data CAutolab TestDate Demoacv05 bow Filename CAutolabs TestDate DemoacvlS bow maa Number of columns E Fotential array Cv Current lt array A ocan lt array gt Index lt Array iws E ai heat Figure 62 The GPES data buffers bcw can now be imported into NOVA When importing data buffer files the additional files with cv1 cv2 etc must be located in the same folder as the bcw file 51 Page A Warning It is not possible to import data buffers containing data obtained using the cyclic voltammetry current integration method When importing data buffers containing a second signal accurate conversion of the second signal cannot be fully guaranteed It is recommended to review the imported data 52 Page NOVA 1 10 5 Release notes Released 15 10 2014 Introduction The 1 10 5 NOVA release adds the following improvements e Warning provided on Windows XP computers e Support for signal averaging for Avantes spectrometers e Control of the Metrohm 6 2148 010 Remote box e Improvements to the Metrohm Liquid Handling support e Automatic repair of pX1000 checksum error Installation prerequisites In order to run properly Nova 1 10 5 the following components need to be installed on the computer e
8. The Liquid Handling setup window shown for a Metrohm 858 Professional Sample Processor The following settings can be specified see Figure 45 e Name of the device e Parallel execution e Rack type using the provided dropdown list e Lift rate shift rate and swing rate for each tower e Lift work position and maximum position for each tower e The presence of pumps valves stirrer peristaltic pump 858 only and injection valve 858 only using the provided checkboxes e Towers can be deactivated if needed using the provided checkbox When a Metrohm 858 Professional Sample Processor is used Tower 2 is deactivated by default 37 Page An important parameter which can be defined for each connected device is the Parallel execution mode When this setting is active a Liquid Handling device will not block the procedure while it is executing an action allowing the next command to run and the procedure to continue If this setting is not active the device will hold the procedure until the action being carried out by the device is finished One additional command Wait for Metrohm device has been added to force the procedure to wait for a Metrohm device with the Parallel execution enabled To illustrate this four examples are illustrated in Figure 46 In this figure the duration of the Dose commands is shorter for Dosino 1 than for Dosino 2 Dosino 1 Dose Dosino 2 Dose CV Staircase A 3 Time Dosino 1 Dose Dosino 2 Dose B
9. 200 Page External devices support This version of NOVA also supports the RS232 communication protocol which can be used to control external devices like water baths stirrers valves etc The External devices commands are located in the External devices group see Figure 271 ee External devices External device initalize External device send External device receive External device close Figure 271 The External devices commands can be used to setup a RS232 communication protocol More information about the External devices control can be found in the External devices tutorial 201 Page NOVA 1 3 Release notes Released 01 04 2008 Introduction These notes provide an overview of the new features introduced in NOVA 1 3 compared to the previous release The following items have been added to NOVA 1 3 A number of tutorials available from the Help menu Support for the modules e Booster 10 A e Booster 20A Support for the instruments e PGSTAT 100 e PGSTAT 30 302 N e PGSTAT 12 Improvements and additions e NOVA 1 2 and NOVA 1 3 on the same computer e Improved Chrono methods e SCANGEN SCAN250 together with the ADC164 e New linking behavior e Printing links procedure setup e Reverse compatibility with version 1 2 e Diagnostics e Signal set s for each measurement command e More than one signal set in the measurement view e Clear plot measurement e Manual scaling during measurement
10. Improved Autolab control interface The Autolab control command is available from the measurement group in the commands browser This command defines hardware settings of the instrument like the selected current range the cell status the bandwidth of the potentiostat galvanostat etc The Autolab control command is already available in NOVA 1 2 This version of NOVA introduces some user interface changes To use this command click on the tJ button located on the right hand side see Figure 299 223 Page Procedure Values New procedure Remarks End status Autolab Collection m Signal sampler Time WE 1 Current m Options No options m E Timed procedure Autolab control Figure 299 Opening the Autolab control user interface Figure 300 shows a typical view of the Autolab control interface For each hardware module with manual settings a list of items are available in Figure 300 the settings for WE 1 WE 2 and DIO are available Autolab control WE 1 WE 2 DIO 1 P1 A Direction Unchanged PF1 A Wnrte Unchanged P1 B Directon Unchanged P1 B Write Unchanged P1 CLower Direction Uncha Cell Unchanged Cell Unchanged Current range Unchanged Bandwidth Unchanged Mode Unchanged Current range Unchanged Potential Unchanged BA Mode Unchanged IR compensation Unchange FRA input Unchanged IR compensation value Unc FRA input Unchanged External input Unchanged scangen input Unchanged Oscillat
11. Measurement View Analysis View ser lag Fil Autolab display F10 FRA manual control MEE manual control lt ru e 00 fs Add remove MUs manual control panel in Autolab display Figure 185 Adding the MUX manual control panel to the Autolab display Another example is shown in Figure 159 and Figure 160 see section 0 Each panel provides additional manual control over the instruments or the accessories connected to the instrument see Figure 186 Autolab display A Autolab manual control AUTS30 2 status current range A MUA manual control Ative channel Select 0 4 MUX L Figure 186 The MUX manual control panel provides a direct interface to the MUX module 139 Page At any time the panels can be collapsed and expanded by clicking the button in the top left corner of each panel see Figure 187 Autolab display A Autolab manual control AUTS30 2 status current range a w MUX manual control Figure 187 Collapsing the MUX manual control panel Pressing the button expands the panel again Current interrupt and positive feedback procedures Two current interrupt procedures i Interrupt and i Interrupt high speed are now provided in the Autolab group of procedures These procedures can be used to determine the uncompensated resistance of the cell using the current interruption method The i Interrupt high speed procedure uses the fast sampling ADC module ADC10M or ADC75
12. Maximum time 3 10 Filter On ma Filter time 3 0 02 WEN Fotential lt empty Cv ovfoE lt empty s v t lt array gt 5 ith E ws E maj 1 Build E vs t plot A Calculate signal thal th aa E ws t m lt gt Figure 53 Overview of the PSA procedure The PSA command also provides a filter option default on When the filter is on the filter time can be specified The default filter time is set to 20 ms for 50 Hz line frequency or 16 67 ms for 60 Hz line frequency The voltage measurement E vs t is used to calculate the retention times dt dE vs E Figure 54 show an example of the E vs t measurement and the resulting peak shaped plot 44 Page Deposition time Potential stop Time stop dt dE Peak voltage Figure 54 Schematic overview of a PSA measurement E vs t measurement top and dt dE vs E plot bottom The Peak voltage position is characteristic of the substance the Peak area is proportional to its concentration Time derivative signals added to Signal Sampler For each signal provided by the Signal sampler with the exception of the time signal itself the time derivative can now be sampled and displayed in real time see Figure 55 45 Page Pi Edit Sampler 0 Signal sample Optimized didt Sampler configuration WEI Current Sampler WE 1 Potential Segment WEG Power fe AWE 1 Potential WE 1 Resistance segment Optimized WE 1 Charge o WE Current E
13. Simplified interface with Profile menu A profiling scheme has been added to Nova Using this tool it is possible to hide some commands in order to simplify the user interface The profiles can be adjusted using the dedicated Profile menu see Figure 101 File View Profile Run Tools Help be Te Plas Harchvare basecd Basic X Intermediate Advanced Corrosion Education Electroanalysis Energy Interfacial electrochemistry Semiconductors Reset user profile Import user profile Export user profile Hide Ctrl H Unhide Ctl Shift H Show all Figure 101 The profile menu can be used to set the user profile The profiles are grouped in three sections e Level based mandatory set to Intermediate by default e Hardware based optional e Application based optional 3 Please refer to the Getting started manual for more information 79 Page Level based All the commands and the procedures in Nova have been tagged with three levels basic intermediate and advanced When the basic profile is active only a few simple commands are shown when the advance profile is active all the commands are shown see Figure 102 Commands Procedures Commands Procedures Favorite commands l Favorite commands l l Control Control Metrohm devices External devices i Measurement general z Set potential e Timed procedure Set current Autolab control Setcell e Bet potential
14. iy Downloads l Subfolder 2 7 8 2013 11 21 File folder Recent places Subfolder 3 7 8 2013 11 21 File folder Dropbox Libraries amp Computer a Network 3 items Figure 34 Subfolder can be created in the root folders used in the Database manager of NOVA Commands Frocedures 5 Subfolder 1 fn ox module tutorial Cyclic voltammetry with pes be pss UU0 module tutorial Cyclic voltammetry with p71 000 Subfalder 2 z MUs tutorial 1 Control of the bilis through an Input box e MU tutorial 2 Control of the Wis through the Autolab control command 2 H MUX tutorial 3 Control of the MU through the Repeat tor each value command 5 Subfalder 3 m Booster 0A test CY i Booster 0A test CY H My procedures Figure 35 The subfolders created in the root folder defined in the Database manager of NOVA are displayed in the procedure browser Note A subfolder will only be displayed if there a procedure files located into the folder Note A subfolder cannot be created in NOVA The folders must be created in Windows Explorer 27 Page Multiple warning error validation tooltip in procedure editor The procedure editor of NOVA validates the procedure in the background and displays warning symbols or error symbols where applicable When the mouse pointer is now located on top of one of these symbols the tooltip shows up to three errors or warnings in the same tooltip see Figure 36 Co
15. or versus the measured open circuit potential When the potential is specified versus the reference electrode REF the potential will be applied on the cell using an implicit offset potential of O V When the potential is specified versus the open circuit potential the potential will be applied using an implicit offset potential equal to the OCP value Note An OCP determination command must be present in the procedure in order to be able to specify a potential versus OCP For all the measurement commands that allow the potential parameters to be edited in the procedure editor the right click menu can be used For the Chrono methods command which uses a dedicated editor this toggle is provided in the editor itself as shown in Figure 38 30 Page hers Chrono methods editor 0 Step lt Basic Text Step Step Potential 0 v Jocp Step X Duration 0 01 5 Sample Yes Interval time 0 0001 5 Estimated number of points 100 w Advanced ee av Figure 38 The REF OCP toggle is provided in the Chrono methods command editor A Warning The method described in the Open circuit potential measurements tutorial of NOVA is still supported Using the method described in the tutorial will overrule the new settings provided by this minor update of NOVA The REF OCP toggle is not available for the pulse potentials used in Square wave voltammetry Differential pulse voltammetry Differential normal pulse and Norm
16. the data point is not stored This new sampling option can therefore be used to sample baseline data using a large interval time and sample transients on this baseline with a much higher Sampling rate An example is shown in Figure 60 gt cn i E 1 Potential v 0 44 0 46 0 468 0 5 0 52 0 Set 0 56 0 58 Corrected time 5 Figure 60 Comparison of a normal Chrono potentiometric measurement blue and a Chrono potentiometric measurement using the derivative based recording red 50 Page Both curves shown in Figure 60 are recorded using a Chrono potentiometry measurement The current applied goes from 0 A to 4 mA using a dummy cell consisting of a 1000 Ohm resistor in series with a 10 uF capacitor in parallel with a 1000 Ohm resistor see Figure 61 R 1 00k0 C 10 0 uF Figure 61 The dummy cell used in the example shown in Figure 60 The blue curve is recorded using a fixed 20 ms interval time the red curve is recorded using the same settings when the derivative of the WE 1 Potential signal is lt than 2 V s When the derivative is larger than this value the values are recorded using the fast interval time of 2 ms This leads to more data points in the potential transient region Import GPES data buffer The mport GPES data command is now also able to import data buffer files The data is converted to a single data set in the NOVA file Data buffer files have the ocw extension see Figure 62
17. wAutolab III Booster 10A F Booster2 0A Power Supply Frequency Import FRA Calibration C Documents and Settings All Users Application Data Eco Chemie HardwareSetup40 xml Figure 273 The hardware setup window NOVA 1 2 and NOVA 1 3 It is possible to install both packages of the NOVA software on the same computer Installing version 1 3 does not upgrade version 1 2 However it is not possible to use both software packages at the same time and data sets obtained with NOVA 1 3 cannot be used with version 1 2 The opposite situation is possible using the conversion tools that are installed together with version 1 3 see page 9 Improved Chrono Methods The Chrono methods command introduced in NOVA 1 2 had a USB timeout limitation which meant that measurements longer than 25 seconds could not be performed This limitation was not practical for long measurements and it has been resolved in NOVA 1 3 Using the Chrono methods command it is now possible to measure the response of the electrochemical cell as long as required Figure 274 shows the potential profile for a Chrono methods measurement with a total duration of 60 seconds 40 repetitions of a sequence of three potential steps total number of points 60 000 204 Page a es 8 aaa 40 45 50 55 60 Figure 274 The potential profile obtained with a 60 s chrono methods command Note to ensure that the timing of all the events during the chrono methods
18. when NOVA is used with the instruments mentioned above in combination with the NOVA only driver the initialization of the instrument will be stopped until the firmware is updated see Figure 99 77 Page User log message Time Date Command J Outdated firmware detected on USB interface in combination with NOVA only drivers PL 11 55 34 10 13 2011 SS Outdated firmware detected on USB interface in combination with NOVA only drivers Please close the software and run the Diagnostics application to update the firmware recommended or switch to GPES compatible drivers using the Driver Manager refer to the Getting Started for more information Figure 99 The initialization of the instrument is blocked when the outdated firmware is detected on an instrument controlled through the NOVA only driver During Diagnostics an update message will be displayed if the outdated firmware is detected Clicking the Yes button when prompted will silently update the firmware see Figure 100 G Diagnostics AUT84529 File Edit Tests Results H A Windows Information mbedded Processor Test H P Embedded Processor Test adi iran niar ation a Firmware upgrade available There is a new firmware available for the USB interface Would you like to upgrade to the latest version recom m ended te Figure 100 An upgrade message is displayed when the outdated firmware is detected The firmware update is permanent and needs
19. 3 Demo Database Demo 07 High speed chrono methods ADC750 C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 08 Chrono methods ADC 164 20 steps n C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 09 Chrono methods ADC 164 with variabl C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 12 Imported pcPt GPES data nox C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 13 Imported pcPt GPES data nox C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 14 Imported GPES data nox lt Add files to list Remove files from list Create backup s Override backup s Figure 249 Adding the files to the list Note the original files will not be removed which means that you can still access the data from previous NOVA versions Click the Start button to initiate the conversion to the NOVA 1 4 file format It is possible to create a backup of the source files and to overwrite the backup files if they are already found in the source folder It is also possible to create a log file which can be useful if the conversion fails During the upgrade step the progress is displayed in real time see Figure 250 EB Upgrade to NOVA 1 4 File File C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 01 Copper deposition nox Finished C Documents and Sett
20. Description RQ Validate Circuit a R RQ R R 500 Q CNRC Ri 5 RG RCW Y0 1 00 uMho R RQ RQ R RQ Q RL R RQ Q R RL R RQ RQ RQ RQ RQ Q RT C RW C RL Figure 317 Selecting an equivalent circuit from the pre defined list Once the equivalent circuit is defined it is possible to define the initial values of the variable s of each element of the circuit To do this click an element in the frame on the left The properties of the selected element will be displayed in the frame on the right see Figure 318 FE circuit definition Mima Circuit Description Validate Circuit g R RQ R R 500 Lower limit Unit Freed S Q YO 1 00 uMho N 1 000 Upper limit User limits Value O YO Lower limit Unit Fred Upper limit User limits Value Figure 318 Displaying the parameters and properties of the selected element note the two variables used in the definition of the Q element 237 Page The following settings can be edited for each individual element e Lower limit defines the lowest possible value for the variable of the element to be used during the fitting of the data e Unit defines the unit used for the element e Fixed true false defines whether the value of the variable can be changed during the fitting of the data The default setting is false e Upper limit defines the highest possible value for the variable of the element to be used during the fitting
21. Logi vs Logit E vsi Evst E vs Logi E vs Logit Figure 114 Each icon in the popup menu is assigned to a specific action This popup menu system can be used to facilitate procedure construction and data analysis 88 Page Add comments to My commands To simplify the organisation of commands saved in the My commands group remarks can now be added to each command as shown in Figure 138 E Save command in My comm ands lo mxs Mame My command Remarks A comment can now be provided for commands saved in the Wy commands group Figure 115 Remarks can now be added to commands saved in the My commands group The remarks provided upon saving the command are displayed in a tooltip in the commands browser see Figure 116 L Commands Procedures n Favorite commands Control Metrohm devices External devices Measurement general MMeasurement cyclic and linear sweep voltammetry Measurement voltammetric analysis Measurement chrono methods Measurement impedance Data handling Analysis general Analysis baseline correction Analysis corrosion Analysis impedance Plots general Plots impedance b My commands S hiy command A comment can now be provided for commands saved in the My commands group Figure 116 The remarks are displayed in a tooltip for each command saved in the My commands group H A H H H H P H H A H H A A E Furthermore
22. NET Framework 4 e Visual C 2008 x64 When these components are not installed the Nova installer will start with the Prerequisites installation Wizard see Figure 63 Welcome to the Prerequisites Wizard The setup has determined that some of the prerequisites needed to run this program are missing This wizard will assist you in getting and installing those prerequisites Click Next to continue to the list of prerequisites Click Finish at any time to completely skip the installation of prerequisites and jump to the installation of the main program Click Cancel to cancel the installation and exit the Setup Wizard Figure 63 Prerequisites installation Wizard Click the Next button to start the Wizard Figure 64 will appear Select the Required Prerequisites and click the Next button The Wizard will detect automatically which prerequisites are already installed on the PC 53 Page Se 2 Metrohm These programs are needed for the application to run Click on the che next to a prerequisite to select it for install or to skip it Au tolab B V Name Version Action NET Framework 4 0 Required 4 0 or higher Fo Skip Visual C 2008 x64 Required 9 0 or higher Fo Install Press the Next button to install the prerequisites Figure 64 Prerequisites selection Installation of NET Framework 4 The installation of the NET Framework 4 is described in Chapter 1 3 1 of the Getting Starte
23. Page The circuit definition window will be displayed see Figure 315 This window can be used to define the equivalent circuit used to fit or to simulate the data as well as the initial conditions for the calculation E Circuit definition R RQ Validate Circuit i Lower limit Unit R R 500 0 Fixed S Q Y0 1 00 uMho N 1 000 Upper limit User limits Value E YO Lower limit Unit Fred Upper limit User limits Value Figure 315 The circuit definition window To define the equivalent circuit click the Circuit description field in the top section of the window and type the expression used to define the circuit The following convention is used e Items between are in parallel e Items between are in series For example the equivalent circuit displayed in Figure 316 is defined by e R RQ where the first R corresponds to Rs the second R corresponds to Rp which is in parallel with a constant phase element Q Oa Rp Figure 316 A simple equivalent circuit Randles cell 236 Page Once the equivalent circuit is defined click the Validate circuit button to create the circuit It is possible to choose an equivalent circuit from a pre defined list of typical circuits To do this click the drop down list button in the Circuit description field and select the required circuit from the list Figure 317 Press the Validate circuit button to create the circuit EE Circuit definition Circuit
24. Simulation data analysis tool for impedance spectroscopy data Using this tool it is possible to create an equivalent circuit graphically using the individual circuit elements and connections between these elements see Figure 195 Equivalent Circuit Editor _ OK Circuit Edt Tools Properties C F Fitted E C Fixed Iw 7 Apply limits YO 100 pMho input 7 Output ae Figure 161 A graphical circuit editor has been added to the Fit and Simulation analysis tool Note equivalent circuits can also be created using the traditional CDC syntax Fit results can be exported easily using the included reporting tool see Figure 162 123 Page a Circuit Report mj X Estimated Error 74 Wncompensated resistance R 75 878 0 265 Nereis Palorzaionesitence R 28s o2 Element Parameter Walde Figure 162 The Circuit Report tool can be used to view the results Moreover an additional user defined database in which equivalent circuits can be stored for future use has been created This database can be defined through the database manager see Figure 196 Database management Procedures standard CADocuments and settings Usernhy Documents My Procedures 1 6 standarc cal ser CADocuments and Setings UJsern My Documentsi My Procedures 1 6 Procedures Measured data Data CADocuments and Settings UsernMy Documents My Procedures 1 6 Novea Commands Commands CADocuments and Seting
25. Validation results 0 The following problems were encountered during validation Message Command AUTS0002 amp Cell is switched off Optimize current range CV staircase Hoane Dy OK Cancel Figure 14 Right click a warning in the validation screen to ignore it It is not possible to hide Error messages It is also possible to reset the warning levels back to normal This can be done by opening the NOVA Options from the Tools Options menu In the NOVA options dialog click the l button located next to the Hidden warning Reset option see Figure 15 11 Page Nova options n Graphics 4 Basic Auto save measured data Yes Clear measurement plot before start Yes Hidden warnings Reset Ea Switch to measurement view when stat measurement Yes Time out in seconds for the validation dialog 30 o Expert Figure 15 Click the button to reset the hidden warnings Link to Windows Explorer for database A direct shortcut to the location of a procedure file or data file has been added to the right click menu in NOVA Right clicking a procedure entry in the Setup view or a data entry in the Analysis view provides a Show in Windows Explorer option see Figure 16 Commands Procedures H Avutolab 5 Standards S My procedures g ser manual example Export procedure Delete proceclure s a A Show in Windows Explorer Figure 16 A shortcut to the location in Windows Exp
26. analysis tool is also available as a command in the Analysis general group of command This analysis tool can only be used in combination with data sets that include the Time WE 1 Current and WE 1 Potential or ECN 1 Potential see Figure 178 133 Page a Chrono amperometry At gt 1 ms a iwst Plot Options Properties Add Windower Generate index Add Plat Show All Plots Hide All Plots Save in My commands A Delete Remove all from View Figure 178 The ECN Spectral noise analysis command has been added Typical electrochemical noise analysis options are available in this analysis tool It can be used to construct power spectrum density plots of potential current and impedance for graphical analysis of noise data Additional statistical indicators like noise resistance pitting index kurtosis and skewness are automatically calculated see Figure 179 ECN Measurement Record signals gt 1 ms Hem E vst Hem vst 0 1 oa log E PSD vs logi A 0 01 log l PSD vs logg logih vs logi 0 001 Skewness E 0 110425 Kurtosis E 2 42045 skewness 0 0634856 Kurtosis 1 43283 Noise resistance 266 631 Pitting index 0 532564 1E 5 1E 6 1E 0 0001 1E 5 1E 6 Potential PSD V Hz Current PSD A Hz 1E f 1E 8 1E 9 1E 10 0 01 0 1 1 10 Frequency Hz Figure 179 An example of ECN spectral noise analysis data Pl
27. are currently selected indicators are now displayed on the right hand side of the status bar These indicators facilitate the identification of the active profile in NOVA see Figure 75 User log message Command gt Start Ready Harchvare basecl Basic Electroanalysis Figure 75 Active profile indicators are now shown in the status bar Hidden commands warning Depending on the active profile some commands can be hidden from view in the procedure editor To warn the user about this a message is now displayed in the status bar of NOVA see Figure 76 User log message Time Date Command i Autolab USB connected u34UT 70530 11 56 38 3 26 2012 gt Start Ready Some commands or command parameters are hidden by the active profile Basic Figure 76 A warning is shown when commands are hidden by the active profile To reveal the hidden commands select the Show all option from the Profile menu or adjust the active profile using the same menu Check for update on startup If the computer is connected to the internet NOVA will check if a new version is available for download from the Metrohm Autolab website on startup If a new version is available an indication will be displayed in the connection manager in the lower right corner of the screen see Figure 77 Autolab interface A new version of Nova is available 1 9 Click here for more information Connected devices 0 Figure 77 A messag
28. available for Avantes spectrometers A new command parameter has been added to the Arantes initialize command see Figure 70 E Avantes initialize z Seral number Start wavelength nm 250 stop wavelength nm 600 Integration time ms 500 Number of averages gt Figure 70 The number of averages parameter has been added to the Avantes initialize command This parameter can be used to specify the number of averages to use when acquiring a spectrum according to the method specified in the External devices tutorial available from the Help menu in NOVA The use of the averaging option can improve the signal to noise ratio of the measured spectra as shown in Figure 71 57 Page 2200 2000 1800 1600 1400 Measured value a u 1200 1000 VV yl ll Al if Wi HL 600 300 290 40g 450 S00 S20 BOO 650 Wavelength nm Figure 71 Example of data acquired using the Avantes spectrometer blue curve no averaging red curve 100 averages Note Each acquired spectrum stored in the Avantes spectrometer will be the average of the number of specified number of averages When the averaging option is used the total integration time used for each averaged spectrum is given by the specified integration time multiplied by the number of averages A Warning It is necessary to update the firmware of the Avantes spectrometers to version 000 031 000 001 Contact Metrohm Autolab info metrohm autolab com for mo
29. backup s Override backup s Idle Figure 251 When the upgrade application has finished the converted nox files will be ready for NOVA 1 4 Note if the location of the NOVA source database is the My Documents My Procedures 1 x folder the converted files will be automatically copied to the My Documents My Procedures 1 4 folder If the source database is located in another folder the same folder will be used as location for the NOVA 1 4 nox files New data analysis framework and data analysis tools The data analysis framework has been redesigned It is now possible to add data analysis tools directly to the data in the Analysis view by using a context menu By right clicking on a plot in NOVA in the data explorer frame it is possible to add analysis tools directly to the plot see Figure 252 Demo 01 Copper deposition CV staircase 0 0009 fr Evst H E vs i 0 0008 H ivst 0 0007 o Plot Options Properties SG Smooth Show All Plots Baseline Correction Hide All Plots Save in My commands Regression X Delete Derivative EENAA Integrate LL Corrosion Rate gt Z 0 Hydrodynamic i vs Vw 0 0001 Energy vs Power 0 0002 0 0003 0 0004 0 2 0 02 04 0 6 0 8 1 Potential applied V Figure 252 Adding a peak search to a CV staircase plot 2 Analysis tools added to a plot are displayed directly in the data explorer frame and the control parameters of the selected tool are acces
30. can be used to troubleshoot an instrument or perform individual tests to verify the correct operation of the instrument It requires the standard dummy cell with the WE lead and the S lead if present connected to the a circuit of the cell It also requires a BNC cable connected between the ADC164 channel 2 to the DAC164 channel 2 on the front panel of the instrument In order to perform the tests the diagnostics tool must be configured according to the instrument type The configuration of the diagnostics tool is done using the select menu see Figure 285 211 Page 4s Diagnostics UAutolab UAutolab FRA DA Converter Test Potentiostat Test Noise Test AC Voltammetry Test Galvanostat Test Progress PO Figure 285 Setting the hardware selection in the diagnostics tool from the Select menu For all the PGSTATs the Autolab setting should be selected For the uAutolab and the pAutolab with FRA module a specific setting should be used instead Pressing the start button will initiate all the selected tests The connection with the instrument will be established by the diagnostics tool during the Embedded Processor Test During the test the progress will be displayed and a successful test will be indicated by a green symbol see Figure 286 212 Page w Diagnostics Windows Information Embedded Processor Test EEProm Test Timer Test Autolab Test AD Converter Test DA Converter Test Potentiostat Test Noi
31. control panel Potential Stripping Analysis PSA methods The Potential Stripping Analysis PSA and Constant Current Potential Stripping Analysis CC PSA methods have been added to NOVA These methods provide the means to perform a potentiometric stripping analysis with chemical oxidation or with a constant current in order to determine substances in an organic matrix with the aid of mercury film electrodes without prior digestion 43 Page In PSA measurement mode the analytes are deposited at the working electrode with the constant deposition potential during a predetermined deposition time Then the applied deposition potential is switched off and the cell voltage is measured as a function of the time with the highest possible sampling rate In CC PSA the same strategy is applied but after the deposition time a constant current is applied The cell voltage is measured as a function of the time with the highest possible sampling rate The measurement time is limited either by the Potential limit or the Maximum time criterion defined in the procedure see Figure 53 Commands Parameters Links Potentiometric stripping analysis Remarks Potentiometric stripping analysis m End status Autolab aaa signal sampler Mo signals ma Options Mo Options m Instrument UWSALIT 70530 Instrument description Autolab contral J H Set potential 0 800 Set cell On it at time 3 z E Potentiometric stripping analysis Fotential limit v 0 001
32. gt Hz a Fi lt _ array gt m Td lt _ array gt 0 rr Fi lt amay gt 0 m Phase lt _ array gt m Bode plot modulus Graphical settings General settings x Frequency Hz Y Z 0 Z Fhase Bode plot phase Graphical settings General settings m x Frequency Hz Y Phase Fi Z 0 Nyquist plot Graphical settings General settings x Z O Y 0 Fi Frequency Hz Figure 306 The Import FRA data command Find circle for impedance data Analysis of the data obtained during an electrochemical impedance measurement is usually performed by fitting the experimental data with an equivalent circuit based on the Boukamp model In order to help in the estimation of the parameters of the equivalent circuit an electrochemical circle fit tool is available from the Baseline tools This simple tool calculates the values of the elements of the equivalent circuit shown in Figure 307 using the measured data points of a circular portion of the Nyquist plot corresponding to a single time constant a Rs Figure 307 The equivalent circuit used in the Electrochemical circle fit tool 229 Page This circuit includes the following items e Rs Ohm used to simulate the value of the uncompensated resistance e Rp Ohm used to simulate the polarization resistance also referred to as the charge transfer resistance e CPE the value of the argument of the constant phase e
33. it is possible to edit the remarks assigned to saved commands by right clicking the commands in the My commands group see Figure 117 89 Page s Commands Procedures t Favorite commands Control Metroahm devices External devices Measurement general Measurement cyclic and linear sweep voltammetry Measurement voltammetric analysis Measurement chrono methods Measurement impedance Data handling Analysis general Analysis baseline correction Analysis corrosion Analysis impedance Plots general Plots impedance My commands ze hiy comman Edit Rem arks X Export comm andl xo Delete Figure 117 Right click the commands saved in My commands group to edit the remarks Favorite commands group A new group called Favorite commands has been added to the Commands browser see Figure 139 i Commands Procedures Ep Favorite commands Control Metrohm devices External devices Measurement general Measurement cyclic and linear sweep voltammetry Measurement voltammetric analysis Measurement chrono methods Measurement impedance Data handling Analysis general Analysis baseline correction Analysis corrosion Analysis impedance Plots general Plots impedance My Commands Figure 118 A Favorite commands group has been added to the Co
34. literature A total of six methods are available e Time semi derivative this algorithm uses a semi derivative transformation of a time dependent function f t according to 17 Page d 2 rI dt 2 fC e Time semi integral this algorithm uses a semi integral transformation of a time dependent function f t according to do eee e GO differintegration Grunwald 0 this algorithm can be used to carry out differintegration to any user defined order For the order of 1 the operation is equivalent to a derivative and for 1 to an integration For 0 5 the GO algorithm is the same as the time semi derivative method For 0 5 the GO algorithm is the same as the time semi integral method Error in results increases with the length of the interval and accumulates i e error in latter points is larger than in earlier ones Important advantage is that this algorithm does not require the value of the function for t 0 which makes it very well suited for transformation of chronoamperometric data where i 9 gt 0 The disadvantage of the algorithm is that the total number of operations is proportional to the square of the number of data points so calculation time grows fast with the length of the data set The fundamentals of this algorithm are described in Oldham KB J Electroanal Chem 121 1981 431 e FRLT differintegration Fast Riemann Liouville Transform this is a fast approximate algorithm based on a recursive digital
35. menu It is also possible to Cut Copy and Paste a group of commands Manual control of External devices Manual control of analog controlled external devices is now available like the Autolab RDE or the Autolab LED Driver The parameters of the external device connected to the Autolab can be defined in the Hardware setup see Figure 20 14 Page Hardware setup File Tools Main Module Additional Module s ADC164 1 Y PGSTAT302N _ FRA32M l _ PGSTAT302F FRA Signal name L PGSTAT302 T JADCIOM _ PGSTAT30 M ADC750 Signal unit __ PGSTAT30 AUT T ADC 50r4 l _ PGSTAT128N SCAN25O Conversion slope PGSTAT12 m PGSTATIOON Conversion offset m PGSTAT100 T PGSTAT100 AUTS o aa ADC164 2 PGSTAT101 M101 F120 Filter Signal name T wAutolab Ill __ Fl20 Integrator pAutolab Il __ Booster20A Signal unit _ PGSTAT204 _ Boosterl 0A PGSTAT20 _JEQCM Conversion slope pose ARa Conversion offset ECN J DAC164 1 External cable u utolab eae cable JAutolab Signal neme _ IME663 Signal unit MUX Conversion slope Conversion offset Upper limit Lower limit Power Supply Frequency 50 Hz v Import FRA2 Calibration AT C Program Data Metrohm Autolab 11 0 HardwareSetup xml External 1 v H Y 1 VIV 0 Vv External 2 v H Y 1 MY 0 Vv External 1 v m Vv 1 Vi 0 Vv 0 Vv 0 Vv
36. mode the offset value must first be set to 50 mA using the Autolab control command see Figure 228 Autolab control WE DG DACH Cell Unchanged Current range 10 mA Bandwidth Unchanged Mode Galvanostatic IR Compensation Unchanged IR Compensation value Unchanged Reference potential Unchanged Set Offset Value 0 05 X Figure 228 The offset value must be set to 50 mA in order to apply 100 mA in the 10 mA current range 169 Page Autolab control The Autolab control command has been adjusted for the PGSTAT101 see Figure 229 Autolab control DIO DAC Cell Unchanged Current range Unchanged Bandwidth Unchanged Mode Unchanged IR Compensation Unchanged IR Compensation value Unchanged Reference potential Unchanged Cittset Value Unchanged Cancel Figure 229 The Autolab control window has been adjusted for the PGSTAT101 TTL triggering The PGSTAT101 is fitted with a single non configurable DIO connector The DIO connector has a total of eight write lines and four read lines see Figure 230 170 Page 9 OUT2 3 Isolated GND 6 OUT4 Port A 15 OUT7 14 owe 10 IN4 14 OUT5 DGND 13 OUT3 12 OUT Figure 230 Mapping of the PGSTAT101 DIO connector Note Port A includes 8 write lines and two digital ground pins pin 4 and pin 11 Port B includes 4 read lines and an isolated ground pin pin 3 All pins on Port B are
37. now available from the measurement group in the commands browser This command samples the WE 1 Potential during a pre defined time see Figure 303 S OCP determination 0 000 Signal sampler Time WE 1 Potential ma Maximum time s 120 dE dt limit 1E 06 Use average OCF Yes ca OCF value 00 WE 1 Potential lt _armay gt V Time lt _aray gt s G Evs t Graphical settings General settings m x Time Y WE 1 Potential V Fa Time s Figure 303 The OCP determination command 226 Page The OCP determination command has the following parameters e Signal sampler defines the signals that are sampled during the OCP determination WE 1 Potential and Time are the default settings e Maximum time s defines the maximum duration of the OCP determination e dE dt limit defines an optional cutoff value for the derivative of the OCP if this value is set to O the dE dt limit is not used e Use average OCP yes no this settings defines whether the moving average the OCP values measured during 5 seconds should be used in the determination of the OCP or if the last measured OCP value should be used instead The OCP determination command comes with a signal set which displays the WE 1 Potential versus time during the measurement A second window is also displayed during the measurement displaying real time information about WE 1 Potential and dE dt see Figure 304 OCP determination Latest value Average Min
38. of the data e User limits yes no defines whether the Lower and Upper limit should be used during the fitting of the data Default setting is yes e Value defines the initial value of the variable of the circuit element Note some circuit elements have more than one variable The fitting parameters can be defined for each variable independently see Figure 318 Once the fitting conditions have been defined the calculation can be performed Fitting the data using an equivalent circuit To start the fitting algorithm click the button located in the toolbar This will start the calculation using the defined equivalent circuit and the initial conditions for each element If the fitting calculation succeeds the calculated data points will be plotted in the 2D plot area overlaying the original data set see Figure 319 The area below the 2D plot area is updated after the calculation A table is displayed on the left hand side showing the calculated values of the total impedance the real and imaginary components and the phase angle see Figure 319 The Fit and simulation control interface is also updated and displays the number of iterations required to reach the final result and the final value of the Chi square parameter 2 238 Page 1000 800 600 S N 400 200 0 0 200 400 600 800 1000 Z Q E Input Modulus Imaginary Phase Real Max number of Iterations 100 100 01515328 1 5915
39. see Figure 321 The calculated values and the estimated error are displayed for each element 239 Page EIl Circuit definition Circuit Description R RQ E R RQ ChiSquare 3 800e 010 Iterations 5 1 000 R R 100 Q 0 000 Lower limit 0 RQ Unit R R 1 00 kQ 0 000 Fixed False Q Y0 1 00 Mho 0 000 N 1 000 0 000 Upper limit 10E 0001 User limits Yes Value 0 99999 721732842362 O Yo 1 00 EMho Lower limit 1E 15 Unit Mho Fixed False Upper limit 10E0004 User limits Yes Value 1 0000 18262393 1581E 06 Figure 321 The detailed results of the fit calculation The frame on the right displays the detailed calculated values of each variable for the selected element Note if the fit calculation is not complete after the maximum number of iterations it is possible to resume the fitting using the last calculated values of each element of the equivalent circuit To do this check the Use result as circuit check box in the Results window and press the analyze button to restart the fit calculation using the last values as Initial conditions see Figure 321 To save the results of the fitting click the button located in the toolbar This will add the calculation to the data set which will be available as a new signal set in the data explorer see Figure 322 a New procedure 10 3 2007 10 30 56 PM ew Import FRA data J Bode plot modulus Bode plot phase x Nyquist plot Simulation J Bode
40. 0 These procedures can be used with all the instruments fitted with the iR compensation circuit Figure 188 shows an example of current interrupt measurement recorded using the provided procedure on the Autolab dummy cell gt This option is not available with the PGSTAT10 and the pAutolab III 140 Page V Fotentia Fil J 0 0005 0 001 0 0015 Time from interrupt is Figure 188 Example of data obtained with the i Interrupt high speed procedure The recorded potential transient is automatically fitted and the calculated value of the uncompensated resistance is displayed in the Autolab display window Figure 189 The transient is fitted using an exponential regression and a linear regression yielding values of Ru exponential and Ru linear respectively Note the commands used in the i Interrupt and the i Interrupt high speed procedures are available in the Measurement general group 141 Page Autolab display A Autolab manual control AU T84844 PSTAT status current range Ru exponential Ru linear 99 01 2 121 3 LO _ Figure 189 The results of the fitting of the transient are shown in the Autolab display Additionally a Positive feedback procedure is supplied in the Autolab group of procedures With this procedure it is possible to fine tune the value of the uncompensated resistance estimated from the current interrupt procedures Figure 190 shows an example of four positive feedback meas
41. 01 has been added to the list of devices in the diagnostics application Note the PGSTAT101 is equipped with an internal dummy cell When the diagnostics tests are performed on this instrument the reference RE and counter CE electrode leads must be connected together on one hand and the working WE and sense S electrode leads must be connected together on the other hand Make sure that RE CE and S WE are not in contact A reminder is shown at the beginning of the diagnostics see Figure 227 Please connect the cellconnectors as shown open Figure 227 When the diagnostics are performed with the PGSTAT101 connect RE to CE and S to WE as shown in the visual reminder 168 Page PGSTAT101 test A specific procedure to test the PGSTAT101 has been added to the Module test database default location C Program Files Eco Chemie Nova 7 5 Shared Databases Module test This test procedure can be used to verify the basic functionality of the instrument The test is performed on the internal dummy cell Refer to the Module test documentation for more information available from the Help Tutorials menu Maximum current The highest current range available in the PGSTAT101 is 10 mA This current range has a linearity of 10 times which means that a maximum of 100 mA can be applied to the cell in galvanostatic mode and that a maximum of 100 mA can be measured in this current range in potentiostatic mode To apply 100 mA in GSTAT
42. 1 Current Calculated signals ow WE Charge WE 2 Charge Figure 82 WE X Charge signals are now available in the sampler The WE X Charge signal is a calculated signal and therefore cannot be sampled in optimized mode The calculation is performed in real time which allows these new signals to be involved in the cutoff option as well see Figure 83 A Warning The charge is calculated mathematically using the so called trapezoidal method The accuracy of this method depends on the interval time and on the current derivative In most cases the calculated charge will only be a first approximation of the real charge which can be measured properly using the optional FI20 module or the on board integration 66 Page lt Edit Options Automatic Current Ranging Cutoff Autolab control Automatic Integration Time Cutoff on vvE 1 Current Basic properties signal Action when Value Action Linkable as Eytemal 1 ADCIB4 1 External 1 ADC164 2 Advanced properties Mr of detections 4 Additional cutoffs Mo Cutoff Rernove CK Cancel Figure 83 The calculated charge is available in the cutoff option Automatic offset DAC control The offset DAC described in Chapter 4 of the NOVA Getting started manual is now automatically set by the software whenever required This allows the potential or the current to be set automatically to any value within the app
43. 1000 2000 2004 2000 4000 6000 su00 10000 12000 Z L Figure 129 Zoom in on the data Next right click the plot in the data explorer frame and select the Create Windower from X axis option from the context menu see Figure 130 97 Page i TestFRA a FRA measurement potentiostatic H FRA frequency scan Nyquist 2 v a Bode modulu Bode phase x x pu Plot Options Properties Create VWindower from X axis X F My comm ands 7 Add Analysis Copy Visible Plots to Show All Plots Hicle All Plots Save in My comm andels Delete Remove all fram View Redo Insert Windower Ctl y Figure 130 Select the Create Windower from X axis option to window the visible data The software will then add a Windower item to the data which will contain all the data that fit in the visible range of values for the signal plotted on the X axis In the case shown in Figure 131 the Z values between 9 8 kOhm and 13 2 kOhm have been windowed S00 10000 10500 11000 11500 13000 Z C2 12000 12500 Figure 131 The windowed data 98 Page New plot options It is now possible to change the line plot and the combi plot in order to use a discontinued line instead of regular line see Figure 132 Through a drop down list it is now possible to choose between different line styles Plot Options Flot Flot style Line plot y axis placement Left Li
44. 12 i 0 0005 G lt 0 0001 O z T D S 0 0004 O O 6E 5 O 5 0 0003 ja ng 4E 5 ui gt SED 0 0002 0 2E 5 0 0001 4E 5 0 6E 5 0 8 1 12 1 4 1 6 0 8 1 12 14 1 6 Potential applied V Potential applied Y Figure 57 Example of a real time determination of a derivative left i vs E plot right Q vs E plot and dQ dt vs E plot As observed in Figure 57 the time derivative of the charge provides the same result as the original current measurement Fast options for the Record signals gt 1 ms command The Record signals gt 1 ms command now offers the possibility to define two different interval times e The interval time which corresponds to the time between two consecutive data points This interval time corresponds to the interval time of the previous versions of NOVA This value must be 1 33 ms e The fast interval time which correspond to a new interval time that can be used to run the Options specified in the procedure This new fast interval time must be 1 33 ms and must be an integral fraction of the interval time 47 Page Each Record signals gt 7 ms command offers the possibility to use the fast options through the Use fast options toggle see Figure 58 When the fast options are not used the fast interval time parameter is not shown in the procedure editor Record signals gt 1 ms Duration s p Interval time s 0 2 Estimated number of points ZE oignal sample
45. 1650 Interval time Lis 24400 Signal sampler Time WE 1 Potential WE 1 Current m Fotential applied lt _amay gt V Scan lt aray gt WE 1 Potential _array gt VW array s A i WE 1 Current airay gt A Givs t Graphical settings General settings ca X Time 8 Y WE 1 Current A Fi Potential applied V Set cell Off lt gt lt gt Figure 291 Modifying the links used for the Signal set will change the way the data is displayed during the measurement More than one signal set in the measurement view It is possible to add more than one signal set to a measurement command Each signal set will be displayed in the measurement view which means that it is now possible to plot more than one signal in real time For the Cyclic voltammetry procedure this can be achieved by dragging a Signal set command from the command browser and drop on the CV Staircase command see Figure 292 216 Page File View Run Tools Help ante ee eek ee es a Commands Procedures Control Inputbox Messagebox Repeatn times Repeatfor each value Increment parameters Increment parameters with signal Play sound Measurement Timed procedure Autolab control Set potential Set current Set cell Set reference potential Wait time s CV staircase CV staircase galvanostatic CV linear scan high speed CV linear scan LSV staircase LSV staircase galvanostatic Record signals gt 1 ms
46. 3 0 069135 0 097145 Peak 1 2 0 031234 0 080468 0 0342 0 080772 Figure 254 Data analysis results are available in the data grid 0 33142 0 2124 0 33142 0 00012439 0 20844 Reverse A Base start Base en 0 12512 0 93811 0 11715 0 69809 v gt allows for Peak sum of derivatives 0 0085256 0 1029 0 0073167 0 10011 Furthermore the results of the data analysis tools can be used to generate new plots see Figure 255 It is also possible to use the Calculate signals and Filter and select tools directly without switching to the Data grid 190 Page 1 2 1 1 1 09 0 8 0 7 06 O05 04 03 02 01 O Potential applied V Figure 255 Stacked plots and data analysis tools the red line is the original plot the black line the applied baseline correction and the blue line is the corrected plot New data handling and analysis commands NOVA 1 4 introduces a number of new data analysis commands which can be used to perform automatic data handling and data analysis The following commands have been added e Inthe Data handling group o Import ASCII o Export ASCII o Scan extractor e Inthe Analysis general group o Regression o Integrate o Calculate charge o Energy vs Power o Hydrodynamic i vs Vo e Inthe Analysis baseline correction group o Polynomial fixed order o Polynomial maximum order o Exponential o Circle e Inthe Analysis corrosion group o Corrosion rate
47. 38 40 42 44 46 48 50 52 Time s Figure 294 Real time plot for the Cyclic voltammetry procedure showing two signals plotted at the same time The blue curve corresponds to the WE 1 Potential left axis and the red curve corresponds to the WE 1 Current right axis 218 Page Clear plot during measurement The clear measurement plot button in the toolbar is now available during the measurement If this button is pressed during a measurement the plot will be cleared even if a measurement is ongoing The plotting of the data will resume after the plot is cleared Manual rescale during measurement In NOVA 1 3 it is possible to disable the automatic rescaling during a measurement Any action changing the scaling of the plot during a measurement for example zooming in or out or changing the scaling of one of the axes will interrupt the automatic rescaling feature of NOVA Pressing the F4 key will resume automatic rescaling Mathematical parser as a command The Mathematical parser command is available from the Analysis group in the command browser This command can be used to perform a calculation during the measurement or at the end ot it The mathematical parser command requires a user defined mathematical formula and a source electrochemical signal for each variable in the mathematical expression Figure 295 shows a typical example of the Mathematical parser command In this case the Mathematical parser command has been ad
48. 4 Bit versions of Windows e Convolution analysis method added to the Analysis general group of commands e Options added to the Build signal command Support for Metrohm devices in 64 Bit versions of Windows The 1 10 2 update of NOVA adds support for Metrohm devices in 64 Bit versions of Windows The files required to work with all versions of Windows are installed in NOVA installation folder All the Metrohm devices are supported except the Sample Processors 814 815 and 858 The warnings used in the External devices tutorial regarding incompatibility with 64 Bit versions of NOVA can be disregarded Support for Avantes spectrometers in 64 Bit versions of Windows The 1 10 2 update of NOVA adds support for Avantes spectrometers in 64 Bit versions of Windows The files required to work with all versions of Windows are installed in NOVA installation folder The warnings used in the External devices tutorial regarding incompatibility with 64 Bit versions of NOVA can be disregarded Convolution analysis method added to the Analysis general group of commands The convolution analysis methods have been added to the Analysis general group of commands Convolution methods can be used to eliminate the effect of the decrease of the concentration gradient of the electroactive species from the total response of the electrode For a general description of the use of the convolution methods in electrochemistry we refer the user to the
49. 69073 0 91180223 100 002488939 Circuit 100 02404264 2 003654954 1 14781055 100 003972291 ae ao aaa i 100 03813061 2 592489929 1 44488252 100 006322905 r of iterations giving no improvement m maas 100 06045162 3 175597688 1 81868959 100 010047285 aie oo 100 09581406 3 997751186 2 28895895 100 015948625 a ta Fit or Simulation Fit 100 15183718 5 032854396 2 88045459 100 025301143 Rae PT IT Ee men 100 24056030 6 335921665 3 62391955 100 040122086 S Results 100 38099991 7 976190686 4 55747935 100 063607403 hitia dF neces pa 5 100 60316599 10 04100996 5 72811962 100 100824806 Result ae 100 95426806 12 64030497 _ 7 19278081 100 159806960 Chi square 3 8E 10 Figure 319 The 2D plot area is updated after the fit the black line plot corresponds to the calculated data To view the fitted circuit elements click the button located next to the Result field in the fit and simulation control interface see Figure 320 E Input Max number of Iterations 100 Circuit Circuit Maximum change in chi square 0 001 Maximum number of iterations giving no improvement 100 Fitting style Impedance Use weight factors Yes Fit or Simulation Fit Measurement data format Impedance E Results Number of iterations performed 5 Result Circuit A Chi square 3 6E 10 Figure 320 Opening the results window This opens a new window similar to the one used to create the equivalent circuit
50. A measurements 146 Page Ee Measurement voltammetic analysis Timed procedure for voltammetric analysis Diferential pulse SQUare wae sampled DL Normal pulse Diferential normal pulse Figure 193 The Voltammetric analysis commands Note it is possible to use these commands in polarographic mode refer to the user manual for more information Alongside the VA measurement commands additional commands to control the mercury drop electrode have been added to the Measurement general group see Figure 194 e Purge this command defines the duration of the purge step the stirrer is always switched on when the N purging is on e Set stirrer this command controls the stirrer of the VA stand e Create new drop this command creates n new drop by activating the drop knocker on the VA stand al Timed procedure Autolab control set potential set current set cell Wait time s Optimize current range OCP determination set reference potential set BIFOT potential cet pH measurement temperature Reset EQICM AFrequency Control Autolab ROE switch Autolab ROE otf Control external device DAC aait for DIG tricia fa Furge Set stirrer Create new drop Figure 194 Three additional command related to the control of the mercury drop electrode have been added to the Measurement general group 147 Page Manual control for Mercury Drop Electrode MDE Manual control over the Mercury Drop Electrode MDE is provid
51. B Interval time s 0 01 Estimated number of points ili Signal sampler Time WE Potential WWE Current dw ECT Currentidt Options 1 Options a Use fast options YES a Fast interval time s 0 01 Corrected time lt array gt 5 CWE Currentidt sample threshold As 0 Time lt array gt 3 WWE Potential array gt V4 WWE Current array A cvWwE Currentict array A S Index lt arrary gt 7 1s t z Set cell Off a 4 Figure 59 The sample threshold parameter is available by combining the time derivative sampler with the fast options 49 Page The default value of this new parameter is set to 0 The units of the parameter are indicated in the procedure editor When the fast options are used the fast interval time must be an integral fraction of the interval time parameter When the command is executed the measurement proceeds according to the information provided in Sections Error Reference source not found and Error Reference source not found The derivative s signals are calculated using the fast interval time and compared in absolute value to the specified threshold value for derivative signal after each fast interval time e If the absolute value of the derivative is higher than the specified threshold value a data point is stored e In all other cases the absolute value of the derivative is lower or equal than the specified threshold value or the specified threshold value is 0
52. Chrono methods Chrono methods high speed Optimize current range FRA frequency scan Control external device Analysis Build signal Signal windower Mathematical parser SG Smooth Automatic peak search Derivative Import GPES data Import FRA data Baseline Fit Procedure Cyclic voltammetry Remarks End status Autolab Signal sampler Options Timed procedure Set Potentiostatic and select current range Set cell Wait time s Optimize current range OV staircase A Start potential V Upper vertex potential V Lower vertex potential V Stop potential V Number of stop crossings Step potential V Scan rate V s Total number of points Interval time us Signal sampler Potential applied Scan WE 1 Potential Time WE 1 Current 6 ivs E Graphical settings X Y zZ amp Set cell e S lt gt fe Values Factory standard procedure a Collection Time WE 1 Potential WE 1 Current y Automatic Current Ranging WE 1 1 mA 1 s Time WE 1 Potential WE 1 Current a lt array gt V lt array gt lt array gt V lt array gt s lt array gt A General settings oa Potential applied V WE 1 Current A Time s Off Figure 292 Adding a Signal set command to a measurement command can be done by dragging A new signal set command will be available for the CV Staircase command see Figure 293 It is possible to select whic
53. Cutoff option are now shown in the tooltip Cut Copy Paste option in procedure editor A Cut Copy Paste option has been added to the procedure editor Using the right click menu or the traditional keyboard shortcuts CTRL X CTRL C CTRL V for Cut Copy and Paste respectively it is possible to cut or copy commands in the procedure editor and paste them in the procedure see Figure 19 13 Page Commands Parameters Links Cyclic voltammetry potentiostatic Remarks Cyclic voltammetry potentiostatic ma End status Autolab m Signal sampler Time WE 1 Potential WE 1 Current ma Options 1 Options rr Instrument AUT40008 Instrument description Autolab control Set potential T Epo Set cell On Enabled Save in My commands 0 2 0 1000000 Wait time s Optimize current CV staircase Set cell Delete lt gt Cut Ctrl X Ctrl C N Commands Farameters Links Cyclic voltammetry potentiostatic Remarks Cyclic voltammetry potentiostatic al End status Autolab xa Signal sampler Time WE 1 Potential WE 1 Current ma Options 1 Options c Instrument AUT40008 Instrument description Autolab control z Set potential 0 000 Set cell On j Wait time s 5 Optimize current range 5 CV staircase 0 000 1 000 1 000 0 000 2 0 10000001 lt Set cell Off Save in My commands G Paste Ctrl V Lal Figure 19 A Cut Copy Paste option has been added to the right click
54. II data command The Columns can be linked to the electrochemical signals to export see Figure 267 197 Page E CV staircase 0 000 1 000 1 000 0 000 2 0 10000 start potential V 0 000 Upper vertex potential V 1 000 Lower vertex potential V 1 000 stop potential V 0 000 Number of stop crossings Z Step potential V 0 00244 Scan rate V s 0 10000 Total number of points 650 Interval time Ls 24400 Signal sampler Time WE 1 Current Options 1 Options E Potential applied lt _ armay gt V Time lt _armay gt s WE 1 Current lt _armay gt A Scan lt aray Index lt aray gt ivs E aa S Export ASCII data Desktop Exported ASCII data txt Number of columns 2 Column delimiter Tab E Decimal separator File mode Overwrite Remarks Pre Column 1 Potential applied V Column 2 WE 1 Current A Figure 267 Using the Export ASCII data in combination with a CV staircase command Note exporting data to an ASCII file during a measurement introduces a delay in the timing The duration of the pause depends on the amount of data points G circuit element The Gerischer diffusion circuit element which is used to model the effect of a preceding chemical reaction happening in the bulk solution so called CE mechanism or the behavior of a porous electrode has been added to the list of available circuit elements in the Fit and Simulation tool see Figure 268 r e G Gerischer impedance
55. MDE Contral Figure 198 Manual control of the MUX module is provided in the View menu Through the MUX control it is possible to manually set one of the available MUX channel to active see Figure 235 MUX Manual Control Active channel Select 0 4 MUX 1 Figure 199 The MUX Manual Control can be used to select one of the available MUX channels Note control of the MUX is also possible during a measurement using the Autolab control command see Figure 200 149 Page Autolab control WE DION DACH Set Channel 0 Channel Unchanged Set Channel 0 b Figure 200 Control of the MUX is also available in the Autolab control window New Autolab control command The Autolab control command has been redesigned and now displays the available properties under tabs The number of available tabs depends on the hardware setup see Figure 201 Autolab control WE 2 iadi DACH Cell Unchanged Current range 10 4 booster on Current range Current range Current range Current range Current range Current range Current range 1 AEEA OT ETET Oscillation protection Unchanged Reterence potential Unchanged Figure 201 The new Autolab control command Note more information about the Autolab control command can be found in the Autolab control tutorial 150 Page Autolab display The Autolab display available from the View menu or through the g key has been modifi
56. NOVA Release notes previous versions Table of Contents NOVA 1 10 1 Release notes Released 08 05 2013 oo cccececcaccececeececeeeecueeeseeeens 2 NOVA 1 10 2 Release notes Released 24 07 2013 oo cccccececcecaececeececeeeeeeceeneaes 17 NOVA 1 10 3 Release notes Released 18 10 2013 ceceececcecacceceececeeeeeecueeneaes 22 NOVA 1 10 4 Release notes Released 01 05 2014 ooo ciceccececcecaececeeeeeeeaeeneaes 29 NOVA 1 10 5 Release notes Released 15 10 2014 oo ceccececcecacceceeeeeeeaeeeeaes 53 NOVA 1 9 Release notes Released 26 11 2012 ccccccececcecececcecececeeecesecueaeeess 61 NOVA 1 8 Release notes Released 01 12 2011 ccccccecececcecececcecececeeeecesecueaeeers 77 NOVA 1 7 Release notes Released 01 04 2011 oo ceeececeecacceceececeeeeeeeeeeneaeeeeaes 101 NOVA 1 6 Release notes Released 01 06 2010 0 0 cc ceeceececceceececeeceseeeeensaeeneaes 114 NOVA 1 5 Release notes Released 01 06 2009 00 0 e ce eceececcecacceceececeeeeeeeaeeeeaes 144 NOVA 1 4 Release notes Released 14 09 2008 00 0 eccccececcecacceceececeeaeeeeaeeneaes 173 NOVA 1 3 Release notes Released 01 04 2008 00 0 0 cceceececcececceceeceseeeeeneaeeneaes 202 1 Page NOVA 1 10 1 Release notes Released 08 05 2013 Introduction Thank you for installing this update of NOVA These notes provide an overview of the new features introduced in NOVA 1 10 1 The following improvements have been added to NOVA Support for 64 B
57. New plotting framework A new plotting framework has been implemented in this version of NOVA It is now possible to add pre defined plots to a procedure by dragging and dropping the plot command onto a measurement command If this measurement command provides the required pre defined signals these signals are automatically linked to the added plot The predefined plots are available in two different sections in the command browser The Plots general section contains pre defined plots used in typical DC measurements The Plots impedance section contains pre defined plots related to electrochemical impedance spectroscopy measurements see Figure 241 180 Page Plots general Custom Evs Log i E vs Logi AFrequency vs E Levich plot Power plot Plots impedance Nyquist 2 vs Z Bode modulus Bode phase Nyquist Y vs Y Residual Z Residual Z Epsilon plot MottSchottky Rs Cs MottSchottky Rs Cp Rp Figure 241 The pre defined default plots The pre defined plots are also available in the analysis view Depending on the type of measurement a number of predefined plots are available using the right click menu in the analysis view Figure 242 illustrates this feature on an impedance data set Since the data has been recorded using the FRA frequency scan command NOVA offers a number of impedance related plots Demo 16 FRA impedance oo Plot Options H Prope
58. OVA 1 7 requires the NET Framework 4 0 PGSTAT302F The PGSTAT302F is a special version of the PGSTAT302N This instrument can be toggled from normal operation mode to floating mode The regular use is intended for typical electrochemical cells in which neither the working electrode nor the electrochemical cell itself are connected to ground The floating mode is intended for grounded electrochemical cells or cells in which the working electrode is directly connected to ground Please note that the signal to noise ratio will deteriorate when working with the PGSTAT302F in floating mode When the PGSTAT302F is operated in normal mode the specifications will be identical to those of the PGSTAT302N More information on the PGSTAT302F can be found in the documentation provided with the instrument PGSTAT100N The PGSTAT1OON is the evolution to N form factor of the Autolab PGSTAT100 It can now be selected in the Hardware setup Multi Autolab The Multi Autolab is a generic frame in the same form factor as the PGSTAT302N This frame can be fitted with additional modules see Figure 136 102 Page BA BA EQCM EQCM pX1000 px1000 M101 M101 M101 M101 M101 M101 Figure 136 Example of a Multi Autolab instrument fitted with M101 modules and daughter modules BA EQCM and pX1000 The following modules can be installed in the frame M101 this is a PGSTAT101 module providing control for a single electrochemical cell The specificati
59. Remarks Factory standard procedure m End status Autolab Collection Signal sampler Time WE 1 Potential WE 1 Current a Options Automatic Current Ranging WE 1 1 mA 100 nA a E Timed procedure Set Potentiostatic and select current range m Set potential 0 000 Set cell On Wait time s 5 Optimize current range 5 E CV staircase 0 000 1 000 1 000 0 000 2 0 10000 Start potential V 0 000 Upper vertex potential V 1 000 Lower vertex potential V 1 000 Stop potential V 0 000 Number of stop crossings 2 Step potential V 0 00244 Scan rate V s 0 10000 Total number of points 1650 Interval time Us 4400 Signal sampler Time WE 1 Potential WE 1 Current m Fotential applied lt _ array gt V WE 1 Potential lt _ amay gt V Log of the current lt _amray gt Scan lt aray Time WE 1 Current ivs E B MathParser Current WE 1 Current A Set cell Off a gt ee array Pay A Figure 298 The parameters of the mathematical parser command have to be linked to the source electrochemical signals In the example shown in Figure 298 the Current parameter has been linked with the WE 1 Current electrochemical signal At the end of the measurement the values of the WE 1 Current will be used in the predefined calculation and a new electrochemical signal Log of the current will be added to the data set This calculated signal will then be available for data analysis
60. Store in database Select All b Start Selected Stop Selected Ready Figure 170 The Multi Autolab view provides an interface through which two or more devices can be controlled at the same time Note more information on the control of multiple instruments can be found in the Multi Autolab tutorial available from the Help menu 129 Page Software synchronization command for Multi Autolab measurements The Multi Autolab software synchronization command has been added to the Measurement General group of commands This command can be used create a synchronization point for two or more instruments in a procedure When two or more instruments perform this procedure in Multi Autolab mode the synchronization commands will force the instruments to hold until the number of instruments holding at the synchronization point matches the value defined by the user in the procedure or until the command reaches the time limit if applied see Figure 171 Multi Autolab sofware synchronization 202020222 Number of participating Autolab instruments z Group name Pretreatment synchronization Time limit cjl Use Time limit No a Abort procedure after time out Mo ail lt gt Figure 171 The Multi Autolab software synchronization command can be used to synchronize two or more Autolabs during a Multi Autolab measurement Note the timing accuracy of the software synchronization command is 100 ms More inform
61. T oad Message LJ Time limit s a30 lse time limit Mo ia X Message Enter the strings in the collection one per line This message can be displayed using multiple lines Cancel Figure 32 The Message box and nput box commands now provide editors supporting line breaks Additionally the Message box and nput box commands now auto wrap the complete message and no longer display scrollbars making long texts more readable see Figure 33 AUT40007 AUT40007 This message can be displayed using multiple lines This message can be displayed using multiple lines _ Ok N Cancel Figure 33 The complete text is now displayed in the Message box and the nput box commands Subfolders in the procedure browser The procedure browser of NOVA is now able to display subfolder located in the folders defined in the Database manager This feature can be used to simplify procedure bookkeeping The subfolders created in one of the folders used by NOVA will also be displayed in the procedure browser see Figure 34 and Figure 35 26 Page wR Le Standard Oo File Home Share af J E New item FA Select all F Easy access 7 v E clit Select none Delete Re New Properties b P a p History oo Invert selection Documents gt My Procedures 1 10 gt Standard gt v Search Standard P PS Favorites Name Date modified Type Size E Desktop l Subfolder 1 7 8 2013 11 21 File folder
62. Unchang Figure 301 Changing the settings can be done using the drop down lists To change a setting select the new value from a drop down list Figure 302 illustrates the change of one of the hardware settings Using the drop down lists the active current range for the WE 1 can be set to 10 pA 225 Page Autolab control WE 1 Cell Unchanged Bandwidth Unchanged Mode Unchanged IR compensation Unchange IR compensation value Unc FRA input Unchanged External input Unchanged scangen input Unchanged Oscillation protection Unche Reference potential Uncha WE Cell Unchanged Current range Unchanged Potential Unchanged BA Mode Unchanged FRA input Unchanged DIO 1 P1 ADirecton Unchanged P1AWrite Unchanged P1 B Direction Unchanged P1 B Write Unchanged F1 CLower Direction Uncha F1 CLower Write Unchange F1 CUpper Direction Uncha F1 CUpper Write Unchang P2 A Direction Unchanged P2 A Write Unchanged P2 B Direction Unchanged P2 B Write Unchanged P2 CLowerDirection Uncha P2 CLower Write Unchange P2 CUpper Direction Uncha P2 CUpperWrite Unchang Figure 302 The changes in the Autolab control command are highlighted Note the Autolab control command only displays the settings of the hardware modules defined in the hardware setup OCP integration Open circuit potential measurements are now easier compared to the previous versions of NOVA A new command OCP determination is
63. Wait time s Bet current Optimize current range Bet cell OCP determination oo Waittime 8 e set reference potential Optimize current range Control Autolab RDE OCP determination Switch Autolab RDE off Bet reference potential Purge e Hnterrupt measurement e Set stirrer 2 os Interrupt measurement high speed Create new drop Set BIPOT ARRAY potential e cet pH measurement temperature Reset EQCM AFrequency Control Autolab RDE Switch Autolab RDE off z Create new drop e Determine integrator drift e Muli 4utolab software synchronization e Muli 4utolab hardware synchronization Set ECD current offset Figure 102 Difference between the basic left and the advanced right profile Note the intermediate profile is the default level based profile selected upon installation of Nova Important the selected level based profile is always on Hardware based All the commands and the procedures in Nova have been tagged with a hardware requirement marker When the hardware based profile is active only the procedures and commands that can be executed with the connected instrument are shown In Figure 103 the Autolab procedures are shown without and with the hardware based profile active for a uAutolablll Since the uAutolablll is not fitted with the required hardware several procedures are hidden 80 Page Commands Procedures Autolab e Cyclic voltammetry potentiostatic e Cyclic voltammetry qalvanostat
64. Ze s e Yoa K jo 198 Page FE circuit definition Validate Circuit Upper limit Lower limit Value 0 5 Fixed No Unit User limits Yes E YO 1 00 mMho Upper limit Lower limit Value Fixed Unit User limits Figure 268 The G element is now available in the Fit and Simulation Kronig Kramers calculation The Kronig Kramers KK test tool has been added to the current version of NOVA The KK test is often used to relate the real and imaginary parts of a complex transfer function like electrochemical impedance Z This test can be used to check whether the measured data comply with the assumptions of KK transformation These assumptions are 1 The response is only related to the excitation signal 2 The response is linear or the perturbation is small e g lt 10 mV for non linear systems 3 The system does not change with time 4 The system is finite for all values of including zero and infinity If the investigated system changes with time due to e g ageing temperature change non equilibrium initial state etc the test fails Failure of KK test usually means that no good fit can be obtained using the equivalent circuit method This analysis tool is based on the work of Dr B A Boukamp as published in J Electrochem Soc Vol 142 6 1995 The KK test can be used by using the right click menu and by choosing Kronig Kramers test from the Add Analysis menu see Figure 269 199 Pag
65. _ Interval time s ola a m Farameters Links Cyclic voltammetry potentiostatic no extra modules reguiregd Time YE Potential WE Current ma 1 Options HALT 205350 0 000 On am p p O 000 1 000 1 000 0 000 2 01000000 0 000 1 000 1 000 0 000 2 0 00244 0 1000000 1650 Signal sampler Hide Options ations p Fotential applied Time WE Current ocan WEN Fotential Index Ives E set cell lt gt lt gt array gv arrary gt 5 lt lt lt aray A Array array Cv Array Ott Figure 110 Hiding and unhiding command parameters in the procedure editor Sorting function for the commands browser The possibility to sort the commands in a group is now provided Right clicking a command group displays the different sorting options ascending or descending see Figure 111 It is always possible to return to the original order using the same strategy and using the Original order option provided in the context menu 86 Page Commands Procedures Favorite commands H Control H Metrohm devices H External devices H Measurement general H Measurement cyclic and linear sweep voltammetry H Measurement voltammetric analysis Measurement chrono methods Measurement impedance Scan sel Hide all Pe oe 4 Sort ascending X Calculate ZF Sort descending wimpors v Original order Import FR O
66. a a CV Staircase Dosino 1 Dose CV Staircase C ___________ e Dosino 2 Dose Dosino 1 2 Dose D CV Staircase Figure 46 Experiment flow for four different Liquid handling configurations e Figure 46 A Dosino 1 and Dosino 2 have parallel execution disabled Both Dosino need to finish the Dose command before the CV staircase command can start e Figure 46 B parallel execution is enabled on Dosino 2 and disabled on Dosino 1 Dosino 2 starts dosing immediately after Dosino 1 is finished The CV staircase command starts as soon as Dosino 2 starts dosing 38 Page e Figure 46 C parallel execution is enabled on Dosino 1 and disabled on Dosino 2 Dosino 2 starts dosing at the same time as Dosino 1 Only when Dosino 2 is finished can the CV staircase command start e Figure 46 D parallel execution is enabled for both Dosino 1 and Dosino 2 All three commands start at the same time Once the connected devices are configured in the Liquid Handling Setup tool each device can be manually controlled using a dedicated panel provided in the Autolab display window The Liquid Handling manual control in the View menu provides a list of connected devices see Figure 47 File View Profile Run Tools Help ke Advanced procedure view Setup View Mult Autolab View Measurement View ia Analysis View T User log F11 Ea Autolab display F10 FRA manual control MDE manual control MUX manual control External m
67. a pseudo capacitance of 51 8 nF Change type to Convert to pseudo capacitance a Figure 134 Converting a Q element to a pseudo capacitance 100 Page NOVA 1 7 Release notes Released 01 04 2011 Introduction These notes provide an overview of the new features introduced in NOVA 1 7 compared to the previous release The following items have been added to this release of NOVA Support for the instruments and modules PGSTAT302F Switchable floating version of the PGSTAT302N PGSTAT100N Multi Autolab Multi channel frame with M101 potentio Stat galvanostat Improvements and additions On the fly conversion of procedures and data from previous versions of NOVA Redesign of the pX calibration interface Redesign of Edit Cutoff user interface Reverse on Cutoff Adjustments to the Graphical user interface for Fitting and Simulation of impedance data Improvement of the Peak search analysis tool Driver manager Export to ZView command Integration of My Command s in Analysis view Record signals linkable Faster startup Adjustments to the Windower tool Preview of database names Installation requirements NOVA 1 7 requires the NET Framework 4 0 to be installed This windows update is automatically installed if necessary during the setup of NOVA 1 7 see Figure 135 101 Page 16 Nova 1 7 Setup a Installing Microsoft NET Framework 4 x6 and xb4 T Cancel Figure 135 N
68. ab control set potential set cell Viait time 3 Optimize current range LY staircase set cell lt gt H3ALT 0530 Hide c Redo Delete CV staircase Ctrl Y 0 000 On F z 0 000 1 000 1 000 0 000 2 0 1000000 a Off Sz Figure 123 Using the Redo function 93 Page Modification of the Calculate signal command The Ca culate signal command has been adjusted and now displays the expression used in the calculation in the procedure editor see Figure 140 E CY staircase start potential v Upper vertex potential 0 Lower vertex potential 6 stop potential 0 Number of stop crossings step potential v scan rate vis Estimated number of points Interval time s signal sampler Options Potential applied Time WE Current ocan WE Fotential Logarithm of the current Index E iws E Calculate signal Current U 000 1 000 1 000 0 000 2 0 1000000 0 000 1 000 1 000 0 000 0 00244 0 1 000000 1650 0 024400 Time YE Potential WET Current 1 Options lt aray gt Vi arrary gt 5 Array A erreary gt array Cv errary gt erray gt AA A A NA 10LOG ABS Current l WEI Current 4 Figure 124 The expression used in the Calculate signal command is now displayed in the procedure editor Noise meters added to the Autolab display A bar graph noise meter has been added to the Autolab display to indicate the l
69. after subtraction of the baseline see Figure 41 Demo 10 Differential pulse measurement 3 Differential pulse see H divs E Moving average i H Residual oe 4 9E 7 AE 7 3 5E 7 3E 7 2 9E 7 Corrected Y 2E 7 1 5E 1E 7 5E 8 1 2 1 0 8 0 6 0 4 0 2 0 Fitted x Figure 41 The residual plot is automatically created It is possible to adjust the Window size parameter by change the value shown in the frame on the right hand side of the plot see Figure 42 33 Page mT i x Signal Expression Unit Fitted x Fitted Y Corrected Y Window size 4 1 2 1 0 8 0 6 0 4 0 2 0 Potential applied Figure 42 Modifying Window size parameter The baseline will be recalculated using the new window size and the residual plot will be adjusted Improved controls for Metrohm Liquid Handling instruments This update of NOVA introduces new controls for the Metrohm Liquid Handling tools The new implementation of these instruments deviates significantly from the information provided in Section 2 of the External devices tutorial available from the Help menu in NOVA The main differences are listed here It is no longer required to Initialize and Close Metrohm devices All connected instruments are initialized when NOVA starts and are closed when NOVA is closed Additional devices can be added however this requires all connected devices to be reinitialized All instrum
70. ain No Sample DC Yes Calculate admittance No v Advanced Estimated duration 4 minutes OK Cancel Figure 7 Some parameters of settings are separated into basic and advanced More information on the use of the new user interface for FRA measurement commands can be found in the Impedance measurements tutorial available from the Help menu in NOVA Phase out of the Timed procedure command The 7imed procedure command has been phased out in this version of NOVA The command is no longer required to control the timing of the events programmed in the NOVA procedures All procedures constructed using previous versions of NOVA are converted properly and pre existing 7 med procedure commands are replaced by Nested procedure commands To indicate the timing a new graphical indicator is used Timing guide in procedure editor and managed timing In previous versions of NOVA the 7imed procedure command was used to indicate and control the timing of commands in a measurement sequence To provide a more consistent user interface for the creation of procedures a new timing guide system has been implemented in the current version of NOVA When measurement commands are located in sequence the timing will automatically adjusted in the Same way as in the previous editions with a 7imed procedure No interruption will be observed in the measurement This is indicated now by a green line guide on the left hand side of the proce
71. al commands are located in the Measurement cyclic and linear sweep voltammetry and Measurement chrono methods groups When one of these commands is added to the procedure editor a complete set of commands will be created These commands constitute a complete template for a potentiostatic or galvanostatic measurement see Figure 239 Commands Parameters New procedure Remarks m End status Autolab Collection ma Signal sampler Time WE 1 Current m Options No Options S Timed procedure potentiostatic Autolab control Set potential 0 000 Set cell On c Wait time s 5 Optimize current range 5 Set cell Off ca lt 5 a Figure 239 The template commands can be used to create an almost complete procedure Once a template command has been added to the procedure editor the missing measurement command can be inserted in the template see Figure 240 Additionally the options and the sampler can be defined before the measurement is started Start and stop potentials can be linked to the Set potential command if required 179 Page Commands Parameters New procedure Remarks End status Autolab Collection a signal sampler Time WE 1 Current m Options No Options E Timed procedure potentiostatic Autolab control a Set potential 0 000 Set cell On fal Wait time s 5 Optimize current range 5 C E CV staircase Set cell Off z lt gt lt gt Figure 240 Adding a measurement command to a template
72. al pulse Baseline correction by moving average The baseline correction using the moving average method is now available as command and analysis tool This baseline correction method is very effective when peaks show as shoulders on steep flanks The moving average performs the following steps 1 The source data is grouped into segments of n points where n correspond to the Window size parameter of the Moving average baseline correction tool default value of n is 2 This means that the source data is reduced from m data points to m n averages 2 The average value of each segment is calculated 31 Page 3 Each it average value is compared to the average value of its immediate neighbouring values ati 1 andi 1 a For positive going sweeps if the it average value is higher than the average value of the averages at i 1 andi 1 then the it average value is replaced by the average value of the averages at i 1 and i 1 b For negative going sweeps if the it average value is lower than the average value of the averages at i 1 andi 1 then the it average value is replaced by the average value of the averages at i 1 and pal c Step 3 is repeated for a maximum of 1000 iterations or until the baseline does not change anymore 4 The baseline is interpolated from m n final averages to the original m data points 5 The baseline is subtracted from the source data The moving average baseline
73. al time validation when errors are identified More detailed validation information This version of NOVA adds more information in the validation messages Previous editions of NOVA only reported the nature of an error or warning This version of NOVA now also adds troubleshooting information see Figure 13 Validation results Oo x J The following problems were encountered during validation Message Command AUTS0002 The interval time 0 00122 s is too small With current option CV staircase The interval time 0 00122 s is too small With current options the smallest possible interval time ts 0 001668 s Without Automatic current ranging option the smallest interval time is 0 000466 s Cancel Figure 13 Procedure validation in NOVA now displays possible solutions to an error or warning displayed in the tooltip Hiding warnings in the validation report It is now possible to indicate to the software to ignore warnings during validation This can be useful for measurements which need to be carried out with parameters that fall outside of the normal operation specifications for example with the cell 10 Page off In those cases although the warning message is normal the user can decide to ignore the message until further notice To ignore a message in the validation screen right click the warning message and select the Hide warning option from the context menu see Figure 14
74. an one version of the NOVA software on the same computer Installing version 1 5 does not upgrade previously installed versions However it is not possible to use both software packages at the same time and data sets obtained with NOVA 1 5 cannot be used with previous versions of NOVA The opposite situation is possible using the conversion tools that are installed together with version 1 5 Tutorials New tutorials have been added to this version of NOVA The tutorials are available from the Help menu see Figure 191 Help es 3 Getting started About User manual Fi Check for Updates Command list Release notes 1 5 Release notes previous version Module test with Nova Bipotentostat Booster high current amplifier Chrono methods Chrono methods high speed Cycle voltammetry Cycle voltammetry linear scan Cutoff boundaries ECD low current amplifier ECM electrochemical noise EQCM quartz crystal microbalance External devices F120 filter Impedance spectroscopy MUX multiplexer Open circuit potential px pH and temperature Voltarmetric analysis Figure 191 New tutorials are available from the Help menu Modules support NOVA 1 5 introduces the support for the pX ECN MUX FI20 Filter modules and the for the IME663 and IME303 interfaces to the Hg drop electrode stands Support for the Booster10A in combination with the PGSTAT128N is also pr
75. and linearsweep E hmety H Measurement cyclic and linear sweep voltammetry aa Measurement voltammetric analysis a Measurement voltammetric analysis Measurement chrono methods Measurement chrono methods Measurement Impedance Measurement Impedance Data handling Data handling Analysis general He Analysis general Analysis baseline correction Analysis baseline correction Analysis corrosion HF Analysis corrosion Analysis impedance Analysis Impedance ial Flots qeneral ahl Flots general ahl Flots impedance ahl Flots impedance My commands H My commands Figure 109 Hiding a command left and a command group right When a command group is hidden the whole group will become invisible Finally in the procedure editor it is possible to hide or unhide command parameters using the same method see Figure 110 For example if the interval time is not important it can be hidden from view This can be used to further simplify the user interface 85 Page Commands Cyclic voltammetry potentiostatic Remarks End status Autolab signal sampler Options Instrument Instrument description El Timed procedure Autolab control set potential set cell Viait time 3 Optimize current range CY staircase start potential Upper vertex potential v Lower vertex potential 6 stop potential v Number of stop crossings step potential v scan rate y s Estimated number of points _
76. and the maximum number of devices supported in Multi Autolab mode is 8 It is possible to quickly switch between drivers by using the dedicated driver manager application A shortcut is provided in Start menu All programs Autolab Tools see Figure 143 108 Page lt gt Driver Manager Select the driver used to control your Autolab instrument Nova only recommended setup Select this driver when you only use Nova 1 or higher on your PC Advantages Faster USB data exchange Connect a maximum of 16 Autolab instruments Ready for future applications gt GPES compatible Select this driver when you want to use Nova 1 7 or higher together with Nova 1 6 or lower and or GPES on this PC Restrictions Slower USB data exchange Connect a maximum of 6 Autolab instruments No further developments are done with this driver Nova only instruments 2 GPES compatible instruments 0 Settings Total number of instruments Figure 143 The Autolab Driver Manager application can be used to quickly switch from one driver to the other The Autolab NOVA only driver is recommended Note switch to the GPES compatible driver when using earlier versions of NOVA or when using the GPES or FRA software Improvements to the Peak search tool The Peak search command and the corresponding analysis tool have been redesigned and improved The parameter Mumber of points in search window is now defined in t
77. ands group is located in the commands browser To add a command to the My commands database right click the command in the procedure editor and select the Save in My commands option see Figure 258 Commands Parameters New procedure Remarks aml End status Autolab Collection ia Signal sampler Time WE 1 Current z Options No Options E S Timed procedure 2 Autolab contr Enabled OCP determi Set reference p al Set potential 1 200 Set cell On x Wait time 5 5 Optimize current range 5 lt _ gt lt gt Figure 258 Click the Save in My Commands option to add it to the My commands database You will be prompted to specify a name for the command see Figure 259 Save command in My Commands My Potentiostatic Preconditioning Figure 259 Specify a name for the command In the example shown here the whole Timed procedure will be saved in the My commands database as My potentiostatic Preconditioning see Figure 260 Note a tooltip displays the details of the command 193 Page Control Control Metrohm devices Measurement general Measurement cyclic and linear sweep voltammetry Measurement chrono methods Measurement impedance Data handling Analysis general Analysis baseline correction Analysis corrosion Analysis impedance Plots general Plots impedance My commands S My Potentiostatic Preconditioning My Potentiostatic Preconditioning Timed procedure Autolab control A
78. ans to perform measurements on up to six working electrodes sharing a common reference and counter electrode at the same time Multiple BA modules numbered 1 to 5 can now be selected in the Hardware setup see Figure 166 Hardware setup ok File Tools Main Module Additional Modulets yl PGSTAT101 PGSTAT302N PGSTAT128N wAutolab II PGSTAT100 PGSTAT302 I FRAZ E ADCOM C ADC750 C ADC750r4 C SCANZ50 1 SCANGEN El Wisc Multi BA instrument Yes PGSTATI2 IBA PGSTAT3O BAH LAwtolab Il 7 BA 2 PGSTAT20 PGSTATIO BIPOT ARRAY JEco Fl20 Filter C Fl20 Integrator Booster 04 Booster1 04 EQCM C px1000 LJ px JECN External J IME303 C IMEBES MIL Power Supply Frequency Import FRA Calibration FRA offset DAC range pile Multi BA instrument C Documents and Settings All Users Applicaton Data Eco Chemie HardwareSetup O xml Figure 166 Selecting multiple BA modules for a MultiBA instrument The WE x Current and WE x Potential signals will be added to the Signal sampler These signals can be sampled during electrochemical measurements see Figure 167 127 Page EE Edit Sampler en sample Optimized Sampler configuration WEL a sampler segment WEC Potential WE 2 Potential WE 3 Paotential WE 4 Potential Segment Cotimized e WE 2 Current di Current 3 Current Current Curr
79. anual control Liquicl Handling manual control Analyte 800 9128 X Figure 47 Manual control of the Liquid Handling devices is available from the View menu The devices are listed using the following format Name of the device Metrohm device number type Serial number n the example shown in Figure 47 one Metrohm 800 Dosino with serial number 9128 called Analyte defined in the Liquid Handling Setup Figure 48 shows the manual control panel added to the Autolab displaying the controls for a Dosino 39 Page Autolab display A Analyte Prepare Fill Empty Dose ml 5 Fort Input port Dosediml 5 00 Hola stop 9128 20ml Figure 48 Manual control of a Dosino The Dosino manual control panel provides the following controls e Prepare the Dosino using the e button e Fill the Dosino through the specified filling port using the e Empty the Dosino using the button o button e Specify and dose a volume using the button through the specified port using the provided drop down box e The and buttons can be used to hold or stop the currently running actions on the Dosino Figure 49 shows the manual control panel added to the Autolab displaying the controls for a Stirrer Autolab display stirrer Speed ce lt X 238 Figure 49 Manual control of a Stirrer The Stirrer manual control panel provides the following controls e Specify the stirring rate betw
80. arallel The impedance of series element is given by the sum of the impedance values of each individual element while the impedance of the element placed in parallel is given by the reciprocal of the sum of the reciprocal impedance values of each element In order to use the fit and simulation tool in NOVA load an impedance measurement and select any plot for display in the 2D plot area Click on the analysis toolbar and activate the Fit and simulation method see Figure 311 Brel 1100 1000 F 900 800 700 a iy QO 400 300 200 100 0 600 900 H 4s Analyze Clear Save None None Peak search Regression Baseline Fit 0 200 400 600 800 1000 Z Q Figure 311 Selecting the Fit and simulation tool from the Analysis toolbar Once the Fit and simulation tool has been selected a new area will be displayed at the bottom of the 2D plot area see Figure 312 This area is the control interface for the fit and simulation tool 233 Page 7 Q 0 200 400 600 800 1000 Z Q E Input Max number of Iterations 100 Circuit Maximum change in chi square 0 001 Maximum number of iterations giving no improvement 100 Fitting style Impedance Use weight factors Yes Fit or Simulation Fit __Measurement data format _Impedance Results Number of iterations performed 0 Result Chi square 0 Figure 312 Selecting the fit and simulation tool displa
81. as been modified in NOVA 1 6 This application now supports multiple Autolab instruments When the application starts it detects all available instruments connected to the computer see Figure 173 4a Diagnostics Diagnostics is searching for instruments Figure 173 The Diagnostics application automatically scans for all the connected instruments Note the test can only be performed on a single instrument at a time If more than one instrument is detected a selection menu is displayed before the Diagnostics starts see Figure 174 4a Diagnostics Please select an instrument ALT 635981 LWSALIT 0K30 15671411 Figure 174 A selection menu is displayed if more than one instrument is detected Note instruments with serial number beginning with AUT9 or with u2AUT7 connected through an external USB interface are identified by the serial number of the interface USB7XXXxX Instruments with an internal USB interface or instruments with serial number beginning with AUT7 connected through an external USB interface are identified by their own serial number If the hardware setup of the connected instrument can be located on the computer the diagnostics test can be performed immediately Otherwise the hardware setup for the connected instrument can be defined Select the Hardware setup option from the Select menu see Figure 175 131 Page 4s Diagnostics AUT83072 Select All Tests l Select All Automatic Tes
82. at the problem is Figure 288 shows the output of the diagnostics tool when the test is performed with a faulty USB connection 213 Page w Diagnostics Results Windows Information A Windows Information Embedded Processor Test a Be Embedded Processor Test EEProm Test 2 0 Embedded System Type IF030 USB Timer Test i O F030 USBinitialisation failed Autolab Test 2 O Embedded Processor Test failed AD Converter Test nL Advanced DA Converter Test o Error Communication error Invalid USB handle Potentiostat Test _ EEProm Test Noise Test _ Timer Test AC Voltammetry Test C Autolab Test Galvanostat Test AD Converter Test C DA Converter Test Potentiostat Test Progress Figure 288 A failed test will be indicated in the diagnostics tool It is possible to print the test report or to save it as a text file by using the File menu and selecting the appropriate action see Figure 289 as Diagnostics imi Save Report As Peada in eport is fe eet a fer al Windows Information Tal Embedded Processor Test EEPTOM TEST H A EEProm Test Timer Test H A Timer Test Autolab Test H A Autolab Test AD Converter Test H A AD Converter Test DA Converter Test H A DA Converter Test Potentiostat Test H A Potentiostat Test Noise Test H A Noise Test AC Voltammetry Test J A AC Voltammetry Test Galvanostat Test 8 Galvanostat Test Progress Figure 289 It is possible to save or print the diagnostics re
83. atic Cyclic voltammetry current integration Cyclic voltammetry linear scan e Cyclic voltammetry linear scan high speed Linear sweep voltammetry potentiostatic Linear sweep voltammetry galvanostatic Linear polarization Hydrodynamic linear sweep Differential pulse voltammetry 2 square wave voltammetry 2 sampled DC polarography 2 Chrono amperometry At gt 1 ms e Chrono potentiometry At gt 1 ms e Chrono amperometry fast e Chrono potentiometry fast 2 Chrono amperometry high speed Chrono potentiometry high speed z Chrono charge discharge Hnterrupt interrupt high speed Positive feedback e FRA impedance potentiastatic FRA impedance galvanastatic FRA potential scan Standards i Ady procedures Figure 106 Hiding a procedure from the procedure browser Once an item has been hidden from view it will not be shown until it is unhidden To unhide hidden commands procedures or command parameters select the Show all option from the Profiles menu see Figure 107 File E View 5 DA ag Figure 107 Select the Show all option Profile Run Tools Help Harchvare based Basic Interm ecate Advanced Corrasion Education Electroanalysis Energy Interfacial electrochemistry Semiconductors Reset user profile Import user profile Export user profile Hide Unhicde Show all N from the Profile menu to display all hidden items Ctrl H Col Shitt H 83 Page Hidden items are sh
84. ation can be found in the Multi Autolab tutorial available from the Help menu Instrument serial number and description in the database To simplify data management in the database each experiment is now logged with the identifying serial number and the configuration name if specified in the database frame see Figure 172 This additional information can be used to find data sets more easily It is possible to use the database for sorting the experiments using any of the available columns and to filter the database contents using the provided tools in order to display only specific measurements File View Run Tools Help LEB 2 2 a gt i a ee B D Ei Select instrument AUT40009 Procedure name Time stamp Remarks Instrument Instrument description Cyclic voltammetry potentiostatic 12 24 2009 9 41 094M Cyclic voltammetry potentiostatic no extra modules required AUT40009 Cyclic voltammetry potentiostatic 12 24 2009 9 35 06 4M Cyclic voltammetry potentiostatic no extra modules required AUTS83478 PGSTAT128N FRA2Z Cyclic voltammetry potentiostatic 12 24 2009 9 35 01 AM Cyclic voltammetry potentiostatic no extra modules required AUT40009 PGSTAT101 Figure 172 The database frame includes an Instrument serial number column and an Instrument description column Please refer to the User Manual and the Multi Autolab tutorial for more information 130 Page Multi Autolab support in Diagnostics application The diagnostics tool h
85. ay gt V Scan lt aray WE 1 Potential lt armay gt V lt _aray gt s WE 1 Current lt _array gt A B ivs E Graphical settings General settings c X Potential applied V Y WE 1 Current A F Time 8 Set cell Off a lt gt Figure 290 The Cyclic voltammetry procedure with the default Signal set of the CV Staircase command The signal set s added to a measurement command of a procedure define how the measured data is displayed in real time during the measurement For the CV Staircase command the WE 1 Current signal will be plotted against the Potential applied in real time If the links are changed for example by replacing the Potential applied by the Time the data will be plotted differently during the measurement see Figure 291 215 Page Procedure Values Cyclic voltammetry Remarks Factory standard procedure m End status Autolab Collection m Signal sampler Time WE 1 Potential WE 1 Current Options Automatic Current Ranging WE 1 1 mA 1 a E Timed procedure Set Potentiostatic and select current range m Set potential 0 000 Set cell On Wait time s 5 Optimize current range 5 E CV staircase 0 000 1 000 1 000 0 000 2 0 10000 start potential v 0 000 Upper vertex potential V 1 000 Lower vertex potential V 1 000 stop potential V 0 000 Number of stop crossings 2 Step potential V 0 0024 Scan rate V s 0 10000 Total number of points
86. ble to combine several profiles at the same time intermediate hardware based and energy related Hide Show option To further customize the appearance of the user interface the option to hide and show procedures commands and command parameters has been added To hide an item in Nova simply right click the item and select the hide option from the menu In Figure 106 this option is used to hide the Chrono coulometry fast procedure from the procedures browser 82 Page Commands Procedures Autolab l Cyclic voltammetry potentiostatic Cyclic voltammetry galvanostatic Cyclic voltammetry current integration Cyclic voltammetry linear scan e Cyclic voltammetry linear scan high speed Linear sweep voltammetry potentiostatic Linear sweep voltammetry galvanostatic Linear polarization Hydrodynamic linear sweep Differential pulse voltammetry 2 square wave voltammetry 2 sampled DC polarography 2 Chrono amperometry At gt 1 ms Chrono potentiometry At gt 1 ms e Chrono amperometry fast 2 Chrono potentiometry fast S Chrona coulometry fa Chrono amperometry Hicle Chrono potentiometry high speed Chrono charge discharge interrupt Hnterrupt high speed Positive feedback FRA impedance potentiostatic FRA impedance galvanastatic PRA potential scan Standards i Ady procedures Commands Procedures Autolab l Cyclic voltammetry potentiostatic Cyclic voltammetry galvanost
87. c Summary Current range 100 mA v Bandwidth High stability v iR compensation Off 0 Q v Advanced Cancel Figure 3 The Autolab control editor has been redesigned Additionally a Summary has been added to the editor The summary displays all the specified settings in one clear overview see Figure 4 Autolab control 0 EA PGSTAT204 WE 1 Cell On DIO12 Integrator WE 1 Current range 1mA FRA32M WE 1 iR Compensation On Summary lt WE 1 Mode Potentiostatic OK Cancel Figure 4 A summary has been added to the Autolab control editor It is possible to quickly remove one or more of the settings indicated in the summary by clicking the icon as shown in Figure 4 For more information on the use of the Autolab control command please refer to the Autolab control tutorial available from the Help menu in NOVA 5 Page New user interface for the Chrono methods and Chrono methods high speed commands The Chrono methods and Chrono methods high speed command have been modified and a new user interface has been added to the commands This dialog replaces the previous Chrono methods and Chrono methods high speed editor see Figure 5 ard Chrono methods editor O ES Step A Basic Step Text Step Step Potential 0 V Step Duration 0 01 S Sample Yes Interval time 0 0001 S Estimated number of points 100 v Advanced a TEE Figure 5 A new user interface has been added to the chron
88. cation marker corrosion energy electroanalysis etc When a given application profile is active only the commands and procedures relevant for this application are shown see Figure 104 Commands Procedures Commands Procedures Autolab Auto lat Cyclic voltammetry potentiastatic Cyclic voltammetry potentiastatic Linear sweep voltammetry potentiostatic Linear sweep voltammetry potentiostatic Linear polarization Hydrodynamic linear sweep Hydrodynamic linear sweep Diferential pulse voltammetry Chrono amperometry At gt 1 ms 2 square wave voltammetry Chrono potentiometry At gt 1 ms Sampled DC polarography i FRA impedance potentiostatic 2 i Chrono amperometry At gt 1 ms Standards Standards H My procedures i Ady procedures Figure 104 Difference between the corrosion left and the electroanalytical right profile Note it is possible to combine all the profile schemes at the same time For example it is possible to set the profile to show hardware based and intermediate commands and procedures for the energy application see Figure 105 81 Page File View Profile Run Tools Help Dba adzy Hardware based Basic Intermediate Achanced Corrosion Education Electroanalysis Energy X Interfacial electrochem stry Semiconductors Reset user profile Import user profile Export user profile Hide Ctrl H Unhice Ctl Shitt H Show all Figure 105 It is possi
89. ch row of the table A possible example is shown in Figure 184 In this example the three parameters defined in the table shown in Figure 183 are linked to the Scan rate Upper vertex potential and the Potential value defined in the Set potential command respectively S Repeat for each row Number of repetitions scan rate ys 0 05 Upper vertex potential i Preconditioning potential w 0 1 E Timed procedure Autolab control am set potential 0 000 oet cell On a Vat time s 5 Optimize current ranqe z E CY staircase 0 100 1 000 1 000 0 100 2 00 start potential yj 0 000 Upper vertex potential Vv 1 000 Lower vertex potential 6w 1 000 stop potential v 0 000 Number of stop crossings step potential v 0 00244 ocan rate vfs 0 05000 Total number of points 1650 Interval time s 0 024400 signal sampler Time WWE 1 Current Ootians 1 Options z Figure 184 A possible use of the Repeat for each row command The measurement will therefore be repeated using the values defined in each row for the three parameters Autolab display with collapsible panels The Autolab display has been redesigned in this version of NOVA It is now possible to add or remove panels to the Autolab display by choosing the required options in the View menu see Figure 185 138 Page Fie View Run Tools Help be Advanced command view ay g JID T Advanced procedure view Setup View Multi Autolab View
90. ched off when the timed procedure is encountered If required it is possible to switch off the DSG input on the PGSTAT by using the Autolab control command in the timed procedure 7 Refer to the Impedance tutorial for more information and a practical example 157 Page New FRA commands Two FRA commands have been added to the Measurement impedance group of commands e FRA single frequency e FRA single frequency external These two commands are used in combination with the FRA frequency scan commands potentiostatic galvanostatic or external When more than one FRA single frequency is added to a FRA frequency scan command each frequency in the scan will be measured n times where n is the number of FRA single frequency commands in the scan see Figure 213 FRA measurement potentiostatic Frequency lt errey gt Az Phase lt aray gt lt array gt 2 lt array 02 7 lt array gt 0 Index array FRA frequency scan Collection Frequency table Collection Number of frequencies Estimated duration Timed procedure B Autolab control MUs 1 Channel 2 H FRA single frequency 1 1 10 1 0 Timed procedure Autolab control MUX 1 Channel 2 4 H FRA single frequency 1 1 10 1 0 4 Figure 213 Example of two FRA single frequency commands in a FRA measurement potentiostatic 158 Page Post measurement checks The User log will now displa
91. cilitate bookkeeping of Metrohm Liquid handling devices the connected devices are now identified by Name Device type Serial number in the Liquid Handling setup see Figure 74 Analyte 600 2429 41774 770 41774 Refresh Liquid Handling setup Name Port 1 settings Rate 0 01 ml min 166 ml min Tube length mm Tube diameter mm Port settings Rate 0 01 ml min 166 ml min Tube length mm Tube diameter mm Port 3 settings Rate 0 01 ml min 166 ml min Tube length mm Tube diameter mm Port4 settings Rate 0 07 ml min 166 ml min Analyte 330 0 2 0 150 0 2 0 330 0 2 0 o EE Parallel execution Active Dosing port w Active Fill port k Active Special port ka Active Mone w Cancel Figure 74 Metrohm devices are now identified by Name Device type Serial number Automatic repair of the pX1000 checksum error problem An error in the programming could potentially lead to a write error when saving the calibration data in the on board memory of the pX1000 module This error is now fixed and checksum errors in existing pX1000 modules are automatically repaired 60 Page NOVA 1 9 Release notes Released 26 1 1 2012 Introduction Thank you for installing this update of NOVA These notes provide an overview of the new features introduced in NOVA 1 9 The following improvements have been added to NOVA e Support for 64 Bit versions of Window
92. command is as accurate as possible the Autolab cannot display the measured data points in real time While the chrono methods command is running the Autolab display will indicate a busy timer in the lower left angle see Figure 275 When the chrono methods measurement finishes the rest of the procedure will be executed Autolab display status current range Figure 275 The Autolab display window with the Busy timer in the lower left corner SCAN250 amp SCANGEN in combination with the ADC164 NOVA 1 3 now supports the combination of the SCAN250 SCANGEN with the ADC164 The SCAN250 was previously only available in combination with the ADC750 or the ADC10M A dedicated command CV inear scan is available from the measurement group This command performs a linear scan cyclic voltammogram with the SCAN250 or the SCANGEN module while the electrochemical signals are sampled using the ADC164 205 Page The CV inear scan high speed command can be used to perform a cyclic voltammogram with the SCAN250 or the SCANGEN module while the current and the potential are sampled using a high speed ADC either the ADC750 or the ADC10M New linking behavior Links are an important component of the procedure building process Links are used in Nova to establish a dynamic relationship between two or more parameters or signals To provide a clear overview of the linked parameters or signals Nova 1 3 now highlights a link whenever one of the l
93. correction tool can only be used with data which is presented on a non reversing X axis This means that it cannot be used on a cyclic voltammetry measurement The moving Baseline correction Moving average tool can be added to a data set by using the quick access toolbar or by right clicking the plot and choosing this option from the context menu see Figure 39 B Demo 10 Differential A Y S nent Differential pulse Tr H Smooth gt f Baseline Correction Polynomial fixed order Peak search Polynomial maximum order Regression Exponential Derivative Moving average N Integrate a FFT Analysis i 7 Corrosion Rate gt roy erent O ey LU 156 7 1E 7 5E 8 0 1 2 1 0 8 0 6 0 4 0 2 0 Potential applied W Figure 39 Adding the Moving average baseline correction to the data The moving average baseline correction tool is added to the data set and the baseline is automatically drawn on the plot using the default settings see Figure 40 32 Page S Demo 10 Differential pulse measurement Differential pulse 5E 7 HH divs E Moving average H Residual plot et 4E 7 3 5E 7 E 1 6 Current A ha Sy m a VV amp a ee sos J i oO 1 2 1 0 8 0 6 0 4 0 2 0 Potential applied V Figure 40 The baseline correction tool is added to the data and the baseline is drawn The Residual plot is also added automatically This plot shows the source values
94. d install the latest service packs and security updates for this product For more information visit the following Web site Figure 67 Visual C 2008 Redistributable installation Click the Finish button to finalize the prerequisites setup The setup program will proceed to the Nova Setup automatically see Figure 68 Welcome to the Nova 1 10 Setup Wizard The Setup Wizard will install Nova 1 10 on your computer Click Next to continue or Cancel to exit the Setup Wizard Figure 68 Start of Nova installation Windows XP warning Microsoft has ended support for Windows XP on April 8 2014 It is therefore no longer recommended to keep using this operating system A warning is now provided in the User log indicating that NOVA should no longer be used in combination with Windows XP see Figure 69 56 Page User log message Time Date Command The support for Microsoft XP has ended the 8th of April 2014 Next versions of Nova will no longer be able to run under Windows XP 12 22 50 9 10 2014 ss N The support for Microsoft XP has ended the 8th of April 2014 Next versions of Nova will no longer be able to run under Windows XP Please change your operating system A Figure 69 A warning about Windows XP is npw shown in the User lo Future versions of NOVA may be incompatible with Windows XP Support for signal averaging for Avantes spectrometers Signal averaging is now
95. d manual This component is required for Windows 7 Vista and XP Installation of the Visual C 2008 x64 Redistributable The Visual C 2008 x64 Redistributable is necessary on for 64 bit versions of Windows only The installation Wizard will guide you through the installation process see Figure 65 Figure 66 and Figure 67 When one of the Prerequisites is not installed or not installed properly Nova cannot start and will give an error message 54 Page Welcome to Microsoft Visual C 2008 Redistributable Setup This wizard will guide you through the installation process Be sure to carefully read and understand all the rights and restrictions described in the license terms You must accept the license terms before you can install the software MICROSOFT SOFTWARE LICENSE TERMS MICROSOFT VISUAL C 2008 FEATURE PACK REDISTRIBUTABLE RUNTIME LIBRARIES These license terms are an agreement between Microsoft Corporation or based on where you live one of its affiliates and you Please read them They apply to the software named above which includes the media on which you received it if any The terms also apply to any Microsoft updates cunnlamante v Press the Page Down key to see more text M Ihave read and accept the license terms Figure 66 Visual C 2008 License Terms 55 Page Microsoft Visual C 2008 Redistributable has been successfully installed It is highly recommended that you download an
96. de backup s Figure 282 The upgrade application displays the available nox files in NOVA 1 2 format Using the Aad files to listand the Remove files from the list buttons individual nox files can be added or removed from the list Click the Start button to initiate the conversion to the NOVA 1 3 file format It is possible to create a backup of the source files and to overwrite the backup files if they are already found in the source folder It is also possible to create a log file which can be useful if the conversion fails During the upgrade step the progress is displayed in real time see Figure 250 as Upgrade to Nova 1 3 File File Status C Documents and Settings User My Documents My Procedures 1 2 My example database Measurement 1 nox Busy Converting C Documents and Settings User My Documents My Procedures 1 2 My example database Measurement 2 nox C Documents and Settings User My Documents My Procedures 1 2 My example database Measurement 3 nox C Documents and Settings User My Documents My Procedures 1 2 My example database Measurement4 nox C Documents and Settings User My Documents My Procedures 1 2 My example database Measurement 5 nox Abort Converting C Documents and Settings User My Documents My Procedures 1 2 My example database Measurement 1 nox Figure 283 The upgrade application converts every nox file in the list from the NOVA 1 2 format to the NOVA 1 3 format When all the nox fil
97. ded at the end of the procedure 219 Page Commands Parameters Cyclic voltammetry Remarks Factory standard procedure al End status Autolab Collection m Signal sampler Time WE 1 Potential WE 1 Current m Options Automatic Current Ranging WE D 1 mA 100 nA a E Timed procedure Set Potentiostatic and select current range ma Set potential 0 000 Set cell On Wait time s 5 Optimize current range 5 E CV staircase 0 000 1 000 1 000 0 000 2 0 10000 start potential V 0 000 Upper vertex potential v 1 000 Lower vertex potential v 1 000 stop potential V 0 000 Number of stop crossings 2 Step potential V 0 00244 Scan rate V s 0 10000 Total number of points 1650 Interval time Ls 24400 Signal sampler Time WE 1 Potential WE 1 Current Ea Fotential applied lt _array gt V Scan lt aray gt WE 1 Potential lt _ array gt V Time lt _ amay gt s WE 1 Current lt _array gt A 7 ivs E MathParser Set cell lt _ gt lt _ gt Figure 295 The mathematical parser command added to the Cyclic voltammetry procedure To use this command click the amp button located on the right hand side This will open the Expression builder window in which the mathematical function can be created see Figure 296 220 Page Fe Expression builder E mj E4 Farameters Functions Figure 296 The expression builder window The following items are required e Name
98. ded in the tutorials Autolab test procedures Special procedures are now included in a special Module test database installed with NOVA These procedures can be used to test specific hardware module and the Autolab potentiostat using the Autolab dummy cell see Figure 222 Commands Frocedures Autolak g standards Test4DLslan 5 43 2009 10 06 00 PR TestADCI 0M Deb e00a aare PM TestADC BO 5256 2009 3 3 ar Fil Test4RRaAy 5232009 2 06 20 PM Testa 5 25 2009 3 30 00 Pra TestBlPOT 5 23 2009 2 05 55 PM TestBoosteri DA 5 25 2009 3 38 27 PM TestBooster2 DA 5 25 2009 3 41 37 PM H Testly 5 23 2009 1 11 06 PM z Tesey Pas TA 101 5f23 2009 1 11 06 PM TestElD 5 25 2009 9 20 20 AM TestECN 5 23 2009 3 31 25 PM TestEQlh 5243 2009 10 12 35 PM TestFl 0 Filter 5 25 2009 3 30 59 PM TestFRA 6 4 2009 10 12 20 4M Testis 5 23 2009 4 46 15 PM Testo 5 23 2009 5 06 06 Phl Testps1000 5f23 2009 5 08 24 PM i est sCAMZ50 5 25 2009 5 27 07 PM 3 i TastsCANGEN 5 23 2009 5 21 15 PM i Ady procedures Figure 222 Module test procedures are now included in the software More information can be found in the Module test with Nova document available from the Help menu 164 Page PGSTAT101 support PGSTAT104 uo Figure 223 The new Autolab PGSTAT101 Instrument specifications The PGSTAT101 shown in Figure 223 is a potentiostat galvanostat with USB interface The specifications of t
99. define the number of columns in the GPES data file see Figure 262 This allows you to import GPES data files with a recorded second signal bipotentiostat SPR etc a Import GPES data Filename c i Number of columns Index lt aray Column 2 lt _ amay gt Column 1 lt _ array gt ivs E mg 4 lt _ gt Figure 262 The Import GPES data command Moreover it is possible to assign names and units to the columns located in the GPES file using a dedicated interface accessible by clicking the tJ located on the Number of columns parameter line Using the Signal editor window it is possible to change the name of the columns manually or using a drop down list see Figure 263 195 Page a Import GPES data Potential Current Index ivs E lt gt Filename z lt amar Vv A Signal Editor Number of columns Current A FE Edit Signal Signal name N ay Potental Unit AFrequency Driving force JPH pX Voltage Temperature x T Figure 263 Changing the name of the columns can be done using the Signal Editor window Note using the names from the drop down list allows identifying the signals and ensures compatibility with all the data analysis tools Import and Export ASCII Import and Export ASCII data commands have been added to the data handling command group These two commands can be used to import data from an ASCII f
100. dure editor see Figure 8 7 Page Commands Parameters Links Cyclic voltammetry potentiostatic Remarks Cyclic voltammetry potentiostatic no extra modules required saa End status Autolab aaa signal sampler Time WE 1 Potential WWE 1 Current m Options 1 Options al Instrument Instrument description H Autolab control zj H Set potential 0 000 set cell On m Vat time 3 a Optimize current range a H CY staircase U 000 1 000 1 000 0 000 2 01000000 set cell Ott m lt gt Figure 8 The green timing guide located on the left hand side of the procedure editor replaces the 7imed procedure When non measurement commands are inserted anywhere in a procedure an interruption of the timing must be introduced to execute the non measurement command This is indicated by a break in the timing guide located on the left hand side of the procedure editor see Figure 9 Commands Parameters Links Cyclic voltammetry potentiostatic Remarks Cyclic voltammetry potentiostatic no extra modules required c End status Autolab m oignal sampler Time WWE 1 Potential vWwE 1 Current al Lotions 1 Options m Instrument Instrument description E Autolab control m E Set potential 0 000 Set cell On wWalttime s z H Message box Optimize current range z H CY staircase 0 000 1 000 1 000 0 000 2 01000000 Set cell Ct CRA Figure 9 Inserting non measurement commands in a measurement sequence creates a break i
101. e a i Demo 16 FRA impedance El al Plot Options Properties 7 Add Windower Generate index Add Plot AddAnaiyss Fit and simulation Show All Plots Hide All Plots Flectrochemical circle fit Save in My commands Include all FRA data Delete Potential scan FRA data Figure 269 Adding the Kronig Kramers test to impedance data Note in the current version of NOVA only the impedance Kronig Kramers test which uses a serial RC element sequence is supported More information about the Kronig Kramers test can be found in the Impedance measurements tutorial Metrohm devices support This version of NOVA introduces the support for the Metrohm 800 Dosino Metrohm 801 Stirrer and Metrohm 814 815 858 Sample changer through the Metrohm Serial Bus MSB interface A Control Metrohm devices command group is available in the commands browser see Figure 270 ee Metrohm devices Dosino initialize Dosino prepare Dosino dose Dosino empty Dasino fill Dosino to end Dosino exchange Dosino close Sample processor initialize Sample processor lift Sample processor move Sample processor valve Sample processor pump Sample processor swing Sample processor stir Sample processor close Stirrer initialize Stirer speed stirrer clase Figure 270 The Dosino related commands are located in the Control Metrohm devices group More information about the Dosino control can be found in the External devices tutorial
102. e Convoluted plot item in the data explorer frame see Figure 26 4E 7 3 5E 7 3E 7 2 5E 7 2E 7 1 5E 7 1E 7 5E 8 0 5E 8 Current A Convoluted current 1E 7 1 5E 7 2E 7 2 5E 7 0 0 8 0 6 0 4 0 2 0 0 2 0 4 0 6 0 8 Potential V Potential V Figure 26 Example of a time semi derivative convolution Options added to the Build signal dialog The build signal command has been extended and now also provides the values specified in the Options This only applies to a linkable cutoff option When an linkable cutoff condition is used the value specified in this option will be available in the Build signal dialog see Figure 27 20 Page T Build signal H Measurement cyclic and linear sweep voltammetry Mame H Measurement qeneral n Options 3 Cutoff cu rrent H Untyped filter Search from 1 level s up Sort by order of 1st array high to low Sort by order of 1st array low to high OK Cancel Figure 27 Linkable cutoff options are now listed in the Build signal dialog 21 Page NOVA 1 10 3 Release notes Released 18 10 2013 Introduction The 1 10 3 NOVA release adds the following improvements e Support for Metrohm devices in 64 Bit versions of Windows Sample processors e Increment parameter and Increment parameter with signal back in Control group e Single instance of cutoff e Integrate between markers e Import FRA equivalent circuit e Import Export equivalent circ
103. e 137 103 Page a Import procedure gO gt Libraries gt Organize New folder ij Documents gt My Procedures 1 6 gt Nova gt Libraries Documents library Arrange by Folder v Nova lt Documents a a l TT Name Pictures Demo 01 Copper deposition a Videos Demo 02 Lead deposition EQCM Demo 03 Bipotentiostat measurement PtPt Ring Disc electrode 11 Demo 04 Hydrodynamic linear sweep Demo 05 Fe II Fe M on pcPt Demo 12 Imported pcPt GPES data E amp Computer Network o 6 A Demo 13 Imported pcPt GPES data v a Hl j File name Demo 03 Bipotentostat measurement PtPt Ring Disc elec v INOX Files NOVA 1 3 or late caas Figure 137 It is now possible to import procedures and data from previous versions of Nova directly Please refer to the Upgrading files from previous versions tutorial available from the Help menu Note files from NOVA 1 2 or earlier versions are no longer supported Redesign of the pH Calibration interface The pH Calibration user interface has been redesigned for clarity Redundant information has been removed and the calibration information is now displayed more clearly see Figure 138 104 Page E px Calibration boba Es Settings Calibration Input mode Single Differential Calibration temperature 25 00 C Temperature C
104. e Mathematical parser as a command e Improved Autolab Control interface e OCP integration e Reference voltage command e Import FRA data command e Find circle for impedance data e Fit and simulation for impedance data 202 Page Tutorials A series of short tutorials is available from the Help menu in Nova Each tutorial is dedicated to a specific measurement technique or aspect of the software Some tutorials include procedures that can be used to perform simple measurements on the Autolab dummy cell Help User Manual Fi About Release Notes 1 3 Command list Cyclic voltammetry Chrono methods Impedance measurements Chrono methods high speed Cyclic voltammetry linear scan Booster Open circuit potential measurements Figure 272 A series of short tutorials is available from the Help menu Modules support NOVA 1 3 introduces the support for the current boosters Booster 10A and Booster 20A The boosters can be used by setting the instrument in the highest current range 10 A or 20 A Note the boosters can only be used on DIO connector P1 Hardware support The hardware setup of NOVA 1 3 now includes the PGSTATs 12 30 302N and 100 The hardware setup now separates the choice of the main Autolab module and the additional modules see Figure 234 203 Page EE Hardware setup File Tools Main Module Additional Module s PSTAT10 E PGSTAT10 _ wAutolab Ii _
105. e command can be used to determine the length of an array When linked to an array of value this command will return an integer which corresponds to the number of items in the array Figure 211 shows a possible use for the Get array size command El Timed procedure Autolab control m set potential 0 000 H Set cell On z Vat time 3 z Optimize current range z E CY staircase 0 000 1 000 1 000 0 000 2 01 start potential 0 000 Upper vertex potential fv 1 000 Lower vertex potential 63 1 000 stop potential v 0 000 Number of stop crossings Z step potential v 0 00244 ocan rate v s 0 10000 Total number of points Interval time s signal sampler Time WE 1 Current m Options 1 Options m Fotential applied aray gt p Time lt arrayy gt 5 WE Current lt aray gt 4 ocan lt array gt Array size lt 0 Index lt arrary gt ivs E Ij H Set cell Cit lt gt lt gt Figure 211 The Get array size command used in combination with the CV staircase command The total number of points parameter displayed in the CV staircase command is an estimation of the real number of data points Depending on the scan rate and potential step the real number of data points measured during by the CV staircase command could deviate slightly The Get array size command can be used to determine the real number of data points 156 Page The Get array item command can be used to extract the n value from an ar
106. e is show when a new version if available for download 62 Page Linkable cutoff value in procedure editor The value parameter used in the Cutoff option can now be linked in the procedure editor if a unique identifying name is given to it The Edit Options window now provides an additional field on the Cutoff tab allowing the user to specify the name of the parameter to use in the procedure editor to identify the cutoff limit see Figure 111 lt 4 Edit Options Automatic Current Ranging Cutoff Autolab control Automatic Integration Time Basic properties signal WE 1 Current Z Action when gt 7 Value 0 001 Action Nothing Linkable as Cutoff current Advanced properties Mr of detections 4 Additional cutoffs Mo Cutoff Remove Figure 78 The value of the cutoff is now linkable if a name is provided on the Cutoff tab If a name is provided in the Linkab e as field in the basic properties this parameter will be shown in the procedure editor see Figure 79 Other command parameters can then be linked to this parameter which allows the cutoff value to be modified or specified by other commands while the measurement Is running using an input box or a calculate signal for example 63 Page Commands Cyclic voltammetry potentiostatic Remarks End status Autolab signal sampler Options Instrument Instrument description E Timed procedure Autolab control set potential set cell a
107. e validation will always provide a warning when a measurement is started with the internal dummy cell on see Figure 12 Validaton results The following problems were encountered during validation Message Command AUT40148 A The internal dummy cell is on Set cell a The internal dummy cell is on set cell A The internal dummy cell is on Autolab control Time remaining 30 seconds Cancel Figure 86 A warning is provided during validation when the internal dummy cell is on Optional serial number in legend By default the Autolab serial number is displayed in the legend of any plot to facilitate the identification of the instrument in an overlay plot It is now possible to deactivate this option through the NOVA options see Figure 87 69 Page Nova options Graphics Misc 2 Autolab display Overall graphical settings Advanced settings show serial in legend Figure 87 The NOVA options allow the serial number to be activated or deactivated in the legend Linkable purge time The Duration parameter of the Purge time command is now linkable to other command parameters see Figure 121 E Input box Title of box Message Duration of the purge Time limit 5 lse time lirit Mo E Timed procedure E Purge Duration fs Figure 88 The duration parameter of the Purge time command is now linkable 70 Page Procedure editor in the Multi Autolab view To facilitate editing
108. ease refer to the ECN tutorial available from the Help menu for more information Clear plot button modification The clear plot button available in the Measurement view has been modified in order to allow the user to clear all the plots at once by clicking the clear plot button la or to clear one of the specific plot by extending the context menu by clicking the arrow button 2 located next to the clear button Any one of the four plots can be cleared through this context menu see Figure 235 134 Page File View Pun Tools Help La BE fi hak fia ceo Je Measurement Plat 2 Measurement Plot 3 Measurement Flot 4 Figure 180 It is possible to clear a specific plot in the measurement view by extending the Clear plot button Dynamic command parameters This version of NOVA clarifies the concept of Dynamic command parameters Contrary to normal command parameters belonging to individual commands like the Scan rate parameter for a Cyclic voltammetry command or the interval time in a Chrono methods command dynamic command parameters are parameters that are generated by data handling or data analysis commands during a measurement Dynamic command parameters therefore have no initial values and they are generated during experiments For example the slope calculated by a linear regression on measured data can only be provided once the data is collected and the calculation performed The same applies to the value of a Cons
109. easurement like the linearity or the stability of the system being investigated FRA Sampler Input amplitude Channel gt sample frequency domain P c eo Transfer function Phase Channel z Phase Real Z sample time domain Imaginary Sample nc l Sample frequency domain Figure 155 The new FRA sampler can be used to sample time and frequency domain information during FRA measurements as well as the dc components The FRA related commands have been redesigned and the fundamental parameters of the FRA measurements can now be used in combination with other commands using links For example it is possible to define the amplitude to be used in the frequency scan through an Input box or a calculation see Figure 156 118 Page Commands Parameters FRA impedance potentiostatic Remarks FRA impedance potentiostatic requires FRAZ module s End status Autolab signal sampler Mo signals T Options 1 Options ma Instrument Instrument description Timed procedure E Input box Title of box Amplitude used inthe FRA measurement Message Value ofthe amplitude in volts oe Value 0 01 E FRA measurement potentiostatic Frequency lt arrayy gt Hz Phase lt array gt Time lt array gt 5 Z lt array gt 01 lt array gt 01 E lt array 02 Index lt array gt E FRA frequency scan m Frequency 100000 a Amplitude 0 01 Wave type 0 Number of frequencie
110. ed Two features have been added to the Autolab display Real time display of Voltage and Current The Autolab display can now be used to view the voltage and current values measured by the Autolab when no measurement is running see Figure 202 Autolab display 100 pA 10 pA iA EES 100 mA 100nA 10 mA 1 m status current range Pe LL Figure 202 The Autolab display can be used to view the voltage and current even if no measurement is running Manual control of the instrument The Autolab display can also be used to manually control the potential or the current of the Autolab Depending on the instrument settings PSTAT or GSTAT it Is possible to click the voltage or current label in the Autolab display to edit the value of the applied voltage or current applied on the electrochemical cell respectively see Figure 203 151 Page Autolab display Autolab display current cu re t T oyl ovl T oyl oyl 10 pA Y ovl iR C 1A Y oyl iR 1A HSTAB 100mA 100nA 100mA 100nA 10mA 10nA 10mA 10nA EES 1 mA status current range status current range Ss ee a Figure 203 Clicking the voltage label left or current label right in the Autolab display allows editing of the applied voltage or current Skip button The Skip button has been added to the toolbar This button is active during a measurement and can be used to interrupt the currently executed command in the procedure and immediately mo
111. ed frequencies see Figure 94 G FRA frequency scan editor Il x Frequency range Integration time calculation First applied frequency 100000 Hz Integration time maximum 0 125 S Last applied frequency 0 1 Hz Integration cycles minimum 1 Number of frequencies per decade 10 Frequency step Wave type Significant digits 5 aires a E Amplitude Logarithmic 5 sines Square root 15 sines Amplitude 0 01 y q J RMS Frequencies per decade Replace Add Clear Frequency Hz Amplitude V Wave type Integration time Minimum number of cycles to integrate 100000 0 01 Single sine 0 125 1 75431 0 01 Single sine 0 125 1 56899 0 01 Single sine 0 125 1 42919 0 01 Single sine 0 125 1 32375 0 01 Single sine 0 125 1 24421 0 01 Single sine v 0 125 1 18421 Single sine 1 mal Figure 94 It is now possible to define the frequency scan using a Frequency per decade distribution Using this distribution the actual number of frequencies is defined by the First and Last applied frequencies in the scan 74 Page Merge files option It is now possible to merge files in order to generate a new file which contains the data from the source files This option can be used when data included in one file needs to be used in a calculation involving data from another file The source files are not deleted and a new file is created instead A name for the new fi
112. ed in the Liquid Handling Setup 42 Page Additionally the following commands have been modified with respect to the previous versions Dosino prepare the Mumber of cycles parameter has been added to the command This parameter defines how many prepare cycles should be performed on the Dosino default 1 Dosino dose the Port parameter has been added to the command This parameter defines which of the 4 ports should be used in the dosing command Dosino to end the Port parameter has been added to the command This parameter defines which of the 4 ports should be used in the to end command Two new commands have been added to the Metrohm devices group of commands Sample processor 858 inject valve this command controls the optional injection valve if present Metrohm 858 Professional Sample Processor only The valve can be set to Fill Valve parameter 0 or Inject Valve parameter 1 Sample processor 858 peristaltic pump this command controls the optional peristaltic pump if present Metrohm 858 Professional Sample Processor The speed can be set between 15 and 15 At any moment when one of the connected Metrohm devices is performing an action the status will be displayed in the manual control panel see Figure 52 Autolab display ES A Analyte Frepare Fill Empty Dose ml s Liose Fort Inout port Diosed mij 1 14 Hold stop 9128 BUSY 20 ml Figure 52 The status of each device is displayed in the manual
113. ed in the View menu see Figure 195 This can be used to manually control the Metrohm VA 663 Stand or the PAR 303 303A Stand through the IME663 and the IME303 respectively View Advanced View Setup View Measurement View a Analysis View Ej User Log Fil Autolab Display F10 MUX Control Figure 195 Manual control of the MDE is provided in the View menu Through the MDE control it is possible to manually switch purging and stirring on and off and create new drops see Figure 196 Electrode Control A Newson New drop Stirrer MIDE 1 Figure 196 The Electrode Control can be used switch purge and stirrer on or off and to create a new drop Note control of the MDE is also possible during a measurement using the Autolab control command A specific MDE tab is available in the Autolab control window see Figure 197 The Number of new drops controls the number of consecutive drops to knock off the mercury electrode 148 Page Autolab control DIO DACH Purge Off Stirrer On Set Number of new drops 1 Number of new drops Unchanged Set Number of new drops Figure 197 Control of the MDE is possible through the Autolab control command Manual control for MUX Manual control over the MUX module is available from the View menu see Figure 235 View Advanced View Setup View l La 2 Measurement View Analysis View User Log Fii Autolab Display F10
114. eeds to be checked see Figure 29 3 Edit Options BEE Automatic Current Ranging Suto Autolab control Automatic Integration Time tems Cutot on WWE i Current Add Remove Basic properties signal WE Current we Action when gt Ww Value 0 5 Action Reverse scan direction w ee once Linkable as Advanced properties Mr of detections 4 Additional cutoffs No Cutoff JK Cancel Figure 29 Specifying if the cutoff action needs to be performed only once 23 Page Integrate between markers The Integrate analysis tool has been modified and now provides the means to integrate a curve between two user defined markers The area determined in units of Y axis units of X axis is provided in the data explorer frame see Figure 30 Demo 10 Differential pulse measurement 3 Differential pulse bivSE Integrate Integrate plot 4 5E 7 Area 2 59706E 8 SE 3 5E 7 3E 7 2E VVE 1 6 Current A 1 5E 7 1E 7 5E 8 1 2 1 0 8 0 6 0 4 0 2 0 Potential applied W Figure 30 The Integrate analysis tool now integrates between two user defined markers The markers can be repositioned by right clicking them on the plot The markers can be deleted by clicking the button on the right hand side of the plot Import FRA equivalent circuit Existing FRA equivalent circuits from the GPES FRA software library can now be imported directly into the Fit and S
115. een 15 and 15 using the provided slider or numeric value 40 Page Figure 50 shows the manual control panel added to the Autolab displaying the controls for a Sample Processor Autolab display x A sample processor Tower 1 Rack position 1 48 Lit position 0 125 110 0 Pump Peristaltic pump 01 Hold stop 4589 000010 Figure 50 Manual control of a Sample Processor The Pump checkboxes provided in the manual control of the sample processor correspond to Pump 1 and 2 respectively The same applies to the Valve control not shown in Figure 50 The Sample Processor manual control panel provides the following controls e Move the rack to the specified position with respect to the Sample processor tower using the button e Move the tower to the specified position using the button Three shortcut buttons are available o moves the lift to the Work position defined in the Liquid Handling Setup for the device using the current rack position o moves the lift to the Shift position default 0 mm using the current rack position o 4 moves the lift to the Shift position default 0 mm and moves the rack to position 1 This is defined as the Home position e Switch on or off Pump 1 and or Pump 2 if present using the dedicated checkboxes shown in Figure 50 e Switch on or off Valve 1 and or Valve 2 if present using the dedicated checkboxes not shown in Figure 50 e Set the Stirrer soeed be
116. eight factors will be lower than this value The default value is 0 001 e Maximum number of iterations giving no improvement defines a second stop condition for the fitting calculation This number defines the number of iterations that are allowed during which the Chi square value does not improve When this value is reached the fitting calculation is stopped e Measurement data impedance admittance defines the type of data of the data set e Use weight factors yes no defines whether a weight factor should be used during the calculation If weight factors are used each point is multiplied by a weight factor equal to the inverse of the square of the impedance modulus If this option is not used the weight factor is the same for each point i e the inverse of the square root of the average of the impedance modulus The fit and simulation tool requires the definition of an equivalent circuit as well as initial conditions This can be done by clicking the amp button located next to the Circuit field in the fit and simulation control interface see Figure 314 E Input Max number of Iterations 100 Circuit Maximum change in chi square 0 001 Maximum number of iterations giving no improvement 100 Fitting style Impedance Use weight factors Yes Fit or Simulation Fit Measurement data format Impedance E Results Number of iterations performed 0 Result Chi square 0 Figure 314 Opening the circuit definition window 235
117. ent 1 Potential Ele i WELT WEZI Current WE Fotential WEDS WELS WE 4 J Efa Fotential E 4 Current WEH Potential External 1 400164 1 Externali1 ADC 14 2 Time Current S ITS STIS 1 ES ESI ISIE LINIOISI OSES LIK N Figure 167 The WE x Current and WE x Potential signals are available in the signal sampler Note only the signals of the selected modules are shown In Figure 167 BA modules 2 and 3 corresponding to WE 3 and WE 4 respectively are present in the instrument but not selected in the Hardware setup More information on the use of the MultiBA instruments in NOVA can be found in the MultiBA tutorial available from the Help menu Multi Autolab support Version 1 6 of NOVA includes support for multiple instruments It is now possible to connect multiple Autolab instruments to the same computer and perform measurements using any of the connected devices The maximum number of devices is limited to 8 Selection of the active device is performed using a dedicated toolbar see Figure 168 Available devices are identified by their serial numbers or by the serial number of the external USB interface if applicable File View Run Tools Help ERTES le a laa Sa ea 28 eo Select instrument AUTS3072 m ALTA3G7F2 USB Oye b JAUT 70530 Figure 168 A dedicated toolbar is can be used to select an instrument Measurements can be performed on multiple ins
118. ental settings for the Metrohm devices are now locally stored This means that the device can be operated directly after starting NOVA Manual control for all initialized devices is now available even during a NOVA procedure Full control of all the instrumental settings is now available Several devices can be operated at the same time Control for the Metrohm 858 peristaltic pump and injection valve options has been added All rackcodes are now included in the dedicated hardware setup To define the settings of the connected devices the dedicated Liquid Handling Setup can be used see Figure 43 34 Page File View Profile Run Tools Help ETTE NEE E fa Options Database Manager ET Check Procedure Alt F1 Hardware Setup Liquicl Handling Setup X pH Calibration Figure 43 The Liquid Handling Setup is available from the Tools menu In the Liquid Handling Setup window the settings of each connected device can be defined and stored These settings will be used each time one of the defined devices is connected to the computer A unique identifying name can be assigned to each connected device This ID is stored alongside the device settings The default name is set to the device serial number Figure 44 shows the settings for the Metrohm 800 Dosino 35 Page Refresh Liquid Handling setup Name Port settings Rate 0 07 ml min 166 ml min Tube length mm Tube diameter mm Fort se
119. es have been processed they will be compatible with the NOVA 1 3 format see Figure 251 210 Page EE Upgrade to Nova 1 3 File File C Documents and Settings User My Documents My Procedures 1 2 My example database Measurement 1 nox Finished C Documents and Settings User My Documents My Procedures 1 2 My example database Measurement 2 nox Finished C Documents and Settings User My Documents My Procedures 1 2 My example database Measurement 3 nox Finished C Documents and Settings User My Documents My Procedures 1 2 My example database Measurement 4 nox Finished C Documents and Settings User My Documents My Procedures 1 2 My example database Measurement 5 nox Finished Add files to list Remove files from list Create backup s Override backup s Idle Figure 284 When the upgrade application has finished the converted nox files will be ready for NOVA 1 3 Note if the location of the NOVA 1 2 source database is the My Documents My Procedures 1 2 the converted files will be automatically copied to the My Documents My Procedures 1 3 folder If the source database is located in another folder the same folder will be used as location for the NOVA 1 3 nox files Diagnostics NOVA 1 3 introduces a new version of the diagnostics tool This tool is provided as a stand alone application and can be accessed from the start menu in the Autolab group Start menu All programs Autolab Tools The diagnostics tool
120. es instruments can be controlled by NOVA in combination with the Autolab The commands related to the control of the Avantes instruments have been added to the External devices group of commands see Figure 93 l mer ternal devices Avantes initialize Avantes clase External device initialize External device send External device receive External device close Figure 93 Dedicated commands to control Avantes spectrometers are available in the External devices group of commands Please refer to the GPES User Manual for more information on the file format of the GPES files 73 Page Two commands are available e Avantes initialize initializes the control of a specified Avantes spectrophotometer connected to the computer This command can be used to specify the measurement range the integration time and other data acquisition parameters for the spectrophotometer e Avantes close terminates the control of the initialized Avantes spectrophotometer and recovers the measured data from the spectrometer This data is then associated with electrochemical data from the Autolab if applicable Frequencies per decade in the FRA frequency scan editor It is now possible to specify the frequencies per decade to use in a FRA frequency scan rather than the absolute number of frequencies in the scan When the number of frequencies per decade is specified a logarithmic distribution is used between the first and last specifi
121. evel of noise recorded for both the potential and the current see Figure 125 Autolab display A Autolab manual control AUT64148 94 Page current range Ef Figure 125 Noise meters are now used to display the noise in the measurements The noisier the signal the more bars will be displayed In Figure 125 the noise on the potential is very small one bar while the noise on the current is larger four bars out of maximum of eight Real time modification of the command parameters It is now possible to modify certain command parameters while the measurement is running In the measurement view an additional frame is displayed during the experiment If the running command offers the possibility to modify a parameter in real time the current value will be displayed in the additional frame see Figure 126 File View Profile Run Tools Help File View Profile Run Tools Help Be Te Bere tt eee eee re a Ea MB ET Cyclic voltammetry potentiostatic Cyclic voltammetry potentiostatic Tired procedure Tired procedure 2 Autolab control 2 Autolab control Wait time 3 Wait time s Optimize current range Optimize current range BCV staircase EECV staircase Upper vertex potential v Upper vertex potential v Lower vertex potential v Lower vertex potential v stop potential V stop potential v Number of stop crossings 2 Number of stop crossings 2 step potential V 0 00244 step potential V
122. f the use of the multiple plot option is displayed in Figure 206 153 Page Bode modulus Bode phase Z Q 1000 10000 200 Z Q Frequency Hz 60 3E 5 40 Current resolution 2E 5 lt x lt gt 20 16 5 S 0 5 0 oOo j 1E 5 9 w 20 2E 5 o 3E 5 40 4E 5 SES an 0 01 0 005 0 0 005 0 01 0 015 0 0 0005 0 001 0 0015 0 002 0 0025 0 003 0 0035 0 004 Time domain E V Time s Figure 206 Using the multiple plot feature in an impedance measurement plot 1 top left Nyquist plot plot 2 top right Bode plot plot 3 bottom left Lissajous plot plot 4 bottom right Resolution vs time Note results of calculations and data handling commands are displayed after the data has been collected Additionally it is possible to copy plots from the analysis view into any of the 4 available plots in the measurement view This provides the possibility to create overlays between data points being recorded real time and data points from previous experiments see Figure 207 a Demo 01 Copper deposition E CY staircase Plot Gptons Propertes Add analysis Show All Plots H easurement plot 2 l Hide All Plots Measurement plot 3 Save in My commands Measurement plot 4 Delete Remove all from View Figure 207 Copying visible plots from the analysis view to the measurement view can be done by right clicking a plot in the analysis view and choosi
123. filter It is best suited for differintegration in the range of 0 0 0 5 up to semi integration It is less precise than GO algorithm but the number of operations is linearly related to the number of data points For details refer to Pajkossy T Nyikos L J Electroanal Chem 179 1984 65 e Spherical convolution this algorithm is used to carry out convolution of the data measured using a spherical electrode and staircase potential waveform Values of the diffusion coefficient and the electrode radius are necessary Details of the algorithm can be found in S O Engblom K B Oldham Anal Chem 62 1990 625 e Kinetic convolution this algorithm carries out kinetic convolution according to F E Woodard R D Goodin P J Kinlen Anal Chem 56 1984 1920 This convolution requires the value of the rate constant of irreversible homogeneous follow up reaction ECi mechanism The Convolution command can be added to a procedure to process potential sweep or chronoamperometry data This command requires the Time signal and the WE 1 Current signal The type of convolution used can be specified using a drop down list see Figure 23 18 Page E Convolution Current lt array gt A a Time araw gt s c spherical convolution Electrode radius crn Time semi derivative Diffusion coefficient cm Time semi integral Convoluted current a0 diferinte gration 7 Convolution plot FELT differintegration lt gt spherical c
124. fit o Corrosion rate Tafel slope e In the Analysis impedance group 191 Page o Kronig Kramers test o Include all FRA data Furthermore the following commands have been renamed e Automatic peak search gt Peak search e Mathematical parser gt Calculate signal e Signal windower gt Windower My commands It is now possible to define your own commands using the My commands framework In Nova 1 4 a new database that be used to store your own commands has been added This database can be defined using the database manager see Figure 256 Database management Database locations Procedures standard My Documents My Procedures 1 4 Standard User My Documents My Procedures 1 4 User Measured data Data My Documents My Procedures 1 4 Data Commands Commands My Documents My Procedures 1 4 Commands Figure 256 The database manager can be used to define a Commands database Commands defined using the My commands framework will be stored in the defined database and will be available for procedure building in the commands browser see Figure 257 192 Page Control Control Metrohm devices Measurement general Measurement cyclic and linear sweep voltammetry Measurement chrono methods Measurement impedance Data handling Analysis general Analysis baseline correction Analysis corrosion Analysis impedance Plots general Plots impedance Figure 257 The My comm
125. ftware reads and writes data files In order to ensure backwards compatibility with the previous release version conversion tools are provided Previously recorded data sets obtained with NOVA 1 2 need to be converted using these tools before the data and the procedures can be used by NOVA 1 3 This section describes how to use the conversion tools 207 Page The main difference between version 1 2 and 1 3 is that the former uses a single file database storage system whereas the latter uses a multiple file database storage This means that data sets obtained with NOVA 1 2 have first to be extracted from the database as individual NOVA 1 2 nox files export phase The Nova 1 2 nox files can then be converted into nox files which can be used by NOVA 1 3 conversion phase The two steps are schematically summarized in Figure 247 Export Convert gt yap Pater hth J NOX y NOX EE La NOVA 1 2 object database NOVA 1 2 file database NOVA 1 3 file database My Documents My My Documents My My Documents My procedures 1 2 yap procedures 1 2 nox procedures 1 3 nox Figure 278 Schematic view of the NOVA 1 2 to NOVA 1 3 conversion process After installing NOVA 1 3 start the Export databases 1 2 to files application Start menu Programs Autolab Tools This will start the export application which will display the contents of the default folder containing the NOVA 1 2 databases My Docu
126. galvanically isolated Do not use pin 4 or pin 11 as ground pin for the read lines Important the write lines of the PGSTAT101 DIO connector are capable of supplying a maximum current of 200 mA Suitable pull down resistors should be placed in the write lines of the DIO cable connected to the PGSTAT101 A typical value for the pull down resistance is about 1 kQ Please refer to the user manual of the external device connected to the PGSTAT101 for more information The Autolab contro command only shows a single option in the DIO tab where the 8 write pins of the single DIO connector can be defined see Figure 231 171 Page Autolab control WE 1 DIO0 DAC Set Pl A Write 0 00000000 Figure 231 The 8 pins of the write section of the single DIO port of the PSGTAT101 can be set directly from the Autolab control command The Wait for DIO trigger command available in the Measurement General group of command has also been adjusted Pressing the amp button in the procedure editor opens a dialog window which can be used to identify the available connectors and ports for the instrument in use For the PGSTAT101 a single input port is available on the DIO connector see Figure 232 DIO connector DIO connector port Trigger byte Use time limit Maximum time as DIO connector DIO connector o Trigger byte Maximum time s Figure 232 The new Wait for DIO trigger interface Note
127. ge OCP Yes aay OCP value WE 1 Potential lt _armay gt V Time lt _array gt s B Evs t Graphical settings General settings m x Time 5 Y WE 1 Potential V Fa Time 5 E Set reference potential 0 000 Reference potential V 0 000 1LF lt L Figure 305 Linking the OCP value with the Set reference potential will force NOVA to apply all the potential values with respect to OCP The same command can be used to correct the potential of the working electrode with a user defined offset This offset will be added to all the potential values in the procedure This can be useful if the experimental settings are defined relative to a different reference electrode than the one in use Note in this case it is not required to link the Reference potential parameter Import FRA data command An mport FRA data command has been added to the analysis group of the command browser This command is similar to the mport GPES data It allows importing data files obtained with the FRA software into the NOVA 1 3 database Figure 306 illustrates the use of the Import FRA data command The parameter of the command is the location of the dfr file The command generates a Nyquist plot and a Bode plot automatically Note the Import FRA data command can be used even if there is no instrument connected to the computer 228 Page Import FRA data Filename Filename Filename Frequency lt amay
128. h a short interval time 48 Page When the fast options are used in combination with one or more cutoff options the number of consecutive detections specified for each cutoff no longer relates to the interval time The fast interval time is used instead This means that the number of consecutive detections will no longer match the number of data points recorded after the cutoff condition is met Derivative based recording in the Record signals gt 1 ms command The Record signals gt 1 ms command now provides extra functionality by combining the modifications described in Sections Error Reference source not found and Error Reference source not found of this document When a Record signals gt 1 ms command is executed with the Fast options active and if the time derivative of one or more of the sampled signals is added to the signal sampler the possibility to specify a sample thresho dtor each of the derivative signals is provided see Figure 59 Commands Parameters Links Chrono amperametry At gt 1 ms Remarks Chrono amperometry At gt 1 ms ma End status Autolab al signal sampler Time WE Potential WE Current Options 1 Options Ea Instrument Instrument description Autolab control Set potential 0 000 Set cell On a walt time s 5 Record signals 1 ms 5 0 01 Set potential 0 500 H Record signals gt 1 ms 5 0 01 Set potential 0 500 Record signals gt 1 ms Duration s
129. h electrochemical signals to use for this new signal set by linking the available signals of the CV Staircase to the X Y and Z inputs of the signal set command 217 Page CV staircase Start potential V Upper vertex potential V Lower vertex potential V stop potential v Number of stop crossings step potential V Scan rate V s Total number of points Interval time Ls Signal sampler Potential applied Scan WE 1 Potential Time WE 1 Current B ivs E Graphical settings x Y Z E Signal set Graphical settings x Y Z Set cell lt gt lt _ gt 0 000 1 000 1 000 0 000 2 0 70000 0 000 1 000 1 000 0 000 2 0 00244 0 10000 Time WE 1 Potential WE 1 Current lt _amay gt V _aray gt _aray gt V _array gt 5 _array gt A A A AA General settings Potential applied V WE 1 Current A Time s lt array gt lt array gt lt array Off Figure 293 The new signal set is added to the CV Staircase command Setting up the signal set s more than one plot can be displayed in real time Figure 294 shows an example in which two signals are plotted in the measurement view during the measurement 1 4 1 6E 6 1 2 1 4E 6 1 1 2E 6 0 8 1E 6 0 6 8E 7 0 4 6E 7 S T z 0 2 4 amp 7 Z Cc 0 S 27 Zo 5 O 0 4 in LLU 2ET 0 6 4E 7 0 8 6E 7 1 8E 7 42 1E 6 1 4 Ag 1 2E 6 14 16 18 20 22 24 26 28 30 32 34 36
130. have been condensed into one line commands Figure 235 shows the factory default Cyclic voltammetry procedure The Autolab control Set Cell Wait time and Optimize current range command have been reduced to a single line in the procedure editor see Figure 235 175 Page Commands Cyclic voltammetry potentiostatic Remarks End status Autolab Signal sampler Options E Timed procedure Autolab control Set potential Set cell Wait time s Optimize current range B CV staircase start potential v Upper vertex potential V Lower vertex potential V stop potential V Number of stop crossings step potential V Scan rate V s Total number of points Interval time Lis Signal sampler Options Potential applied Time WE 1 Current Scan Index ivs E Set cell z gt 2s Parameters Cyclic voltammetry potentiostatic no extra modules required Collection Time WE 1 Current 1 Options 5 0 000 1 000 1 000 0 000 2 0 10000 0 000 1 000 1 000 0 000 2 0 00244 0 10000 1650 24400 Time WE 1 Current 1 Options lt _ array gt V _array gt s5 _array gt A array gt _aray gt A AA Off Figure 235 The factory default Cyclic voltammetry potentiostatic procedure New Autolab procedures The following new factory default procedures have been added to the Autolab group see Figure 236 e Cyclic voltammetry with EQCM e Cyclic voltammetry with BA e Cyclic voltammetry w
131. he Analysis view as a quick dial control see Figure 144 109 Page Search mode D Automatic J Manual Base line mode Minimum peak height 0 Minimum peak width 0 Mr of points in search window 3 Number of significant digits 5 D Reset Peak Type Forward Reverse Figure 144 The Number of points in search window parameter can now be adjusted with a quick dial This allows the user to easily modify this parameter and visualize the changes in the peak search results Moreover the search algorithm is now also able to cross over data gaps When encountering data sets with a gap the peak baseline can be extended over the gap if the gap distance is smaller than 3 of the X and Y value range see Figure 145 0 001 0 001 z 0 0005 T 0 0005 j T P L G 0 z 0 mi mi z 0 0005 gt 0 0005 0 001 0 001 0 2 0 0 2 0 4 0 6 0 2 0 0 2 0 4 0 6 Potential applied V Potential applied Y Figure 145 The redesigned peak search tool is able to extend the baseline across data gaps left source data with gap around 0 25 V right result of peak search Export to ZView A dedicated data exporting tool has been added to NOVA Using this tool it is possible to quickly export impedance spectroscopy data to a ZView compatible format see Figure 146 110 Page e il TestFRA a E FRA measurement potentiostatic H FRA frequency scan Plot Options O Nyquist 2 vs 2 Properties Bode modulus l Bode phase E
132. he Nyquist plot Each selected data point will be marked by a black arrow After the third point is clicked the fitted circle will be plotted in the 2D plot area and the calculated values for the fitted circle will be displayed in the bottom area of the 2D plot see Figure 310 231 Page Z Q 0 200 400 600 800 4000 Z 0 E Point selection style SnapToDataset Estimated Parameters 9 974E2 Figure 310 The results of the Electrochemical circle fit are displayed in the area at the bottom of the 2D plot Note it is possible to save the results of the electrochemical circle fit by clicking the save button located in the analysis toolbar Fit and simulation Detailed analysis of the data obtained during an electrochemical impedance measurement is usually performed by fitting the experimental data with an equivalent circuit based on the Boukamp model Many circuit elements can be used to fit the experimental data with a model However the equivalent circuit must be constructed carefully since a given experimental data set can be fitted with more than one unique equivalent circuit The fit and simulation tool allows the definition of an equivalent circuit using the following elements e R resistance e C capacitance e L inductance e Q constant phase element e W Warburg impedance e O Cotangent hyperbolic e T Tangent hyperbolic 232 Page The circuit elements can be arranged in series or in p
133. he device are listed below e Compliance voltage 10 V e Maximum applied potential 10 V e Maximum current 100 mA e Electrode connections CE RE S WE and additional analog ground e Analog 1 0 Eout lout Vin Vout e Digital I O 8 outputs and 4 inputs e Internal dummy cell 100 Ohm 1 MOhm 1 uF e iR compensation Requires optional I O cable 165 Page Hardware setup PGSTAT101 The new Autolab PGSTAT101 is now supported in the latest version of NOVA The instrument can be selected in the hardware setup window see Figure 224 Hardware setup _ ox File Tools Main Module PGSTATIO1 2GSTAT302N PGSTAT128N _ wAutolab III PGSTAT100 PGSTAT302 gt dditional Module s F wAutolab Il _ PGSTAT20 PGSTAT10 Biema IME303 IME663 EEO Power Supply Frequency mpotFRACalibraion FRA offset DAC range EEN C Documents and Settings All Users Application Data Eco Chemie HardwareSetup60 xml Figure 224 The PGSTAT101 is available in the hardware setup Note the PGSTAT101 is not modular and no additional modules except the IME663 and the IME303 can be selected when this instrument is used The PGSTAT101 can be fitted with the optional I O cable This cable provides four additional connections to the PGSTAT101 analog circuits see Figure 225 All the Signals are with respect to Autolab ground and indirectly to protective earth 166 Page Figure 225 The o
134. he progress is displayed in real time When the first step is finished the extracted files can be upgraded to the NOVA 1 3 file format see Figure 281 ad Export NOVA 1 2 database to nox files File Status Message C Documents and Settings User My Documents My Procedures 1 2 My example database yap Done lt gt Add database to list Remove database from list Upgrade files to Nova 1 3 Idle Figure 281 When the extraction process is finished the files can be upgraded to the NOVA 1 3 file format Note the original databases will not be destroyed which means that you can still access the data from NOVA 1 2 Click the Upgrade files to NOVA 1 3 button to continue The Export application will close and the Upgrade application will be loaded The exported nox files will be displayed in the list see Figure 282 209 Page as Upgrade to Nova 1 3 File File C Documents and Settings User My Documents My Procedures 1 2 My example database Measurement 1 nox C Documents and Settings User My Documents My Procedures 1 2 My example database Measurement 2 nox C Documents and Settings User My Documents My Procedures 1 2 My example database Measurement 3 nox C Documents and Settings User My Documents My Procedures 1 2 My example database Measurement 4 nox C Documents and Settings User My Documents My Procedures 1 2 My example database Measurement 5 nox Add files to list Remove files from list Create backup s Overri
135. ic Cyclic voltammetry current integration e Cyclic voltammetry linear scan e Cyclic voltammetry linear scan high speed e Linear sweep voltammetry potentiostatic Linear sweep voltammetry galvanostatic Linear polarization Hydrodynamic linear sweep Differential pulse voltammetry square wave voltammetry e sampled DC polarography e Chrono amperometry At gt 1 ms e Chrono potentiometry At gt 1 ms e Chrono amperometry fast e Chrono potentiometry fast Chrono coulometry fast e Chrono amperometry high speed e Chrono potentiometry high speed Chrono charge discharge Interrupt e Interrupt high speed Positive feedback FRA impedance potentiastatic FRA impedance galvanastatic FRA potential scan Commands Procedures Autolab Cyclic voltammetry potentiastatic Cyclic voltammetry qalvanostatic Cyclic voltammetry current integration e Linear sweep voltammetry potentiostatic Linear sweep voltammetry galvanostatic Linear polarization e Hydrodynamic linear sweep e Chrono amperometry At gt 1 ms e Chrono potentiometry At gt 1 ms Chrono amperometry fast Chrono potentiometry fast Chrono coulometry fast i Chrono charge discharge Figure 103 Overview of the Autolab procedures with a yAutolablll left hardware based profile not active and right hardware based profile active Application based All the commands and the procedures in Nova have been tagged with an appli
136. ignal External 1 ADC164 2 AICUIGIE signals i 1 F ower i 1 Resistance SIOOSSsi8 Sample alternating Cancel Figure 80 WE 1 Power and WE 1 Resistance signals are now available in the sampler These new signals are calculated signals and therefore cannot be sampled in optimized mode The calculation is performed in real time which allows these new signals to be involved in the cutoff option as well see Figure 81 23 Edit Options Automatic Current Ranging Cutoff Cutot on WET Power signal WE 11 WEC I Action when WWE 1 Fotential WE Power Value WE 1 Resistance External 1 4001 64 1 External 1 400164 2 Time Action Linkable as Advanced properties Mr of detections 4 Additional cutoffs Mo Cutoff E Remove Figure 81 The new signals are also available in the cutoff option 65 Page WE X Charge signal The WE X Charge signal in Coulomb has been added to the signal sampler This Signal is available for each working electrode for which the current signal is measured see Figure 82 e Edit Sampler VEC Current Fotential Power Charge Current WE C2 Charge External 1 ADCTE4 1 External 1 ADC1TH4 2 Time l i Resistance l i wWE WE I WECI WE I WEL 2 sample alternating eke sample Optimized Sampler configuratian Wf vf Sampler Segment 2 Current Segment Optimized
137. ile Cy Program FilesfEco Ch 6 0 3530 25445 Infralution Common filen C Program Files Eco Ch 3 10 1 0 Infralution Contrals file yW C Program Files Eco Ch 3 10 1 0 lnfeohitiqwe anterak 4 fie fila tir Sea aro Eila c iE ee ooh 1710 1 A Acknowledgement Figure 217 The hardware configuration is now shown in the About menu alongside software version information 160 Page Improved support for Metrohm devices Support for Metrohm devices has been improved in this version of NOVA The Initialization commands now have a dedicated interface in which the parameters of the device can be easily entered Figure 218 shows the case of the Dosino settings interface Dosino settings Dosina Serial number 9128 Filling port Output pot 1 Output port 2 Fort 1 settings Rate 0 07 mifmin 166 mifrmin TI mmm mi oo ma mJ mD i Tube length mmj a Tube diameter mm Fort 2 settings Rate 0 07 ml min 166 miltrmin Tube length mmj Tube diameter rim Fort 3 settings Rate 0 07 ml min 166 mliimin tT Tube length mm Tube diameter rim D a Cancel Figure 218 Dosino settings interface Autolab control in the options The Options menu has been extended with an additional tab which can be used to set specific Autolab settings at the end of each sampling step see Figure 219 This can be used for example to create a new drop after each sa
138. ile or export measured electrochemical signals to an ASCII file The Import ASCII data has a number of parameters like the number of lines to ignore at the beginning of the file the number of columns in the file the column delimiter see Figure 264 a Import ASCII data Filename sal Number of columns 2 Column delimiter opace c Decimal separator al Number of rows to skip 2 Column 1 lt array gt Column 2 lt array gt Index lt array gt e Figure 264 The import ASCII data command Moreover it is possible to specify the name of the signals using the same interface as the new Import GPES command 196 Page El Import ASCII data Column delimiter Decimal separator Number of rows to skip Column 1 Column 2 Index z gt Filename Space Signal Editor Number of columns Column 1 Column 2 Edit Signal Current Signal name Unit Figure 265 Changing the name of the columns can be done using the Signal Editor window The Export ASCII data command can be used to export measured or calculated electrochemical signals during a measurement The number of columns and the delimiter can be specified as well as the filename see Figure 266 a Export ASCI data Filename Number of columns 2 Column delimiter Tab az Decimal separator File mode Overwrite Remarks za Column 1 lt aray Column 2 lt _ array gt lt gt Figure 266 The export ASC
139. imulation analysis tool in NOVA see Figure 31 24 Page are Equivalent Circuit Editor _ O ES Circuit Edit Tools Se Open Circuit Constant Phase Element Q Insert Circuit la Save Circuit O vertie Name Import Circuit Export Circuit Start 3 13846E 06 Import FRA Circuit N Fitted Ey X Clear Circuit Fixed Start 0 876189 Fitted J Fixed OK Cancel Figure 31 The option for importing FRA equivalent circuits is now available in the Fit and Simulation analysis tool FRA equivalent circuit files ecc files from the FRA software package can be imported directly into the circuit editor The equivalent circuit from the FRA software element is converted to a Q element in NOVA New Import Export equivalent circuits The possibility to import and export equivalent circuits directly from the Fit and Simulation dialog window has been added to this version of NOVA see Figure 31 The equivalent circuits are available as ece files Circuits from older versions of NOVA can be imported into the current version New format for the Message box and Input box commands The Message box and nput box commands are now provided with a text editor that supports line breaks The message to shown in the two commands can now be edited directly into the procedure editor and line breaks can be created using the enter key see Figure 32 25 Page E Message box Tithe of box AL
140. imum Maximum Potential 128 2 pV 133 3 pV 126 2 pV 137 3 pV Time lett 103 25 Time to average 5 dE dt 2 060 pV s Limit dE dt 1 000 p s 2 00 Soe g _ LL Oo Accept on timeout Average OCP Accept on dE dt limit Last OCP Figure 304 The OCP determination window displayed during the measurement During the OCP determination it is possible to check or uncheck the Accept on timeout and Accept on dE dt limit options It is also possible to switch from the average OCP to the last measured OCP The minimum and maximum values represent the lowest and highest value of the WE 1 Potential measured during the OCP determination The green line plotted in the OCP determination window represents the dE dt limit 227 Page Note it is possible to press the Accept button to stop the OCP determination and use the last value of the WE 1 Potential as the OCP Set reference potential command A new Set reference potential command is available from the measurement group in the command browser This command can be used to apply any offset to the potential applied on the working electrode WE 1 in potentiostatic mode This command can be used in combination with the OCP determination command to apply all the potentials with respect to the OCP see Figure 305 E Timed procedure E OCP determination 0 000 signal sampler Time WE 1 Potential Maximum time s 120 dE dt limit 1E 06 Use avera
141. ings User My Documents My Procedures 1 3 Demo Database Demo 02 Copper deposition QCM nox Finished C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 03 Bipotentiostat measurement PtPt Rin Finished C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 04 Hydrodynamic LSV with increasing rot Finished C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 06 Galvanostatic CV nox Finished C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 07 High speed chrono methods ADC750 Finished C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 08 Chrono methods ADC 164 20 steps n Finished C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 09 Chrono methods ADC 164 with variabl Converting C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 12 Imported pcPt GPES data nox C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 13 Imported pcPt GPES data nox C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 14 Imported GPES data nox Figure 250 The upgrade application converts every nox file in the list from to the NOVA 1 4 format When all the nox files have been processed they will be compatible with the NOVA 1 4 format see Figure 251 188 Page EB U
142. inked items is selected see Figure 276 Unselected links are displayed in light grey color Procedure Values Cyclic voltammetry Remarks Factory standard procedure m End status Autolab Collection m Signal sampler Time WE 1 Potential WE 1 Current al Options Automatic Current Ranging WE 1 1 mA 100 E Timed procedure Set Potentiostatic and select current range ma E Set potential 0 000 Setpoint potential V Set cell On Wait time s 5 Optimize current range 5 B CV staircase 0 000 1 000 1 000 0 000 2 0 70000 start potential V 0 000 Upper vertex potential V 1 000 Lower vertex potential V 1 000 stop potential V 0 000 Number of stop crossings 2 Step potential V 0 00244 Scan rate V s 0 10000 Total number of points 650 Interval time Ls 24400 Signal sampler Time WE 1 Potential WE 1 Current Fotential applied lt _array gt V Scan lt _ amay gt WE 1 Potential lt _armray gt V Time lt _ armay gt s WE 1 Current lt _array gt A B ivs E Graphical settings General settings m X Potential applied V Y WE 1 Current A Z Time 5 Set cell Off lt gt gt Figure 276 Links are highlighted whenever a linked parameter or signal is selected Note linking and unlinking is now available through the right mouse button 206 Page Printable links The print procedure option available from the File menu can now be used to print the visible links al
143. ion protection Unche Reference potential Uncha P1 CLower Write Unchange P1 CUpperDirection Uncha Pi CUpperWrite Unchang P 2 A Direction Unchanged P2 A Write Unchanged P2 B Direction Unchanged P2 B Write Unchanged P2 CLower Direction Uncha F2 CLower Write Unchange P2 CUpper Directon Uncha F2 CUpper Write Unchang Figure 300 A typical Autolab control interface window The available settings for each item can be selected from a drop down list see Figure 301 The default status of each item is Unchanged which means that the settings of the instrument will not be changed unless it is required by the user 224 Page Autolab control WE 1 Cell Unchanged Current range Unchanged current range Unchanged ment range rent range rent range rent range Scangen input Unchanged Oscillation protection Unche Reference potential Uncha WE Cell Unchanged Current range Unchanged Potential Unchanged BA Mode Unchanged FRA input Unchanged DIO 1 P1 A Direction Unchanged P1 A Write Unchanged P1 B Direction Unchanged P1 B Write Unchanged P1 CLower Direction Uncha P71 CLower Write Unchange P1 CUpper Direction Uncha P1 CUpper Write Unchang P2 A Direction Unchanged P2 AWrite Unchanged P2 B Direction Unchanged P2 B Write Unchanged P2 CLower Direction Uncha P22 CLower Write Unchange P2 CUpper Direction Uncha F2 CUpper Write
144. it time 3 Optimize current range CY staircase start potential v Upper vertex potential 6 Lower vertex potential 6 stop potential v Number of stop crossings step potential v scan rate y s Estimated number of points Interval time s signal sampler E Options Cutoff current H E T Farameters Links Cyclic voltammetry potentiostath ET Time WWE Fotential WEJ C 1 Options ma 0 000 On weal 5 5 O 000 1 000 1 000 0 000 2 01 0 000 1 000 1 000 0 000 0 00244 0 7 000000 1650 0 024400 Time WWE Fotential WEC C Options Fotential applied Time WE Current Srah WE Potential Index Ives E set cell lt gt lt gt ay array ev array gt 3 Array A errery gt Array Cv STEN gt AA A AN Ott Figure 79 The cutoff limit is displayed in the procedure editor if a name is provided Power and Resistance signals The WE 1 Power signal in Watt and the WE 1 Resistance signal in Ohm have been added to the signal sampler These signal are derived from the WE 1 Potential and the WE 1 Current signals and can only be recorded if both signals are sampled see Figure 112 64 Page a Edit Sampler signal sample Optimized Sampler configuration WE 1 Current Sampler WE1 Potential E Segment WELT Power WEI Potential WE 1 Resistance segment Optimized External 1 ADC164 1 Se 5 Calculated s
145. it versions of Windows for all instruments with USB control Support for the new Autolab PGSTAT204 New user interface for Autolab control command New user interface for Chrono methods and Chrono methods high speed command New user interface for FRA measurement command Phase out of the Timed procedure command Timing guide in procedure editor and managed timing Real time validation in procedure editor More detailed validation information Ignore warnings in validation Link to Windows Explorer for database Cutoff information displayed in options tooltip Cut Copy Paste option in procedure editor Manual control for external devices Support for 64 Bit versions of Windows for all instruments NOVA now includes support for 64 Bit versions of Windows for all instruments This is an improvement with respect to the previous version of NOVA which provided support only for the latest generation of Autolab instruments S Warning The GPES compatible driver cannot be used in 64 Bit versions of NOVA This choice is greyed out in the Driver manager application see Figure 1 Warning Support for third party instrumentation Metrohm and Avantes is not 64 Bit compatible 2 Page Select the driver used to control your Autolab instrument Nova only recommended setup Select this driver when you only use Nova 1 or higher on your PC Advantages Faster USB data exchange Connect a maximum of 16 Autolab instruments Support
146. ith ECD e Chrono potentiometry e FRA impedance galvanostatic Note some of the Autolab factory default procedures have been renamed 176 Page E Autolab Cyclic voltammetry potentiostatic os Cyclic voltammetry galvanostatic Cyclic voltammetry with EQCM Cyclic voltammetry with BA Cyclic voltammetry with ECD Chrono amperometry gt Chrono potentiometry z Chrono amperometry fast Chrono potentiometry fast Chrono charge discharge Linear polarization Hydrodynamic linear sweep z Linear scan High speed linear scan FRA impedance potentiostatic FRA impedance galvanostatic FRA potential scan Figure 236 The Autolab factory default procedures Grouped commands All the commands are now grouped in dedicated sections in the commands browser Additional sections have been added like the analysis sections in which specific analysis commands can be found and the plot sections in which ready made plot commands are located see Figure 237 177 Page Control Metrohm devices External devices Measurement general Measurement cyclic and linear sweep voltammetry Timed procedure potentiostatic CV staircase CV linear scan e CV linear scan high speed LSV staircase Timed procedure galvanostatic CV staircase galvanostatic LSV staircase galvanostatic Measurement chrono methods Measurement impedance Data handling Analysis general Analysis baseline correction Analysis corrosion Corro
147. l will be available in the Autolab display window see Figure 160 Using this panel it is possible to perform manual measurements using the FRA2 module The frequency and amplitude can be directly defined in the panel as well as other relevant parameters 121 Page Autolab display A Autolab manual control AUT amp 30 2 Current ma status current range a A FRA manual control frequency Hz amplitude a a iE UULU Mode Internal Wave type Sine Integration time s Minimum number of cycles to integrate Elapsed time s E D vo ELA Vv KOC LA PACI LAJ 1 880 m 108 1 m 10 53 u Darou dg 4 Freq Hz 9 02 Phasen i 2 0d 1 000 k 20a 1 51 15 ETE 158 1 Figure 160 The Autolab display with the FRA manual control Pressing the FRA ON button switches on the FRA2 module and starts the manual measurement The measured values are displayed at the bottom of the panel It is possible to modify the amplitude or the frequency during the measurement Note the measurements are repeated until the FRA ON button is clicked again to switch off the impedance analyzer More information on the use of the FRA manual control panel can be found in the Impedance tutorial available from the Help menu 122 Page Graphical user interface for Fit and Simulation A graphical circuit editor has been added to the Fit and
148. le must be specified upon merging see Figure 95 File View Profile Run Tools Help ee te Bee eee ae ER Cae ee es ae ee Procedure name Time stamp Remarks Instrument Instrument description Procedure 1 3 20 2012 2 57 34 PM This is the source data from procedure 1 Procedure 2 aa Bt ees the source data from procedure 2 Re stl Set Active Procedure Properties Store in Repository Pro xc Delete from Repository Name Restore from Repository MERGED Procedures Im port Data Enter the strings in the collection one per line Export Data X Delete Data Merge Data Procedure 1 This is the source data from procedure 1 Procedure 2 This is the source data from procedure 2 Cancel Figure 95 Merging data files in the NOVA database A new file is created and added to the database This file contains the data from the merged source files see Figure 96 File View Profile Run Tools Help he Bit a hr IIT SS co eco oi he Procedure name Time stamp Remarks Instrument Instrument description MERGED Procedures 3 20 2012 3 17 53 PM Procedure 1 Procedure 1 3 20 2012 2 57 34 PM This is the source data from procedure 1 Procedure 2 3 20 2012 2 57 09 PM This is the source data from procedure 2 Figure 96 A new merged file is added to the database Wait time and Wait time us command consolidation The Wait time s and Wait time us commands have been consolidated to avoid confusio
149. lement also referred to as a Q element e n the value of the exponent of the constant phase element To use the electrochemical circle fit load an impedance measurement and select the Nyquist plot for display in the 2D plot area Click on the analysis toolbar and activate the Electrochemical circle method from the Baseline fit group see Figure 308 AGS Analyze Clear Save None id None Peak search Regression Circle Fit and Simulation Polynomial known order Polynomial unknown order Exponential 1100 1000 900 800 700 600 Z Q 500 E 400 300 x 200 x 100 0 0 200 400 600 800 1000 Z Q Figure 308 Selecting the Electrochemical circle method from the Baseline fit group Once the Electrochemical circle method has been selected a new area will be displayed at the bottom of the 2D plot area see Figure 309 The mouse cursor changes to a large cross 230 Page To use the Electrochemical circle baseline fit tool three measured data points must be clicked fixing the data points through which the fitted circle must pass 1100 1000 900 800 700 600 500 400 300 200 100 Z Q O 200 400 600 800 1000 Z Q Point selection style Snap T oDataset Farameter Name Estimated Parameters Figure 309 Selecting the Electrochemical circle method displays a control area at the bottom of the 2D plot area Using the left mouse button select at least three data points in t
150. licable range The offset DAC should not be modified when the cell is on during a measurement A warning is provided during validation if the procedure requires the offset DAC to be reset during the experiment see Figure 7 67 Page Validation results Ela The following problems were encountered during validation Messaqe Command AUT40148 AS The Offset DAC will be changed while the cell is on set potential Time remaining 30 seconds Figure 84 A warning is provided when the offset DAC is reset while the cell is switched on Internal dummy cell control for PGSTAT101 and M101 The PGSTAT101 and M101 are both fitted with an internal dummy cell This internal dummy cell can now be controlled through the Autolab contro command as shown in Figure 138 Autolab contral Cell Unchanged Current range Unchanged Bandwidth Unchanged Mode Unchanged IR Compensation Unchanged IR Compensation value Unchanged Reference potential Unchanged Internal dummy cell Off Internal dummy cell Unchanged Internal dummy cell Off Internal dummy cell On Ofiset Value Unchanged Figure 85 The internal dummy cell for the PGSTAT101 and the M101 can now be controlled using the Auto ab control command Using the internal dummy cell toggle it is possible to set the internal dummy cell on or off 68 Page The internal dummy cell must be switched off when measurements are performed on a real cell The procedur
151. lorer is available from the right click menu Using this option it is possible to quickly locate the selected file on the computer see Figure 17 12 Page hl la Procedures o0 fs l Home Share View f o My Documents gt My Procedures 1 10 gt Procedures v Search Procedures P x Favorites Name Date modified Type Size New procedure nox 13 12 2012 06 24 NOX File 55 KB Libraries iM Computer a Network 1 item 1 item selected 54 6 KB Figure 17 The Show in Windows Explorer option allows to quickly locate a file on the computer The link to the file location in Windows Explorer also provides the means to change the name of the nox file Cutoff information displayed in options tooltip The options tooltip now provides more detailed information about the cutoffs used in the procedure editor The limits used in the cutoff option are now shown in tooltip see Figure 18 Commands Parameters Links Cyclic voltammetry potentiostatic Remarks Cyclic voltammetry potentiostatic End status Autolab oignal sampler Time WE Potential vwE 1 Current Options 1 Options Instrument ALT 40008 Instrument description Options Autolab control Cutoff WE 1 Current gt 0 0006 Set potential 0 000 Set cell On Vat time 3 z Optimize current range z CY staircase U 000 1 000 1 000 0 000 2 01000000 7 cet cell Ct lt gt Figure 18 The limits defined in the
152. ly see Figure 246 185 Page FE Determine FRA Range Last appled frequency 0 01 A rms First applied frequency Applied AC amplitude Number of frequencies 3 ms top Freg Amplitude Wave type Frequency step 10000 Hz 0 01 A rms Sine C Linear 1000 Hz 0 07 A rms Sine 100 Hz 0 01 Arms Sine Logarithmic OC Square root Wave type Single sine D 5 sines below 3472 Hz D 15 sines below 315 7 Hz Collection Figure 246 The GSTAT FRA range builder window NOTE Automatic current ranging is not possible in GSTAT mode Reverse compatibility with previous NOVA versions This version of NOVA introduces a large number of changes that affect the way the software reads and writes data files In order to ensure backwards compatibility with the previous versions conversion tools are provided The conversion tool can be used to convert data recorded with previous versions The conversion process is summarized Figure 247 Data from NOVA 1 2 is stored in a single yap file which is first converted to files in the NOVA 1 3 format Data from NOVA 1 3 is available as single nox files can be converted into NOVA 1 4 nox files 13 More information can be found in the NOVA 1 3 release notes 186 Page NOX Convert Convert NOX yap op Y A Previous NOVA NOVA 1 3 file database NOVA 1 4 file database versions My Documents My My Documents My procedures 1 3 nox proced
153. ments My Procedures 1 2 All the NOVA 1 2 databases in this folder will be displayed see Figure 248 EE Export NOVA 1 2 database to nox files File Status Message C Documents and Settings User My Documents My Procedures 1 2 My example database yap lt gt Add database to list Remove database from list Upgrade files to Nova 1 3 Idle Figure 279 The contents of the My Procedures 1 2 folder are displayed in the Export application Using the Add database to list and the Remove database from the list buttons databases can be added or removed from the list The conversion involves two steps The first conversion step converts the selected database s to individual nox files and the second conversion step converts the NOVA 1 2 files to NOVA 1 3 files 208 Page Having selected the databases that have to be converted from the 1 2 format to the 1 3 format click the Convert to files button to start the first conversion step see Figure 280 Depending on the number of databases and the size of the selected databases this step could take several minutes EE Export NOVA 1 2 database to nox files File Status Message C Documents and Settings User My Documents My Procedures 1 2 My example database yap Exporting Abort conversion MARAA Idle Figure 280 During the first conversion step the contents of the selected database s are exported to individual nox files During the conversion step t
154. mmands Parameters Links Cyclic voltammetry potentiostatic Remarks Cyclic voltammetry potentiostatic ail End status Autolab m oignal sampler Time WE 1 Potential vWE1 Current m Options 0 Options m Instrument ALITSOO02 Instrument description E Autolab control m WE Mode Galkanostatic WE 1 Bandwidth High stability WE Current range 1 mA Set potential 0 000 set cell Ott m Wattne 3 a A Optimize current range z e C staircase Tror Instrument mode Is not set correctly The instrument must be set to Potentiostatic mode Warning Cell is switched off Warning signal is not linked Figure 36 Up to three errors and or warnings are displayed in the tooltip in the procedure editor Note Errors are always shown before warnings 28 Page NOVA 1 10 4 Release notes Released 01 05 2014 Introduction The 1 10 4 NOVA release adds the following improvements e New OCP potential integration e Baseline correction by moving average e Improved controls for Metrohm Liquid Handling instruments e Potential Stripping Analysis PSA methods e Time derivative signals added to Signal Sampler e Fast options for the Record signals gt 1 ms command e Derivative based recording in the Record signals gt 7 ms command e Import GPES data buffer New OCP potential integration This update of NOVA introduces a new way to specify the potential values to be applied during any potentiostatic measurement If an OCP de
155. mmands browser The Favorite commands group automatically displays the ten commands with the highest ranking see Figure 119 90 Page Commands Procedures i Favorite commands Autolab control m My command Timed procedure Set potential Bet cell e Optimize current range OCP determination e set reference potential Control Autalab RDE Wait for DIO trigger Control Metrohm devices External devices Measurement general Measurement cyclic and linear sweep voltammetry Measurement voltammetric analysis Measurement chrono methods Measurement impedance Data handling Analysis general Analysis baseline correction Analysis corrosion Analysis impedance Plots general Plots impedance My commands H Wy command Figure 119 The Favorite commands group displays the ten most used commands User defined commands stored in the My commands group of commands are also listed in the Favorite commands if applicable It is possible to manually remove a command from the Favorite commands group by right clicking the command see Figure 120 91 Page Commands Procedures Favorite commands Autolab control S hiy commant gt Timed proce Remove from Favorite comm ancdls X m Set potential Edit Rem arks Det cell Optimize cur Export comm andl OCF determ X Delete e set reference potential Control Autolab RDE Wait for DIO trigger Control Metrohm devices
156. mpling step in sampled DC polarography 161 Page EE Edit Options Automatic Current Ranging Cutoff Autolab control Properties Autolab control Autolab control WEC DIO0 DACH Purge Unchanged stirrer Unchanged Set Number of new drops 1 Number of new drops Unchanged oet Number of new drops 1 b Remove Figure 219 The Autolab control command is now available in the options Wait for DIO trigger A wait for DIO trigger command has been added to the Measurement General group of commands With this command it is possible to force the procedure to hold until a predefined DIO trigger is detected on one of the DIO connectors of the Autolab see Figure 220 Wart for DIO trigger F 1 Fort A so0onnnc DIO connector F z DIO connector port Fort a Trigger byte SOO Use time limit Mo T Maximum time s z Figure 220 The Wait for DIO trigger command is now available for receiving triggers For the trigger byte it is possible to define the sequence using 1 pin up O pin down or x wildcard Additionally it is possible to define a maximum time limit for the command If the predefined sequence is not detected within the time limit the measurement will continue While the software is waiting for the DIO trigger the current connector status is displayed in the lower right corner of the Autolab display see Figure 221
157. n Both commands are now replaced by a single Wait time s command which accepts decimal values The accuracy of the wait time is 1 ms New circuit element for Fit and Simulation The library of circuit elements has been expanded by adding the B2 circuit element The B2 circuit element available in the Fit and Simulation analysis tool is a transmission line element derived from the classical model for a porous or mixed phase electrode of thickness L see Figure 97 75 Page Figure 97 Overview of the B2 circuit element This transmission line has been integrated in NOVA In the literature this denomination is also extended in the world of DSC and in general systems that analyze the combination of charge transport accumulation and recombination More information on the B2 circuit element can be found in the Appendix of the Impedance measurements tutorial available in the Help menu in NOVA Clear measurement plot command A Clear measurement plot command has been added to the Control group of commands see Figure 98 Control 2 Input box 2 Message box a Seng e mail Repeat n times Repeat for each value 2 Repeatfor multiple values Increment parameter Figure 98 The Clear measurement plot command has been added to the Control group of commands This command can be added anywhere in the procedure to clear the contents of one of the four available plots or all plots at once 76 Page NOVA 1 8 Release n
158. n the frame on the right hand side of the Hardware setup window see Figure 152 More information on the use of the integrator module can be found in the Filter and Integrator tutorial available from the Help menu 117 Page Serial number recognition Version 1 6 stores hardware setup profiles for each connected instrument If the hardware setup is defined and saved on the computer for a specific instrument this configuration file will be automatically loaded whenever the instrument is connected to the computer The FRA2 calibration file is also associated with the identifying serial number of the device Note it is not necessary to reboot the software whenever the hardware setup is adjusted Redesign of the FRA measurement commands This version of NOVA includes a set of completely redesigned FRA measurement commands The data acquisition speed has been significantly improved with respect to the previous versions of NOVA without compromising data quality Software overhead times have been reduced resulting in a dramatic increase in data acquisition speed The default Test FRA2 procedure provided in the Module test database will now take approximately four minutes instead of roughly ten minutes in the previous versions Through the added FRA sampler time and frequency domain raw signals can be easily added to the measurement see Figure 155 This additional information can be used to evaluate important experimental settings during m
159. n the timing and in the timing guide Furthermore when measurements are carried out with a very large number of data points the software may enforce mandatory timing breaks in a measurement sequence to allow the on board memory of the instrument to be cleared These breaks are indicated by a horizontal green break line across the procedure editor see Figure 10 Note The enforced timing break is automatically handled by the NOVA software 8 Page Commands Parameters Links Chrono amperometry At gt 1 ms Remarks Chrono amperometry A gt 1 ms nO End status Autolak ma oignal sampler Time WE 1 Potential WWE 1 Current Lotions 1 Options ma Instrument ALT 40008 Instrument description Autolab control ma set potential 0 000 Set cell On m Wait time 3 A Record signals gt 1 ms 500 0 01 set potential 0 500 Record signals gt 1 ms 500 0 01 set potential 0 500 Record signals gt 1 ms 500 0 01 Set cell Cit sae lt 3 Figure 10 A mandatory timing break is indicated by a horizontal green line Real time validation in procedure editor NOVA 1 10 now validates the procedures designed in the procedure editor in real time Errors or warnings are indicated on the left hand side of the procedure editor These messages can be used to identify problems in the procedure quickly see Figure 11 Commands Parameters Links Cyclic voltammetry potentiostatic Remarks Cyclic voltammetry potentiostatic
160. naming a drop down list displaying the list of files 112 Page already present in the database starting with the same name typed in the Procedure name field is automatically generated see Figure 150 o Save measured data Procedure name Dema Demo 07 High speed chrono methods F Demo 08 Chrono methods ADC 164 21 Remarks Demo 10 Differential pulse measuremen Demo 11 Hydrodynamic FRA with OCP dl Figure 150 The Save measured data now automatically displays a list of file names already present in the database 113 Page NOVA 1 6 Release notes Released 01 06 2010 Introduction These notes provide an overview of the new features introduced in NOVA 1 6 compared to the previous release The following items have been added to NOVA 1 6 Anew set of tutorials available from the Help menu Support for the modules FI20 Integrator and on board integrator Improvements and additions 114 Page Serial number recognition Redesign of the FRA measurement commands Single frequency FRA measurements Manual control of the FRA through Autolab display Graphical user interface for Fitting and Simulation of impedance data Simplified commands and parameters MultiBA module support Multi Autolab support Software synchronization command for Multi Autolab measurements Serial number and instrument description in the database Multi Autolab support for Diagnostics application New user interface for the
161. nd for DAC control in the End Status Autolab which is useful for safety reasons Note only DAC channel 3 can be used using this control 182 Page Autolab control WE 1 Cell Unchanged Current range Unchanged Bandwidth Unchanged Mode Unchanged IR compensation Unchange IR compensation value Unc External input Unchanged Oscillation protection Unche Reference potential Uncha DIO 1 P1 A Direction Unchanged P7 A Write Unchanged P1 6 Direction Unchanged P1 B Write Unchanged P1 CLowerDirection Uncha P1 CLower Write Unchange P1 CUpper Direction Uncha Pi CUpper Write Unchang P2 A Direction Unchanged P2 A Write Unchanged P2 B Direction Unchanged P2 B Write Unchanged P2 CLowerDirection Uncha F2 CLower Write Unchange P2 CUpper Direction Uncha F2 CUpper Write Unchang DAC 1 oltage Unchanged Voltage Unchanged set Voltage 0 Figure 243 DAC control in the Autolab control window Cutoffs The options available in NOVA have been augmented with a Cutoff interface It is now possible to define any cutoff condition in a procedure The cutoff conditions can be defined for the whole procedure or a specific measurement command It is possible to group cutoff conditions using OR and AND operators Moreover users can define the number of cutoff conditions detections required to trigger the cutoff actions Finally when a cutoff condition is met the user has the choice to stop the command st
162. ne Line style Line color Line size Advanced Reset values cancel Figure 132 A line style drop down list has been added to the plot options 99 Page Linkable interval time in Record signal gt 1 ms command The interval time parameter of the Record signals gt 1 ms command can now be linked to another parameter The interval of the command can therefore be specified using an input box for example see Figure 148 E Input box Tithe of box SALT 20530 Message Interval time s Malue E Timed procedure E Record signals gt 1 ms 5 Duration s z o Interval time 3 Estimated number of points 500 oignal sampler Time WEC1 Current m Options Mo Options al Corrected time array gt 5 Time lt array gt 5 WE Current array gt 4 Index lt array gt lve t z lt gt 4 3 Figure 133 The interval time parameter of the Record signals gt 1 ms command is now linkable Pseudo capacitance calculation for RQ circuit The fitting and simulation tool for impedance spectroscopy now offers the possibility to convert a Q element in parallel with a resistance to a pseudo capacitance according to the following calculation 1 1 Crad Yo l R This option is shown in Figure 134 For example a Q element with a Yo value of 1 uMho and a n factor of 0 75 in parallel with a resistance of 1000 Ohm will be converted to
163. nformation Reverse on Cutoff The redesign of the Edit Cutoff user interface now also includes a command specific action field which can be used to trigger a specific action when a user defined cutoff condition is met during the execution of a specific command Presently only the CV staircase and the LSV staircase commands make use of this option For both commands the possibility to trigger a reversal of the scan direction is provided This Reverse on cutoff action is only available in the Edit Cutoff dialog specified for CV staircase and LSV staircase see Figure 140 106 Page o Edit Options Automatic Current Ranging Cutoff Autolab contral Automatic Integration Time Cutoff on WEY Current Remove Figure 140 The Reverse scan direction action can be specified in the cutoff for CV staircase Basic properties Signal WEN Current ka Action when gt x Value Nothing otop command stop timed procedure procedure Mr of detections Additional cutoffs Mo Cutoff Cancel and LSV staircase commands Please refer to the Cutoff tutorial available from the Help menu in NOVA for more information Adjustments to the Graphical user interface for Fitting and Simulation of impedance data The Graphical user interface for the fitting and simulation of impedance spectroscopy introduced in NOVA 1 6 has been adjusted The following modifications are included in this release e Unlinked c
164. ng the location of the plot in the measurement view Note this option creates an exact copy of the selected plot s including any additions to the plot s 154 Page Send email It is now possible to send an email using a dedicated command during an experiment see Figure 208 This feature can be used to inform the user about the progress of a measurement when the experiments is very long E Send e mail To recipient domainname subject Measurement is finished Message body The measurement is finished and t Outgoing mail server SMTP smtp example com From e mail address senderadomainname gt Figure 208 It is now possible to send emails during an experiment Check for update An online check option is available from the Help menu see Figure 209 and Figure 210 This option can be used to verify if a new version of NOVA is available This option requires an internet connection Help 4 Tutorials About aes ee Figure 209 Online check for updates Version control l Your current version 1 5 3330 25457 is up to date Figure 210 The current version is up to date If a new version is available visit the www metrohm autolab com website to download the update 155 Page New data handling commands Three new data handling commands have been added to the Data handling group of commands e Get array size e Get array item e Get first array item e Get last array item The get array siz
165. ngle frequency command available from the Measurement impedance group of commands it is now possible to perform a single frequency measurement It is not necessary to setup the complete FRA frequency scan command for this type of measurement see Figure 158 Be FRA singte frequency Input frequency Hz 100 Input amplitude 0 1 Input wawe type single sine m FRA sampler m Options Mo Options m Frequency lt array Hz E lt array gt 02 say array gt 02 Z caray 02 Phase lt array gt i Time lt array 3 Fotential DIC array gt Vv Current D array A AA Figure 158 Single frequency measurements are now possible using the FRA single frequency command 120 Page Manual control of the FRA through Autolab display A panel system has been added to the Autolab display window It is now possible to add or remove additional panels to this window by picking the corresponding item in the view menu see Figure 159 File View Run Tools Help be Advanced command view te a e a JIE a Advanced procedure view Setup View Mult Autolap View Measurement View Analysis View User log Fil Autolap display F10 lt FE aa Add remove FRA manual control panel in Autolab display Figure 159 Adding the FRA manual control panel to the Autolab display MDE manual control MUX manual control When the FRA manual contro option is selected an additional pane
166. no extra modules required End status Autolab m oignal sampler Time WE 1 Potential WE 11 Current m Options 1 Options aaa Instrument Instrument description Autolab control set potential 0 000 e Set cell E at time s p A Optimize current range A CY staircase 0 000 1 000 1 000 0 000 2 0 1000000 Ott SH Set ce Cell is switched off Figure 11 The procedure is now validated in real time warnings and errors are indicated on the left hand side of the procedure editor In the example shown in Figure 11 the warnings are provided because the cell is not switched on during the procedure Since this is not an error the warning symbol is shown A If an error is detected as shown in Figure 12 the error symbol is shown instead 9 Page Commands Parameters Cyclic voltammetry potentiostatic Remarks Cyclic voltammetry potentiostatic no extra modules required End status Autolab oignal sampler Time WE 1 Potential vwE1 Current Options 1 Options Instrument Instrument description Autolab control Links E ait Instru WE Mode Galvanostatic WE 1 Bandwidth High stability WE Current range 1 mA set potential 0 000 set cell Ott ait time 3 a Optimize current range z CY staircase O 000 1 000 1 000 0 000 2 0 1000000 ment mode is not set correctly The instrument must be set to Potentiostatic mode Figure 12 An error symbol is provided by the re
167. nt amplifier ECM electrochemical noise EQCM quartz crystal microbalance External devices F120 filter and integrator Impedance spectroscopy I compensaton Muli Autolab MUBA MUX multiplexer Open circuit potential pox pH and temperature Voltarmmetric analysis Figure 151 New tutorials are available from the Help menu 115 Page Modules support NOVA 1 6 adds support for the analog integrator part of the optional FI20 module It also includes support for the on board integrator of the yAutolab type II and III as well as the PGSTAT101 see Figure 152 Hardware setup OX File Tools Main Module Additional Modulets A Ir gt Fe PGSTATIO1 C FRA PRSTATSOUZM 4ADCIOM El Misc Calibration factor PGSTAT128N wAutolab II PGSTAT100 PGSTAT302 PGSTAT12 PGSTAT3O WAUtolab Il PGSTAT20 LJ ADC750 LJ ADC7SOrd SCAN250 C SCANGEN a _ BA C BIPOT ARRAY CECD Fl20 Filter FGSTAT10 Fi20 Integrator gmoostercUA Booster1 04 EQCM External C IME303 C IMEBES KALI Fower Supply Frequency Import FRA Calibration FRA offset DAC range Sia Calibration factor CADocuments and Settings 4ll Users Applicaton DataEco Chemie HardwareSetup 0 xml Figure 152 The integrator module is now supported in NOVA The integrator module can be used to measure the charge and perform chrono coulometry e
168. o amperometry fast Chrono potentiometry fast Chrono coulometry fas z Chrono amperometry F Unhide p Chrono potentiometry high speed X e Chrono charge discharge Hnterrupt Hnterrupt high speed Positive feedback FRA impedance potentiostatic FRA impedance galvanostatic i PRA potential scan Standards i My procedures Figure 108 Right click hidden items to unhide them To unhide a hidden item right click the item and select the unhide option from the context menu as shown in Figure 108 Note it is also possible to hide items using the CTRL H keyboard shortcut and to unhide items using the CTRL SHIFT H keyboard shortcut In the commands browser it is possible to hide single commands from a given group using the same method It is however also possible to completely hide a command group from the browser see Figure 109 84 Page Commands Procedures Commands Procedures Favorite commands H Favorite commands H Control H Control H Metrohm devices H Metrohm devices H External devices gt Estermal device External device initialize External d Hide all gt External device send External d 2 External device receive 2 External d 4 Sort ascending External device close Extemald 2 Sort descending fee Eternal device specia e External d 4 Measurement qeneral Hide H Measuremer Original order H Measurement cyclic
169. o methods command This interface conveniently separates the basic and the advanced parameters More information on the use of the Chrono methods command can be found in the Chrono methods tutorial available from the Help menu New user interface for the FRA measurement commands A new editor has been added to the FRA measurement commands to allow the specification of all relevant experimental parameters in a single form see Figure 6 A FRA editor 0 Ea OE First applied frequency 100000 Hz Sampler Options Last applied frequency 0 1 Hz Plots Number of frequencies 50 Summary Frequency step Amplitude Wave type Estimated duration 4 minutes Linear Logarithmic _ Square root _ Frequencies per decade 0 01 V RMS Single sine 5 sines 15 sines Cancel Figure 6 A new user interface has been added to the FRA measurement commands 6 Page The new interface brings all the important parameters and settings into one location The settings are specified in different sections depending on the type frequency scan options etc Where applicable some of the parameters have been separated into basic and advanced parameters to simplify everyday use of these parameters and commands see Figure 7 ave FRA editor oO E3 Frequency scan Q Basic Sampler Options Plots Maximum integration time p 125 S Minimum integration cycles 1 Summary Sample time domain No Sample frequency dom
170. of multiple procedures in the Multi Autolab view a simplified procedure editor is available in this view to edit existing procedures To open this editor click the button located next to the specified path see Figure 140 Instrument 1 Description Procedure Ch Cyclic valtammetry potentiostatic nox Browse Use active procedure Plot Optians Instrument Output L3AUT 0530 v v Store in database Instrument 2 Description Procedure CAUs FRA impedance potentiostatic nox Browse Edit Use active procedure Plot Options Instrument Output AUT64148 v v Store in database Figure 89 Clicking the button in the Multi Autolab view opens a simplified procedure editor Clicking the button opens a popup window displaying a reduced form of the setup view Through this window the procedure can be modified Commands and links in the procedure can be edited and the changes can be saved to file see Figure 90 G 2 i 2 A l i EY Procedure Editor CAUsers User Desktop Cyclic voltammetry potentiostatic nox o hoea FALCK IGE Commands Commands Parameters Links Favorite ada Cyclic voltammetry potentiostatic Control Remarks Cyclic voltammetry potentiostati Meiran devices End status Autolab Eia External devices Signal sampler Time WE 1 Potential WE 1 C Measurement general cent 1 Options s Measurement cyclic and linear sweep voltammetry ana of Measurement voltamme
171. on is switched off the user will be prompted at the end of each experiment to provide a name and a comment for the measurement If the data Is invalid or if saving the data is not required an additional option to discard the measurement is provided Figure 216 159 Page FE Save measured data Procedure name Remarks Cyclic voltammetry potentiostatic no extra modules required Figure 216 When Automatic save is disabled the user is prompted to specify name and remarks for the experiment The user can also discard the data if it is invalid Note pressing the Discard button will delete the measured data points immediately These data points cannot be recovered Version and hardware overview in the About menu The Help about menu now displays extensive version and hardware configuration information see Figure 217 FE About NOVA General Application NYA ersion esi Company Eco Chemie BY Embedded application ADK AST version 2 0 d030 24051 Embedded version 2 0 3330 24075 ADK wersion 2 0 3330 24075 IF030 version alz Autolab serial number ALT83079 Licensed since 2 0 2009 11 03 30 AM Autolab modules PiasTATa0e ECD ADC1B4 DACTE4 External DIO45 Liperating system Microsoft Windows lt P Name Location Version Accessibility fle VCO AVIN DOW S assembly U 0 0 buwelf2 fle VO AVINDOW Sfassembly U 0 0 EcoChemie Sharedbl filed Program FilesfEco Ch 5 0 3350 2545b EcoChemiebti f
172. ong with the rest of the procedure see Figure 277 All the links will be printed on the right hand side A print preview is available from the File menu Procedure Values Cycle voltammetry Remarks Factory standard procedure End status Autolab Collection Signal sampler Time WE 1 Potental WE 1 Curent Options Automate CurentRanging WE 1 1mA 10_ Timed procedure Set Potentiostatcand selectcurent r Set potental 0 000 Setpoint potental v 0 000 Set cell On H Wart time 5 5 Optimize current range 5 CV staircase 0 000 1 000 1 000 0 000 2 0 10000 Start potential Vv 0 0900 Uppervertex potential Vv 1 000 Lowervertex potential 0 1 000 Stop potental V 0 000 Numberof stop crossings 2 Step potental V 0 0024 Scan rate V s 0 10000 Total number of points 1650 Interval time us 24400 Signal sampler Time WE 1 Potential WE 1 Curent Potentalapphed lt amay gt W Scan lt anmay gt WE 1 Potental lt _amay gt A Time lt _amay gt s WE 1 Curent lt amay gt A ivs E Graphical settings General settings x Potential apphed M WE 1 Current A Fa Time s Set cell Of irt Figure 277 Print preview of the cyclic voltammetry procedure with the links on the right hand side Note only the visible links will be printed Maintaining reverse compatibility This version of NOVA introduces a large number of changes that affect the way the so
173. onnections are now identified in a unique way when connections in the graphical user interface are not combined properly in an equivalent circuit they are indicated by an open circle C rather than a closed circle This allows the user to identify the invalid connections more quickly see Figure 141 C 1 00 pF Figure 141 Invalid connections are now indicated by an open circle left C element not connected properly right C element connected properly 107 Page e The x value is now included in the Report the calculated y value is now included in the report created by the Fit and Simulation tool see Figure 142 kava Circuit Report File Edit Element Farameter Value Estimated Error 75 R 86 087 1 875 246 1 665 6 O120E 06 off 0 0015453 1 975 0 054454 Figure 142 The calculated x value is now automatically included in the report generated by the Fit and Simulation tool Driver manager The Autolab requires specific USB drivers in order to operate properly Presently two different drivers are provided for the Autolab e NOVA only driver recommended this driver is only supported in NOVA It provides faster USB data transfer with respect to the GPES drivers and provides support for up to 16 Autolab instruments connected to the same computer e GPES compatible driver this driver is recommended for users that want to switch between NOVA and GPES This driver provides slower data transfer
174. ons of the M101 module are identical to the specifications of the PGSTAT101 Up to 12 M101 modules can be installed in a Multi Autolab frame providing connections for up to 12 independent electrochemical cells Daughter module it is possible to install an optional module in the module bay directly on the right hand side of aM101 module The daughter module can only be installed in an even position identified by a letter on the front panel This means that every M101 module installed in an odd module bay in the Multi Autolab frame identified by a number on the front panel can control a single daughter module installed in the even position directly on the right Any of the following modules can be installed in this position BA EQCM pX1000 and MUX The M101 modules and optional daughter modules are used through the Multi Autolab view Please refer to the Multi Autolab tutorial for more information Previous NOVA versions and NOVA 1 7 It is possible to install more than one version of the NOVA software on the same computer Installing version 1 7 does not upgrade previously installed versions However it is only possible to use one version of the software at a time and data sets obtained with NOVA 1 7 cannot be used with previous versions of NOVA The opposite situation is possible using the conversion tool that is installed together with version 1 7 or by using the Import data and Import procedure tools available in the software see Figur
175. onvolution XN Kinetic convolution J Figure 23 The convolution command can be added to the procedure In the analysis view the Convolution command can be added to a data set which includes the Time and WE 1 Current signals using the quick access menu or the right click menu see Figure 24 QSwerair B 5 Cyclic voltammetry pe 0112 1 1 29 AR 5 gl C staircase Convolution X H ivsE ECN Spectral noise analysis Calculate charge IR drop correction Cyclic voltammetry potentiostatic AT 63478 14 5 2013 11 32 45 S C staircase H iveE Plot Options Properties Add VWincdower Generate index Add Plot b Add Analysis Convolution My comm ands i ECN Spectral noise analysis Show All Plots Calculate charge Hide All Plots IR drop correction Save in My commands Delete Remove all from View Figure 24 Adding the convolution command to a data set The convolution item will be added to the data set The type of convolution can be specified using a dedicated drop down list on the right hand side of the plot in the analysis frame see Figure 25 19 Page Type Time semi dervative Time semi dertvate Time sembintegral a0 diferintegratian FALT differinteqration Spherical convolution Kinetic convolution Figure 25 Specifying the type of convolution in the Analysis view The result of the convolution algorithm can be displayed as a plot by clicking th
176. op the timed procedure or stop the whole procedure see Figure 244 183 Page FE Edit Options Automatic Current Ranging Cutoff Properties E Misc Stop command Action when gt Additional cutoffs No Cutoff Nr of detections 4 Signal WE 1 Current Value 1 Remove Figure 244 The Cutoff interface More information about the cutoffs can be found in the Cutoff tutorial Simplified FRA frequency range editor The determine FRA range window has been simplified The amplitude range builder has been removed The possibility of defining more than one amplitude is still available using the Add button Moreover it is now possible to define the amplitude of the FRA frequency scan in absolute value top or root mean square value rms The tooltip displays both values see Figure 245 184 Page FE Determine FRA Range 1A First applied frequency Applied AC amplitude Last applied frequency 0 01 Vitop Number of frequencies 3 Oms top Frequency step P Linear Logarithmic 100 Hz 0 01 V top 0 007071 V rms OC Square root Wave type Single sine D 5 sines below 3472 Hz D 15 sines below 315 7 Hz Figure 245 The simplified determine FRA range window FRA Galvanostatic support A dedicated FRA measurement galvanostatic command has been added to the command list This command can be used to define a frequency scan in galvanostatic conditions The amplitude can be defined in A direct
177. ord signals command 5 i Renee Value El Timed procedure E Record signals 1 ms Duration f s Interval time s 1 Estimated number of 30 oignal sampler Time WE 11 Current ma potions Mo Options m Corrected time lt array 5 Time lt array gt 5 WE Current lt aray 4 Index lt Array gt ws t zj lt gt Figure 148 The duration parameter of the Record signals gt 1 ms command is now linkable Faster startup of Nova The boot sequence of the software has been improved with respect to the previous versions Nova will now start considerably faster and the startup time Is independent of the number of files in the database Adjustments to the Windower tool The Windower command available from the Data handling group has been modified The boundaries defined in the command can now be linked in the procedure editor to other parameters The linkable boundaries are shown in the procedure editor after definition of initial values in the command see Figure 149 e Windower Source lt array gt Boundaries Collection Err Begin 1 End 1 1 Begin 2 2 End z b gt Figure 149 The boundaries defined in the Windower tool are now available in the procedure editor Preview of database names When the Automatic save option is set to off through the Tools Options menu the Save measured data dialog window will be displayed at the end of each measurement To facilitate file
178. otential tv 0 000 Upper vertex potential 0v 1 000 Lower vertex potential w 1 000 stop potential v 0 000 Number of stop crossings 2 step potential v 0 00244 ocan rate v s 0 10000 Estimated number of points 1650 Interval time s 0 024400 oignal sampler Time WWE Potential vvwE 1 Current m Options 1 Options m Fotential applied lt array gt Time lt array gt 3 WEH Current lt array gt 4 Scan lt arrary gt WE 1 Potential lt array 0 Average current lt array 4 lndex lt array gt Ive E al E Calculate signal al i WEJ Current 4 Set cell Cit maj lt gt Figure 181 An example showing the four types of parameters in the procedure setup In this example WE 1 Current is shown in red because it is a measured value scan rate is shown in black since it is a command parameter the interval time is shown in grey because it cannot be edited and it is calculated from the values of the scan rate and the step potential The average current is a calculated value generated by the Calculate signal command and it is therefore shown in blue This parameter is a dynamic parameter since it is calculated during the experiment Dynamic command parameters are very useful for advanced procedure building Figure 182 shows an example of the dynamic command parameters used in a procedure Impedance measurements are repeated a number of times and fitted using a R RQ equivalent circuit The fitted
179. otentiostatic procedure Note the well known CTRL Z keyboard shortcut can also be used Cyclic voltammetry potentiostatic Commands Remarks End status Autolat signal sampler Lotions Instrument Parameters Links Cyclic voltammetry potentiostatic no extra modules required muaj Time WE 1 Potential vWE 1 Current a 1 Options H3ALT 0530 Instrument description Timed procedure E E E E E ce Autolab control mna Set potential Undo Delete CV staircase Ctl zZ Set cell 7 asl Viait time 3 a Optimize current range z set cell Ott m 4 3 Figure 122 Using the Undo function Similarly it is possible to redo an undone action by clicking the button in the toolbar or by right clicking anywhere in the procedure editor setup view or the data explorer frame analysis view and select the Redo option from the context menu In Figure 123 this tool is used to redo the delete action performed on the CV staircase command of the Cyclic Voltammetry potentiostatic procedure Note the well known CTRL Y keyboard shortcut can also be used Cyclic voltammetry potentiostatic Commands Remarks End status Autolat signal sampler Options Instrument Parameters Links Cyclic voltammetry potentiostatic no extra modules required muaj Time WE 1 Potential vWE 1 Current m 1 Options m Instrument description E Timed procedure H E E E E Autol
180. otes Released 01 12 2011 Introduction These notes provide an overview of the new features introduced in NOVA 1 8 compared to the previous release The following items have been added to this release of NOVA Support for the instruments and modules e FRA32M New impedance analyzer module Improvements and additions e Automatic update tool for USB interfaces e Automatic Hardware setup e Simplified interface with Profile menu e Hide Show option e Sorting function for the Commands browser e Import Export Profiles e Context sensitive popup menu e Add comments to My Commands e Favorite commands group e Basic Undo Redo functionality e Modification to the Ca culate signa command e Noise meters added to Autolab display e Real time modification of the command parameters e Add plots in real time e Modification of the plot options in real time e Create Windower from X axis e New plot options e Linkable interval time in Record signals gt 7 ms command e Pseudo capacitance calculation for RQ circuit Automatic update tool for USB interfaces Autolab PGSTAT302N and PGSTAT100N with serial numbers gt AUT84440 and PGSTAT128N with serial numbers gt AUT84460 need a firmware update to avoid a potential USB communication problem This update is only required for the above mentioned instruments when used in combination with the NOVA only drivers An automatic update tool is included in the Diagnostics application Note
181. ovided 145 Page Hardware support The hardware setup of NOVA 1 5 now includes support for the ADC750 rev 4 ECN pX FI20 filter and MUX modules The PGSTAT101 is also supported The external signals can now be conveniently edited using a dedicated menu see Figure 234 A special conversion function is provided for eSPR signals Hardware setup T mj bd File Tools Main Module Additional Module s External Adc Channel3 Offset 0 Multiplier 1 Unit Vv _ eSPR Multiplier COS Signal Offset Externale Adc Channel4 Offset 0 Multiplier 1 Unit L _ eSPR Multiplier COS Signal Offset Power Supply Frequency Import FRA Calibration FRA offset DAC range saa C Docurnents and Setings 4ll Users Application Data Eco Chemie HardwareSetup60 mil Figure 192 The hardware setup window Voltammetric analysis techniques This new version of NOVA introduces the most commonly used voltammetric analysis VA techniques These techniques can be used on solid electrodes or on a mercury drop electrode The following techniques are now supported e Sampled DC e Normal pulse e Differential pulse e Differential normal pulse e Square wave The commands required for these measurements can be found in the Measurement voltammetric analysis group of commands see Figure 193 The Timed procedure for voltammetric analysis provides a generic template for V
182. own in green see Figure 108 Commands Procedures Autolak in Cyclic voltammetry potentiastatic be Cyclic voltammetry qalvanostatic be Cyclic voltammetry current integration ie Cyclic voltammetry linear scan H Cyclic voltammetry linear scan high speed Linear sweep voltammetry potentiostatic Linear sweep voltammetry galvanostatic Linear polarization Hydrodynamic linear sweep e Differential pulse voltammetry e square wave voltammetry sampled OC polarography Chrono amperometry At gt 1 ms Chrono potentiometry At gt 1 ms Chrono amperometry fast e Chrono potentiometry fast he nrana coulometre tazi e Chrono amperometry high speed e Chrono potentiometry high speed Chrono charge discharge Interrupt e Interrupt high speed Positive feedback FRA impedance potentiastatic FRA impedance qalvanastatic FRA potential scan Standards m My procedures Commands Procedures Autolak Cyclic voltammetry potentiostatic ie Cyclic voltammetry qalvanostatic be Cyclic voltammetry current integration z Cyclic voltammetry linear scan e Cyclic voltammetry linear scan high speed Linear sweep voltammetry potentiostatic Linear sweep voltammetry galvanostatic Linear polarization Hydrodynamic linear sweep e Diferential pulse voltammetry square wave voltammetry sampled DC polarography Chrono amperometry At gt 1 ms Chrono potentiometry At gt 1 ms Chron
183. pgrade to NOVA 1 4 File File C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 01 Copper deposition nox Finished C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 02 Copper deposition QCM nox Finished C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 03 Bipotentiostat measurement PtPt Rin Finished C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 04 Hydrodynamic LSV with increasing rot Finished C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 06 Galvanostatic CV nox Finished C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 07 High speed chrono methods ADC750 Finished C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 08 Chrono methods ADC 164 20 steps n Finished C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 09 Chrono methods ADC 164 with variabl Finished C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 12 Imported pcPt GPES data nox Finished C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 13 Imported pcPt GPES data nox Finished C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 14 Imported GPES data nox Finished lt Add files to list Remove files from list Create
184. plot modulus Bode plot phase Residual plot 2 A Residual plot 2 F E Figure 322 The saved results of the fit are added to the data set The added signal set contains the calculated Bode and Nyquist plots as well as the residual plots for Z and Z 240 Page Simulating the data using an equivalent circuit The simulation tool can be used to calculate the expected behavior of a user defined equivalent circuit To use the simulation tool the equivalent circuit must first be defined in the same way as for the fitting procedure However the Fit or Simulation parameter in the control interface must be set to Simulation see Figure 323 El Input Max number of Iterations 100 Circuit Circuit Maximum change in chi square 0 001 Maximum number of iterations giving no improvement 100 Fitting style Impedance Use weight factors Yes Fit or Simulation Measurement data format E Results Number of iterations performed Result Chi square Figure 323 To use the simulation tool the Fit or Simulation parameter must be set accordingly To start the simulation algorithm click the button located in the toolbar This will calculate the expected behavior of the equivalent circuit using the initial parameters for each of the circuit elements Figure 324 shows an example of simulated data 241 Page 7 Q 1000 800 600 400 200 0 0 200 400 600 800 1000 Z Q E Inp
185. port Signal set s for each measurement command It is now possible to define one or more signal set for each measurement command which will be created during the measurement Each measurement command has a default signal set which can be edited The signal set s added to a measurement command can use any electrochemical signal defined in the sampler of the command Figure 290 shows the default signal 214 Page set used for the CV Staircase command The signal set vs uses the following electrochemical signals e X Potential applied V e Y WE 1 Current A e Z Time s The definition of the electrochemical signals used in the signal set is achieved using links Procedure Values Cyclic voltammetry Remarks Factory standard procedure al End status Autolab Collection Signal sampler Time WE 1 Potential WE 1 Current ma Options Automatic Current Ranging WE 1 1 mA 1 a E Timed procedure Set Potentiostatic and select current range an Set potential 0 000 Set cell On Wait time s 5 Optimize current range 5 E CV staircase 0 000 1 000 1 000 0 000 2 0 10000 start potential V 0 000 Upper vertex potential V 1 000 Lower vertex potential V 1 000 stop potential V 0 000 Number of stop crossings 2 Step potential V 0 0024 Scan rate V s 0 10000 Total number of points 1650 Interval time Ls 24400 Signal sampler Time WE 1 Potential WE 1 Current ma Potential applied lt _ar
186. procedure validator FFT Analysis and FFT Smoothing ECN Spectral noise analysis Clear plot button modification Dynamic command parameters Repeat for multiple values Autolab display with collapsible panels Current interrupt and positive feedback External NET applications support Avantes spectrometer support Previous NOVA versions and NOVA 1 6 It is possible to install more than one version of the NOVA software on the same computer Installing version 1 6 does not upgrade previously installed versions However it is not possible to use both software packages at the same time and data sets obtained with NOVA 1 6 cannot be used with previous versions of NOVA The opposite situation is possible using the conversion tool that Is installed together with version 1 6 Please refer to the Upgrading files from previous versions tutorial available from the Help menu Tutorials New tutorials have been added to this version of NOVA The tutorials are available from the Help menu see Figure 191 Help Tutorials N Getting started About 5 User manual Fl Check for Updates Command list Release notes 1 6 Release notes previous version Module test with Nova Upgrading files from previous versions Autolab control Bipotentostat Booster high current amplifier Chrono methods Chrono methods high speed Cycle voltammetry Cycle voltammetry linear scan Cutoff boundaries ECD low curre
187. ptional I O cable for the PGSTAT101 With the optional I O cable the following signals are available Eour This output corresponds to the differential potential of RE versus S The output voltage will vary between 10 V lour This signal corresponds to the inverted output of the current to voltage converter circuit of the PGSTAT101 A 1 V signal corresponds to 1 x the selected current range Vour This output corresponds to the DAC output It is controlled by software and is meant to be used to control external devices like the rotating speed of a Rotating Disc Electrode RDE The output level varies between 10 V Vin This input corresponds to the ADC input This input can be used for measuring a second signal The input range is 10 V More information about the PGSTAT101 hardware can be found in the PDF version of the Getting started available from the Help Tutorials menu 10 The Eou value corresponds to WE 1 Potential 11 The iout value corresponds to WE 1 Current Current range 167 Page Diagnostics The diagnostics application has been adjusted and the PGSTAT101 has been added to the list of devices available in the test see Figure 226 4s Diagnostics Select Al Tests Deselect Optional Tests Autolab PGSTAT101 b UAutolab Type II UAutolab Type II gT zi iL o oqo 2 ag i B Ag e DA Noise Test Galvanostat Test Frogress Doo Figure 226 The PGSTAT1
188. r Time WE 1 Fotential WEOQ Current m potions Options m Use fast options No m Corrected time lt array gt 5 Time array gt 5 WE Fotential array Cv WE Current lt array A Index lt array gt h vs t z Record signals gt 1 ms Duration s z Interval time s 0 2 Estimated number of points 23 oignal sampler Time WE 1 Fotential WEOQ Current m potions Options m lse fast options Yes m Fast interval time s 0 02 Corrected time array gt 5 Time lt array 5 WE Potential array Cv WE Current array 4 Index lt array gt h ws t al Figure 58 The Use fast options toggles the fast interval time off top or on bottom Using the fast interval time does not increase the number of data points recorded This option only changes the behavior of the Options Automatic current ranging Cutofts etc e lf the fast options are not used the Options specified in the command will be executed at the end of each interval time e lf the fast options are used the Options specified in the command will be executed at the end of each fast interval time The fast options therefore allows a complete decoupling of the sampling of the data and the execution of the options This is particularly useful for experiments during which data points need to be recorded for a long time with a large interval time while the properties of the cell need to be controlled wit
189. ray while the Get last array item automatically looks for the last value in an array Both commands can be used to extract specific values from a list of measured or calculated signals and use these values as parameters in the procedure Timed procedure in FRA frequency scan It is now possible to add a Timed procedure to a FRA frequency scan Commands located inside the timed procedure are executed for each frequency in the scan see Figure 212 El FRA measurement potentiastatic Frequency lt array gt Hz Phase lt aray gt 7 Z lt array gt 02 E lt array 02 E samar 02 Index lt arrary gt E FRA frequency scan Collection m Freguency table Collection ma Number of frequencies Estimated duration FRA single frequency 1 1 10 1 0 El Timed procedure E Record signals 1 ms 5 1 Duration s 5 Interval time s Total number of points signal sampler Time External ADC Tb4 1 a Options 2 Options mf Corrected time lt array gt 3 a Time lt arrayy gt 5 Oodans Exteralf1 A0C164 1 lt array gt Vv WEL 1 4 100 nA WE 1 Current caray A LEUTO WELD current Index lt anay e E ys t zx Figure 212 Timed procedures can be added to the FRA frequency scan This feature can be used to record external signals during a frequency scan or to test measured signals against a cutoff condition as shown in Figure 212 Note the DSG of the FRA2 module is not swit
190. re information on firmware modifications of the Avantes spectrometers Control of the Metrohm 6 2148 010 remote box This update of NOVA provides support for the Metrohm 6 2148 010 Remote box with MSB connection This device can be connected to any available MSB port and provides one additional spare MSB connection for additional hardware see Figure 72 58 Page Figure 72 Support for the Metrohm 6 2148 010 Remote box with MSB is now available This device can be used to send and receive digital signals from other Metrohm devices The Remote box is controlled during a measurement using the dedicated Remote inputs and Remote outputs commands provided in the Metrohm devices group of commands see Figure 73 Remote inputs Device name DigitallO_1 m Inputs Remote outputs Device name DigitallQ_1 al Outputs 1000000000000 T Figure 73 The Remote inputs and Remote outputs commands are used to control the Remote box The Metrohm 6 2148 010 has a total of 8 read lines the status of which can be acquired using the Remote inputs command It also has a total of 14 write lines which can be set using the Remote outouts command For both command the high state is represented by a 1 and a low state is represented by a 0 The Metrohm 6 2148 010 Remote box Is identified in the Liquid Handling setup as a 770 device type see Section 5 4 59 Page Improvements to thea Metrohm Liquid Handling support To fa
191. rform simple measurements on the Autolab dummy cell Help About Getting started User Manual Fi Command list Release notes 1 4 Release notes previous versions How to test a module in Nova Bipotentiostat Booster high current amplifier Chrono methods Chrono methods high speed Cyclic voltammetry Cyclic voltammetry linear scan Cutoff boundaries ECD low current amplifier EQCM quartz crystal microbalance External devices Impedance Open circuit potential pX1000 pX pH and temperature Figure 233 A series of short tutorials is available from the Help menu Modules support NOVA 1 4 introduces the support for the ECD pX1000 and EQCM modules Hardware support The hardware setup of NOVA 1 4 now includes the PGSTAT128N and PGSTAT20 see Figure 234 12 With serial number gt 960350 174 Page EE Hardware setup File Tools Main Module Additional Module s PGSTAT302N _ wAutolab II PGSTAT100 PGSTAT302 PGSTAT12 PGSTAT30 wAutolab II PGSTAT20 PGSTAT10 PSTATIO pA 10 d Common Module s Power Supply Frequency Import FRA Calibration FRA offset DAC range 5V 5V sf C Documents and Settings All Users Application Data Eco Chemie HardwareSetup50 xml a Figure 234 The hardware setup window Simplified user interface NOVA 1 4 introduces a lighter user interface A number of commands
192. riginal order Import ASCII data Export ASCII data Export to 2view Generate index Analysis general Analysis baseline correction Analysis corrosion Analysis impedance Plots general Plots impedance Wy Commands Commands Procedures Favorite commands H Control H Metrohm devices H External devices H Measurement general Measurement cyclic and linear sweep voltammetry Measurement voltarnmetric analysis Measurement chrono methods Measurement impedance Build signe Hicle all Calculate s 4 4 Sort ascending pe Export Ast 7 TE pa Exportto Z 4 Sort descending Generate il Original order oo mpor AS i gt Import FRA data Import GPES data Scan selector n Winidower Analysis general Analysis baseline correction Analysis corrosion Analysis impedance Plots general Flots impedance My commands Figure 111 Sorting the commands in a group in the commands browser Import Export profiles It is possible to hide any number of items in Nova and to create a new profile for this customized view Using the Profile menu it is possible to import and export user profiles see Figure 112 File View ae Te S Profile Basic Run Tools Help Harchvare based Interm eciate Advanced Corrosion Education Electroanalysis Energy Interfacial electrochemistry Semiconductors Reset u
193. rties Add Windower Generate index Add Plot Custom ada Aras nase vs2 Show All Plots Bode modulus Hide All Plots Bode phase Save in My commands Delete Figure 242 Adding a pre defined plot to a data set The Custom plot is an empty plot with undefined X Y and Z signals It is possible to add it using the list provided by the Add Plot menu or by clicking the Add Plot option in the right click menu The name of the plot can be changed using the right click menu properties option 181 Page Note Signal set which was used in the previous versions of NOVA as name for a plot has been renamed to Plot Previous NOVA versions and NOVA 1 4 It is possible to install both packages of the NOVA software on the same computer Installing version 1 4 does not upgrade previously installed versions However it is not possible to use both software packages at the same time and data sets obtained with NOVA 1 4 cannot be used with previous versions of NOVA The opposite situation is possible using the conversion tools that are installed together with version 1 4 DAC control in Autolab control For external devices controlled through a DAC voltage set using the Control external device command a set DAC control field has been added to the Autolab control interface see Figure 243 This allows for direct control of the DAC in a chrono methods required for fast transient acquisition involving an external device a
194. s e Active profile indication in the status bar e Hidden commands warning e Check for updates on startup e Linkable cutoff value in procedure editor e Power and resistance signals added to the signal sampler e WE X Charge signal added to the signal sampler e Automatic offset DAC control e Internal dummy cell control for the PGSTAT101 and the M101 e Optional serial number in legend e Linkable purge time e Procedure editor in Multi Autolab view e iR drop correction analysis tool command e File extension identification in mport GPES data command e Dedicated Avantes spectrometers support e Frequencies per decade distribution in the FRA frequency scan editor e Consolidation of the Wait time s and Wait time us commands e Distributed circuit element added to Fit and Simulation tool e Clear measurement plot command Support for 64 Bit versions of Windows NOVA now includes support for 64 Bit versions of Windows for selected instruments Please refer to for a list of compatible instruments see Table 1 Instrument type PGSTAT10 20 PGSTAT12 30 302 100 PGSTAT302N PGSTAT128N PGSTAT100N PGSTAT302F PGSTAT101 Multi Autolab M101 UAutolab II and III 64 Bit compatible No No Yes Serial number gt AUT84440 Yes Serial number gt AUT84460 Yes Serial number gt AUT84500 Yes Yes Yes No Table 1 Windows 64 Bit compatibility table 61 Page Active profile indication To indicate which NOVA profiles
195. s 64 bit Windows l Ready for future applications GPES compatible Select this driver when you want to use Nova 1 7 or higher together with Nova 1 6 or lower and or GPES on this PC Restrictions Slower USB data exchange Connect a maximum of 6 Autolab instruments Doesnt support 64 bit Windows No further developments are done with this driver Nova only instruments 1 GPES compatible instruments 0 Total number of instruments 1 Figure 1 The GPES compatible driver cannot be used in 64 Bit versions of Windows 3 Page Support for the new Autolab PGSTAT204 This version of NOVA provides support for the new Autolab PGSTAT204 see Figure 2 Figure 2 The Autolab PGSTAT204 This new compact instrument can be used stand alone or in combination with one of the following modules e FRA32M Electrochemical impedance analyzer module e BA Dual mode bipotentiostat module e EQCM Electrochemical quartz crystal microbalance module e MUX Multiplexer module e pX1000 pH and temperature measurement module New user interface for Autolab control command The editor for the Autolab control command has been redesigned and will now display the settings in well defined areas of the interface see Figure 3 Basic and advanced parameters are now shown in clearly separated sections 4 Page are Autolab control Oo ES PGSTAT204 A Basic ps cel off Integrator FRA32M Mode Potentiostati
196. s Bl Estimated duration pr FRA single frequency lt gt Build siqnal hhyquist 2 vs 2 Bode modulus Bode phase lt gt Timed procedure lt gt Figure 156 Linking an Input box to the amplitude used in the FRA measurement Single frequency measurements are now also possible as well as time scan FRA measurements The Time signal is sampled for each impedance data point This Signal consists of the total elapsed time since the beginning of the experiment This allows the user to track the progress of the measurement in long experiments or in time scan experiments Impedance measurements requiring connections to and from external devices are now easier to configure The FRA sampler has been designed to allow the user to specify all the parameters of the external transfer function from one single location see Figure 157 119 Page a FRA Sampler Input amplitude Channel gt _ Sample frequency domain Transfer function Oxe Ove or Phase Channel r Real Sample time domain Imaginary F sample frequency domain sample OC i Cancel Figure 157 The FRA sampler used for measurements in combination with a Kikusui PLZ164WA electronic load The commands required for these measurements can be found in the Measurement impedance group of commands and more information about impedance spectroscopy measurements can be found in the Impedance spectroscopy tutorial Single frequency FRA measurements Using the FRA si
197. s UseriMy Documentsi My Procedures 1 6 Commands cal Circuits Circuits LADocuments and settings UsernhMy Documents My Procedures 1 6 Circuits cul mae Figure 163 The Circuits database has been added to the database manager Note more information about the new Fit and Simulation tool can be found in the Impedance spectroscopy tutorial 124 Page Simplified commands and parameters For more clarity some advanced parameters have been hidden from view in the default procedure setup These advanced parameters are still available and can be modified if required but the modification of these parameters is only required for advanced measurements It is possible to switch from the default view to the advanced command view by using the toggle available in the View menu see Figure 164 File View Bun Tools Help cf e do gly i a show hide advanced commands and parameters Advanced procedure view Setup View cE Mult Autolab View Measurement View a Analysis View E ser log Fii Autolab display F10 FRA manual control MDE manual control MLS manual control Figure 164 The Repeat for each row command provides a table of one of more parameters Switching to the Advanced command view displays the advanced commands in the commands browser and the advanced parameters in the procedure setup frame Figure 165 shows a side by side comparison of the FRA single freguency command in normal mode and in advance command vie
198. scan rate V s 0 1000000 scan rate V s O ay Figure 126 The additional frame located in the measurement progress frame displays the list of modifiable command parameters left original parameters right modification of the scan rate In the example shown in Figure 126 the modifiable command parameters of the CV staircase command are displayed To change a parameter change the value and press the button see Figure 126 Note only the parameters of the active command can be modified If the modified parameter is linked to other parameters in the procedure the modification is applied to the linked parameters as well The modification of the parameters only affects these parameters during the ongoing measurement The original parameters defined in the procedure in the Setup view or not affected Add plots in real time 95 Page It is now possible to add new plots to a given command in the measurement view while the command is running if the command provides data that can be plotted Right clicking the command in the measurement progress frame displays a context sensitive menu through which the type of plot and location can be chosen see Figure 127 File View Profile Run Tools Help Bt Bere eee eae ee re Cyclic voltammetry potentiostatic Tired procedure Autolab control if i i 4 Set potential Bet cell Wait time 8 Optimize current range me oY staircas ebeell Add Flot to MeasurementPlotl
199. se Test AC Voltammetry Test Galvanostat Test Results A Windows Information H A Embedded Processor Test J A EEProm Test J A Timer Test J A Autolab Test J A AD Converter Test H A DA Converter Test H A Potentiostat Test a al Noise Test al AC Voltammetry Test 3 Galvanostat Test Progress Figure 286 The diagnostics report after all the tests have been performed successfully If all the tests succeed the instrument is working correctly It is possible to verify the results of a specific test by clicking open the details in the diagnostics tool see Figure 287 w Diagnostics Results Windows Information H A AD Converter Test Embedded Frocessor Test F vil DA Converter Test EEProm Test be O DA Converter Test succeeded Timer Test 2 Ka Advanced Autolab Test 2 2 DAC 4 ADC 4 V 100 V 100 005 V AD Converter Test DAC 4 ADC 4 V 4 999 V 5 000 005 V DA Converter Test DAC 4 ADC 4 V 4 999 V 5 000 005 V Potentiostat Test DAC 4 ADC 4 V 001 V 000 005 Vj Noise Test 2 2 DAC 4 ADC 4 V 499 V 500 005 V AC Voltammetry Test 2 2 DAC 4 ADC 4 V 500 V 500 005 V Galvanostat Test 2 DAC 4 ADC 4 V 900 V 900 005 V DAC 4 ADC 4 V 699 V 900 005 V g T Fotentiostat Test Progress Figure 287 The diagnostics tool displays the details of all the tests If one or more of the tests fails a red symbol will be used to indicate which test failed and wh
200. sed using a dedicated interface in the Analysis frame see Figure 253 189 Page Demo 01 Copper deposition CV staircase H A Evst H E vsi H ivst H Standard CV WE 1 Current A 0 0009 0 0008 0 0007 0 0006 0 0005 0 0004 0 0003 0 0002 0 0001 0 0001 0 0002 0 0003 0 0004 0 2 0 0 8 0 2 0 4 0 6 Potential applied V v7 i x Signal Expression Unit Index Peak posit Peak height Peak area Base start Search mode Automatic O Manual Base line mode Minimum peak height Minimum peak width Nr of points in search window Number of significant digits Peck Type Peak position Index gt 0 24017 0 19226 0 24017 2 3 4 0 19424 1E 05 lo B 5 Forward Peak height Peak area 0 00021219 0 00092294 0 00020283 0 00091457 1 5448E 05 0 00013739 1 5915E 05 Figure 253 Adding a peak search analysis tool to a CV staircase 2 2 The results of the data analysis tools are available in the data grid This easy export of the results to an ASCII or xls file see Figure 254 Peak position 0 24017 0 19226 0 24017 Peak height Base start Peak area 0 00021219 0 00092294 0 00020283 0 00091457 1 5448E 05 0 00013739 1 5915E 05 0 00012439 0 33142 0 2124 0 33142 0 20844 0 93811 Base end Penk width half 0 12512 0 06295 0 11719 0 69809 0 09670
201. ser profile Import user profile Export user profile Hicle Unhicle Show all Ctrl H Ctl Shitt H Figure 112 Importing and exporting user profiles 87 Page This means that any number of profiles can be created and used at any time using this method It is possible to reset the user defined profiles to default by using the Reset user profile option from the Profile menu Figure 112 Context sensitive popup menu A new context sensitive popup menu window has been added to Nova This popup appears as soon as any item supporting this feature is clicked see Figure 113 Commands Parameters Links Cyclic voltammetry potentiostatic Remarks Cyclic voltammetry potentiostatic no extra modules required s End status Autolab m oignal sampler Time WWE Potential vwE 1 Current m Options 1 Options m Instrument Instrument description E Timed procedure Autolab contral set potential 0 000 set cell Ge 0 1 000 0 000 2 0 1 000000 Set cell lt 3 lt 3 Figure 113 Clicking an item in Nova now displays a popup menu window for supported items only This popup menu displays a number of icons related to context sensitive actions In the example shown in Figure 113 a total of eight action buttons are shown in the popup menu These actions are the most commonly encountered for the CV staircase command see Figure 114 E Os w P a 7 B Add plot j vst Log i vs E
202. sible through the External NET commands For more information contact Metrohm Autolab B V nova metrohm autolab com This information can be found in the Shared DataBases Tutorials External DOTNET DLL folder located in the installation folder 143 Page NOVA 1 5 Release notes Released 01 06 2009 Introduction These notes provide an overview of the new features introduced in NOVA 1 5 compared to the previous release The following items have been added to NOVA 1 5 Anew set of tutorials available from the Help menu Support for the modules pX ECN FI20 Filter MUX IME663 amp IME303 Booster10A for the PGSTAT128N ADC750 revision 4 0 PGSTAT101 Improvements and additions 144 Page Voltammetric analysis techniques Manual control of the Hg drop electrode IME663 or IME303 Manual control of the MUX New user interface for Autolab control command Manual control of the instrument through Autolab display Skip button Reverse button Multiple plots in measurement view and overlays Send email command Check online for updates New data handling commands Timed procedure inside a FRA frequency scan New FRA commands Post measurement check Save data option Hardware summary in the About menu Improved support for Metrohm devices Autolab control in options Wait on DIO trigger New Autolab procedures Test of Autolab modules Previous NOVA versions and NOVA 1 5 It is possible to install more th
203. sion rate fit Corrosion rate tafel slope Analysis impedance Plots general Plots impedance Nyquist 2 vs Z Bode modulus Bode phase Nyquist Y vs Y Residual Z Residual 2 Epsilon plot MottSchottky Rs Cs i MottSchottky Rs Cp Rp H My commands Figure 237 The new commands browser showing the details of the Cyclic and linear sweep voltammetry measurement section the Corrosion analysis section and the Impedance plots section Procedure templates A series of special commands called template commands have been added to the command browser in the Measurement cyclic and linear sweep voltammetry and in the Measurement chrono methods group see Figure 238 e Timed procedure potentiostatic e Timed procedure galvanostatic These commands are complete templates that can be used to construct procedures quickly 178 Page Measurement cyclic and linear sweep voltammetry S Timed procedure potentiostatic CV staircase CV linear scan CV linear scan high speed LSV staircase Timed procedure galvanostatic gt CV staircase galvanostatic L LSV staircase galvanostatic Measurement chrono methods gt Timed procedure potentiostatic Record signals gt 1 ms Chrono methods Chrono methods high speed i Timed procedure galvanostatic z Record signals gt 1 ms galvanostatic z Chrono methods galvanostatic Chrono methods high speed galvanostatic Figure 238 Speci
204. tant phase element impedance obtained by fitting experimental data NOVA now allows the user to use these dynamic command parameters in the same way as any other parameter The results of calculations or data handling steps can be linked to other parameters or can be plotted during a measurement For example the result of a linear regression can be used in a procedure plotting the intercept versus the square root of the scan rate To identify dynamic command parameters in the procedure editor these parameters are now shown in blue Other parameters are shown according the following color convention e Red parameters measurable electrochemical signals through the signal Sampler or a dedicated sampler e Black parameters command parameters that can be edited e Grey parameters command parameters that cannot be edited and are calculated based on the user defined command parameter values Figure 181 shows an example of the four types of parameters in the procedure editor 135 Page Commands Parameters Cyclic voltammetry potentiostatic Remarks Cyclic voltammetry potentiastatic no extra modules required sy End status Autolab m Signal sampler Time WWE 1 Fotential WE 1 Current ma Options 1 Options m Instrument Instrument description E Timed procedure Autolab control m set potential 0 000 oet cell Cin T art time 3 a Optimize current range A E CY staircase 0 000 1 000 1 000 0 000 2 0 10000 start p
205. termination command is used in a procedure all consecutive commands that specify a potential to be applied on the cell can be adjusted using a right click menu see Figure 37 29 Page Commands Cyclic voltammetry potentiostatic Parameters Links Remarks Cyclic voltammetry potentiostatic ma End status Autolab aaa oignal sampler Time WE 1 Potential vWE1 Current m Options 1 Options m Instrument ALIT4000 Instrument description H Autolab control m OCF determination 0 000 Set potential 0 000 cet cell On E at time 3 A Optimize current range z E CY staircase O 000 1 000 1 000 0 000 2 0 1000000 start potential v 0 000 Upper vertex potential v4 anr Lower vertex potential 0 Versus REF stop potential 6 Versus OCP Number of stop crossings Step potential 0 Hide ocan rate v s Estimated number of paints kK Undo Insert OCP determinaton Ctl4 Z Interval time s 0 024400 oignal sampler Time WE 1 Potential vWE 1 Current al Options 1 Options m Fotential applied array Cv Time lt array 5 WE Current lt array A ocan lt array gt WE Potential array Cv Index lt arrary gt H iws E zj E ws t ial Set cell Cit lt gt Figure 37 Each applied potential value can now be specified versus the OCP or versus the reference electrode REF Each potential to be applied can be specified versus the reference electrode REF
206. the trigger byte consists of 4 bits for the PGSTAT101 172 Page NOVA 1 4 Release notes Released 14 09 2008 Introduction These notes provide an overview of the new features introduced in NOVA 1 4 compared to the previous release The following items have been added to NOVA 1 4 Anew set of tutorials available from the Help menu Support for the modules pX1 000 e EQCM e ECD Support for the instruments e PGSTAT20 e PGSTAT128N Improvements and additions e Tutorials e Simplified user interface e New Autolab procedures e Grouped commands e Procedure templates e New plotting framework e Installed on same computer as previous releases e DAC control in Autolab control e Cutofts e Simplified FRA frequency range editor e FRA Galvanostatic support e pH calibration e Data repository e Reverse compatibility with previous NOVA versions e New data analysis framework and data analysis tools e New data handling and new data analysis commands e My commands e Improved Import GPES command e Import and Export ASCII e G circuit element in Fit and Simulation e Kronig Kramers calculation e Metrohm liquid handling support e External devices control 173 Page Tutorials A series of short tutorials is available from the Help menu in Nova see Figure 233 Each tutorial is dedicated to a specific measurement technique or aspect of the software Some tutorials include procedures that can be used to pe
207. this is the name of the electrochemical signal generated by the calculation e Unit this is the unit of the calculated signal e Expression this is the mathematical expression used for the calculation The functions provided in the two lists on the right hand side of the expression builder window can be used to build the expression The unit group can be used to assign a unit to the calculated electrochemical signal The unit can be selected from the drop down list or it can be entered manually The parameters field which is updated once a formula has been entered provides a list of all the variables that are used in the calculation In Figure 297 the expression builder is used to calculate the logarithmic value of the absolute value of the current The formula has only one parameter the Current see Figure 297 221 Page FE Expression builder _ ox Expression 10LOG ABS Current Parameters Functions Figure 297 The expression builder and the formula used in the Mathematical parser When the mathematical expression has been entered the expression builder can be closed by clicking the OK button The Mathematical parser command will be updated see Figure 298 A list of parameters will be displayed under the Mathematical parser command Each of these parameters has to be linked to the source electrochemical signal that has to be used in the calculation 222 Page Commands Parameters Cyclic voltammetry
208. ting the measurement FFT Analysis and FFT Smoothing Two FFT related analysis tools with matching commands in the Analysis general group of commands have been added e FFT Smooth Applies a smoothing on the measured data to filter out noise and spikes The frequency domain data Is first calculated through an FFT One of four type of filtering strategies can be applied low pass high pass band pass and band stop The filtered data is reconverted to time domain after the filtering is applied e FFT Analysis Calculates the frequency domain data from source time domain data through a FFT Both tools can be selected from the right click menu see Figure 177 or can be added as commands in a Nova procedure Chrono amperometry At gt 1 ms ll Record signals 1 ms Plot Options Properties sinc TY sc smooth Copy Visible Plot s to Baseline Correction Show All Plots Peak search Hide All Plots Regression Save in Mly commands Derivative Delete Integrate Remove all from View sal cuales Corrosion Rate Figure 177 Both the FFT Smooth and FFT Analysis tools have been added More information on the use of these tools can be found in the User Manual Chapter 4 ECN Spectral noise analysis A dedicated spectral noise analysis command has been added to Nova This analysis tool can be used to analyze electrochemical noise data obtained using the ECN module or measured through the Autolab PGSTAT This
209. to be carried out only once The update will take about five seconds FRA32M The FRA32M is the new impedance analyzer module for the modular Autolab PGSTAT instruments and the Multi Autolab instruments It replaces the FRA2 module and it is compatible with all the commands and procedures used in combination with the FRA2 module The FRA32M is fitted with a frequency generator that reaches 32 MHz However when the FRA32M is used in combination with the Autolab PGSTAT the maximum frequency that can be applied in a measurement is 1 MHz For measurements involving external devices the frequency can be increased The maximum frequency that can be used in combination with the FRA32M depends on the highest achievable bandwidth of the Autolab PGSTAT Please refer to the Getting started manual for more information 78 Page Please refer to the Impedance spectroscopy tutorial available from the Help menu for more information Automatic Hardware setup Whenever an Autolab is connected to the computer for the first time Nova will try to configure the instrument automatically by reading out the on board EEPROM information This allows the software to pre configure the hardware setup without user intervention For old instruments and old modules this automatic configuration can sometimes not be done accurately For this reason it is always recommended to verify that the configuration is accurate after initialization of the instruments
210. tric analysis i vie eet aan an Measurement chrono methods apy marme som Measurement impedance Eo AO aS ii Data handling Set potential 0 000 7 Analysis general wane a I Analysis baseline correction mea Analysis corrosion Optimize current range 5 Analysis impedance H CY staircase 0 000 1 000 1 000 0 000 2 01 Plots general Sada Off a Plots impedance gt My commands Figure 90 A simplified view of the setup view is shown when the button is clicked iR drop correction tool The R drop correction command and analysis tool have been added This tool can be used to automatically correct the data after the measurement is finished for iR drop This tool requires the user to manually set the value of the uncompensated resistance to use in the calculation The tool calculates an adjusted value of the applied potential given by 71 Page Ecorrected Eapplied iR Where R is the resistance value specified by the user The command can be found in the analysis general group of commands The analysis tool can be added to a measured data set directly see Figure 91 Cyclic voltammetry potentiostatic CY staircase ivsE Plot Options Properties Add Windower Generate index Add Plot gt Add Analysis gt ECN Spectral noise analysis Show All Plots Calculate charge Hide All Plots iR drop correction N Save in My comm ands
211. truments in the same way they are performed when a single instrument is connected to the computer A single 128 Page procedure can run on any of the available devices However only one instrument can be used during the measurements in this mode It is also possible to control more than one device at the same time in order to run the same or different procedures This can be done by using the Multi Autolab view The Multi Autolab can be selected using the View menu or by clicking the amp button in the toolbar see Figure 169 File View Run Tools Help Si T EE Ll ES Multi Autoalab view Figure 169 The Multi Autolab view can be accessed using the View menu or the dedicated button in the toolbar This view provides a dedicated interface through which two or more devices can be controlled see Figure 170 File View Run Tools Help Ns ES E a TEE Configuration name Multi Autolab example Remarks This is an example of Multi Autolab configuration using A uAutolablll FRAZ APGSTAT302N FRA2 A PGSTAT10 with USB interface C Instrument 1 Description Procedure Use active procedure Plot Options AUT 2527 Store in database Instrument Output Instrument 2 Description Procedure Use active procedure Plot Options Instrument Output AUT83072 Store in database _ Instrument 3 Description Procedure Use active procedure Plot Options Instrument Output W3AUT 70530
212. ts Deselect Cptonal Tests Select instrument Autolab Test AD Converter Test DA Converter Test Potentiostat Test Noise Test Galvanastat Test Integrator test Frogress Eas Figure 175 Adjusting the hardware setup for the connected instrument Procedure validation screen The procedure validation screen has been redesigned in order to present errors and or warning in a clear way If errors or warnings situations are detected during the validation step a window showing these errors and or warnings will be displayed see Figure 176 Procedure checking The following problems were encountered during validation Message Command Errors Automatic current ranging can not be used when the filter ECD is switched on LY staircase Warnings a Selected filter time constant EOD too slow to measure properly with the specif CW staircase i selected filter time constant ECD is too slow to measure properly with the specified interval time scan rate or frequency tis possible to continue but the measured data could be invalid ou can change the filter time constant in the Autolab control or adjust the interval time scan rate or frequency Figure 176 The redesigned procedure validation screen now groups errors and warnings messages 132 Page If only warnings are detected the procedure can be started by pressing the OK button although it is recommended to verify the warning messages before star
213. ttings Rate 0 01 mifrmin 166 ml min Tube length rim Tube diameter mmj Port 3 settings Rate 0 07 rmilmin 766 ml min Tube length mm Tube diameter mm Fort 4 settings Rate 0 07 mifmin 166 ml min 330 0 2 0 150 0 200 0 2 0 330 0 2 0 20 0 BE _ Parallel execution Active Dosing port ka Active Fill port w Active special port Active None JK X Cancel Figure 44 The Liquid Handling setup window shown for a Metrohm 800 Dosino The Dosino setup provides the possibility to define the role of each port of the device Make sure that the roles are defined properly since this will have an influence on the Prepare Fill and Empty commands The following settings can be specified see Figure 44 e Name of the device e Parallel execution e Role of each port using the provided dropdown list e Rate Diameter and Length for each port e Ports can be deactivated if needed using the provided checkbox 36 Page Figure 45 shows the settings for the Metrohm 858 Professional Sample Processor Liquid Handling setup 0 ES Mame sample processor Parallel execution Rack type 62041350 W Tower 1 setings Active Lift rate 3 mms 25 mm s 3 Pumps Shift rate 3 s 20 s 3 Valves Swing rate 10 s 55 s 10 stirrer Work position rim 100 Peristaltic pump Position limit rim 100 Injection valve v 3 v J v 10 v 100 100 Refresh JK Cancel Figure 45
214. tween 15 and 15 if present not shown in Figure 50 e Set the Peristaltic pump speed between 15 and 15 if present only for the Metrohm 858 Professional Sample Processor 41 Page e Set the Injection valve to Fill or Inject position if present only for the Metrohm 858 Professional Sample Processor not shown in Figure 50 The commands described in the External devices tutorial are still available and can be used to perform the actions as indicated in this document However the Metrohm devices commands have all been modified and now provide a list of available devices in the procedure editor When using a command to control a Metrohm device it is possible to type the name of the device directly in the procedure editor Device name parameter or click the button to display a list of available devices see Figure 51 Commands Farameters Links New procedure Remarks aa End status Autolab zz oignal sampler Time WwE 1 Current m Options Mo Options Err Instrument Instrument description Dosino prepare Dosing 1 Dosino_1 Cycles 1 a lt gt Device name Please select one item sample processor stirrer Figure 51 A list of available devices is displayed in the procedure editor Select the name of the device to control and click the __ button to close the editor The procedure editor will be updated The name displayed in the Device name dialog correspond to the names for each device specifi
215. uit e New format for Message box and nput box commands e Subfolders in procedure browser e Multiple warning error validation tooltip in the procedure editor Support for Metrohm devices in 64 Bit versions of Windows The 1 10 3 update of NOVA adds the support for the 814 815 and 858 Metrohm Sample processors Increment parameter and Increment parameter with signal back in the Control group of commands The ncrement parameter and Increment parameter with signal commands have been added again to the Control group of commands These two commands were missing in the initial release of NOVA 1 10 Single instance of cutoff The possibility to perform a specific action specified in a cutoff option only once has been added This is particularly useful in combination with the Reverse scan direction action for staircase cyclic voltammetry or linear sweep voltammetry This option is useful for corrosion experiments requiring the scan direction to be reversed once a threshold current is reached as shown in Figure 28 22 Page 0 1 0 01 0 001 current density mA cm 200 0 0 0001 potential in mV vs SHE _ E E 400 600 800 1000 1200 redox potential limit potential redox potential 250 mV Figure 28 Example of a corrosion experiment requiring the scan direction to be reversed once a threshold current is reached To indicate that the specified action needs to be executed only once the Only once checkbox n
216. urements performed on the Autolab dummy cell using compensated resistance values of 0 95 98 and 102 Ohm respectively The correct value of the uncompensated resistance can be determined by trial and error by detecting the point at which the response of the cell becomes a ringing oscillation 142 Page 0 6 Evst 0Q 1 0 6 Evst 95Q 0 4 0 4 gt gt w 0 2 w 0 2 5 5 0 E 0 Wi 9 2 Wi 9 9 0 4 0 4 0 0 005 0 01 0 015 0 0 005 0 01 0 015 Corrected time s Corrected time S 06 E vst 98 Q 3 l E vyst 102 9 0 4 0 2 0 2 0 4 1 Potential W D VVE 1 Potential V gt 0 005 0 01 0 015 0 0 005 0 01 0 015 Corrected time s Corrected time s Figure 190 Four different positive feedback experiment plot 1 green line 0 Ohm plot 2 blue line 95 Ohm plot 3 orange line 98 Ohm plot 4 red line 102 Ohm More information on the use of the i Interrupt and Positive feedback procedures can be found in the iR Compensation tutorial available from the Help menu External NET applications support External applications can be used from NOVA using dedicated commands This option is for advanced applications only and requires the user to be familiar with software programming A tutorial and some examples are provided in the installation folder Avantes spectrometer support Basic support for Avantes spectrometers is available Presently support of these devices is pos
217. ures 1 4 nox Figure 247 Schematic view of the conversion process to NOVA 1 4 from previous versions After installing NOVA 1 4 start the Upgrade files to NOVA 1 4 application Start menu All Programs Autolab Tools The Upgrade to NOVA application will be started see Figure 248 To use the upgrade function files from older NOVA version must be added to the application as individual nox files FE Upgrade to NOVA 1 4 Add files to list Remove files from list Create backup s Override backup s Idle Figure 248 The Upgrade to NOVA 1 4 application To add files to the list press the Add files to list button Navigate to the folder containing the files to upgrade from previous NOVA versions to 1 4 see Figure 249 187 Page EB Upgrade to NOVA 1 4 File File C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 01 Copper deposition nox C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 02 Copper deposition QCM nox C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 03 Bipotentiostat measurement PtPt Rin C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 04 Hydrodynamic LSV with increasing rot C Documents and Settings User My Documents My Procedures 1 3 Demo Database Demo 06 Galvanostatic CV nox C Documents and Settings User My Documents My Procedures 1
218. ut Imaginary Phase Real Max number of Iterations 100 1 59152693 0 182373089 500 00506596 _ Circuit Circuit 2 00359429 0 229590078 500 00802890 e e AE o 2 52239742 0 289035645 500 01272530 e r of iterations giving no improvement 3 17544783 0 363859949 500 02016775 sng siye P 3 99749440 0 458040077 500 03196196 ao eeki ican zae Fit or Simulation Simulation 5 03239327 0 576591909 500 05065509 e deat anes 6 33506375 0 725789471 500 08027895 5 Results 7 97455430 0 913506746 500 12721940 iden sik S EEE EA 5 10 0378363 1 149633422 500 20159760 Result Circuit 12 6340838 1 446527582 500 31944423 Chi square 3 8E 10 Figure 324 The results of the simulation are displayed in the same way as those of the fitting The results of the simulation are displayed in the same way as those of the fitting calculation Clicking the save button located in the toolbar will save the results of the simulation 242 Page
219. utolab control OCP determination OCP determination OCP value 0 000 set reference potential Set reference potential Reference potential V 0 000 Set potential Set potential Setpoint potential V 1 200 Set cell Set cell Cell status On Wait time s Wait time s Duration s 5 Optimize current range Optimize current range Number of optimize steps 5 Figure 260 The command is added to the My commands database Once a command has been added to the My command database it can dragged into the procedure editor as any other command In the example shown in Figure 261 the My Potentiostatic Preconditioning command has been added to a new procedure 194 Page Commands Parameters New procedure Remarks aa End status Autolab Collection al Signal sampler Time WE 1 Current m Options No Options m S My Potentiostatic Preconditioning Autolab control z OCP determination 0 000 7 Set reference potential 0 000 Set potential 1 200 Set cell On c Wait time s Optimize current range 5 oe lt gt Figure 261 Adding a My command into the procedure editor creates a copy of the original command Note saving a complete Timed procedure instead of a single command allows you to very quickly group commands This simplifies the procedure building process especially for routine measurements Improved Import GPES command The import GPES command has been improved It is now possible to
220. values of the circuit elements are dynamic command parameters and can be used to create plot 3 and plot 4 showing the fitted values versus the repeat number 136 Page 1200 1000 800 600 400 200 Phase 200 400 600 0 500 1000 1500 0 1 1 10 100 1000 10000 Z Frequency 0 9995 1200 1E 6 Q 0 9993 0 9992 130 9 5E 7 0 9991 1100 0 999 9E 7 0 9989 1050 Polarization resistance R Q Constant phase element N 0 9988 8 5E 7 Uncompensated resistance R Constant phase element YO Mho 0 9987 1000 9 0 9986 6 8 6 8 Repeat Repeat Figure 182 Using Dynamic command parameters during a measurement plot 1 and plot 2 show raw impedance data plot 3 and plot 4 show calculated values dynamically added by the Fit and simulation command Repeat for multiple values A new type of repeat loop Repeat for multiple values has been added to the Control group of commands This command is similar to the Repeat for each value command The difference with respect to the latter is that the Repeat for multiple values command can be used to define a Table of values containing one or more columns see Figure 183 Edit table t Figure 183 The Repeat for multiple values command provides a table of one of more parameters 137 Page Note the number of values in each column must be the same During the measurement the commands in this new type of repetition loop will be repeated for ea
221. ve on to the next command Note the Skip button does not change the settings of the Autolab The instrument will remain in the settings encountered immediately before the skip button is pressed Reverse button Nova now provides an additional button in the Autolab display that can be used to reverse the scan direction of linear sweep and cyclic staircase voltammetry commands see Figure 204 This button is available both in potentiostatic and in galvanostatic mode Note the Reverse button is not available for cyclic voltammetry measurements performed using the linear scan generator module SCANGEN or SCAN250 and for the Voltammetric analysis commands 152 Page Autolab display 100 m 100nA 10 mA CELL ON oe status current range Reverse rr Figure 204 The reverse button is now available in the Autolab display Multiple plots in measurement view This version of NOVA introduces the possibility of displaying up to 4 plots at the same time in the measurement view Each plot can be configured independently and can be used to display measured data points or results from data handling commands or calculations During the experiments it is possible to change the arrangement of the plots using dedicated toolbar buttons see Figure 205 aw NOVA File View Run Tools Help he Si a T ah R223 J Show four plots during measurement Figure 205 The dedicated toolbar buttons for multiple plots An example o
222. w 125 Page FRA single frequency Input frequency Hz 100 Input amplitude 0 1 Input wave type Single sine a FRA sampler Options No Options 3 Frequency lt array gt Hz Fad lt array gt 0 TAL lt array gt 9 F lt array gt 0 Phase lt array gt Time lt array gt s Potential DC lt aray gt V4 Current DC lt aray gt A lt gt Input frequency Hz 100 Input amplitude 0 1 Amplitude in RMS Yes y Amplitude unit Y Input wawe type Single sine as Input connection Internal eo Integration time s 1 Minimum number of cycles to integrate 1 Number of cycles to reach steady state 10 Maximum time to reach steady state s 1 with a minimum fraction of a cycle 0 FRA sampler Options No Options c Lowest bandwidth High stability a Frequency lt array gt Hz Pil lt array gt 0 TA lt array gt 0 PA lt array gt Q Phase lt array gt Time lt array gt s Potential DC lt array gt 0 Current DC lt array gt A lt gt Figure 165 Comparison of the FRA single frequency command shown in default simplified 126 Page mode left and in the advanced command view right Support for MultiBA instruments Version 1 6 of NOVA includes support for MultiBA devices The MultiBA instrument is a special version of the modular Autolab PGSTAT except the PGSTAT100 in which more than one BA module is installed This provides the me
223. xperiments It can also be used to perform so called Cyclic voltammetry Staircase current integration experiments Two default Autolab procedures have been added to illustrate the use of this module Warning the integrator must be calibrated before it is used The calibration of the integrator is performed in the Diagnostics application Make sure that the Integrator test is selected in the diagnostics application see Figure 153 Refer to the Getting started manual for more information on the Diagnostics application 116 Page 4s Diagnostics 3AUT70530 File Select Tests Results Windows Information Embedded Processor Test License information EEProm Test Timer Test UAutolab Type Ill Test AD Converter Test DA Converter Test Potentiostat Test Noise Test Galvanostat Test Integrator test Frogress Ea Figure 153 The integrator test is used to determine the calibration factor of the integrator When the integrator test is finished a window will be shown indicating the currently used calibration factor and the measured calibration factor see Figure 154 Integrator calibration Calibration factor currenti 1 Calibration factor measured 1 06 Save measured tactor X Figure 154 The stored and measured calibration factors are shown at the end of the test The new value can be stored by clicking the OK button This value will be shown i
224. xport to AView Adel Wincdower Generate index Aclel Plot Add Analysis Show All Plots Hide All Plots Save in My comm ands Delete Remove all from View Figure 146 A direct Export to ZView tool has been added Using this tool it is possible to create an ASCII file directly readable by the ZView software A matching Export to ZView command has been added to the Data handling group of command in the Setup view My Commands integration in Analysis view User defined commands created in the Setup view or in the Analysis view using the My commands framework can now be accessed from the Analysis view using the right click menu see Figure 147 Cyclic voltammetry potentiostatic C staircase 3 ivs E Plot Options Properties Le H Add Windower Generate index Add Plot Add Analysis My comm ands My analysis comm and Show All Plots N Hide All Plots Save in My comm anes Delete Remove all from View Figure 147 Commands created using the My commands framework in the Setup view are now available in the Analysis view 111 Page Linkable duration in Record signal gt 7 ms command The Duration parameter of the Record signals gt 1 ms command can now be linked to another parameter The duration of the command can therefore be specified using an input box for example see Figure 148 E Input box Title of box Duration Messaqe setthe duration of the Rec
225. xteral 1 External 1 al ulate a signas n GWE 1 Currentfat Inte grator 1 Charge Integrator Integrated Current KOUKI Time _ Sample alternating JK Cancel Figure 55 The time derivative signals can be selected in the Signal sampler The derivative signals are calculated in real time Just like any other signal the derivative signals can be plotted in real time and can be used as a cutoff value as shown in Figure 56 3 Edit Options 0 Automatic Current Ranging Suto Autolab control Automatic Integration Time tems Cutoff on cE Currentict Basic properties oignal dW ECY Currentiet v Action when gt w Value 0 001 Action stop command v _ Only once Linkable as Advanced properties qF Mr of detections 4 Additional cutofis Mo Cutoff Add Remove Cancel Figure 56 The derivative signals can be used for cutoffs 46 Page The derivate signals obtained in real time will be noisier than the calculated derivatives obtained using the derivate analysis tool because the latter uses a windowing function to that includes also the data points ahead of the data point at which the derivative is calculated This function is not available in the real time calculation which can only take into account the values preceding the data point at which the derivate is calculated An example of a plot of a time derived signals shown in Figure 57 0 00018 0 0007 0 00016 0 00014 0 0006 0 000
226. y messages after the measurement finishes advising to change the experimental condition if applicable The example shown in Figure 214 suggests changing the current range used in the measurement as an overload was detected during the previous experiment ser log message Time Date Command WU Autolab USB connected e0708 PMO 2 5 2004 J Autolab initialization finished 2 07 19 PM 2 5 2009 amp Overload occurred in 100 nA current range try using a higher current range 2 08 33 PMO 2 5 2009 LY staircase Figure 214 Post measurement check Note it is possible to copy paste the contents of the User log using the right click menu Save data at the end of the measurement By default NOVA saves all the measured data points at the end of the experiment It is now however possible to switch this feature off This can be trough the options menu see Figure 215 Nova options Graphics Colors Advanced settings Clear measurement plot before start File name of embedded executable Log tracing Switch to measurement view when start measurement Time out in seconds for the validation dialog 30 Trace level Warning URL of the external version information http www ecochemie nl download content Version Nova URL of the internal version information http softwareserver updateserver Nova Auto save measured data Figure 215 The Automatic save feature can be switched on or off in the options menu When this opti
227. ys the large control window below the 2D plot area The Fit and simulation control interface has a number of values and settings see Figure 313 E Input Max number of Iterations 100 Circuit Maximum change in chi square 0 001 Maximum number of iterations giving no improvement 100 Fitting style Impedance Use weight factors Yes Fit or Simulation Fit Measurement data format Impedance Results Number of iterations performed 0 Result Chi square 0 Figure 313 The detailed view of the Fit and simulation control interface 234 Page The following parameters define the calculation method used in the fit and simulation tool e Fit or Simulation defines the calculation method Using the Fit methods the software will try to find the most suitable values for the parameters of each element defined in the equivalent circuit starting with initial user defined values The simulation method simply calculates the impedance values for the equivalent circuit as it is defined by the user e Fitting style impedance admittance defines whether the calculation should use the impedance or the admittance values during the fit e Maximum number of iterations defines the number of consecutive calculations used during the fitting calculation The default value is 100 e Maximum change in Chi square defines one of the convergence criteria The fitting will not be finished until the absolute change in the Chi square parameter including w

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