Home

Express Software Users Manual

image

Contents

1. P1 and S1 leads to the working electrode S2 lead to the reference electrode P2 and S3 leads to the counter electrode 2 1 3 1 2 CE to Ground mode EC Lab Express Software User s Manua Cell Connection WE sal Ene P1 51 52 33 BE P Fig 11 Standard mode connection for SP 300 technology This mode of connexion is dedicated to special applications such as for example bipotentiostat mode In the bipotentiostat mode two working electrodes are present in the same bath whereas only one counter electrode and one reference electrode are used For VMP3 technology Disconnect the cables from the cell select Electrodes connection CE to ground and reconnect the cell as follows CA1 CE and Ref3 leads to the working electrode Ref2 lead to the reference electrode GROUND and Ref1 leads to the counter electrode For SP 300 technology Disconnect the cables from the cell select Electrodes connection CE to ground and reconnect the cell as follows P1 and S1 leads to the working electrode S2 lead to the reference electrode GROUND and S3 leads to the counter electrode Cell Connection CE CAT refs E Mc a HE Ter CE ref ground Fig 12 CE to ground connection mode for VMP3 technology Cell Connection F1 5 MIE 59 Ece 53 CE ground Fig 13 CE to ground connection mode for SP 300 technology To set the standard connection proceed in the same way dis
2. aPont 4369 at the beginning of the selected zone and ending at se 05187 Y the max current value to the end of the zone The ie 0 092 26 mA data point zone for the analysis is shown in the Total points 456 Selection frame by the extreme points Results The results of the analysis are displayed in the Position 0 231 5 Results frame Several values for the peak are Height 0 224 m displayed the position E height width 1 2 el dua que e E Ep2 charge pos and charge neg These values Bie ies e IC are explained below Ghee Men Uae The results can be copied to the clipboard to be pasted in the print window comment zone or a text file They can also be saved in a text file 7 Fig 82 Peak results tab 3 3 3 1 3 Results of the peak analysis using a linear regression baseline The following figure shows the result of the peak analysis performed on a cyclic voltammetry data file The baseline used for the analysis is a linear regression baseline CV_Fe_basique_1_n mpp vs Ewe cycle 2 Marker Data point selected zone I mA Regression line Ewe V Fig 83 Oxidation peak analysis on a cyclic voltammetry experiment using a linear regression baseline 69 EC Lab Express Software User s Manual The different values in the result frame of the peak analysis window are as follows Position is the potential E corresponding to the max current value determined according to the basel
3. Minimize Stop 50 100 sin ampl mV 7 Fig 127 VASP plot and VASP Fit window 3 3 5 5 Constant Amplitude Sinusoidal microPolarization CASP The relationship describing the potential modulation vs the sinus of the frequency is given by 105 EC Lab Express Software User s Manual E Ecor E sin 2zfst Then by applying a Fourier Transform to the former relationship the resulting current can be described by the following equation 3 4 I t l of sin ot l cos2at of sinBat Where the fundamental is 6 o and the three first harmonics are h lz O 3 respectively 3 3 5 5 oh ZI RE b pE ag oO OE al ba be ba bc 48 l2 to OE E 7 3 3 5 5 l3 bof aE p tO aps 2 24 384 In order to prevent the polarization of the sample the intensity of the sinusoidal excitation Va has to be chosen so as to have a value of the three first harmonics 6 2 9 3 and 6 3 not null and the rest of harmonics equal to 0 The f is determined by EIS technique The simulated harmonic plot is given in vs Time The CASP fit tool allows the user to find the corrosion current and the anodic and cathodic tafel parameters into a versus time presentation In the analysis menu select the CASP Fit tool T The CASP Fit window is displayed The user could receive a warning message to switch to the versus time graph representation Fig 84 CASP Fit Selection Trace sz tim
4. damping factor The following table gives typical frequency bandwidths of the control amplifiers poles for the VMP3 VMP2 Z VSP SP 150 SP 50 HCP 803 and BiStat Bandwidth 7 6 5 4 3 2 1 Frequency 680 kHz 217kHz 62kHz 21kHz 3 2kHz 318 Hz 32Hz Note e Refer to the SP 300 VSP 300 SP 200 or SP 240 installation and configuration manual for details about bandwidth definition for these instruments e When the mouse pointer stands for several seconds max 20 on a box a hint see Fig 33 appears The hint is a min 20 visual control text that gives the user information about the box It shows the min and the max values Fig 33 Hint of the variable and the value that cancel the box 2 2 5 Running acquisition Click on the Run button P to launch the experiment A filename selection window will appear 2 EC Lab Express Software User s Manual My Recent Documents My Network File name EV mpr ll Placez Save as hype EC Lab raw files MPR Cancel Fig 34 Filename selection window The default folder to save data in My document is called EC Lab Express Data The user can choose and create another folder to save his data files Clicking on the Save button or pressing on the ENTER key will start the experiment Two files are created when running the experiment a binary raw data file with a mpr extension automatically added and a LOG file which is a reminder of the experimental settings
5. Ewe V Fig 86 Wave analysis on a curve resulting from a RDE experiment E is the half wave potential obtained by the intersection of the curve with the median between both linear regressions la is defined by the current value for E E on the top linear regression for the oxidation reaction 71 EC Lab Express Software User s Manual 3 3 3 3 CV Sim CV Sim is a tool designed for the simulation of cyclic voltammetry curves It is a useful tool to elucidate the mechanism of an electrochemical reaction To perform the simulation it is assumed that e Only one specie Red or Ox is initially in the solution e The Initial current is equal to zero So the voltage sweep will start from the open circuit voltage First to perform the simulation the user has to define the number of electron transfer steps that are involved in the mechanisms via the combo box E represents a mechanism with one electron transfer E and so on up to 5 electron transfer EEEEE Depending on the number of electron transfers selected the corresponding number of tabs appears Example Select Example s elect Mechanism E Mechanism EEEE setup E ez es es sew Reaction Reaction Reduction A ze4 Reduction A ze gt B z mE z 1 EO De VW EQ oz VW ko nno cm s ko nno cm s a o5 a o5 Species Species Ca initia
6. 3 3 4 3 1 Mott Schottky relationship and properties of semi conductors 92 33 432 The MOU SCHOUKY DIOE orien e Re Etre etc e Ente Eat io teed 93 9 99 9 ME MOIESCHONKV FI usc icon E pn e a nU E ER Qe tnu E Re tonus ended 94 3 3 4 3 4 Saving Fit and analysis reSultS o ccconnccconccconcnccnonnnoncncnnnnnnoncncnnnnnonanoss 95 3 3 4 4 Kramers Kronig transformation ooccconcconcconcconiconoconoconoconononocanonanonanenanenones 96 905 COMODOS lt el eel EE neers 98 cs AAA eE EEE EG e ee eee ee oe 98 Se OL eS 101 Some as 103 dee WIAIMIZO PUN cacon 103 JS COM Ma oc 104 3 3 5 4 Variable Amplitude Sinusoidal microPolarization VASP 105 3 3 5 5 Constant Amplitude Sinusoidal microPolarization CASP 105 3 3 5 6 Electrochemical Noise AnalySIs ccccccscccscecececeeeceeeceeeceeeceeecseeseeenseenes 107 GOS SAN Y Me 109 O A 113 EC Lab Express Software User s Manual Introduction EC Lab Express software has been designed to control single channel potentiostats SP 50 SP 150 SP 200 SP240 and SP 300 But it is also compatible with the other potentiostats of our range VMP2 Z BiStat VMP3 VSP and VSP 300 Each channel board of our multichannel instruments is an independent potentiostat galvanostat board that can be controlled by EC Lab Express software Once the techniques have been loaded and started
7. Bod AXIS A iu du Em E M 46 3 2 5 2 How to create your own graph representation for a specific technique 47 3 2 5 3 How to create a Graph Style sanna O 48 320 MLS RIT 50 S COPY ODIOS cedo iii 51 32 a Standard COPY OPIO Susini aii 52 a JAUValicedacopy ODIOLIS eiecerunt atear m srr eens boonies anna 52 92 9 cg 19126 8 19 Ae en en eM ee eM er eM eer eM ene 52 3 2 9 Multiple graphic in O da ii 53 3 3 Graph Tools Analysis TOO S 55 ioa cceeveueioudnsaseeaseuaiondacasneestenadenessueneeedeucdoudasuency 54 Sal ZOMG SCICCU OM uisa bed eu tou isa aad eui utrunque duties Ee 55 232 A 57 3 0 22 Min and Max determination oocccccccccncccncccnocononononononononononononnnonnnnnnnnnnnnnnnnns 57 ORE WING Tr iai RON REESE ESTEE 58 JOLI O 6 E Ie n ooo 59 3 0 2 4 Linear interpolation id 60 J29 UDa c IT e 60 A o EE EE E E E E E E E E E EE 61 332 ECU A o s 63 oo gl uper batida bios 65 3 9 2 9 Mllti Exponenllal SIM escocia airline e eh 66 29 2 10 Mi lti EXDOHenDttal Pla 66 3 3 3 General Electrochemistry SectiON occccoccccoccncocccnconcncnonononannnnonnnonncnnnnnnnonncnnnononos 67 3 3 3 1 Peak irc Ss 67 3 3 3 1 1 Baseline selection usina codiciados 67 3 3 3 1 2 Peak analysis results cccccecccscccseeceeeseeeceeecececeeeceeecseecseeseeenseeneeeses 69 3 3 3 1 3 Results of the peak analysis using a linear regression baseline 69 3 3 3 1 4 Results of the peak analysis using a polynomial base
8. File SPE diode mpr Matt 5chattky Analysis 12 02 05 15 31 parameters Temperature 25 0 C Dielectric constant 1 000 Surface Area 0 001 cof results File CNEC Labec lab v9 10D ata S PELIS diode mpr Range 0 020 05 W 0 300 1 Vv Frequency 100 000 kHz Flatband potential 0 756 5 Donor density 0 683 5ez1 cm 3 Frequency 31 622 kHz Flatband potential 0 750 2 Donor density 0 685 1821 cm 3 Frequency 10 000 kHz Flatband potential OTE Donor density 0657 bee cm 3 gt wh 2 By x Fig 118 Analysis Results window This text file shows the file name and the analysis performed on the curve with the date and time at the top If several fits were made successively on the curve the user can display every analysis one after the other using the Next button The results can be printed edited to be copied or deleted 3 3 4 4 Kramers Kronig transformation According to several conditions on the studied system it is possible to determine the imaginary part of the impedance from the real part and vive versa The system must be causal stable linear and invariant in time and the impedance must be finite when w 0 or Q This transformation is sometimes used in electrochemistry for the validation of experimental results For example the impedance imaginary part can be calculated from the real part or conversely with the equation Re Z x Re Z 0 2 2 00 Im Z T X 0 0 The
9. Integral tool available with the graphic display used to integrate curves Kramers Kronig transformation tool very helpful to validate impedance measurements done on electrochemical systems Linear Fit tool available with the graphic display used to fit a curve as a straight line Linear Interpolation the linear interpolation allows the user to space out regularly each point of the data file The user can select to interpolate data by a defined number of points or a regular time between each point LOG function of the graphic display that open the log file mpl containing details and settings of the experiment without any data points Loop protocol available in the linked experiments and used to repeat one or more experiments It is different from the cycle in an experiment Low current option providing a sub pA resolution that can be added to each channel This option extends the current range down to 1 nA This option can be added both to standard or Z option channel boards 110 EC Lab Express Software User s Manual Min Max graphic tool to determine the min and max values on a selected zone of the curve Mott Schottky graphic display of 1 C vs Ewe or 1 C vs Ewe curve and corresponding linear fit to determine slope and offset Option EC Lab Express software window in the Config menu used to choose the automatic reconnection of the software to the device Peak analysis graphic tool used on a I E curve to dete
10. al 2 Hm a in 3 S Potential steps Nose Add noise Noise level 000 000 m i 0 000 mv m E Lalculate Copy Copy Sa Fig 89 Setup tab of CV sin e Electrode Geometry of the electrode can be linear semi infinite or spherical semi infinite The surface area of the electrode is calculated from the value of the radius of the electrode e Experimental conditions Temperature in degree Celsius Ro the resistance in Ohm Double layer capacity in UF e Potential scan Scan type linear or sinusoidal scan respectively for CV or LASV simulation Scan rate in V per second The initial and the two vertex potential in V Number of scans performed for the CV or LASV simulation e Sampling The user defines the number of points needed per scan to perform the simulation The total number of points the resolution in time and in voltage is indicated e Noise Some noise in current or in voltage can be superimposed to the simulated curve 73 EC Lab Express Software User s Manual When all the parameters are set the user has to click on the calculate button to display by default the simulated CV curve CVsim mpr vs Ewe 10 000 Example Select 5 000 Reduction A zeAH E 0 z i lt a E 5000 Ko ao a af 10 5 Species 10 000 Ca initial fel DA eS 15 000 Dp eE 20 000
11. cycle s Method Randomize Simplex m z Randomize E udi z Pa l Stop randomize on h 0000 iterations Fj dl Stop fiton 5000 iterations v Fi Weight El v x 11 99e 6 XN 0 314 8e 3 Iterations 5000 Simplex Cycle MEK Fig 103 Fit results with a combination Randomize Simplex 83 EC Lab Express Software User s Manual The randomization was stopped after 2000 iterations and the fit after 5000 iterations In that case the y value is related to a weight 1 for each point The more the number of points selected for the fit the higher the 7 value will be In the case of a weight Z considered the 7 value tends toward zero In any case the value must be the smallest possible The results can be copied to the clipboard or saved in a fit file filename fit When the mpr file is displayed the fit results can be reloaded with the Show analysis results button Note that ZFit can be used with data represented with the Bode plot or the Nyquist plot 3 3 4 1 13 Fit on successive cycles ZFit tool includes an option to fit successive impedance cycles For example in the case of potential steps with EIS measurements on each step we can make an automatic data fitting on each cycle successively without any action by the user The EIS spectra obtained on each step can be seen on the graph at left hand corner on the figure below The potential was scanned from 0 to 1 V with 20 steps of 50 mV We can see the 21 EIS spectra t
12. nce ClO CU OG dd 21 FSI SLO a cea E E nee cede I mr 77 Right click PGC OMAN IRR TETTE a a cee tute utes 35 piloremel tc clo AA A PE ee ee eee ee TL EP 35 CUE AAA a E II II A 35 Right Click MOUSE MOS MMC 34 An A RUE 27 ee TT 27 AAA n A o T RM ORTI NHIEU URN RAS 32 SAV TUE ENERO ES PO PEO E Tm 95 6 0 Rarer ue ME MM rR ee ee oe re ee eee ee ee eee ee 34 LS Meme ten eee N M ULL te Ls tL Lm Meme ee em eee 24 A A IM I M LL E 36 PNG T M 37 Cele 37 Tilo O EE EE Ee 3 114 EC Lab Express Software User s Manual PRC HNO VC saree Saat e E ROA O O ech eet eh as 3 LOO e 37 SOW d Goolge rcc ES 34 Standard Mode to UU mm 11 SUT ARG Gear Mode lisa oi 98 104 wijegcteumi ceb T 60 SU ACO AC MARO A RECON 99 ui il PPP e e E E E 98 ls AAA RM RR O IA TRETEN 103 A A o on A ee 103 Vell A I c TN 30 PROGESSEO MAMA a UL IECIT I EMI IM 30 bg Nee s Bec ET 6 Warburg for Convective diffusion Wd ccoocccccoccnccocnnccncnnnoncnonncnnonnnnonnnnnnnnnnnnncnnnnnnonancnos 80 DUO e de ode old ee 79 Wave analysis A i fata Gace Gta XE mU 71 WE TO GOUNA MOC Ge acs A 13 ZFit Description code SM ica 90 A A 84 A M 34 jue T tas 87 D CSCHIDTION e AA E EEES EEEE AN ETNEN 90 115
13. 12 CaCI Nate ll EE 21 AAG OT SIC ISS envoie ne rU ei nb aeree onte pr e ance tp tcp Gre cd RS e Eau 43 CONDI MLS cect O crete O No A creche dues a etui Due t M Lu dUE 38 Ed ud MM LM MM M MEE 39 Connection Ele eR A 5 Connections 2 e 11 ELECTIONS seorsan A ih Muir Md tenuit nu dutacu uia d du 11 Constant Amplitude Sinusoidal microPolarization CASP eese 105 A A UR 52 Copy Ell Data COnGecom HT 52 CODY GM tia oi 52 Gopy Graph Advanced smart a 52 Sopy Z Data Z2SIMPIWIN besooo tliicdd 52 alo PP m 26 euge A o A 34 A ON 72 ON A A PP a ate estore entation eat acinar eit ae 72 CONCENTAUO qu I A 76 CUNO oett EM UE LI EM Id ee ets ICM 74 O NERA NM AME ERE IDCM pP NE 76 A a Hn 73 BrrmSereM E M S 36 Data 1 OIC soetdio nw bros o S DINNER OI U e o III 28 32 DEN SI NERONE ted T 21 99 EO LADE SA A o DIU II 5 Electrode SUnacE FS as i a O 43 ES OLIV AIG FG NCIC burro cisentd San bans basando Sass bus basada bus bue buscada buda bu basas Sia buda brazo basas AD Cad ia dad cad as 99 Ml eii 65 Finite length linear diffusion M ooccconcccncconcconnconcconnconnnonnnonnnoncnnnnonnnnonnnonononnnonnnonnnannnnnnnos 80 FOUTS TV LN SUOMI ss sess uncut od a tcl mistiaraata seat wetaraietaats E E en sacs ane S alatutd dui PE olam eeaamedtas 63 e Sie a at E TT T ne T T UT Tm 81 Graph SNCS d ERROR TR 5
14. 22 co so agr Ss 5 L LILA ZA N o o P cycle number i 1000 40000 100000 freqiHz log spacing SPEIS mpr D co 3 N co a o 4 cycle number Oo 2 n 100 1 000 10 000 100000 Y freqiHz log spacing Fig 42 Bode diagram displayed in the 3D representation Once on the 3D representation it is possible to reach the 3D menu by right clicking on the graph Fig 43 Thanks to this menu it is possible to come back to the 2D representation or to display simultaneously 2D and 3D graphs As for the 2D representation it is possible to copy and print the graph as explained in section 3 2 7 page 51 The Graph properties menu for the 3D representation is the same that the Graph properties menu for the 2D graph and this menu is detailed in the following paragraph Ol v 3D 20 30 Copy d amp P Print Ctrl P Graph Properties Fig 43 3D menu Note that to display a data file with the 3D function the number of points should be inferior to 15000 points 40 EC Lab Express Software User s Manual 3 2 4 Graph properties On the graphic window right click on the mouse and select Graph properties This Graph properties window Is divided into 5 themes Traces Axes Units Graph and Options Each of them allows the user to define properties of the graphic display Graph properties The Traces window allows the user to define all the Predefined Graph Style properties of the selected C Custom
15. C Every 0 001 V Close Fig 70 Subtract files window EC Lab Express Software User s Manual lt l gt vs Ewe z CV_1inA_10Vs_solution mpr cycle 2 z CV_inA_10Vs background mpr cycle 2 z CV_1inA_10Vs_solution z_CV_1nA_10Vs_background mpp lt l gt nA O I aS Nem ars e ME 0 Ewe V vs SCE AA ee A a 0 2 0 4 Fig 71 Use of the Subtract Files tool on the blue and red curves The Obtained curve is given in green color 3 3 2 6 Integral In the same way as the Linear Fit method the user can selected trace between two makers On the graphic display select the Integral with the Integral button 2 in the math section and with the mouse right click on the data points where the fit will be performed The Integral analysis window is displayed Click on Calculate Two markers delimit the integrated trace The markers can be moved to adjust the selected fit zone The fit is updated automatically The integral is calculated according to X axis A pinkish area is displayed on the integrated zone The units of the integral fit result depend on the plotted data points For a cyclic voltammetry the units will be A V The results can be copied to the clipboard to be pasted in the print window comment zone or a text file They can also be saved in a text file calculate the integral value of a Integral Selection Trace leo vs Ewe From Point 5887 AS 83b V ab 0
16. Calculate Copy I Save 0 5 0 05 EwelV 7 Fig 90 CV simulation with two electron transfer It is also possible to display the interfacial concentration of the electroactive species involved in the mechanism The resulting curve can be saved as mpr file 74 EC Lab Express Software User s Manual File Selection Wanablez CAU zer ADocumentsEC Lab Express Data sim mpr Representation Custom Pa timers E we m cycle number LAZmol L 1 CB mol L 1 CC mol L 1 E3ESIESESEEREESE E FEES E ss ss 3 3 3 3 Same selection for all files Hide Additional Variables keep previous axes process keep previous zoom Fig 91 Variable selection window to display concentrations CVsim mpr vs Ewe CA vs Ewe CBvs Ewe CCvs Ewe 14 10 000 12 5 000 10 0 8 8 lt 3 E 5000 2 6 10 000 4 15 000 2 20 000 0 Ewe V T Fig 92 Interfacial concentration variation versus electrode potential 19 EC Lab Express Software User s Manual Several examples are available in the CVsim window To display an example one has to click on the select button on the top of the CVsim menu Then CVsim examples window appears to select the mechanism of interest CVsim Examples E DLSI Mechanism EE El DLSI Rohm FelIII Fell El El DLSI Rohm Cdl Reaction Reduction A ze lt gt B 1 ED 20 2V ko 0 1cm s 1 af 20 5 9 EEE DLSI Species 1
17. Electrode surface area geometric surface of the working electrode It is a value that is used to represent current density or charge density File Load the load function allows the user to load a data file mpr a setting file mps a linked experiment setting file mpls or a report file Filter this filler can be used as off line filter many times after the experiment but also just after the recording of the data by ticking a box on the Advanced Setting window Many methods and windows are available Fit graphic tool used to determine kinetic or experimental parameters Fourier Transform tool used to apply a Fourier transform to recorded data many windows are available General Settings window in EC Lab Express in which the user can set all parameters about the electrode Graph Type tab tab which contains 3 themes graph properties representation and techniques and allows to define the graph parameters and to attribute to each technique a special representation Group option used in a multichannel mode to start at the same time different experiments on the selected channels Hint small box appearing under the box pointed by the mouse It indicates the min and the max values accepted in the box range current range used in the experiment It is related to the current resolution Impedance defined by the ratio E I Info tab in the graphic display that give the number of points and the size of the raw data file
18. Express Software User s Manual Ato Pf p 1 9 ay exp 2i f At k 1 In the Parameters part of the window Fig 84 two choices are available Doing the analysis on the cycle displayed on the graph selecting Current cycle s Doing the analysis on all the cycles selecting All cycle s In this case the analysis will be performed in all the cycles in a sequential way the result of each cycle will be saved automatically Before to perform the analysis it is possible to remove the trend of the signal potential and current by using a linear fit or a second order polynomial fit A description of the analysis windows that can be used is detailed in the section Fourier transform 3 3 2 7 page 63 Example of electrochemical Noise Analysis is given in Fig 132 References Bertocci U Frydman J Gabrielli C Huet F and Keddam M Journal of Electrochemical Society 145 1998 2780 2786 Mansfeld F Sun Z and Hsu C H Electrochim Acta 46 2001 3651 3664 Lee C C and Mansfeld F Corrosion Science 40 issue 6 1998 959 962 CA R 100mHz 01 mpr Mnise Analysis Ewe vs time vs time 3 A A A A Selection f f A f Trace vs time 0 1 f EwelV Ez Cycle AM From point 3 A Bs i i i i i i ye 58 79e 6 m s To paint 113 A 111 4 s ae 0 019 42 m Total points 111 Parameters Select all chcle s CA R 100mHz 01 ena psd mp
19. Istack A lEstack magnitude of voltage fuel cell stack Estack V I stack Magnitude of the current fuel cell stack I stack A Range current range Range 2 3 3 Data recording In all the technique sequences the user is able to define different modes for data recording The main mode corresponds to decide the recording resolution of the measured variable potential current with at least a recording every predetermined time interval dt from 0 1 to 9999 s This last condition gives a minimum of recorded points in the case where the variation of the observed variable is less than the chosen resolution for a long period of time potential close to equilibrium process leading to a potential plateau etc For open circuit voltage OCV period nothing is controlled and the potential is recorded The recording conditions for OCV periods are in time variation dt and or in potential variation dE For techniques with potential control two different recording conditions are available on a time variation and or an instantaneous current variation dl 31 EC Lab Express Software User s Manual For techniques with current control the recording conditions are on a time variation dt and or potential variation dE Recording conditions are described in the application section for each technique If the user wants to force a periodic recording in time he has to set a large value in the recording resolution of the variab
20. Kramers Kronig transformation can also be verified in an admittance plot If we consider the previous data file ZPOT Fe Basique mpr the Kramers Kronig transformation applied to the whole point series gives the following results 96 EC Lab Express Software User s Manual POT Fe basique 1 mpr Im Z vs frea log spacing SPOT Fe basique 1 kk mpp Im z vs freg log spacing SPOT Fe basique 1 kk mpp Deka Im di vs freg log spacing Y 20 40 50 50 Imi Z VO hm 96 412 Mu eae d LS e a 120 mibi 0 1 1 10 100 1 000 10 000 100 000 lfreq Hz log spacing Fig 119 Result of the Kramers Kronig criterion applied to the data points with the experimental Im Z part the calculated one and the relative error One can see that the Kramers Kronig criterion is not applicable to this system because in the low frequency range the impedance doesn t tend towards O For the high frequency range the imaginary parts tend to 0 So the precision is not significant Kramers Eronig Results zh Rele 3 36 lt A Imi 24 3b 4 lt A Ele 3 84 zx A Phasel z 24 ar The results of this test are displayed as an averaged relative error for each parameter Re Im Z and phase References H W Bode Networks Analysis and feedback Amplifier design Van Nostrand New York 1945 R L Van Meirhaeghe E C Dutoit F Cardon and W P Gomes Electrochim Acta 21 1976 39 D D MacDona
21. Photovoltaic Fuel Cells section SS including Photovoltaic Analysis o Corrosion analysis tools section including Tafel Fit Rp Fit Corr Sim VASP Fit CASP Fit Electrochemical Noise Analysis Fit The user can select the cycle to display with the Show option v Show 4 1 gt This graph window can be maximized using the top right corner button m Note that the user can also have all the point coordinates by hovering the mouse over a point while holding the SHIFT key of the keyboard A comment box is displayed 3 1 1 The graphic window right click menu The graphic menu window can be obtained by clicking on the right button of the mouse 34 EC Lab Express Software User s Manual Flot b 3D Comments d Hide OCW Points Load Files Alto 55 add Files A Remove Trace AlE R E Save Data File As Ctrles LOG History Y Edit surface and Mass dnd Active Trace d Ea Add Graph Copy d Print Ctrl F v Graph Properties AlE P Fig 36 Mouse right click on the graphic window On this right click several frames are displayed x 1 for plot and Graph type selection m 2 for the addition of comments on the graph with the possibility to Add and delete a comment zone and to paste a comment from the clipboard m 3 for showing or hiding OCV points and artefact data points that the user wants to remove before an analysis or a print a 4 for file selection with Load files Ad
22. Preview a Copy EIT Data Condecan Fig 57 Copy option and copy graph advanced menu 91 EC Lab Express Software User s Manual 3 2 7 1 Standard copy options On the top of the menu two standard options either copy the graph or copy the data The Copy Graph option will copy the graph in the clipboard as displayed on the computer screen in an enhanced metafile format emf The user can paste the file in the software he wants The Copy Data option will copy the data selected on the graph if data points are selected or data as they are displayed on the screen in a text format in two columns with X and Y only Data can be directly pasted into spreadsheet software 3 2 7 2 Advanced copy options Three advanced copy options are also available 3 The Copy Graph Advanced option offers eight different file formats for the graph copied Bitmap enhanced metafile PostScript SVG PCX PNG GIF and JPEG with a possibility to choose the size of the picture in pixels The Copy Z Data ZSimpWin option is a gateway to ZSimpWin software This copy option is only available with impedance data files Three data rows frequency Re Z and Im Z are copied in the ZSimpWin format and can be pasted by the user in this software If the impedance experiment is repeated several times only the displayed cycle is copied The Copy EIT Data Condecon option is a gateway to Condecon s
23. REF in V Ece V Mode Intentio Potentio Relax State byte bits n 1 and 2 mode 30 EC Lab Express Software User s Manual variable description Variable name forward in pulsed techniques current measured at the end of the I forward A pulse reverse in pulsed techniques current measured on the reverse part I reverse A delta difference between forward and reverse delta A E step in sweep pulsed techniques potential step increment E step V variable description Variable name Cycle number cycle number Power in CPW calculated by E P W Energy in CPW calculated by E t Energy W h Rp polarization resistance in corrosimetry RO Icon Corrosion current resulting from Rp calculation laced A Ecorr corrosion potential resulting from R calculation Eso V C Inverse of square capacitance for Mott Schottky plot C F C Inverse of capacitance for Mott Schottky plot C F variable description Variable name Frequency in Hz freq Hz E4 module of Ewe V Ewel V I module of in A N A Phase of Z in degrees Phase Z deg Z module of Z in Q IZQ Re Z real part of Z in Q Re Z O Im Z imaginary part of Z in Q Im Z Q Re Z real part of Z in Q Re Zoe O Im Zee imaginary part of Z in Q IM Loe O lt Eye gt averaged Ewe value for each frequency lt Ewe gt V lt l gt averaged value for each frequency lt l gt A Voltage fuel cell stack Estack V Current fuel cell stack
24. Tafel parameters In this technique a potential sinusoidal wave is applied around the corrosion potential Ecorr with N amplitudes increasing from Vamin to Vamax For each amplitude the polarization resistance Rp is determined and Rp versus applied potential amplitude is plotted For a negligible Ohmic drop Re 0 the Rp parameter can be expressed by the relation below 5 6 1 pit b Lor 2 E a zh Rp 27 kt k 1 The VASP Fit allows user to fit data from VASP VASP Fit measurements by clicking on the VASP Fit button in the Sea corrosion section of the analysis tools menu Trace Rip vs sin ampl The software deduces the current corrosion leor and the Tafel From point parameters p4 and p A 4 3 4e 3 my The results can be copied to the clipboard to be pasted in the Je 1 3 3 Ohm To point 14 print window comment zone or a text file They can also be i i e 0 1 my saved in a text file 258 4 Ohm The Fit accuracy can be estimated with the y parameter Vibe nane 20 according the following equation IE 1 N 2 Y ar 2 Gs X aici 1 E EUH pan piel P E ione Ys 5 K Darowicki Corrosion Science Vol 37 n 913 925 tao 2 Kt HD 1995 Use B and B 6 J P Diard B Le Gorrec C Montella Comments Corrosion jJ Use b and be Science 40 495 1998 x WVASP 01 mpr WASP4 01 VASPfit mpp 2 000 1500 lterations xxx 1 000 Calculate Lopy Save Close Rp Ohm
25. an existing file the user can also click on the B Load Settings in the file menu and then select a mpr raw file corresponding to the desired technique and click OK 2 2 4 Parameter Settings description When a technique is selected the parameter frame displays the technique as boxes to complete 25 EC Lab Express Software User s Manual Note Most of the techniques use sequences D that can be added up to 100 Parameters Description Apply Ey i000 000 V Vs Eref for t 0 500 000 sec sf Record every dl 10 1 00 lA or dk 10 010 00 3 Repeat n 0 times Range 5 Auto range E Range GG 25V Bandwidth 8 Update Fig 31 Chronoamperometry parameters EC Lab Express software techniques are made of sequences in which the potential to apply and the duration can be changed Other conditions can be added such as recording conditions repeat options and potentiostat parameters These parameters are the same for all the sequences To add sequences in the technique click on the button Tabs with number are added The recording conditions are the same for all sequences and are defined either in time or in current when the control is in potential or in potential when the control is in current The instrument hardware parameters are defined as follows Range The current range has to be determined by the user When the current is measured the measured values can be twice gre
26. and of the changes done during cycling 2 2 06 Running synchronized experiment This option is available in the advanced interface It is possible to synchronize several experiments together on different channels of an instrument for example in a bipotentiostat experiment The setup procedure is the following Create several experiments one for each channel and select the related device for each of them Automatically when more than one experiment is set the software will offer the possibility to synchronize both experiments 28 EC Lab Express Software User s Manual 4 EC Lab Express V5 50 File Config Help d Device Channel Ewe Current Time Ece 0506V lrange 10 mA Connection Standard DA Freq 100 000 Hz Rcomp 0 2 E a 0 608 V 0 000 A Os bu gt PAT QAR E N Parameters Description 5 6 Experimentl wk VSP 300 0001 V Vs Techniques Set Ewe 10 000 000 s Eref 9 Lv Wait fort 1 000000 2 G Experiment3 E E VSP 300 0001 Record every dl f 000 S Techniques or dt 0 100 00 s v 3 Scan from fj 100 000 KHz v to ff foo Ha vw with Ny Bl points points spacing Logarithmic sinus amplitude V4 noo mV wait for pu 0 10 period s before each frequency average Na f measure s drift correction v Range 6 Auto range Bandwidth G8 4 0 Click on the Run button of t
27. at regular intervals Fluctuations in current and potential are called current and potential noise Three methods are available to calculate the electrochemical noise Standard deviation With the two standard deviation values current and potential it is possible to apply the Ohm s law relationship and to obtain the parameter Rn A ve with Ol cEg e And o obtained with the formula c E Dx x xp where x x is the average PSD with DFT It is also possible to calculate the standard deviation from the Power Spectral Density PSD indeed according to the Parseval theorem it is possible to link variance c and Power Spectral Density of the x variable P f ena Note that P f x t X f where X f is the Fourier transform of PSD with MEM The Maximum Entropy Method MEM is an estimation of the PSD suggested by information theory Calculation of the PSD can be done with the following relationship Moise Analysis Selection Trace Cycle From point wa Es To paint E E yz time 111 4 x Wc 0 019 42 m Total points 111 Parameters Select eyelets Ewe trend removal None trend removal Method PSD with DFT window Rectangle REM order Results Ewe average 2 445e 3 average O 4 73 5e 6 4 O E we 2 039e 3 4 Ex l 0 402 6e 6 4 An 5 065 Ohm 7 Fig 131 Electrochemical Noise Analysis window 107 Close EC Lab
28. combination of randomize followed by Simplex fitting combination of randomize followed by Levenberg Marquarat fitting 82 EC Lab Express Software User s Manual Fit se Method Randomize Simplex yt Randomize Simplex Randomize Levenberg Marquardt stop randomize on h 0000 iterations ae Bs arquardi Weight ate i mins Iterations www Cycle sex Fig 102 Fitting method selection lf ALL cycles are selected for the fit the user will have the possibility of selecting the randomization on the first cycle only or on every cycle For both randomisation and fitting the user can define the number of iterations and for the fit he can also select a relative error Another option Weight is available with two choices either 1 or Z resulting in a different weight of data points at high and low frequencies During the fitting process the iteration number is displayed at the bottom of the window To start the operation click on Minimize 3 3 4 1 12 Application Considering the data file PEIS Fe basique mpr below The following result may be obtained using the Randomize Simplex option with the default parameter values Selection Results Equivalent circuit R1 02 R24w2 ims ies Beis param sel sign value ZPO e jag 1 Inm Pe 47 57 Dhm 0 784 3 iml 17 096 F s a 1 0 150 9e 6 0 885 0 5131 70 94 Ohm 0 746 3 85 33 Ohm s 1 2 0 109e 3 m F T e Fit J sol Select current
29. from the PC the experiments are entirely controlled by the instrument s on board firmware Data are temporarily buffered in the instrument and regularly transferred to the PC which is used for data storage on line visualization and off line data analysis and display This architecture ensures very safe operation since a shutdown of the monitoring PC does not affect the experiments in progress The computer can be connected to the instrument through an Ethernet connection or with an USB connection The application software package provides useful protocols for general electrochemistry corrosion electroanalysis and fuel cell testing otandard graphic functions such as re scaling zoom linear and log scales are available The user can also overlay curves and make various data analyses peak and wave analysis Tafel Ry linear fits An EIS data analysis tool is included in the package for full treatment of data recorded The aim of this manual is to guide the user in EC Lab Express software discovery It is assumed that the user is familiar with Microsoft Windows and knows how to use the mouse and keyboard to access the drop down menus WHEN A USER RECEIVES A NEW UNIT FROM THE FACTORY THE SOFTWARE AND FIRMWARE ARE INSTALLED AND UPGRADED THE INSTRUMENT IS READY TO BE USED IT DOES NOT NEED TO BE UPGRADED WE ADVISE THE USERS TO READ AT LEAST THE FIRST THREE CHAPTERS BEFORE STARTING AN EXPERIMENT EC Lab Express Software User s Manual
30. in the low frequency range 3 3 4 1 9 Gerischer element G The Gerischer circuit element arises when an electroactive species undergoes a chemical reaction in the bulk Description 3erischer Ir j Impedance Elec A 11 2x T3f MNyquist Diagram Im z vs Rel N Fig 101 Gerischer Diffusion element EC Lab Express Software User s Manual Note This list can be continued by new electric elements whenever our customers define a significant one 3 3 4 1 10 Z Fit selection window The Z Fit selection window enables the user to edit and create a circuit For more details about the circuit editing window please refer to the previous section In the equivalent circuit frame the table presents each parameter in raw and for each of them offers the ability to select it in order to be adjusted during the fitting the ability to define the sign of the value between by double clicking in the box the unit and the standard deviation calculated when the Levenberg Marquardt algorithm is used When the selection box is not ticked the parameter value set in the cell will be considered as the correct value It will not be modified during the minimization The Calculate button will calculate and plot the data points for the parameter values set in the table without to randomizing or fitting 3 3 4 1 11 Fitting methods The Zfit tool can perform successive fits with the same model on successive curves in the same data fi
31. of parts could expose live conductors Only qualified personnel who should refer to the relevant maintenance documentation must do adjustments maintenance or repair EQUIPMENT MODIFICATION To avoid introducing safety hazards never install non standard parts in the equipment or make any unauthorised modification To maintain safety always return the equipment to Bio Logic SAS for service and repair GUARANTEE Guarantee and liability claims in the event of injury or material damage are excluded when they are the result of one of the following Improper use of the device Improper installation operation or maintenance of the device Operating the device when the safety and protective devices are defective and or inoperable Non observance of the instructions in the manual with regard to transport storage installation Unauthorized structural alterations to the device Unauthorized modifications to the system settings Inadequate monitoring of device components subject to wear Improperly executed and unauthorized repairs Unauthorized opening of the device or its components Catastrophic events due to the effect of foreign bodies EC Lab Express Software User s Manual IN CASE OF PROBLEM Information on your hardware and software configuration is necessary to analyze and finally solve the problem you encounter If you have any questions or if any problem occurs that is not mentioned in this docume
32. possible to display the two Y axes on the same graph or to separate them selecting the Separate traces box Graph Representations Ewe vs y m Bode Impedance Ewe vs t Ewe vs lve Ewe delta vs Estep Logli vs Ewe Representation Advanced YT asis Ye anis Ewe vs Loalll 4 0 hm Phase z deg O vs t log Y Hp vz t Bode Impedance _ separate traces Nuguist Impedance Black Impedance El vs t s ais Matt Schattkuy req Hz Bode Admittance Nyquist Admittance log spacing Black Admittance Mame Representation Advanced YT axis Ye as 10 hm Fhase z deq lag r1 Lo ui S Bis req Hz log spacing Fig 50 Graph representations window 45 EC Lab Express Software User s Manual 3 2 5 1 Axis processing As shown previously it is possible to apply a mathematical function on each axis By default standard functions such as log X X X 1 X are proposed Fig 51 Nevertheless it is possible for the user to define his own processing function using the Custom menu Then in the window given Fig 51 the user can define an operation in the Variable box in this example it is the et box Mathematical functions are available ticking the box more Graph Representations Black Impedance Black Impedance odd D 7 vs t Mott Schottky Bode Admittance Nyquist Admittance Black Admittance E Phase z error xvzl MH ame YT axis Wm Ece vs t Ewe Ece vs
33. t Bade Al cycle vs time freg vs time IE wel vs freq Il vs freq E wel I vs freq Calculator Mathematical expression Operands Variable NOOO Wr oo Hane Dios Oteo menm Representation Advanced Ex cu e freg Hz Jog spacing l expt sqrt sqrt abst roundi trunci Int log 10 loghi X sini cost Fani arcsint arccost arcani sinh cosht tanh arcsinhi arccosht arckanht PI degtoradt radtodegt x Y 2 AMIS Phase z deg v custom exponential of a number square of a number square root of a number absolute value round to the nearest integer Eruncates a real number bo an integer natural logarithm logarithm base 10 logarithm For a specified base Logh Base X sine of an angle in rad cosine of an angle in rad tangent of an angle in rad inverse sine in rad inverse cosine in rad inverse Fangent in rad hyperbolic sine of an angle in rad hyperbolic sine of an angle in rad hyperbolic tangent of an angle in rad inverse hyperbolic sine in rad inverse hyperbolic cosine in rad inverse hyperbolic tangent in rad 3 141589265358979323855 conversion of degrees to radians conversion of rad to degrees Fig 51 Axis processing window and available mathematical functions 46 EC Lab Express Software User s Manual 3 2 5 2 How to create your own graph representation for a specific technique To facilit
34. the button the user can either add a new technique to the existing experiment or add a new experiment labelled experiment 2 to the existing experiment experiment 1 The button will remove the selected technique or the selected experiment The two arrows buttons are used to move up and move down techniques in the list 2 2 2 2 1 Cell description part In this part you can either fill blank boxes entering comments and values or load them from a mps setting file or a mpr raw file using Load Setting on the main menu This window allows the user to e add information about the electrochemical cell material initial state electrolyte and comments e set the electrode surface area the characteristic mass the equivalent weight and the reference electrode used in the experiment when defined these parameters are automatically used to calculate the corrosion rate after a Tafel Fit They are also used for density plot 21 EC Lab Express Software User s Manual Cell Properties s Cell description Electrode material Initial state Electrobte Commentz Cell characteristics Electrode surface area 0 001 Characteristic mass 0 001 Reference electrode unspecified e Offset potential vs NHE 0 000 w Fig 27 Cell properties window 2 2 2 3 Parameters frame This frame contains the parameters to be adjusted for the experiment To display parameters for each technique the user has to select th
35. through the counter electrode in standard mode e GND BLACK Ground For SP 300 technology SP 200 SP 300 SP 240 VSP 300 e S1 RED Sense 1 for the control and measurement of the Working electrode potential e S2 WHITE Sense 2 for the control and measurement of the Reference electrode potential e S3 BLUE Sense 3 for the control and measurement of the Counter electrode potential e P1 RED Power 1 for the current control and measurement flowing through the Working electrode e P2 BLUE Power 2 for the current control and measurement flowing through the Counter electrode e GND BLACK Ground 2 1 3 1 1 Standard mode This mode of connexion is the one used for most of the electrochemical applications In the standard configuration a measurement channel has 5 lead connections to the electrochemical cell 4 are used in the cell control loop 2 for the current and 2 for the potential while the 5 lead permits simultaneous recording of a supplementary cell potential Cell Connector For VMP3 technology select Electrodes connection Standard uds and connect the cell as follows ERI CA2 WE and Ref1 leads to the working RE ref electrode Fre Ref2 lead to the reference electrode s n CA1 CE and Ref3 leads to the counter electrode Fig 10 Standard mode connection for VMP3 technology 11 For SP 300 technology Select Electrodes connection Standard and connect the cell as follows
36. user has to select the analysis and then select the data points to fit or select the data points before choosing the fit To select the peak analysis click on the button in the graphic tool bar or select peak analysis in the right click analysis menu When this first part is done the peak analysis consists of two steps First the user must choose the baseline and second click on calculate to have the results 3 3 3 1 1 Baseline selection 67 EC Lab Express Software User s Manual When selected the peak analysis window is displayed with two tabs Baseline and Peak In the Baseline tab the user must select the baseline type Three selections are available no baseline linear baseline and polynomial baseline If the user selects NO the analysis will be performed according to the abscissa axis lf the user select LINEAR three different baselines can be set A manual mode with markers locked on the curve or regression mode with a linear regression made on the capacitive part of the curve before the peak or in a free mode two cursors defining a straight line unlocked to the curve If the user selects Polynomial type a polynomial baseline is plotted and adjusted to the data points in the following way two data zones are used for the polynomial fit at the beginning and at the end of the selected zone twenty first points and twenty last points of the selected data zone The selected data zone and the polynomial fit are limited by t
37. 0 EEE DLSI Rohm Cdl CAO 0 01 mol L 1 11 EEE DLSI Fe IID Fe ID Fe D Fe DA 10e 6 cm2 s 1 12 EEEE DLSI 5e6 0m2 5 1 13 EEEEE DLSI EZ 14 EEE DLSI e 111 Reaction 15 EEE DLSI e 123 Reduction B ze lt gt C z 1 E0 0 3 V k 2 0 1cm s 1 af 20 5 Title Species EE DLSI Rahm Cdl u n 3e 6 cm2 s 1 Comments Geometry Linear Semi nfinite Radius 0 1 cm Surface 0 031 42 cm2 Experimental Conditions Temperature 25 deg RB hm 30 Thm Fig 93 CVsim examples window 15 examples are available in this window The corresponding parameters are displayed on the right column When clicking the Add button the corresponding curve is displayed 3 3 4 Electrochemical Impedance Spectroscopy section 3 3 4 1 ZFit EIS analysis tools are powerful tools to determine the kinetic of an electrochemical reaction and values of the kinetic parameters Electrochemical impedance data analysis allows the user to propose an electrochemical reaction mechanism To be interpreted electrochemical impedance data points need a comparison with an electrical circuit simulating the electron and electroactive species at the electrode surface solution interface Indeed this process is assumed to be represented by an equivalent circuit of resistors capacitors inductors and diffusion elements The total current is in most cases the sum of distinct contributions from the faradic process and doubl
38. 161 48 3 m To Paint b z AS 0 166 V as 2 215e 3 m Total paints 135 Results Integral 3 531 14e 3 m Fig 72 Integral window 61 62 lt l gt pA 20 25 30 EC Lab Express Software User s Manua CV platinum 10 cycles n mpp al vs Ewe cycle 1 Integral Selection Trace Fram paint A ke To point A Te l gt vs Ewe 106 0 591 5 0 86 pA 209 0 076 49 3 211 p Total points 104 Results Integral 0 0 5 EwelV vs SCE Fig 73 Integral determination on a trace 1 950 23 p V EC Lab Express Software User s Manual 3 3 2 Fourier transform Fourier Transform FT Selection This mathematical tool i allows the user to calculate the Trace TUN discrete Fourier transform DFT which is a specific kind of From point 44 Fourier Transform It transforms one function into another M Xie which is called the frequency domain representation or Ys 8 28 3 m simply the DFT of the original function But the DFT Topoint 80 requires a discrete input function and whose non zero a fas values have a limited duration Po gode mA Total ports 37 The calculation is done following the formula zo Testing Parameters 1 N 1 XA T ip x exp 2izft with window X ae y Xy X ty x kdt Frequency range e Auto Freg Min Hz When a data point zone is selected click on Calculate Freq Mas 50 Hz Once the zone selected it is possible
39. 2 EC Lab Express software settings 2 1 Starting the Program Double click on the EC Lab Express icon on the desktop The EC Lab Express software s Device window will be displayed EC Lab Express V5 50 NES Fos mcm File Config Help Channel Ewe Current Time Ece 0 674 mV lrange 10 mA Connection Standard a Freq 100 000 Hz Rcomp 0 Q v 0 109mV 0 000A Os Buffer Experiment ERE RA 4 G Experimentl gt wh VSP 300 0001 D Ondine 4 Techniques m cem L2 OV Comm Device amp ddress Serial number Ethernet SP 300 192 109 209 215 0154 Ethernet VMP4 132 103 208 223 Bogdan Ethernet VMP3 192 109 209 235 0230 Ethernet CLB 500 192 109 209 238 1005 if 192 109 209 239 Lj Custom IP address 192 168 0 1 Refresh Modify Off line virtual potensiostat MP3 Options Cell Connection Electrodes Connection Standard P1 al WE Channel G Grounded v E T go We Filtering G 50 kHz E ce ULC measurement G Highspeedscan v ES CE Apply Configuration i Fig 1 Device EC Lab Express window 2 1 1 Connection with the instrument To see all the instruments present in the network click on Refresh of course only one is displayed in case of direct connection The automatic search frame shows the name of the instruments detected with their serial numbers A Mac address is given to each instrument at the factory The Mac address
40. 5Vs sans compensation 1nA mpr cycle 3 UME_5Vs_avec compensation 1nA mpr cycle 3 2 4 M idi gt L ALT N 0 l l o2 o 04 Ewe V vs SCE Fig 16 CV carried out with Ultra Microelectrode of 10 um in a solution of ferrocene in EtOH with TBAP as supporting salt The range of current is 1 nA and scan rate is 5V s The value of current scan where the correction must be applied depends on the intrinsic characteristics of the cell type of electrode distance between electrodes A correction is offered in the Hardware configuration window in the menu ULC measurement This option is automatically selected when Ultra Low current option is connected ULC measurement 3 High speed scan Standard High speed scan Note that if the Ultra Low Current option box is selected the data may be noisier especially for ranges below 1 nA see figure below It is possible to reduce the noise by filter the data available in the Math menu of the Analysis menu 15 EC Lab Express Software User s Manual lt l gt vs Ewe OV THF Fc 1Vs 100pA avec toutes corrections mpr cycle 3 CV_THF_Fc_1Vs_100pA_sans correction mpr cycle 2 Ewe V Fig 17 CV carried out with Ultra Microelectrode of 10 um in a solution of ferrocene in THF without any supporting salt The range of current is 100 pA and scan rate is 1V s 2 1 4 Recording options This part of the device fra
41. 9 ig He 61 PP A o RP a a a a a ia 58 AULT 7A AYA Fe D REORUM 57 ETO MEM MEE MM 36 AP er A 98 EC Lab Express Software User s Manual A PET HT IO Seatac aac weet m 44 Graph DIO DCINCS NE TTE ELDER 41 AXIS NO Em 42 A E EM EM 44 UN A emer enc q ro eee eee ae 44 Bro fe O 41 SAA A A A RACE E E UN RACE N E UN RACE RUN NA E E AES 43 Caraphbre preset QUOI S aceite testa udis dtt ads cio eact ia 45 Graph hepresentatlOliS tdt S erai dea bmi ld did Seed asta 33 allg er e C Y 27 Impedance A NS A UN 76 Mpo taata MM a o e pel E a o e o e Sees 18 oo E 78 io V 61 Bild A AA y A EET EE 58 car Interpol OM is 60 LOG NISTON aia T Um m M Cm 50 MEMO SIZO OEC OE EO ED OD a ala taa did 32 MIMAX dec 57 Mott Schottky A ER IE E EN MEM ss 94 mo e gq T T E E 93 PTE OTS iii 92 MOUSSE SCHO uestes ecg a see tested ne set O ted ees t E A E D E 34 M ltiexbonenualoltri Elt paria 66 C DTOMS WINGOW ME ENT ica 19 A O LE MM M LM IDE 25 Peak analysis nij rr 69 OME COOOIN Alina 34 PON Seleollolasseondastpmttdie gunt o io P un DU WEITAR e PO 34 FOlAIZ AMON Resistance 101 Potential COMMON lCSOIUMON et tL t mE 26 Mibi nutu ect LM C M LL M LE M Lu Ce 52 o bees darn Seed Sac beet ace et TER 85 Record CONAN Susi a TD UE a 31 RETET
42. C Lab Express Software User s Manual Ewe vs log lt I gt Ewe vs log sls LP iron corrosion_tafel mpp 4 log I7 mA Fig 123 Tafel Fit on the Ewe vs log l graph 3 3 5 2 R Fit For E sufficiently close to Eco it is possible to simplify the Stern and Geary equation such as Pa E In10 Ps E o T D D This equation is commonly presented with E as a function of l I Bab du I uU P 1n10 When expressed this way it is easy to see that E E for 0 The slope of this equation is termed the polarization resistance because it has the unit of a resistance and is commonly abbreviated R Polarization resistance R Oo PB vor IT B B InlO 101 EC Lab Express Software User s Manual For the Rp Fit the user has to select the data points and then fit with the R fit button as described before Then click on Calculate The software will automatically find a potential value E on the curve for 0 Two circle markers are set in a x25 mV potential range around E This range and p4 and p values used for the fit are defined in the Parameters frame The R Fit calculates the polarization resistance Ap and the open circuit potential Eco by a linear regression around E 25 mV on an vs E plot All the data points in the potential range are used for the linear regression R is given by the inverse of the linear fit slope and Eor by the potential value cal
43. EC Lab Express Software User s Manual Version 5 5x November 2011 BioLogic Science Instruments N EC Lab Express Software User s Manual Equipment installation WARNING The instrument is safely grounded to the Earth through the protective conductor of the AC power cable Use only the power cord supplied with the instrument and designed for the good current rating 10 Amax and be sure to connect it to a power source provided with protective earth contact Any interruption of the protective earth grounding conductor outside the instrument could result in personal injury Please consult the installation manual for details on the installation of the instrument General description The equipment described in this manual has been designed in accordance with EN61010 and EN61326 and has been supplied in a safe condition The equipment is intended for electrical measurements only It should be used for no other purpose Intended use of the equipment This equipment is an electrical laboratory equipment intended for professional and intended to be used in laboratories commercial and light industrial environments Instrumentation and accessories shall not be connected to humans Instructions for use To avoid injury to an operator the safety precautions given below and throughout the manual must be strictly adhered to whenever the equipment is operated Only advanced user can use the instrument Bio Logic SAS
44. Fig 120 warning message to switch the graph representation Fig 121 Tafel Fit window Answer Yes to the previous message The fit can be minimized with simplex method The results can be copied to the clipboard to be pasted in the print window comment zone or a text file They can also be saved in a text file Note One can manually select the log versus E representation In graph properties axis axis processing select log 1 for Y1 The equivalent weight density and surface area used for the corrosion rate calculation can be defined before the beginning of the experiment in the Cell characteristics window The Tafel graph Fig 122 is displayed in log vs Ewe Two linear regressions are automatically made using the least square method Each linear fit is limited with two circle markers that can be moved 99 EC Lab Express Software User s Manual log lt I gt vs Ewe logt I j vs Ewe LP 01 tafel mpp 2 9 log lt I gt pA 35 45 EwelV Fig 122 Tafel graph Results of the Tafel Fit are calculated whenever a marker is moved The default positions of the markers are 80 mV and 200 mV around E o The software deduces the open circuit potential Eo from the linear regressions intersection the corrosion current value leor and the Tafel constants Ba and e The Fit accuracy can be estimated with the y The Tafel Fit also works with the plot Ewe vs log I 100 E
45. Graph Style traces Select the trace Traces Mame yOU wish to modify in the Axes 1 asique mpi Trace Name frame Units The available trace Graph properties are the plot style Line Style Line Markers Markers Pot Lines BI Undersarnping Posed line properties solid ash color and size the marker properties Maker X B Ene 2 i rectangle circle color and size Options An undersampling option LJ Hide DCV Points is available iiie lies are Draw only li 10000 ints Note Ads o e ae plotted not with markers parameters for all Undersample traces over 25000 ponts graphic windows Options Fig 44 Traces window In the Options window it is possible to choose to hide OCV point or to draw only lines over a number of points or to undersample traces over a number of points or to scroll graph over a number of point Note that the two last possibilities should be the same for all the traces The undersampling traces over and the scroll graph over are incompatible options The user must choose one of the two options Note When several traces are plotted on the same graph the user can change the active trace with a left click on the desired trace when the mouse becomes a hand with a pointed finger It is also possible to select between four styles already defined Line style only blue solid line Line Markers style blue line circle markers XY prop style blue line circle markers a
46. Im z 35 Delta I Delta Phase 14 lt LI LI LI LI d E LI LI L JEJE JESIE TE TE TE TE MSIETJETJETETE TE TET Same selection for all files Hide Additional Variables Fig 108 Selector for the Zfit mpp file offering the possibility to display the relative errors These additional plots may be very useful in evaluating the acceptability of the equivalent circuit selected and the relevance of the measured data points 3 3 4 2 ZSim In order to define the equivalent circuit after an impedance experiment the user can create an electrical circuit and plot the corresponding Nyquist impedance diagram in a given frequency range To illustrate the capabilities of this tool lets consider and fit the PEIS Fe basique mpr data file below The aim of this section is to define the appropriate circuit for the fit 87 EC Lab Express Software User s Manual The data file that will be used in the simulation section and the fitting section has been made from an iron solution on a gold disc working electrode in a pure diffusion regime in the potentio mode at the open circuit potential Open the PEIS_Fe_basique mpr data file in the File menu Load data file The following window will be displayed ZPOT Fe basique 1 mpr miZ vs Retz Im Z 0 hm 50 100 150 200 Re Z Ohm Fig 109 Experimental Nyquist impedance data file This is a typical impedance data file performed in a pure diffusion reg
47. ZA AC Rda Ri L2 R2 RH1 M1 Rl M2 Rz H1 1 Alt A 3H SZ Ri 4 4 HC SR 5 R1 Q1 R2 C2 R34L4 Ri 44 C 5 R5 H1 1 R2 C3 83 2c mA D gm an Display The Circuits ith d 5 A Element s d Element z All The Circuits Fig 111 ZSim ZFit Circuit Edition window The circuit base contains more than 130 circuits The user can create his circuits to be added in blue to the list The main circuits have been described on the right side of the window circuit scheme faradic impedance equation and impedance Nyquist diagram 3 3 4 2 2 Circuit selection To select a circuit in the list the user can select the displayed circuits according to the number of elements or the specific elements in the circuit number of resistances number of Capacitors 3 3 4 2 3 Description code If the required circuit doesn t appear in the list the user can create it He must write it in the first frame top with several rules 1 For elements in series the used sign is For example for R in series with C the equivalent circuit will be R1 C1 2 For elements in parallel the sign is f For example for R in parallel with C the equivalent circuit will be R1 C1 3 If several elements are in series or parallel with each other then the considered elements must be set between brackets For example for R2 and C2 in series together and in parallel with R1 the equivalent circuit will be R1 R2 C2 4 To w
48. a text file They can also be saved in a text file CV Fe basique 1 mpr Min Max ES zl vs Ewe Selection Trace I vs Ewe From point f z A f y ges e f To point A n its dem Total points Results Minimum point 5157 A 0 092 62 V Ts 224 7 pA Maximum point 2083 X 0 232 5 V Y 203 2 pA lt I gt IpA EwelV vs SCE Selection Trace lo vg Ewe From Point 3551 0 299 4 V 0 088 92 m 5550 0 300 5 Vv 0 089 07 m Total points 000 Results Minimum 8157 0 092 62 Vv D 224 7 m 4087 0 236 8 V 0 207 E m Close Fig 63 Min Max fit window Fig 64 Min Max determination on the graph 57 EC Lab Express Software User s Manual 3 3 2 2 Linear Fit Linear Fit When the zone to fit is selected click on Calculate in c election the linear fit window Fig 65 A straight line is displayed SE Imz vs Retz as a result of the linear regression between two green From Point 27 circles with the least square method fit Fig 66 A 130 5 Ohm Move the circles with the mouse by holding the left zou ag mouse button to modify the range of data points be 224 8 Ohm selected for the fit The new linear regression is T 108 8 Ohm automatically calculated when one of the circles is Total paints 12 moved i i Results The coordinates of the first and last data points used for a 0 982 7 Ohak the fit are displayed as well as the number of point
49. ab Express Software User s Manual On the top of this graphic frame the classical tools are displayed e The scroll li used to move the curve on the graphic window le p e The cursor allows the user to display for each point its coordinates and the number of the point When you right click on the mouse a comment is added on the graph given the coordinates of the point e The selection pu allows the user to select a zone of the curve data points either before a fit or analysis or to hide bad data points f i e Zoom andZoom are used either with a zone selection smoothing or by left clicking on the part of the curve that you want to zoom e Zoom Back is very useful when you have zoomed in an undesired zone It is not limited in the number of actions The Mouse Rescale is made of different scaling functions according to each axis These buttons allow rescaling on X axis E Y1 axis Y2 axis and every axes aS at the same time Five section of fitting tools are available o Maths tools section 2 including Min Max determination linear and circle fit linear interpolation file subtraction integral Fourier Transform Filter Multi exponential Sim and Multi exponential Fit o General Electrochemistry section a and CV Sim o Electrochemical Impedance Spectroscopy section including Z Fit Z Sim and Mott Shottky Fit and Kramers Kronig analysis including Peak Analysis Wave Analysis o
50. accepts no responsibility for accidents or damage resulting from any failure to comply with these precautions GROUNDING To minimize the hazard of electrical shock it is essential that the equipment be connected to a protective ground through the AC supply cable The continuity of the ground connection should be checked periodically ATMOSPHERE You must never operate the equipment in corrosive atmosphere Moreover if the equipment is exposed to a highly corrosive atmosphere the components and the metallic parts can be corroded and can involve malfunction of the instrument The user must also be careful that the ventilation grids are not obstructed An external cleaning can be made with a vacuum cleaner if necessary Please consult our specialists to discuss the best location in your lab for the instrument avoid glove box hood chemical products EC Lab Express Software User s Manual AVOID UNSAFE EQUIPMENT The equipment may be unsafe if any of the following statements apply Equipment shows visible damage Equipment has failed to perform an intended operation Equipment has been stored in unfavourable conditions Equipment has been subjected to physical stress In case of doubt as to the serviceability of the equipment don t use it Get it properly checked out by a qualified service technician LIVE CONDUCTORS When the equipment is connected to its measurement inputs or supply the opening of covers or removal
51. ata file is created with the following name filename intpl mpp This tool is very useful to subtract two data files Indeed subtraction between two file is only possible when the files present the same regular distancing between each point 3 3 2 5 Subtract files A tool for subtracting curves is available in math section of analysis tools menu The raw data files are not changed after this analysis Indeed for some applications it could be interesting to subtract two curves The Subtract Files tool is available in the Math section The two files to subtract are selected as File 1 and File 2 Then the resulting file File 1 File 2 is displayed The sampling rate of the resulting file in filter mpp format is defined by e the sampling rate of file 1 or and file 2 e the total number of the points of the resulting curve File 1 File 2 The spacing can be defined in a linear or logarithmic spacing e aconstant time step The results can be copied in the clipboard to be pasted in the print window comment zone or in a text file They can be saved in a text file 60 Selection Trace From point A bos To paint AS Wes T atal points Sampling Ouput file Nb Points 86 O Sampling Fig 69 Linear interpolation window Subtract Files Selection z LV Tn 1 OV ckground me File 1 File 2 sampling O Same as File 1 Same as File 2 3 Same as File 1 and File 2 Q i 00 points
52. ate data treatment it is possible to create a specific representation for each technique For this the user has to click on Add in the bottom of the Graph Representations window then a User x variable is automatically created The user can change the name of the display He must select variables to be displayed on X axis and on Y1 and Y2 axes in the Representation window He can also define a processed display for each axis in the Advanced window Once definition of each axis done it is possible for the user to define the Graph style but also the techniques to which apply this process The selection of the Graph Style can be done on the Advanced menu as shown in Fig 52 As mentioned in the Graph properties part the user can choose amongst four available Graph Styles or define himself a Graph Style that can be associated with defined techniques This can be done by selecting the Edit menu see following paragraph for more details about the Graph Style creation Clicking on the second Edit button allows the selection of the desired technique Once the selection done techniques are displayed in the Selected techniques box as shown in the Fig 52 Graph Representations ES lve Ewe Mame PA oe Logll vs E we Ewe vs Loglll O ve t Ap vet Bode Impedance Mygquist Impedance Representation Advanced L Graphic style association Stile zHone Technique qid Line Mark
53. ater than the chosen Range without current overflow error message In this case the potential range is reduced to 9 V instead of 10 V The maximum measurable current is 2 4xl Range For example with Range 10 mA the current measured can be 24 mA with a potential range 9 V The same thing is possible when the current is controlled E Range adjustment E Range can be defined by the user selecting three ranges of potential already defined 2 5 V 5 V 10 V or the custom range With the custom range depending of the application it is possible for the user to adjust carefully the potential range and then to increase the potential resolution from 305 uV to 5 uV for VMP3 technology and from 333 uV to 5 uV for SP 300 technology Note that two gains are available with the SP 300 technology allowing to reach voltages as small that 250 mV or 25 mV 26 EC Lab Express Software User s Manual E mas 20 Ey E min po Ely 2 Custom Control resolution ans2 TU Measure resolution p Fig 32 E Range selection and Custom window 20 Bandwidth The VMP3 VMP2 Z VSP SP 150 SP 50 HCP 803 and BiStat devices propose a choice of 7 bandwidths damping factors and 9 for SP 300 VSP 300 SP 200 and SP 240 devices in the regulation loop of the potentiostat The frequency bandwidth will depend on the cell impedance and the user should test filtering effect on his experiment for choosing the
54. atinum 10 eycles mpr Test Box 4 SPEIS mpr l gt vs Ewe x Imi ve Re z 2 500 A A 2 000 5 a ed A ds x E 1500 x sex A 000 e Est n x di X x li i um x p 500 M w 2 000 4 000 Ewe V vs SCE Re z yohm Fig 59 Multigraph window To display several graphs in the same window right click on the graphic window select Add Graph and choose the data file to display One graph is active on the window with a red frame in the left bottom corner Other graphs are not active In the multigraph mode fits and analysis remain possible on the active trace of the active graph The graph properties can be modified for each graph independently Graph Tools Analysis tools EC Lab Express software contains powerful analysis tools These analysis tools are divided into five sections Math General Electrochemistry Electrochemical Impedance opectroscopy Photovoltaic Fuel cells and Corrosion Each section contains its specific analysis tools or process For example in the corrosion section it is possible to perform Linear Fit Circular Fit Tafel Fit Ry Fit corrosion data can also be analyzed with efficient simulating program Corr Sim The analysis tools will be detailed in the following paragraphs 94 EC Lab Express Software User s Manual h Selector hd Show Pd v Selector y Show Math Y Math X I General Electrochemistry b mi General Electrochemistry d Electroc
55. between the high X intercept and low X intercept C is the Capacitance determined for the experimental point in the selected zone where Im Z is the maximum Rc 1 The parameters and results can be copied to the clipboard to be pasted in a comment zone the print window or a text file They can also be saved in a text file PEIS Fe basique 1 mpr Im Z vs Re Z 100 90 80 TO 60 50 z 40 un o N o E 20 o apo 10 0 20 30 40 50 100 150 Re Z Ohm Fig 68 Circular Fit on the graph Circle Fit Selection Trace mz vs Rele From point 5 48 15 Ohm Yi 0 963 5 Ohm To point 2a k 120 6 Ohmi sie 15 33 Ohm Total points 24 Parameters lterative algorithm Results Center X Br 35 Uhm Center Y 11 2 Ohm Diameter B3 Std Deviation 0 305 2 Depression a Low intercept 47 02 Ohm High x intercept 127 7 Ohm A 280 66 Ohm B b 254e b F Close Fig 67 Circular Fit window 200 EC Lab Express Software User s Manual 3 3 2 4 Linear interpolation An interpolation tool LE is available in math section of Analysis tools menu The raw data file is not changed after this analysis When a data point zone is selected click on Calculate The linear interpolation allows the user to space out regularly each point of the data file The user can select to interpolate data by a defined number of points or a regular time between each point Then a processed interpolated d
56. cle6 mpr 1 04 1 02 N i wl l i iN T El WU 20 98 n y 0 96 Rut 0 92 98 98 5 time s Fig 77 Filter result Red curve is the raw data file and the blue one is the filtered curve 65 EC Lab Express Software User s Manual It is possible to model data with multiexponential behavior up to order 6 with EC Lab Express software This tool is particularly interesting for conductivity measurements A simulation tool Multi Exponential Sim and a fitting tool Multi Exponential Fit are available in the math section of Analysis tools menu 3 3 2 9 Multi Exponential Sim The Multi Exponential Sim tool allows user to plot a Multi Exponential Sim curve from a multi exponential equation First of all ibi order of the multiexponential equation is selected up to 6 Several units for x or y axis can be chosen for the output graph The window of the simulation is defined between X min and X max In the third block of the N y afk xg t LD ae 1x0 param walue window it is possible to add noise if the box Add noise Gomis is ticked Click on the Calculate button to obtain am simulated curve 1 5 em 1 z axis 3 3 3 2 10 Multi Exponential Fit eet NM min 100020 As previously the user can select the order of the xma on exponential up to 6 In the table Fig 99 a line is Nb points foo created for each parameter Clicking on Calculate the dee calculation without randomiza
57. connect the electrodes from the cell select Electrodes connection standard and set the next connections Refi and CA2 WE leads to the working electrode for VMP3 technology or P1 and S1 leads to the working electrode for SP 300 technology Ref2 lead to the reference electrode for VMP3 technology or S2 lead to the reference electrode for SP 300 technology EC Lab Express Software User s Manual CA1 CE and Ref3 leads to the counter electrode for VMP3 technology or S3 and P2 leads to the counter electrode for SP 300 technology Then click on Apply configuration button Refer to the Installation and configuration manual for more details on the CE to ground connection Warning it is important to disconnect the electrodes from the cell before changing the electrode connection because of the difference between the leads assignment the OCV may not be properly applied Note with CE to ground connection CE vs WE compliance is set to 10 V The CE to ground option is not available with the ZRA protocol Zero Resistance Ammeter 2 1 3 1 3 48 V control mode This connexion mode is only available with the SP 300 when a 1 A 48 V is present inside the chassis Cell Connection Disconnect the cables from the cell select E WE Electrodes connection 48 V control and reconnect the cell as follows oe P2 and S3 leads to the working electrode ce S2 lead to the reference electrode sl LE P1 and S1 leads t
58. culated from the linear equation for 0 The correlation coefficient shows the accuracy of the linear regression It is also possible to determine kor by adjusting the Tafel coefficients Ba and Be previously determined by the Tafel Fit The results can be copied to the clipboard to be pasted in the print window comment zone or a text file They can also be saved in a text file p Graph ie pu vs Ewe LP iron corrosion bis mpry c mA 04 3 Ewe V Selection Trace l gt vs Ewe From Point 40 A 0 350 9 Y fae 0 427 18 3 m To Pont E S 1 238 4 Vv is 0 395 18 3 m Total ports 22 Parameters LE 1200 mW Bs 1200 mW Range 25 0 mW Results Ap 63 155 8 Ohm Ecorr 324 552 mv Correlation 0 998 3 corr 0 413 057 pa Close Fig 124 R Fit window 02 Fig 125 Linear polarization curve of an iron electrode in H2SO 0 1 M 102 EC Lab Express Software User s Manual Note the user can adjust the R Fit He must grab and move markers The fit result is automatically updated It is not necessary to click on Calculate another time one could use the Linear fit to get the same results but the R fit is more convenient for the R calculation 3 3 5 2 1 Corrosion rate Finally the corrosion rate CR is calculated according to the next equation I K EW CR ETIN in millimeter per year mmpy or milliinches per year mpy m corrosion curr
59. d files Remove trace Save Data Files as LOG history 5 for the graphic display with the Active trace Add graph and Remove graph Ewe vs time aj_03 mpr This option shows the active trace that can switch a Iys time aj D4 mpr to one of the other traces with a click 6 for Copy and Print tools 7 for the Graph properties 3 1 2 Loading a data file With the EC Lab Express software the user can reload data files previously recorded following the link File Load Data File or in the graphic window with the mouse right click menu item Load Files The following window appears 35 E C Lab Express Software User s Manua Look in Samples amp t hy Recent Documents Desktop My Documents Mu Network Places Ej 185650 cyclage 260504 GCPL_1 IQx mpp 16650 zPOT l mpr APGC GsMdischarge_1 mpr Ej 18650 GITT D30604 1 cxR mpp 18650 GITT 030604 1 IQx mpp Ej 18650 GITT 180604 1 IQx mpp E CV Fe basique 1 cnG mpp es CV Fe basique 1 n mpp PITT 300604 1 cqrx mpp E 18650 cvclage 760504 GCPL_1 mpr Ed 18650_GITT_030604_1 mpr 18650_GITT_180604_1 mpr Ed 18650 linked 1 GCPL icorr mpr Ed 18650 linked 2 ZPOT 1 mpr 18650 linked 3 GCPL i1corr mpr 18650 linked 4 ZPOT 1 mpr 18650 linked 5 GCPL_1corr mpr lt i E CA Fe l mpr Ej CA loop Fe 1 mpr es CP RAGONE mpr CV Fe basique 1 mpr s DPv Fe basique 1 mpr Ed PITT 2300604 1 mpr s pyr Cw mpr pyrtest
60. density 2 M1del2 cm the Least square method fit Move the circles with the mouse by holding the mouse left button to modify the gt range of data points selected for the fit The new linear E regression is automatically calculated upon moving a ela ESOS Close circle Fig 116 Mott Schottky results window 94 EC Lab Express Software User s Manual The potential range used for the analysis is shown in the Results frame For each selected frequency the flat band potential is determined by extrapolation of the linear regression to C 20 The donor density is calculated from the slope of the linear regression at 25 C according to the dielectric constant of the material and the surface area of the semi conductor defined in the Parameters frame C 2 pF 2 04 053 02 01 0 lt Ewe gt V Fig 117 Mott Schottky Fit The results of the fit flatoand potential donor density can be copied to the clipboard to be pasted in the print window comment zone or a text file They can be saved in a text file 3 3 4 3 4 Saving Fit and analysis results All the fits described above can be saved in a text file Click on save to create a fit file fit in the same folder as the raw data file When the data file is displayed a function Show Analysis Results is available on the right click menu Select this function to display the fit results window 95 EC Lab Express Software User s Manual Analysis Results
61. e From point 833 SS Su ss nee 0 542 de 3 m To paint FER SX a cies 0 011 54 m Total points br24 Input potential H B8 PHMssn iZ fti Fig 128 CASP Fit warning message Auto detect Wa 50 000 mit z loni Hz Answer Yes to the warning message WEN The Fit can be done by clicking on calculate button 511 0 011 26 m ola 0 267 Fe 3 m DI 1 3e 6 m Icom 14 53 pA The CASP graph Fig 85 is displayed in vs time representation ba 8826 W 1 The software deduces the current corrosion leor and the ce i OR PUN Tafel parameters p4 and p Bc 3309 mv The results can be copied to the clipboard to be pasted in eror 1 947 2 the print window comment zone or a text file They can also be saved in a text file The Fit accuracy can be estimated with the y parameter Fig 129 CASP Fit window 106 EC Lab Express Software User s Manual File CASP mpr SVM ZU time s Fig 130 CASP graph 3 3 5 6 Electrochemical Noise Analysis 1 000 The study of corrosion phenomena by electrochemical noise involves the analysis of random Current or potential fluctuations To study these fluctuations the tool Electrochemical Noise Analysis AY was introduced into EC Lab in the version 10 00 Electrochemical noise method requires three electrodes to establish a parameter known as the noise resistance R Two of these are working electrodes and current is measured between them
62. e double layer capacitance the double layer capacitance contribution to the total capacitance is negligible Therefore the capacitance value calculated from this model is assumed to be the value of the space charge capacitance b The equivalent circuit used in this model is a series combination of a resistor and a capacitance the space charge capacitance The capacitance is calculated from the imaginary component of the impedance Im Z using the relationship 1 AG This model is adequate if the frequency is high enough on the order of kHz 3 3 4 3 2 The Mott Schottky plot The Mott Schottky plot presents 1 C versus Eye or 1 C versus Eye for each frequency with C l calculated from the previous relationship Im Z 2414 4C Frequencies v 100 000 kHz 68 125 kHz 46 406 kHz ah a When this plot is selected the window on the left is 14 681 kHz displayed to select the frequencies The user can select v 10 000 kHz i 6 016 kHz several or all frequencies Click on Ok to display the 4 542 kHz Mott Schottky curves The selection is the same for the 3 160 kHz 2 153 kHz time evolution of the impedance or of the phase 1 467 kHz 1 002 kHz All frequencies Cancel Fig 114 Mott Schottky frequency selection window Then the graphic window shows one trace per frequency Use the shift key to display the frequency 93 EC Lab Express Software User s Manual gt C 2 ye Ewes SPEISdiode mp
63. e settings cooomccnonnnnonanonanancananannananaa nnne nnn nane nana natns ranas 2 1 Staring the a 16 2 rt tee 2 1 1 Connection with the instrument cococccocnccocnconcncccnncncnnonnnnonnnonnnonannnnnnnonnnnnnnonnnononos 2 1 1 1 Instrument IP address and gateways change network connection 221 2 Selection or tie chanel uote oae toto aaa ida 2 1 3 Hardware configuration resonar 2 1 3 1 Electrodes CONNOR ross 2o ki Standard mode aoo stan a idad danita cicaitacao siii 2 1 9 1 2 GEO Groundifiode a o caua 2olado las A48 V COMO MOS ia a laadi 2 1 3 1 4 WE 10 Ground mode eint tnde nt ped Conus en Pn Con eagle initis 21 32 a 2 o EC MEI cloro e iced accede E nade E EE E E 2 1 3 4 Ultra Low Current ULC MeasureMent occcoccncccccnccccnccncnncnnnncnnnononannnoncnonanenos 21 RECON ODL OMS oe m c EET 2 2 Preparing and Running an Experiment with EC Lab Express software 2 2 Nhe Bar MENU rural out zeta The Flemmen eese eter oia A 22d INS CONO nelli zceisdeiunitensteicut iun ber a iua i or potui 2 2 2 EC Lab Express main windOwW seeeeeeneeneeneeennn eene 2 2 2 1 DEVICE TAM Cusine II 22 2 2 EXDOHITIeit TEGITIG na ii ia sii tica 2 2 2 2 1 GOldescripion par io dete o e trait to e etra ts 2 2 2 9 Parameters rame simi ER MEC AFIN EET OSEE 2 2 9 PEC a tecliplds casse onus o oo de e la 2 2 4 Parameter Settings description ooccccoccncccnncoccnn
64. e grounded or floating mode The analog filtering The ULC measurement option if a ULC option is connected to the select channel Options Cell Connection Electrode Connection 3 Standard v P1 1 WE Channel G Grounded e E ce ULC measurement G High speed scan Ww F CE Apply Configuration Fig 9 Hardware configuration window 0 EC Lab Express Software User s Manual 2 1 3 1 Electrodes connection Four connection modes can be used with EC Lab Express the standard mode for general purpose the CE to Ground mode more dedicated to special measurement such BiStat measurements the 48 V control used with a booster 1 A 48 V and the WE to ground mode dedicated to experiments like hydrogen permeation To be easily identified each lead has an associated color and label For each mode of connexion depending of the technology labels on the leads are different For VMP3 technology VMP2 VMP3 BiStat VSP SP 150 SP 50 e Refi RED Reference 1 for the control and measurement of the working electrode potential e Hef2 WHITE Reference 2 for the control and measurement of the Reference electrode potential e Ref3 BLUE Reference 3 for the control and measurement of the Counter electrode potential e CA2 RED Control Booster for the current control and measurement flowing through the working electrode in standard mode e CA1 BLUE Control Booster for the current control and measurement flowing
65. e layer charging 3 3 4 1 1 Electric equivalent elements description 76 EC Lab Express Software User s Manual The impedance analysis tool contains currently 8 different electric components These components are R resistor L self inductor C capacitor Q constant Phase Element CPE W Warburg Element simulating the semi infinite diffusion Wd Warburg Diffusion Element simulating the convective diffusion WM restricted Linear Diffusion Element G Gerischer Element 3 3 4 1 2 Resistor R Description Resistor Impedance zl FH Mygquist Diagram Ir z vs Rel o Fig 94 Resistor element description The resistor element is defined as a passive component with a constant value when frequency varies The Fig 102 describes the resistor with Its symbol its faradic impedance and a view of its Nyquist representation The resistor element is characterized by a constant value that can be measured in the Nyquist diagram by the Real part Re Z for an imaginary part to zero Im Z 0 3 3 4 1 3 Inductor L 17 EC Lab Express Software User s Manual Description Inductor L1 Sn Impedance ZJ L 2xf Mygquist Diagram Ir z vs Rel 0 Fig 95 Inductive element description The inductive element has impedance with a frequency dependency as shown on the faradic impedance equation The Nyquist plot of an inductance is a vertical straight line in the imaginary negat
66. e technique in the experiment frame The parameters are described deeply in the EC Lab Express Software Techniques and Applications manual For each selected technique a description is available EC Lab Express software offers a classical right click on each box of the parameter window to copy cut paste and select values Note that parameters can be changed on the fly Once it is done click on the Update button to validate the changes 22 EC Lab Express Software User s Manual Parameters Description Paramet Initial Potential E 000000 V ys l Parameters Description Vertex Potential Ey 1 000 00D Y Vs Emf ww m Vertex Potential Ey 1 000000 V Ys Eref v gt Final Potential Ee 0000000 Y Ve Eret E Scan with dE dt 11 00 000 o E E Record every dE 11 0 000 mM e Average Ez Measure from 50 of step ETS Cyclic voltammetr CV is the most widely used technique Far ta IO ost acquiring qualitative informations about electrochemical 2 d j reactions CY provides informations on redos processes Repeat n E times heterogeneous electron transter reactions and adsorption processes It offers a rapid location of redox potential of the electraactive species LY consists of scanning linearly the potential of a stationary E Range working electrode using a trianqular potential waveform During the potential sweep the patentiastat measures the bandwidth current resulting from electroche
67. ent in A K constant that defines the units of the corrosion rate EW equivalent weight in g equivalent d density in g cm A sample area in cm K CR units 3272 mm A cm year mm year mmpy 1 288x10 milliinches A cm year milliinches year mpy 3 3 5 2 2 Minimize option Nevertheless results may be different from what is expected for two reasons 1 The linear parts of the plot are not recorded 2 The potential scan range is too large and an additional electrochemical reaction appears that does not fit the Stern Geary model In these cases it is possible to reduce the error between the model leaci and the measured data lmes by minimizing the following value N 2 T Ci mz A N 2 Ic This is obtained in clicking on the Minimize button The Nelder and Mead Simplex method cf ref was used to minimize the y value Keep the button pushed lt Enter gt or lt Alt M gt keys until the Stern and Geary parameters Egor lo Ba and p are stabilized Then a theoretical Tafel graph is displayed this graph is displayed in agreement with parameters obtained with minimize button Note that the Simplex method may not succeed if the initial values are too much different from the minimum ones it may fall into a local minimum of y Ecorr corr Ba Be or if the I Ewe curve is linear around E In that case the following message will be displayed The trace KE appears to be linear within the selected zone The mi
68. er points graphic windows Traces Name Style Flot Undersampling Fig 55 Definition of traces properties in Graph style definition 3 2 6 The LOG History file The log file summarizes all parameters used for an experiment with the possible modifications on line Log displays the history of the experiment from its beginning 90 EC Lab Express Software User s Manual CY_02 mpr LOG File CV 02 mpr 9 20 points 233 604 bytes Cyclic Yoltammetry Run on channel 2 User CE vs WE compliance from 10 Y to 10 Y Electrode connection standard Experiment Limits Ewe min 1 00 Y Ewe max 1 00 Y for t gt 10 ms Acquisition started on O6 O3 2005 17 12 40 saved on File CV z mpr Directory C XELC Lab vSberaz Data Host 192 109 209 50 Device VMPZ v Fig 56 Experiment history window The parameter modifications while the experiment is running are added to the end of the file The number of points and the file size are displayed on the top of the window near the file name 3 2 7 Copy options On the graphic display several copy options are available When the user right clicks on the mouse the following copy options can be found in the copy menu 2 Copy Graph Advanced Picture Format Options size as GIF llas JPEG Colors Default as Metafile as PCY F Monochrome Copy Graph AlE as PNG Copy Data Alt D as PostScript as Sa Copy Graph Advanced
69. ers style Ar prop style Monochromatic style Black Impedance 7 vs t Matt S5 chottky Bode Admittance Mugquist Admithance Black Admittance 2 Phase error Select B atter ser Voltage control f Electrochemical Techniques Ee Voltamperometic Techniques Open Circuit voltage OC Cyclic S altammetre Cy C Cyclic Yoltammety Advanced CA Chronoamperomety Chronacaulametry CA C Chronopotentiometry CP C Staircase Voltammetre SW Impedance Spectroscopy Pulsed Techniques Graph Representations ES Black Impedance ipe Black Impedance add A El we t Moott S chottky i Advanced deas ooo Nyquist Admittance Graphic style association Black Admittance EI Phasze z error Stole Line style t x ved Ece wz t Technique s association Ewe Ece vs t Selected techniques Bade Al CV cycle vs time CA freq vs time IE voe we freq I ve freq E we l ve freg Fig 52 Graph Style and technique selection 47 EC Lab Express Software User s Manual Note this graph representation will only be available if the variables to display are recorded in the current mpr file for which the representation will be applied 3 2 5 3 How to create a Graph Style It is often convenient to display the obtained data with the same way same trace color same markers same units For this it is possible with EC Lab Express t
70. ftware automatically displays a newsletter announcing news about Bio Logic Product range Newsletter BioLegic hog ce dra New distribution network Beginning on October 1 2007 Bio logic SAS is pleased to announce that it will begin marketing its products directly to customers through its own distribution network Please see our distributors web page Mew instruments 5 P 30 simplicity and Performance aE 150 Sample and Powerful in a versatile chassis EC T 30 Compact Fuel Cell Test Station for 504 cells Mew software E Lab Express Easy to use electrochemistry software for new users and fast setups E Lab V9 4 New software release available Mew application notes AHEL Two questions about Eramers Eronig transformations A4nN414 ZFit and equivalent electrical circuits Ex Close window Fig 7 Newsletter EC Lab Express Software User s Manual 2 1 2 Selection of the channel Once the connection with the instrument is done the connection window is automatically closed The Channels selection window is automatically opened as shown Fig 8 Selecting a channel allows the user to select the hardware configuration In case of a Bipotentiostat experiment the user has to define the master channel Master Channel for stackbipot techniques only Fig 8 Channels selection window 2 1 3 Hardware configuration Once a channel is selected user can access the selection of The electrodes connection Th
71. g electrode controlled potential control V the working electrode measured potential Ey V the average current average values on every potential steps lt l gt mA and the state byte Other variables such as cycle number may be displayed depending on the protocol of the experiment The state byte includes the variables mode ox red error control changes and counter inc cycle increment that indicate different statuses of the experiment Most of the time the user may not be interested in showing the state byte that is more dedicated to internal files processing So the option Hide Additional variables is checked by default Unchecking the option will add the variables to the file selection window oeveral commands are available to use files e Load replace all files by others Add add file s to the list in order to overlay curves e Remove remove the selected file from the list e Undo undo the last operation done e Clear remove all files from the window X Y1 and Y2 represent the X axis and two different Y axes left and right EC Lab Express users are able to plot data in X Y1 coordinates or in X Y1 amp Y2 coordinates Select the variables to be displayed on a given axis by clicking the corresponding box click again to deselect Select Same selection for all files to get the same axis display for several files A shortcut scroll menu allows for quick selection of the graph plot When a data file is displayed in the grap
72. ght click on the zone and select Edit comments The following window is displayed 38 EC Lab Express Software User s Manual Comment M y comment on this anodic current peak Properties Font Mame Anal Font Style Standard Font Size Alignment Align Lett Font Color go Black Background Color Custom Transparency Show Arrow Fig 41 Edit Comment zone The user can paste analysis results or other comments into the text frame Several comment zone properties are available and the user can display an arrow and direct it to the desired part of the curve To remove comment zones right click on the zone and select Delete comment Note The comment zone is automatically printed on the graph With the Suppr button of the keyboard it is possible to delete the comments 3 2 3 Three Dimensional graphic A 3D representation is available by right clicking on the graph menu After clicking on the 3D menu the Selector menu is available and allows the user to choose the variables to display An example of the Bode diagram obtained with the 3D representation tool is given in Fig 42 39 EC Lab Express Software User s Manual SPEIS mpr Sag EG LIRR 72 Z0 4 E 22777 77 C2 SO II
73. hat can be fit one by one at the user s convenience Selecting all cycles for the fit and randomisation on only the first cycle will lead to an automatic fit When the Minimization is launched a new graph is added at the bottom right hand corner This graph will display the equivalent circuit parameters obtained by the fit in this case H1 H2 R3 C2 C3 versus potential or time The user can have a time evolution or a potential evolution of the desired parameter ae Graph 1T ee ei ghee da ET SR A EST 0c FH vgquist Impedance vt Show Im vs Reiz SPEIS Test Box 3 Circuit 3 mpr cycle 21 PEIS_ Test Baox 3 Circuit 2 zfit mpp z 2 000 1 500 a 1 000 S00 Im 2 0 hm 2 uuu 4 000 Reiz Ohm SPEIS Test Box 3 Circuit 3 _zittparam mpp Rahm vs Eywvez CAF ve Evwez X R3 0hm JU z2 ol 0 5 11 Ew oc c SUM Fig 104 Successive fits on cycles with randomization on the first cycle 84 EC Lab Express Software User s Manual We can see the potential evolution of the resistance R3 and the capacitance C2 The parameters of the equivalent circuit components are stored for each cycle in the Filename_Zfitparam mpp file Note that the fit results are automatically saved in case of multi cycles treatment References W H Press S A Teukolsky W T Vetterling B P Flannery Numerical Recipes in C The Art of the Scientific Computing Cambridge Univers
74. he Experiment frame Experiment Synchronization window appears In this window user selects the directory location and experiments which should be synchronized by ticking the corresponding box name can be modified in the Filename Prefix One file is saved for each experiment Experiment Synchronization Directory CuDataExpressitestBatch5 50 Experiments Selection Experiments Mame Filename Prefix C Experiment Experiment 1 C Experiments Experiment Copy Names b Run Experiments are launched when the user click on the Run button on the window above 29 EC Lab Express Software User s Manual 2 3 Data properties 2 3 1 Type of data files Several files using your filename with different extensions mp are created File oer atene o description Raw data binary file which contains the current parameter settings refreshed mpr at each modification of the detailed flow diagram and of the cell characteristic windows This file includes all the information of the mps file Temporary binary file available for particular protocols derived from the mpr file This file is used for real time displaying of parameters obtained by raw dioi data processing e g the integrated charge since the starting of the experiment the average current between two recordings chronocoulometry mpt The mpt file is a text format file generated when the user exports the raw mpr i file in text format This file is ge
75. hemical Impedance Spectroscopy gt i b e Electrochemical Impedance Spectroscopy dedo s a Corrosion Tafel Fit F4 Photovoltaic Fuel Cells U Rp Fit E l Show Analysis Results e SPR D Corrosion d S Corr Sim A VASP Fit Pu Show Analysis Results lr CASP Fit m Electrochemical Noise Analysis F9 Fig 60 Analysis tools menu g y Fig 61 Corrosion section of Analysis tools menu First of all before any analysis select the trace to fit if several traces are displayed on the graphic window or the cycle if the trace contains several cycles There are two different ways to make a fit on a trace with EC Lab Express software Two steps must be considered the zone selection and the fit choice One can be made before or after the other The two ways to proceed are as follows 1 Click directly on the selection button of the graphic tool bar On the graphic window select the zone that needs to be analyzed by holding the left mouse button The cursor will draw a rectangle around the chosen zone Once it is done release the mouse button The part of the curve selected should be highlighted in red and ready for analysis Then select the required tools with the mouse right click 2 In the Analysis menu select one of the analysis tools The mouse selection mode is automatically selected The user has just to start a zone selection as described above Now a zone is selected on the trace and a fit window is displa
76. hic window the user can modify the graph properties for a better representation of the curve The graphic parameters are automatically saved in a 3 EC Lab Express Software User s Manual graphic file Then when the user reopens the same data file in the graphic window the graphic parameters defined before will be kept 3 2 Graphic facilities 3 2 1 Show Hide points The EC Lab Express software is equipped with a show hide option on the right click menu Aberrant points can now be hidden on the graph in order to perform data processing without any troubling points The hidden data points are not removed from the data file They are only graphically hidden for better processing The data points must be selected with the selection mouse mode before being hidden Then click on Hide selected points to mask the points 3 2 2 Add comments on the graph The graphic package offers the ability to add comment zones on the graph The number of comment zones that can be added on the graph is not limited Wy Comments on le IIFFSrt maa CUF ent He T mA Peak Analysis 05 04 06 11 01 height 0 2 l m i l dt h 1 Ep cha ch 0 3 0 2 0 1 j 0 1 2 0 3 0 4 os 0 6 oy Ewe V Fig 40 Comment zones on the graph To add Comment zones to the graph the user must right click and select Add comments Then an empty comment zone appears on the graph To modify this zone double click on it or ri
77. iHz Frequency range Auto Freg Min Hz Freq Max Hz Nb Points E Fig 75 Fourier transform analysis 64 EC Lab Express Software User s Manual 3 3 2 8 Filter Data may be distorted by external perturbation for Filter instance the 50 or 60 Hz frequency signal coming from Selena the electrical grid The Filter tool Y available in math de menu allows the user to remove this additional signal 0 and then yield to smoother results i To point several filtering methods can be set gt e Moving average method For this method the Total points 35984 window size must be defined es e Savitzky Golay method This method is based Vistos on polynomial calculation in a defined window The window size and the polynomial order have Freg min 0 055 55 Hz 7 siena band Mica thod Freg max 999 5 Hz e Low high pass or band pass reject methods ES These methods are based on Fourier Transform ub The window Rectangle Barlett Hann frequency band Hamming Blackman Welch and the cutoff 50 000 ALE frequency ies have to be defined please refer 60 000 max to the Fourier transform part for more details on 5 i agression this point SUE T l LETTE The results can be copied in the clipboard to be pasted ae ES in the print window comment zone or in a text file They TT can be saved in a text file ATA Fig 76 Fourier Transform window lt I gt vs time cv noise cycle6 filter mpp 7 cv noise cy
78. ic reaction predominates ImIQ10 for E gt Econ E E oorr I 1 10 forE Egor corr So in a log versus E representation one should see two linear parts for E gt Eco and E lt Ecorr for E gt Ecorr corr log RI log a for E lt Ecorr corr 3 log RI log C Tafel Fit window The Tafel Fit window allows the user to find the anodic and cathodic Tafel coefficients into a log I versus E representation Tafel Graph 98 EC Lab Express Software User s Manual On a linear polarization trace select the Tafel Fit with Tafel Fit the Tafel Fit button X in the corrosion section of the Stop Minimize On Analysis menu In the log l versus E representation Me 20 relative error the user has to select the data points centered around 1000 iterations Default Ecorr Point for 2 0 then click on Calculate The EE software will automatically find Ba and B values used T sees PETS Ewe for the calculation of the corrosion current hor The 7 Econ 324688 m Tafel Fit analysis window is displayed Fig 80 ZI U33 wA Note The user will receive a warning message to J Ba lier nave switch to the log I versus Eye graph representation Jp 205 mv x 381 505 EC Lab ES x JM 1 235 32 died 0 000 geq Cannot perform tafel fit with the representation selected Density o oo g cm3 Switch the representation to log I vs Ewe Surface area 0 001 cnr Corrosion rate
79. ime in a solution containing both Ox and Red species of a redox system 3 3 4 2 1 Z Sim window 1 step To simulate a curve with the same shape as the previous experimental results click on ZSim icon A in the Analysis tools menu Then the ZSim selection window appears with the corresponding graphic window This window shows the simulated graph of the circuit with the values selected 88 EC Lab Express Software User s Manual Zsim mpr mid vs Re Z Set Frequencies 40 from F 100 000 3 a E T Toc a with 10 points per decade Y 20 t Equivalent circuit n a R1 01 R2 C3 R3 v Edite 10 parameter value Im Z Ohm 1 050 1100 Re zyohm Fig 110 ZSim menu and the graph corresponding to the selected circuit Note the default opened simulation circuit is the last one used in the previous simulation 2 step In the frequency frame set the frequency range between 500 kHz and 10 uHz with the number of points per decade and the spacing logarithmic or linear Select an equivalent circuit in the list If the required circuit is not in the list then the user can create his circuit in the Edit window Click on Edit to display this window 89 EC Lab Express Software User s Manual Equivalent Circuit Edition Circuit 83 153 Description RH1 51 B2 C3 R3 Add FISC2 R24C3 R HESA FSCZ RZ C3 R3 M4 Al C2 A2 CVA ed IRFTAC2 R24C3 R3w dd AICA R24 3 7 R34 C 4 84 RTCA R
80. ine Height is the current value for the potential E always according to the baseline E Width 1 2 is the potential peak width determined when it is possible at half the peak height parallel to the baseline e E Ep is the semi width for the growing part of the peak e Charge Pos is the charge corresponding to the integration of the peak versus time according to and above the baseline in the case of an oxidation peak The part of the peak considered for the calculation of the charge is limited to the green circle markers This zone can be adjusted by moving the markers e Charge Neg is the complementary part of the charge in the case where the selected zone crosses the baseline below the baseline for an oxidation peak Note it is possible to save the results of the analysis to a text file using the copy option The results are copied to the clipboard and can be pasted in notepad or other software 3 3 3 1 4 Results of the peak analysis using a polynomial baseline In fact it is often difficult to apply a linear regression to simulate the capacitive part of a curve or remove the beginning increasing part of a second current peak A polynomial baseline could lead to a more significant fit On the following figure a polynomial baseline has been used to do a peak analysis The oxidative peak of a polypyrrol film is analyzed using a polynomial baseline With this baseline we can avoid taking into account the beginning part of
81. ircuit Voltage Techniques Hx DV Cyclic Voltammetry DV Cyclic Voltammetry SL C Chrono amp mperometry Il CA Chrono mperometry SL CP ChronoPotentiometry IL CP ChronoPotentiometry PD YN Potentiodynamic PDYN Potentiodynamic GDYN Galvanodynamic GDYN Galvanodynamic LASY Large Amplitude Sinusoidal Voltammetry v LASY Large Amplitude Sinusoidal Yoltammetry Il MOD Modular Pulse Il MOD Modular Pulse L Impedance Spectroscopy Impedance Spectroscopy L Pulsed Techniques Pulsed Techniques L Stack Techniques 4c Corrosion Techniques Corrosion Techniques Ohmic Drop Determination Techniques 15 Ohmic Drop Determination Techniques Le Trigger L Trigger HL d4c L Bipotentiostat 15 Bipotentiostat b LOOF Loop 4 LOOP Loop Fig 22 Main window in standard Fig 23 Main window in advanced interface mode interface mode The Representations menu allows the user to define his own graphic display More details are given in section 3 2 5 page 45 19 EC Lab Express Software User s Manual 2 2 2 EC Lab Express main window 2 EC Lab Express V5 50 coe E File Config Help Device Channel Ewe Current Time Ece 13 329 pV lrange 10 mA Connection Standard 7 2 Freq 100 000 Hz Rcomp 0 Q v 0 196 mV 0 000A Os Buffer n E ICE NM t T Pa ameters Description Pa xperimen Show 4 b gt wk VSP 300 0001
82. is used to detect the instrument in a LAN even if its IP Address is not valid in the network It is also used for the detection of instruments connected by USB It is why when the connection is done by USB the kind and serial number of the instrument are displayed with the IP address equal to O like shown in Fig 2 whereas when the EC Lab Express Software User s Manual connection is done by Ethernet all the information kind serial number and IP address are displayed Device i On line Ethernet W5P 192 109 209 190 0401 Ethernet WSOP 192 109 209 191 0399 Ethernet MP3 192 109 209 192 0406 Ethernet WIF 192 109 209 193 040 2 Ethemet WMP3 192 109 209 216 0413 El IP address mae O Offline virtual potensiostat MP3 A Fig 2 Device selection window Choose one instrument in the list and click on Connect The Connect button becomes a Disconnect button and the light on the button is green the instrument is connected Fig 3 Device On line ELI mi T m Offline virtual potensiostat Y MF Info 3 Disconnect Fig 3 Instrument connection To disconnect the instrument click on the Disconnect button Note Ethernet connection is possible only if the computer has a valid IP Address in the same network as the instrument The user can work with EC Lab Express software off line without being connected The software will work as if it was connected to a virt
83. ith a fit the corrosion current the corrosion potential and the polarization resistance Tafel graph off line processing function allowing the user to display on the graph the logarithm of the current Tafel plot Traces processing tool allowing to apply a mathematical function to the axes Units graphic function used to modify the axis units VASP Fit tool available in the Analysis tool menu It allows user to determine corrosion current and tafel parameters 111 EC Lab Express Software User s Manual Wave analysis graphic tool used on curves obtained in a convective regime and returning the limit current and the half wave potential Zfit once the equivalent circuit defined the Zfit tool allows to identify parameters of the elements with experimental data points ZSim Simulation tool uses to define the equivalent circuit after an impedance experiment ZsimpWin software delivered by PAR and used to fit impedance curves with electrical circuits 112 EC Lab Express Software User s Manual Index mor mpe MpL GK INO Ds alonso peca 30 Ed DN COBLTOLIOOOS utente roii ibo eai arta tact daran tati a eiua tasti ac ud S 13 ACIUB uc ud MI EE M I MU M I MUI 44 ADE Cte ee eee ene CR ame don e ELE CM ene een eR eT p ELA Ec E 34 AVS EEEE E E EE TE T FEE E E TE T FEE E ET 95 Axis MOUSSA US NN NNUS 42 e UV AW VAs asus aou ues intu E ERA IMEEM EM ain aria mn cade ane EM MM EN UN ra 27 oana eOr O EP cs 78 CETO Oround ModE mE
84. ity Press Cambridge UK 2 Edition 1992 E Walter and L Pronzato Identification of Parametric Models from experimental data Springer 2006 J P Diard B Le Gorrec C Montella Cin tique lectrochimique Hermann 1996 E Barsoukov and J Ross Macdonald Impedance Spectroscopy Theory Experiment and applications Wiley interscience 2 Edition 2005 3 3 4 1 14 Pseudo capacitance ZFit calculates the pseudo capacitance associated with a CPE This value can be calculated only for an equivalent circuit R1 R Q This calculation corresponds to the determination of a capacitance value C at a frequency fy corresponding to the maximum imaginary part on the Nyquist circle obtained by fitting with the equivalent circuit R1 R Q This value is the solution of the following equation 1 1 2x RQ 2xRC with a and Q the CPE parameters Considering the previous example from the first frequency down to 20 Hz the equivalent circuit could be R1 R2 Q2 Im Z vs Re Z POT Fe basique 1 mpr POT Fe basique 1 zfit mpp BO a0 100 120 Re Z Ohm Fig 105 Fit results with an R1 R2 Q2 circuit 85 EC Lab Express Software User s Manual Selection Results Equivalent circuit RI Q2 R2 4673 Ohm 04762 31 82e5 F s a1 6 715e 6 09103 0 548 8 2 8158 Ohm 1 224 Equivalent circuit RH1 L2 R2 Pseudocapacitance O O O O O O Fit Select current cycle s Method Randomi
85. ive part Im Z lt 0 3 3 4 1 4 Capacitor C Description Capacitor Ly Impedance 1 MIS Myquist Diagram Im z vs Rez Fig 96 Capacitor element description The capacitor impedance is also frequency dependent The Nyquist plot of such an element corresponds to a vertical straight line in the imaginary positive part Im Z gt 0 The faradic impedance decreases when the frequency increases 78 EC Lab Express Software User s Manual 3 3 4 1 5 Constant phase element Q Description Constant Phase Element CPE RE Impedance 1 zi d 3 i 2 E 71 Mygquist Diagram Im z vs Rel Fig 97 Constant Phase Element description The CPE impedance is also frequency dependent The Nyquist plot of such an element corresponds to a straight line in the imaginary positive part Im Z gt 0 with a az 2 angle with the real axis The faradic impedance of the CPE decreases when the frequency increases 3 3 4 1 6 Warburg element for semi infinite diffusion W The Warburg element can be used to simulate a semi infinite linear diffusion that is unrestricted diffusion to a large planar electrode Description Warburg MW A AL Impedance zii BT jet Nyquist Diagram Im vs Reli Fig 98 Warburg diffusion element description 79 EC Lab Express Software User s Manual The Warburg impedance is an example of a constant phase element for which the
86. l Het Ca initial Het DA Hes DA le5 DB 5eb DB Be6 Calculate Copy Save Fig 87 CVSim window with a single Fig 88 CVSim window with several electron transfer electron transfers For each step the type of reaction and the species characteristics are set in two different frames 1 Reaction Reduction or oxidation has to selected by the combo box z represents the number of electron involved in the electron transfer E is the standard potential of the electron transfer step k is the heterogeneous rate constant ais the charge transfer coefficient in the forward direction 72 EC Lab Express Software User s Manual 2 Species Cx Is the concentration of the specie x As it is assumed that only one specie is initially in the solution concentration is only set in the first step of the mechanism Dx are the diffusion coefficients of the specie x The experimental conditions are set in the Setup tab which is divided into five blocks Example Select Mechanism E Setup Electrode Geometry Linear Semi infinite Radius Surface 3 142 cn E perimental Conditions Temperature An Double layer capacity Potential 5can Scan type Scan rate E init Vertex 1 Vertes 2 Number of scans Sampling Number of points per scan Total number of paints Sampling time oe E amp OF S Ole ol o y G 5 uo B to
87. ld Electrochim Acta 35 1990 39 J P Diard P Landaud J M Le Canut B Le Gorrec and C Montella Electrochim Acta 39 1994 2585 97 EC Lab Express Software User s Manual 3 3 5 Corrosion section The Tafel Fit and the R Fit are both based on the Stern and Geary equation developed here Stern and Geary ref 1 proposed a model of a corroding system that involves two electrochemical reactions an oxidation process and a reduction process This model is based on the Tafel equation that predicts that the logarithm of the current observed in an electrochemical process is directly related to the difference between the applied potential and the open circuit potential The Stern and Geary equation can be expressed as follow EE oon EE cor lE jSL 40 fe 10 Le where I E is the total current at a specific applied potential E Esorr is the open circuit potential of the system Ba and B are the Tafel constant for the anodic oxidation and cathodic reduction reactions and are defined as positive numbers lcorr IS the corrosion current corresponding to the anodic and cathodic current at E Egor The total current I E orr results from the difference of the anodic and cathodic current being null as expected Stern M and Geary A L J Electrochem Soc 104 56 1957 3 3 5 1 Tafel Fit The Stern and Geary equation predicts that for E gt Ego the anodic reaction predominates and that for E lt Esor the cathod
88. le 2 3 4 Data Saving Each channel has its own memory buffer to store data points This memory can receive 40 000 data points When the memory is full data points are rejected until the memory is a little emptied and could receive data points 32 EC Lab Express Software User s Manual EC Lab Express software Graphic Display The Graphic window The EC Lab Express application includes a graphic facility to display experiments on line and off line The user has also the ability to add graphs to an existing graphic window In that case the window Is divided in two or more graphs depending on the number of graphs When an experiment is running the graphic window is automatically opened to display the corresponding result file s Default graphic parameters have been chosen for example plot vs E for the CV technique The user can replace the default graphic parameters by his own parameters To do so he has to select the menu Representations in the Options menu and define his custom settings In case of linked techniques two different graphic windows will be displayed one for all voltamperometric techniques plot versus time and one for the impedance spectroscopy plot versus frequency Gin Graph kan RA EN A vs Ewe v CV Fe basique 1 mpr als vs Ewe i lt l gt mA 1 0 158563 V Tyr 0 130422 mA Point 1091 0 2 0 4 0 6 Ewe V vs SCE Fig 35 Graphic window 33 EC L
89. le The first thing to be defined by the user is the cycle to do the minimisation either one fit made on the current cycle displayed on the graph or the successive fits made on ALL cycles of the experiment Default values are set for every parameter but they never fit properly with the real experimental values Before to do the fit and in order to help the algorithm to find the best values it is necessary to find a couple of values as close as possible to the real one Default values too far off will result in a divergence of the algorithm A randomization has been added before the fitting to select the most suitable couple of parameter values with the lower y value The y equation used in this method is defined as follows 2 j O l with Z 1 is the measured impedance at the f frequency Z mode J param is function of the chosen model f is the frequency l param is the model parameters ex R1 R2 C1 Q1 o is the standard deviation It can be assimilated to the weight of the impedance data points It can be selected by the user to be 1 or Z Moreover two fitting algorithms are available and the user can select between the Downhill simplex algorithm and the Levenberg Marquardt algorithm Both of them can be tried successively to choose the best results In the fitting method the user can select between different combinations only Randomize only Simplex fitting only Levenberg Marquardt fitting
90. le The new parameters will be implemented when clicking on Calculate To store this simulation the user will have to give another name to the data file because a simulation is always created in the Zsim mpr file 3 3 4 3 Mott Schottky Fit Only the instruments equipped with the EIS measurement option have the capability of Mott Schottky fitting 3 3 4 3 1 Mott Schottky relationship and properties of semi conductors The Mott Schottky relationship involves the apparent capacitance measurement as a function of potential under depletion condition 2 7 E E 5L Co SEN e Where Cs is the capacitance of the space charge region e Is the dielectric constant of the semiconductor o Is the permittivity of free space 92 EC Lab Express Software User s Manual N is the donor density electron donor concentration for an n type semi conductor or hole acceptor concentration for a p type semi conductor E is the applied potential Erg is the flatband potential The donor density can be calculated from the slope of the 1 C vs Eye curve and the flatband potential can be determined by extrapolation to C 0 The model required for the calculation is based on two assumptions a Two capacitances have to be considered the one of the space charge region and the one of the double layer Since capacitances are in series the total capacitance is the sum of their reciprocals As the space charge capacitance is much smaller than th
91. les File 1 GEIS 25cm2 1 ElSG 0 1 mpr 2 458 points 39 697 bytes File 2 GEIS 25cm2 1 ElSG 1 1 mpr 408 points 31 217 bytes Fig 20 Import data file window 2 2 1 2 The config menu This menu allows selecting Options like the Automatic reconnection at start up or the interface Two EC Lab Express interfaces exist Fig 22 and Fig 23 Most of the menus are available in both interfaces In standard interface only one experiment can be performed whereas in the advanced interface two experiments can be settled simultaneously Note if not connected to the instrument all techniques are displayed even in the standard mode 18 EC Lab Express Software User s Manual Options General Device Automatic reconnection at startup Device communication time out mm sec Interface Advanced interface Fig 21 Options window Two interface modes are available in EC Lab Express Standard interface mode and advanced interface mode The figures below present the screenshot corresponding to each mode A Load previous settings de Load previous settings G Experimenti lection Cell Characteristics a ak VMP3 0230 amp JA SP 300 0001 a E E Techniques selection a Techniques selection ocy p ory EM 3 6 Experiment2 Sl Voltamperometric Techniques t Voltamperometric Techniques L VMP3 0230 OC Open Circuit Voltage DCV Open C
92. line 70 2992 EIL Ife reais E A a meee ae 71 SO MEC e A A ee ere ree 72 3 3 4 Electrochemical Impedance Spectroscopy SectiON ccoccccoccccncncoonccncnconcncnancnncnnnons 76 D MEAT ms 76 3 3 4 1 1 Electric equivalent elements description sesssuusssse 76 iz LII PARE T UU UU MES 77 SR A ee ee ee ee 77 IA r 6 lon Oe ere ere re ieee epee ent rere ere renee eee eee 78 3 3 4 1 5 Constant phase element Obreros 79 3 3 4 1 6 Warburg element for semi infinite diffusion W sssssese 79 3 3 4 1 7 Warburg element for convective diffusion W ooccooccociconconiconcos 80 3 3 4 1 8 Linear diffusion element M oocccocccccncccncccncocncccnnonnocnnnnnnnonnnonnnonnnonnnos 80 9 94 19 Gescher element Gi dcos dott A 81 3 3 4 1 10 Z Fit selection WINKOW ccceccceccceeeceeeceeeceeecseeceeeceeecseesseesseesseeneeenes 82 9 9 4 T 11 Fitting Medline 82 9 94ET 12 JADDIICATOLL eisin tin ea E Pevdadus ttu eai essa tui Dt ri DM DesVa tiU Dtu rH Deega ES a3 Sotelo Fiton successive CYC Shure a a a a 84 9 9 4 1 14 ESelldoscaDacltall o mresa as ace S 85 3 9 451 15 Additional DIOLS iia 86 ORE MEM A A T T A A 87 Sabe Z V Rare nani n 88 334 22 Circuit Select A 90 9 942 9 DCSCMONOMN Code rori e tient hate Desc detinere Du 90 EC Lab Express Software User s Manual 4 9 94 9 WOT SEMOUKY FIGs ert A e er O CO CO Asc Das EM EA acetate 92
93. me offers the possibility to the user to record the potential of the counter electrode record external signals pH T P using the analog input 1 and input 2 Add an external signal to the voltage or current control connection is done via analog Input2 For the current control the resistance of interest is defined in the table below have an additional parameter corresponding to the control mode record the charge Q record the range in the mpr file Ece C Analog IN 1 G 10v v Analog IN 2 External Control Control charge LI IRange Fig 18 Record External control options window 2 2 EC Lab Express Software User s Manual Current range resistance 1A 1 Ohm 100mA 10 Ohm 10 mA 100 Ohm 1 pA 1 MOhm Preparing and Running an Experiment with EC Lab Express software This chapter is designed to guide users through the use of EC Lab Express software 2 2 1 The Bar menu da ipad seima Bio Logic Home Page de Load Data File Check For Updates EM Import Data File Newsletter mport Data File X Options ewsletter Exil Representations About Fig 19 The three menu items in the menu bar The menu bar offers the ability to load settings or data file previously stored and to import data file but also to choose to use the advanced browser or specific graph Representations but also to check for manuals and updates 2 2 1 1 The File menu The File menus offe
94. mical reactions consecutive to the applied potential The cyclic voltammogram is a current response as a function of the applied potential Fig 28 Parameter and description tab of the parameters frame 2 2 2 4 Graphic frame The graphic package is a complete tool This is the same as EC Lab software It will be described in a following section 23 EC Lab Express Software User s Manual oe Graph PEJA A R g bollvs Ewe C Show ls CV Fe basique 1 mpr ele vg Ewe Ew e V vs SCE 0 5 Fig 29 Graph displaying frame with tool bar 2 2 3 Selecting a technique When a channel is selected the user can either select a new technique from the list of techniques with default parameters or load an existing setting previously built To select a new technique click on the Techniques line The technique selection window appears 24 EC Lab Express Software User s Manual T Experiment Techniques 3 Load previous settings Cell Characteristics Selection E oh SP 0218 a Techniques Techniques selection DD Il C Adv E Voltamperometic Techniques E les Impedance Spectroscopy Se PEIS Potentio Electrochemical Impedance Spectroscopy GEIS Galvana Electrochemical Impedance Spectroscopy Se SPEIS Staircase Potentio Electrochemical Impedance Spectroscopy SGEIS Staircase Galvana Electrochemical Impedance Spectroscopy E 5 Pulsed Techniques p DPY Diffe
95. mpr Ej POT_Fe basique 1 mpr s zpotb 10loops mpr ZpokBornierz 1 mpr File name EV Fe basique 1 mpr Files of type EC Lab data files MPR MPP MPT Fig 37 Open file window Select the data file you want to open and click on Open 3 1 3 The data file and plot selection window Right click on the mouse the following menu appears In the Plot menu select Selector The following window will be displayed 36 3b Comments d Hide OCW Points i Load Files AJO 55 add Files A Remove Trace AlE F E Save Data File As Ctrles LOG History Y Edit surface and Mass ae Active Trace Ea Add Graph Copy d Eh Print Ctrl P e Graph Properties Alt P Ewe ws E Tvs E Ewe Iws t Ewe vs 1 I v5 Ewe lag I vs Ewe Ewe vs lag I Selector Fig 38 Plot menu ka Alt4 5 EC Lab Express Software User s Manual File Selection Variables 1 LA Documents and Settings test express sFilellb2 mpr cum E n2 mode times control Ewes I mA cycle number IL JISIL IL IET gt JSIE TL IL TE JLJEIE IE TE Same selection for all Files Hide Additional Variables Fig 39 File selection window The user can choose to plot another visualization for example time s for X Ewe V for Y1 and lt l gt uA for Y2 The loaded file contains the recording of the following variables the time time s the workin
96. nd proportionality between X and Y axes Monochromatic black line The other curves in this style will be in black with dash or dot lines This style is specially dedicated to scientific articles Nevertheless the user can define his own style defined with all the functions of the Graph Properties window Traces Axes Units Graph Options e Creation of a new graph style is possible with the button This new graph style will be recorded automatically 41 EC Lab Express Software User s Manual Graph properties Predefined Graph Style All the Axes properties can be changed in this 2210 tab Select the axis you Custom Graph Style want to modify in the Traces Mls t 1 asiz er index tabs es It is possible to change Title p g p Cw t the title of the axis but Graph scale 32006138001 gt 71974596001 also to adjust the axis Options _ Scientific Notation range to the user s v Process f convenience The user O Invert Axis can also change the v Grid notation to scientific mode or invert the axis EE positive values on the scr Proportional left and negative values O Shift Y axes on the right oi The grids can be hidden while deselecting the box Font The user can choose the color and the style of the grid Fig 45 Axes window In the option part the user can choose to display his data with the X and Y axes proportional generally used for Nyquist
97. nect it to a power source provided with protective earth contact Any interruption of the protective earth grounding conductor outside the instrument could result in personal injury Guarantee and liability claims in the event of injury or material damage are excluded when they are the result of one of the following Improper use of the device Improper installation operation or maintenance of the device Operating the device when the safety and protective devices are defective and or inoperable Non observance of the instructions in the manual with regard to transport storage installation Unauthorised structural alterations to the device Unauthorised modifications to the system settings Inadequate monitoring of device components subject to wear Improperly executed and unauthorised repairs Unauthorised opening of the device or its components Catastrophic events due to the effect of foreign bodies ONLY QUALIFIED PERSONNEL should operate or service this equipment EC Lab Express Software User s Manual Table of contents EquUIPmentinstalal O aaa Enea de CE elk tat sul Intended use of the equipMeNt cccoocncccnccccnocncncnonccncononnnonononnnnnnnnonnrnnnnnnnnnnenarnnnanonos IiSraodons TOUS Suicidio iE Sut vn uA DU bras General safety CONSIAeratiONS cooocccccccnccccnnccncncnnnnnonnnnnnonnnonnnnononnnonnnnononnnonncncnnnos la MTP OCUCU ON e EET Lt Tem 2 EC Lab Express softwar
98. nerated when the user makes one or several fits on a mpr or a fit mpp data file The results of the fits are saved one after the other when the user clicks on the Save button This file is a text file that can be open Each fit result can be printed alone or with other fits During the experiment e Data from measurement results are appended to the mpr file e Possible modifications of parameter settings are updated in the mpl file and replaced in the header of the mpr file The mpl file is then the Log of the experiment During the experiment this file can be read with a text editor but users should not try to write in this file or to save it because any modification will make it unserviceable by the EC Lab Express software 2 3 2 Variables description oeveral variables are standard and common in every technique and application in the software Every data file contains state bytes that can be hidden in the selector Several additional variables are dependent of the technique used cf additional variables Depending on the techniques some processed variables can be created either automatically or by the user For EIS techniques the variables are related to Z and admittance variables are processed Variable description Variable name Time in s time s I current in mA mA Ewe WE potential versus REF in V Ewe V Ean potential control in V control V la current control in mA control mA E e CE potential versus
99. new Graph Style For this example a Graph style named Style example is defined in such a way that the curve 1 is defined as red solid lines and fushia triangles markers and the curve 2 is defined as blue solid lines and blue sky diag cross marker Fig 55 The Graph Style definition includes all the graph properties These properties were previously defined in the section 3 2 4 Once the definition of the Traces Axes Units Graph and Option has done the user has to click on OK and the new graph style is added to the Graph Style list 49 EC Lab Express Software User s Manual Graph Representations Name Ewe vs t Ewe vs SS i Advanced vs Ewe Representation delta vs Estep Graphic style association Logll vs Ewe G i raph properties x Ewe ve Lodi Se lt None gt J O vs t Predefined Graph Style Techniques association Ap vs t se Line style Bode Impedance E Selected techniques Bode Impedance odd Nyquist Impedance Nyquist Impedance oc Traces Name Black Impedance Axes Black Impedance odd Zl vs t Mott Schottky Graph UE Options Add Remove Style Plot Lines Markers v Line Solid v Ped a a Marker GET y E Red ali Units Options Hide OCY Points Draw only lines over fono points Note common parameters for all Undersample traces ov
100. nfiguration button Refer to the Installation and configuration manual for more details on the WE to Ground connection mode Warning it is important to disconnect the electrodes from the cell before changing the electrode connection because of the difference between the leads assignment the OCV may not be properly applied 2 1 3 2 Channel This menu is only available for the SP 300 technology The Channel menu permits the selection between Grounded and Floating mode for the used channel Floating mode is recommended only when the studied cell is grounded for example autoclaves pipeline f Grounded 3 Floating 2 1 3 3 Filtering This option is only available for the SP 300 technology It is possible to filter potential E and current I by hardware with low pass filters Three filters exist 5 Hz 1 kHz and 50 kHz It is also possible to obtain the raw data by selecting No filter None none 2 1 3 4 Ultra Low Current ULC measurement This option is only available with the SP 300 technology and more especially when the Ultra Low Current option is connected to the channel Two modes are available Standard and High Speed Scan This High Speed Scan option is necessary when low current ability at relatively 14 EC Lab Express Software User s Manual high speed is required In these extreme conditions measurements may be distorted For instance a loop appears at the vertex lt l gt vs Ewe UME
101. nimization maw Fail Do vau want to proceed anyway 7 Fig 126 Tafel Fit minimization message For this reason it is possible to enter directly Egor lcorr Ba and Be values and then continue the minimization Unchecking the boxes around Egor li Ba and Be will remove the 103 EC Lab Express Software User s Manual corresponding value from the minimization And at any time one can restart the calculus from the linear fits by clicking on the Calculate button Reference Press W H Teukolsky S A Vetterling W T Flannery B P Numerical Recipes in C second edition Cambridge University Press section 10 4 408 412 1999 3 3 5 3 Corr Sim The Corr Sim tool allows user to simulate data All Corr Sim these methods are based on the Stern and Geary model Stern and Geary ref 1 proposed a model of a corroding system that involves two electrochemical reactions an oxidation process and a reduction process This model is based on the Tafel equation that predicts that the logarithm of the current observed in an electrochemical process is directly related to the Parameters Econ EE mv corr 3 000 Tn Q Hee D and Bo e se b and B difference between the applied potential and the open circuit potential b E 10 000 V b E 30 000 sel Output The Stern equation can be expressed as follow E Econ _E Ecory K E Lo 10 f 10 Technique ALE Ecorl A LE Frew Wd NE p where I E is the t
102. nt please contact your local retailer list available following the link http www bio logic info potentiostat distributors html The highly qualified staff will be glad to help you Please keep information on the following at hand Description of the error the error message mpr file picture of setting or any other useful information and of the context in which the error occurred Try to remember all steps you had performed immediately before the error occurred The more information on the actual situation you can provide the easier it is to track the problem The serial number of the device located on the rear panel device gt Model SP 150 s n 0001 Bio Logic SAS Power 110 240 Vac 50 60 Hz Fuses 10 AF Pmax 650 W www bio logic info CAUTION CE DO NOT OPEN ATTENTION RISQUE DE CHOC ELECTRIQUE NE PAS OUVRIR The software and hardware version you are currently using On the Help menu click About The displayed dialog box shows the version numbers The operating system on the connected computer The connection mode Ethernet LAN USB between computer and instrument EC Lab Express Software User s Manual G eneral safety considerations Y Class WARRANTY The instrument is safety ground to the Earth through the protective conductor of the AC power cable Use only the power cord supplied with the instrument and designed for the good current rating 10 A max and be sure to con
103. o create a Graph Style In the menu bar select the Representations menu The Graph Representations window will be displayed in this window select the Advanced tab and the four already predefined Graph Styles will be displayed Fig 53 To define your own Graph Style click on the button the window Graph Properties will be displayed as shown Fig 54 Graph Representations Ewe vs Ewe vs lve Ewe delta vs Estep Graphic style association Loglll vs Ewe Representation Advanced Ewe vz Lodg ll Bl G ws None gt Rip vs f Technique Line style Line Markers style Bode Impedance Select Y prop style Bode Impedance odd Monochromatic style Nyguist Impedance Nyquist Impedance oc Black Impedance Black Impedance add vs t Mott Schottky Fig 53 Graph Style selection 48 EC Lab Express Software User s Manual Graph properties Predefined Graph Style Les AAA Traces Traces Name Axes Urita Graph Options Style Flot Undersampling Options Hide OLY Paints points Note common parameters for all points graphic windows Draw only lines over Underzample traces aver JU Graph style name Name Style example Fig 54 Graph Properties window in the Graph Style creation When clicking on the e button a Graph Style name window appears then the user can choose the name of the
104. o the counter electrode Fig 14 48 V control mode for SP 300 technology To set the standard connection proceed in the same way disconnect first S1 S2 and S3 from the cell and only after disconnect P1 and P2 select Electrodes connection standard and set the next connections P1 and S1 leads to the working electrode S2 lead to the reference electrode S3 and P2 leads to the counter electrode Then click on Apply configuration button Refer to the Installation and configuration manual for more details on the 48 V control connection mode 2 1 3 1 4 WE to Ground mode This connection mode is only available with SP 300 and SP 200 instruments for special experiment such as Hydrogen permeation 13 EC Lab Express Software User s Manual Disconnect the cables from the cell select Cell Connection Electrodes connection WE to Ground and reconnect the cell as follows Ground and S1 leads to the working electrode S2 lead to the reference electrode P1 and S3 leads to the counter electrode ground WE 51 Co sal Exe 53 El Fig 15 WE to Ground mode for SP 300 technology To set the standard connection proceed in the same way disconnect the electrodes from the cell select Electrodes connection standard and set the next connections P1 and S1 leads to the working electrode S2 lead to the reference electrode S3 and P2 leads to the counter electrode Then click on Apply co
105. ococnnnonononannnonnnnnnnnnnnonnnonacnnonannos 2 2 5 Running ACQUISITION cccccecccececeeeceeeceeeneeeseeeseeeseeeseeseeeseeesseeseeeseeeseeeseeeneeeseeenes 2 2 6 Running synchronized experiment ccccccceeccceeeceeeeceeeceeeeceueeseeeeeueesueeseeeseneeseess 2 3 Data pro Pen SS sec ies es ths Acacias D ON DN age AAA AA ee 2 3 2 Variables CESCHIDUOM i200 euis dessus ketoecdi tinae eu clos pa CR anu SR ben tacclu ee aanudest 2 9 9 Dala TECOFGING cousssassxes ovest ent pore prae Erat dd td Pra EUA pdas diga 2 0 0 Dala VIA israel recado 3 EC Lab Express software Graphic DiSplay mmmccommccnsccnnnsccnnaannnnaann nana nrnnrcn rana caninos 3 1 Te Graphic WANGON ciri 3 1 1 The graphic window right click MenNu occcocccocncocncccncnccncocncncnnononnnnnncnonnnonnnonanonannns 3 422 Loading adata Mes dis 3 1 3 The data file and plot selection WINdOW ccoocccocnccocncccnccocnconcnnnnnonnnncnnconnanonncnnnnos 3 2 210 fee 2 el ote te Minter tee ern oe rt at A E 3 2 1 Sh WHide DONS eee Ee EE Ere ooo ev PR a ee ede a 3 22 Add COMMENTS ondhe graph sesso cde oa o endete ae ede ecd eae benda adc EC Lab Express Software User s Manual 3 2 3 Three Dimensional graphic ccccscccscccececeeecececeeecececeeeceeecececeeeceueseeeseeeseeeseeenes 39 9 2 4 Graph properties carrere tds tux pud tir ita 41 3 2 5 Graph Representation Tent ooo e o Fere ete Eee te Peta ade Doe Ro ec bate Dae dde Cuv ues 45
106. odify the IP Address to have a valid address in your network Repeat this procedure with the Gateway and click on Modify device A warning message is displayed click on OK When the process is in progress an orange message is displayed and when the instrument receives the new IP address a configuration changed message is displayed in green oeveral Bip sounds are emitted indicating that the communication board is reinitialized with the new IP Address Configuration changed appears at the bottom of this window Advanced ethernet settings Device 5P 300 0002 MAC address 00 14 D 8 01 03 8E Warning IP address 192 109 209 222 Metmask 205 255 255 0 A WARNING modify configuration of the device selected Gateway 192 109 209 222 Modify device Advanced ethernet settings Device SP 300 HOD MAC address O00 14 D 8 01 03 8E Configuration in progress Cloze EC Lab Express Software User s Manual Device gt Advanced ethernet settings Device S5P 300 0002 MAC address 00 14 08 01 03 8E IP address 192 109 209 222 Metmask 255 255 255 0 Gateway 132 103 203 222 Modity device Configuration changed Close Fig 6 Instrument new configuration Then click Close to display the New Device window where you have to click Refresh to refresh the window and select your instrument IP address Now the instrument is ready for use When connected to the web the so
107. oftware This copy option is available only with data files including potential current and time Three data rows are copied in the clipboard in the following order E and t This option only copies the data points corresponding to the displayed points on the graph 3 2 8 Print options Print menu displays the print wndow The user can print only the graph He can also choose to print the log file and some comments added by the user in the comments tab All will be printed on the same paper page The printer setup is also available with the setup button A print preview is available to see the different parts of the page 92 EC Lab Express Software User s Manual Printer ES A HF Laserlet 4100 Senes PS Setup Preview Log Comments Print Graph PETENS i o es 2 iv Print Comments P gui que once die We Print LOG Fig 58 Print window Note the date is displayed and printed automatically in the top right corner 3 2 9 Multiple graphic in a window The EC Lab Express software graphic window is capable of displaying several different and independent graphs Four graphs can easily be displayed in the same window o3 3 3 EC Lab Express Software User s Manual we Graph ES PBR S ES E gt Ng Test Box 4 GEIS mpr CV Fe basique 1 mpr Im Z vs Re Z l gt vs Ewe 2 500 2 000 900 L 1000 n i ag 500 500 2 000 4 000 Re Z 0hm Ewe V vs SCE CV pl
108. otal current at a specific applied Ecor 00 000 mw potential E Eco is the open circuit potential of the Nb points iQ system Ba and p are the Tafel constant for the anodic oxidation and cathodic reduction reactions and are Moise defined as positive numbers 4a lcorr IS the corrosion current corresponding to the anodic and cathodic current at E Eco The total current Noise level 1 000 p Il Ecorr resulting into the difference of the anodic and cathodic current being null as expected Fig 1 Corr Sim window The three proposed methods are presented hereafter The appropriate method has to be selected in the combo box of the output frame Noise in current in potential or in resistance depending on the technique can be superimposed to the resulting simulated data Clicking on the Calculate button gives the simulated curve according to the parameters set The ouptut plot depends on the type of the techniques used The results can be copied in the clipboard to be pasted in the print window comment zone or in a text file They can be saved in a text file Heference 1 Stern M and Geary A L J Electrochem Soc 104 56 1957 104 EC Lab Express Software User s Manual 3 3 5 4 Variable Amplitude Sinusoidal microPolarization VASP Variable Amplitude Sinusoidal micro Polarization VASP is a non linear EIS technique used as a corrosion technique to determine the corrosion current and the
109. p Ewe vs freq lll vs freq E we trend removal time s 0 02 Moner we 0 01 trend removal AEN Mane bl Method PSD with DFT v MEM order Results Ewe average 2 448e 3 V average 0 473 5e 6 A G Ewe 0 935 7e 3 V ol 0 184 Se b 4 An 5 061 Ohm T Fig 132 Electrochemical Noise Analysis on system with a 100 mHz electrochemical noise Ewe V ha viii freqiHz 108 EC Lab Express Software User s Manual 4 Glossary This glossary is made for the user to understand most of the terms of EC Lab Express software and the terms mentioned in the manual Classification is done in the alphabetical order Absolute value mathematical function that changes the negative values in positive ones Amplifier current power booster that can be added to each channel individually Bandwidth represents the frequency of the regulation loop of the potentiostat It depends on the electrochemical cell impedance The bandwidths values are going from up to 8 with increasing frequency CASP Fit tool available in the Analysis tool menu It allows user to determine corrosion current and Tafel parameters Channels each one of the boards corresponding to an independent Potentiostat galvanostat Characteristic mass total mass of the species in the electrochemical cell in most of the cases It is different from the mass of electroactive material This mass is used in the graphic display to represent mass cu
110. phase angle is constant z 4and independent of frequency The Warburg is unique because absolute values of the real and imaginary components are equal at all frequencies 3 3 4 1 7 Warburg element for convective diffusion W The Warburg element for a convective diffusion is an approximation mainly used in case of diffusion on a Rotating Disk Electrode in a finite length The mass transport is Supposed to happen only by diffusion in the Nernst diffusion layer and the solution is considered homogeneous outside this layer The impedance when the material diffuses through the Nernst Diffusion Layer is described by W Description Diffusion convection Impedance UICEENEEIE A73 Zn Myquist Diagram Im z vs Rel zii Pai Fig 99 Warburg element for convective diffusion The Warburg element for convective diffusion is equivalent to the Warburg element in the 2 54 2T high frequency range f 3 3 4 1 8 Linear diffusion element M This diffusion element is used for finite length linear diffusion for example in the case of insertion reactions 80 EC Lab Express Software User s Manual Description Linear diffusion My Impedance 211 Pas cath 2E Vra ent Muquist Diagram Irm z vs Reli Fig 100 Linear Diffusion element The linear diffusion element is equivalent to the Warburg element in the high frequency 3 88 LNT 4 range f and to an R and C in series circuit
111. presented variable Specific units are available for current and charge on one hand and for power and energy on the other hand For current and charge the user can select a current density or a charge density according to the electrode area or to the electrode characteristic mass The Electrode Surface area and Characteristic Mass window is used in the unit window for area charge or current density plot The characteristic mass is also used for specific power or energy plot The user has to set the working electrode surface area characteristic mass and choose the unit Clicking OK will modify the graph according to the new surface but this area is not saved in the raw file Click on Save to file to save the surface in the raw data file 43 EC Lab Express Software User s Manual Title The user can show or hide the graph legend He can CV Fe basique 1 mpr define the position the font dle vs ff Ewe name style and size the apn eS background color and the transparency of this Predefined Graph Style mw Os Pole _ A title can be added to the Custom Graph Style graph to describe the aces v Legend experiment The text must fees Position v be typed in the box The Units Font Name Arial v user can choose the title s Font Style a a format font font style size Options Background Owie ow and color To improve contrast and legibility for a presentation Transparency JJ v Ti
112. r i e C 2 vs Ewe SPEISdiode mpr i gt e C 2 vs Ewe SPEISdiade mpr 3 140 000 120 000 100 000 so 000 60 O00 40 000 20 000 04 03 02 1 O lt Ewe gt V Fig 115 Mott Schottky plot It is possible to set the surface area and plot a capacitance related to the surface 3 3 4 3 3 The Mott Schottky Fit Motk Schottky The Mott Schottky Fit His a graphic tool introduced Parameters with the SPEIS technique to determine semi Temperature 25 0 C conductors parameters flatband potential and donor Dielectric constant 10 density based on the Mott Schottky relationship from Surface Area 5000 cm a Mott Schottky plot Before using this fit a Mott Results Schottky plot 1 C vs Ewe of the experiment must be File CXECLabeclab v3 10 displayed on the graph This plot shows one trace for Range 0 020 16 V 0 260 1 V each selected frequency Frequency 100000 kHz The Mott Schottky Fit corresponds to a linear fit for Flatband potential 0 2611W Donor density ff ofel2 cm each trace one trace for each selected frequency The same potential range is used for every trace Frequency 46 406 kHz Flatband potential 0 765 2 Donor density 2 ald3elz cm When a data point zone is selected click on Calculate Frequency 10 000 kHz A straight line for each trace is displayed as a result of Flathand potential 0 748 V the linear regression between two green circles with Donor
113. rential Pulse Yoltammetry pl Siwy Square Wave Voltammety anl HPY Normal Pulse Yoltammetry anl ANPY Reverse Normal Pulse Woltammetry ail ONPY Differential Normal Pulse Volkanimetry mu DRA Differential Pulse Amperometry ee Stack Techniques E 4 Corrosi n Techniques EWT Ecorr vs Time LP Linear Polarization GC Generalized Corrosion CPP Cyclic Potentiodynamic Polarization POP Potentiodynamic Fitting PSP Potentiostatic Fitting RA Zero Resistance Ammeter CASG Constant Amplitude Sinusoidal ul alyvanopolanzation CASP Constant Amplitude Sinusoidal Polarization VASP Variable Amplitude Sinusoidal pPolarization E Ohmic Drop Determination Techniques E Trigger Ea E Bipatentiastat Fig 30 Techniques selection window To add a technique click on the F button and select the desired technique line on the Technique selection window and double click on it To remove a technique select it in the Experiment tab and click on the button Techniques available with EC Lab Express software have been separated in several fields voltamperometric techniques impedance spectroscopy pulsed techniques corrosion techniques ohmic drop determination techniques and triggers techniques stack bipotentiostat and multiplexer techniques if the advanced interface is selected On the top of this window the user can choose to add a technique from file already used before with parameters To select settings from
114. representation and to differentiate from the rest of the grid the axis origin color style or line size The font type and size is also available from this option menu Note On the graph the user can move one of the Y axes with the mouse left click in order to adjust the origin of both Y axes Put the mouse on the axis to see the e and move the axis 42 EC Lab Express Software User s Manual Graph properties e Predefined Graph Style rese A O Custom Graph Style Traces Graph Units Axes Time Graph Current Options C Charge Frequency Resistor Power Energy Capacity i Potential vs Reference Electrode Offset potential vs Normal Hydrogen Electrode 0 000 Edit Surface 4nd Mass Fig 46 Units window Power and energy can be plotted according to the electrode characteristic mass In such a case the software will ask for the electrode surface area or for the characteristic mass The following window will be displayed Edit parameters File CY Fe basique 1 mpr Parameters Electrode surface area Characteristic mass 0 001 cof oom g v Fig 47 Electrode Surface Area and Characteristic Mass window Graph Units window is used to choose the correct graph units for the different variables he default units are in gray boxes If the user chooses another unit he must activate his choice by ticking the box corresponding to the re
115. rite circuits it is necessary to give a number for each element to separate the different elements If the syntax is not correct an error message will be displayed 90 EC Lab Express Software User s Manual EC Lab Express 6 Circuits created by the customer will be stored in the list in blue They can be modified removed from the list or moved in the list 7 For the selected file ZPOT Fe basique mpr find the correct circuit Randles Circuit R1 Q2 R2 W2 8 Click on Calculate to show the corresponding curve on the graphic window Zsim mpr l Im Z vs Re Z Set Frequencies from F 500 000 with ID points In spacing Equivalent circuit ATAZAA ZWZ v parameter Ohm F s a 1 Ohm Dhm s 1 2 1 050 1 100 Re Z Ohm x Fig 112 ZSim Circuit Edition window 91 EC Lab Express Software User s Manual 9 To adjust this curve to the experimental one the user must adjust values for each parameter as described in the window below and click on Calculate Zsim mqg Im Z vs Re Z Set Frequencies from F 11 00 000 with 10 paint Equivalent circuit ALSO 2 R24w2 v Edi rts dmi Z O hm parameter value Ohm F s a 1 Ohm DIhm s 1 2 Reizyohm Fig 113 ZSim Circuit Edition window with adjusted parameters The results can be copied to the clipboard and saved in a Zsim mpr file The user can modify parameters as much as he wants in the tab
116. rmine the peak current the peak potential exchanged charge quantity and several other parameters Record in each protocol the command to define the number of points in the data file The user can define several recording conditions with potential or charge variation depending on the galvano or potentio mode and with time frequency These data recording option reduces the number of points without loosing any interesting changes in the curve Reference electrode in EC Lab Express software the user can choose a reference electrode in the list or add its own reference electrode R Fit tool available with the graphic display used to calculate a polarization resistance Run button that starts the experiment Scan rate speed of the potential sweep defined with the smallest possible step amplitude Selector window in the graphic display allowing the user to load add or remove a data file from the graph and to choose the axis parameters Smooth option that calculates and displays sliding averaged values with n previous values Specifications characteristics of the instrument such as cell control or current and potential measurement Stern and Geary model model of corroding systems based on the Tafel equation Stop button that stops the experiment Subtract files this tool allows the subtraction of two curves for example to subtract a background from a curve Tafel fit tool available with the graphic display used to determine w
117. rrent density or mass charge density Compliance correspond to the potential range of the counter electrode versus the working electrode potential This option is used in molten salt electrochemistry where the potential decreases a lot between the counter and the reference electrode Cell connection connection of the instrument channel board to the electrochemical cell with five leads Circular fit tool available with the graphic display used to fit a curve and to determine the parameters of the circle such as the capacitance Cycle inside a protocol this term is used to describe a sequence repeated with time Cycle number processed function that allows the user to display on the graphic one or several cycles chosen in the raw file The selected cycles are lightened and the others are hidden Cyclic voltammetry CV this protocol consists in scanning linearly the potential of the working electrode and to measure the current resulting from oxydo reduction reactions Cyclic voltammetry provides information on redox processes electron transfer reactions and adsorption processes Description tab in the experiment selection window that describes the chosen protocol Device EC Lab Express software window in the Config menu used to add new instrument IP address to be connected to the computer E range potential range used in the experiment It is related to the potential resolution 109 EC Lab Express Software User s Manual
118. rs the ability to load settings or data files previously stored and to import data files from other software such as FC Lab Power Suite GPES CONDECON etc The import data file window is shown in Fig 20 In a first time the file to convert has to be loaded and the first lines of this file are displayed in the frame of the Input Text File part To import data in a right way the user has to define in the Importation parameters part the file format the columns separator and the format number of column columns type Note that if the format file to export is already in the database of EC Lab Express selection of the format is automatic Then to finish push the Import button and the file will be exported in EC Lab Express format mpr file 17 EC Lab Express Software User s Manual Import Data File Input Text File File GEIS 25cm2 elt Load Directory C Program Files FCLab 5 10 2 Data S amples Size 161 107 bytes Show Tab and Space FC Lab ASCII FILE File Version 5 001 Date 04 06 2007 Time 15 09 48 Importation Parameters File format FC Lab Columns Separator Tab v Colums Frea Hz IEwel v llwel amp Theta we rad Ewe dc V lwe_dc 4 Range we Eceli Automatic detection Number of columns Columns type Column DE Variable Input file current polarity convention Positive oxidation standard IUPAC convention Positive reduction inverted convention Importation Imported Fi
119. s used aiet sire Clam for the fit in the Selection frame Correlation 0 9999 The results can be copied to the clipboard to be pasted in the print window comment zone or a text file They can also be saved in a text file Fig 65 Linear Fit window PEIS_Fe_basique_1 mpr Im Z vs Re Z 130 120 110 100 S 90 gt 80 TO Z O 60 N E 50 40 30 A o o 20 o o o opos 10 p 01 ms 20 50 100 150 200 Re Z Ohm Fig 66 Linear Fit on the graph 98 EC Lab Express Software User s Manual 3 3 2 3 Circle Fit When the zone to fit is selected click on Calculate in the Circle Fit window Fig 67 A part of a circle curve is displayed as a result of the regression between two green cursors with the Least square method fit Fig 68 Move the cursors with the mouse by holding the left mouse button to modify the range of data points selected for the fit The new regression is automatically calculated when one of the cursors is moved The coordinates of the first and last data points used for the fit are displayed as well as the number of points used for the fit in the Selection frame In the Parameters frame an iterative algorithm allows for the adjustment of the results using a minimization with the simplex method The results displayed are the parameters of the circle The depression is the angle between X axis and the diameter defined from low X intercept R is the difference
120. the pyrrol monomer oxidation The result variables are the same as for the analysis with a straight baseline pyr4 1 nOd mpp ys Ewe cycle 16 I mA Ewe V Fig 84 Peak analysis on a cyclic voltammetry experiment using a polynomial baseline 70 EC Lab Express Software User s Manual 3 3 3 2 Wave analysis The wave analysis is the most useful tool for the analysis of experiments performed in a hydrodynamic Wave Analysis regime specially a rotating disk electrode Selection Results When a data point zone is selected click on Results Calculate E1 2 0 4001 Y The wave analysis is made according to two straight lines These lines are defined using a linear regression fit The software will automatically find the two parts of the curve with the weakest slope for the fit For the first regression the first 20 of the selected data points are taken into account The last 20 of the selected data points are taken into account for the second regression The data point zone for the analysis is shown in the Selection frame by the extreme points a O23 me Ne he Results of the analysis are displayed in the Results frame Several values for the wave are displayed Ej and the limit anodic and cathodic currents The results can be copied to the clipboard to be pasted in the print window comment zone or a text file 7 Fig 85 wave results tab They can also be saved in a text file l mA
121. tion or fit of the ES parameters will be done If the result is not acceptable Noise level 100 S em it is possible to reach a better fit by clicking on Minimize This minimization is only possible when the box associated to the value to minimize is ticked Fig 78 Multiexponential Sim window The Multi Exponential Fit is able to perform a fit on Multi Exponential Fit every data displayed in EC Lab software The combo um E box in the Fit block offers two possibilities to initialize From point O the fit from the Auto estimate values or from Current co parameters boar Note that the x0 value cannot be fit and must be set Y 21725 0m1 Total points 1000 manually by the user Parameters A The results can be copied in the clipboard to be pasted y a k xy b 2 cg A E in the print window comment zone or in a text file They s can be saved in a text file m Lam S em 1 zs S cm 1 S cm 1 5 1 S cm 5 1 Fit Init Auto estimate bul Y 1 574 Iterations 321 Fig 79 Multiexponential Fit window 66 EC Lab Express Software User s Manual Conductivity vs time MExpSim mexpfit mpp MExpSim mpr Conductivity S cm 1 5 10 time s Fig 80 Multi Exponential fit result 3 3 3 General Electrochemistry section 3 3 3 1 Peak Analysis A peak analysis tool is available with the EC Lab Express software Like other analyses with the EC Lab Express software the
122. tle for example the user can Text change the color of the Font Mame Arial v graph background Font Style Bold 16 amp Note When several traces FontColor Mines v are plotted on a graph the user can select the active Graph trace by clicking on the E corresponding legend Fig 48 Graph window Graph properties e Predefined Graph Style l This window allows the 3 user to choose to work in Custom Graph Style inverted convention for the Traces Current polarity convention current polarity Anes Positive oxidation standard IUPAC convention It is also possible to adjust Units O Positive reduction inverted convention the graph size to the Graph monitor format ps bons Monitor format Note common para Fig 49 Options window 44 EC Lab Express Software User s Manual 3 2 5 Graph Representation menu It is possible for the user to define fast graphic displaying modes with the Representation tool in the Config menu The Graph Representations window already offers some standard representations For each representation a scheme of the axes is given For example in the Fig 50 the Bode impedance representation is given This representation is defined as the frequency value on the X axis This value is processed with the log spacing function the IZI value on the Y1 axis This value is processed with the log function the Phase Z value on the Y2 axis It is
123. to choose the shape of the window where the calculation will be done In signal WE Points processing a window function also known as an apodization function or tapering function is a function that is zero valued outside of some chosen interval When another function or a signal data is multiplied by a window Rectangle Y function the product is also zero valued outside the i interval B arlett Hann The 6 windows possibilities are described below M relationship only valid within the interval 1 1 and O Welch outside Fig 74 Fourier Transform window Rectangle w t 1 Barlett w t 1 Hann w t 0 5 0 5cos zt Hamming w t 0 54 0 46 cos zt Blackman w t 0 42 0 5cos 11 5 0 08cos 2 rt Welch w t 1 vt The processed DFT data file is created with the following name filename_dft mpp This tool is very useful to determine if the measurement is affected by environmental noise like 50 or 60 Hz 63 EC Lab Express Software User s Manua CA R 100mHz 01 mpr Ewe vs time vs time 2 AAAAAARARA VVV VV VV V V pm VA 0 02 100 0 1 EwelV C v ull time s CA R 100mHz_01_dft mpp ll mA vs freq Fourier Transform Selection Trace vs time From point O 0 003 A Oz ie O m Ed To point 113 E 0 002 A 1114 Nes 0 019 42 m Total paints 114 0 001 Sampling 0 986 1 s 1 014 Hz Parameters 0 Ee ESE A Windos freq
124. ual potentiostat The user just has to define the device he wants to simulate and click on the Connect button EC Lab Express Software User s Manual The Info button give all the necessary information on the instrument like the serial number the number of channels the firmware version the IP address Device Information Sele o General information Instrument senal number Number of channels 2 Humber of slot 2 Ram size 32 MB CPU 3200 Firmware version 101 Firmware date released on Y 8 2011 Communication Type TLP IP IP address 192 109 209 239 MAC address 00 1408 01 07 FC Metmask 255 255 255 0 Gateway 192 109 209 239 Close Fig 4 Information window 2 1 1 1 Instrument IP address and gateways change network connection If the default IP address of the instrument is not compatible with the network IP addresses it is possible to change the IP address of the instrument This change can be done in the Device window Fig 2 Select the desired instrument and click on Modify The following window then appears EC Lab Express Software User s Manual Advanced ethernet settings Device MAC address IP address 132 103 203 233 Metmask 255 255 255 0 Gateway 192 709 209 233 Modity device Close O un D D EN LI e g ra ce co o amp 8 MEO ca rm Fig 5 Modify window of the Device window used to change the instrument IP Address M
125. wo cursors that can be adjusted for a better fit The polynomial fit used is defined as follows y ax bx cx d The results of the fit are automatically calculated when a cursor is moved Peak Analysis Baseline Peak Baseline Palunamial Hesults Fram Paint e To Port 5 ee ae Total points 2 Slope 0 120 3 m Offset 0 04 1 m Correlation 1 Falyname T Fig 81 Baseline selection tab In the manual mode the baseline is defined by two points represented by circles and set on the curve at the extremities of the zone of selected points In the regression mode the regression straight line determination is made with the least square method Data points used for the regression are automatically selected in the 25 first percentage of the total point number between the beginning of the selected zone and the point corresponding to the max current value The results frame displays the baseline equation and the data point zone used for the regression 68 EC Lab Express Software User s Manual 3 3 3 1 2 Peak analysis results Peak Analysis Baseline Peak When the baseline type is selected click on Calculate i Selecti The software will automatically find the max current edd E lene value in the selected zone according to the baseline From Point 3814 Data points used in the peak analysis are selected by A 0 053 b4 Y default from 35 96 of the beginning of a zone starting ice Mense
126. ye Techies Rest for tp f 1 000 000 e DOCV Record every dEp 100 000 mV or dtp lo 0 010 00 E Range QG 25V Y X 0 vY1 0 Fig 24 Main window when EC Lab Express is connected to the potentiostat EC Lab Express displays only one mask This software is recommended for electrochemistry teaching and new users This window shows the menu bar with File Config and Help and 4 frames Device Experiment Parameters Graph 2 2 2 1 Device frame Device Channel Ewe Current Time Ece 0 040 Y Erange 2 5Y 2 5 Connection Standard a Freq 100 000 Hz lrange 10 mA 1 1 294 mV 0 000 A Os Buffer comp 12 Fig 25 Device frame 20 EC Lab Express Software User s Manual In the Device frame are displayed the channel selected in the list displaying all the channels available in the instrument the amplifier connected to this channel board current values time Ewe l Buffer filling Erange lange the connection mode standard CE to Ground WE to Ground 2 2 2 2 Experiment frame The experiment frame displays the instrument type SP 200 SP 300 VMP3 It is used to build the experiment by linking techniques with the buttons atthe top 7 tr Experiment de m A G Experiment H SP200 0006 Se Techniques Experiment Cell Characteristics E JL SP200 0006 E Techniques E Fig 26 Experiment frame standard and advanced By clicking on
127. yed 3 3 1 Zone selection On the graphic display the zone selection can become very complex when several cycles or loops have been made during the experiment or when several zones are selected at the same time In such a case the software will ask you to select only one trace before doing a fit 55 EC Lab Express Software User s Manual CV platinum 16 cycles mpr ale vs Ewe 20 Selection Paints Selection Select zone E b 312 lt I gt HA 05 1 EwelV vs SCE Fig 62 Zone selection on the graph In this example the selection has to be done between 12 zones To select the zone on which he wants to work the user has to visualize all the zones and select the good one for example the sixth zone displayed in red Then the user has to accept the selection by clicking on OK 96 EC Lab Express Software User s Manual 3 3 2 Math section 3 3 2 1 Min and Max determination On the graphic display select Min Max with the Min Max button or with the mouse right click and the data points where the fit will be performed The Min Max analysis window is displayed Select the zone to fit on the trace and click on Calculate The Min and Max values are automatically detected The minimum and maximum coordinates are displayed in the fit window The minimum and maximum points are highlighted in red on the trace The results can be copied to the clipboard to be pasted in the print window comment zone or
128. ze Simplex Randomize Stop randomize on h 0000 iterations Stop fit on 16 3 relative error Y Weight 1 v rd 14 37 Iterations 163 Simplex Cycle xxxx Fig 106 Fit results and pseudo capacitance calculation The results can be copied and pasted in another document 3 3 4 1 15 Additional plots POT Fe basique 1 zfrt mpp Delta Phase Z1 vs freq log spacing x Delta Zi vs fred lag spacing x D eltai Phase Zi deg es zl eue d 0 1 1 10 100 1 000 10 000 100 000 lfreq Hz log spacing Fig 107 Plot of the relative error on Z and phase vs frequency log spacing 86 EC Lab Express Software User s Manual The equations used for this calculation are described below The same error plot exists for the real part and the imaginary part of the impedance The error is calculated for each frequency IZ meas B Z calc i A Z Z x100 Alp lp meas le calc Re Z Re Z Im Z Im Z ARe Z uu Alim Z E 100 Right click on the graph to see the menu and select Selector to display the following window offering the possibility to display the relative errors The same window can be accessed from the rapid graphic selection bar select Custom File Selection Variables SEL Lab sDrata sS amples POT Fe basique 1 zfit mpp A Fi freg Hz RelZ10hm Imi Ohm 710 hmm Fhase z deq Delta Re z7 D elta

Download Pdf Manuals

image

Related Search

Related Contents

Jura F7 PDF - 1st in Coffee  Rust-Oleum American Accents 215191 Use and Care Manual  - Haag  Service Manual - Manuals, Specs & Warranty  ImageMaster 2D Platinum 7.0 - GE Healthcare Life Sciences  Dell™ W1700 LCD TVユーザーズガイド  SSV7 TROUBLESHOOTING  Burnham PF-5 Series Installation and Operation Manual  EPC II User Manual  

Copyright © All rights reserved.
Failed to retrieve file