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1. 1500 2000 0 time sec Figure 2 4 Hydrogen charging current curve under control of square wave Due to diffusion rate limitation of the hydrogen atoms there will be a current delay on the hydrogen detection side with the phenomenon that anode current gradually increases with time on the rising edge or decreases on the falling edge According to delay duration of the hydrogen detection current and the current value users can figure out the concentration of hydrogen in the metal as well as the diffusion rate and further determine certain corrosion inhibitors effect on hydrogen permeation 49 User s Manual E Hydrogen Diffusion New Data File Filename Comments OCP V 0 80063 Data Acquisition Hydrogen Atom Oxidation Main Unit f Interval l a Applied E v 0 20 f Frequency Hydrogen ions Reduction Slave Unit 1 When residual hydrogen charging BiStat Config Peak Current 5 Time 1 Valley 0 Time 2 Unit mA Unit Hours Slave units Cycles am Cell E Axis Type vs Time 5 ES 11 1 1 Data File When the experiment is performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This is particularly useful if you forget the file names you have already used However before CorrTest begins performing the firs
2. 100000 AC Amplitude 10 FinalFreq Hz 0 01 Petat Gstat Cell C Linear Logarithmic 10 Steps Decade OCP will display the current open circuit potential of the electrolytic cell updated per second It is particularly useful for the users to determine whether the working electrode is stable for impedance test 12 1 1 Data File When the experiment 15 performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This 15 particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file already exists 12 1 2 Polarization DC potential is the set DC polarization potential of the working electrode during impedance test If the test needs to proceed under the open circuit potential OCP then you can enter 0 and select relatively open circuit potential in the drop down box This moment the potentiostat will automatically give a total output of the pen circuit potential and the DC potential to the working electrode If you need to do the impedance test under 50mV DC potential of anodic polarization you can enter 0 05 V for DC potential If the test needs to be carried out at a fixed potential such as 0 5V vs SCE you can select relative reference electrode in the drop down box a
3. 50 Hz 4st Pulse Width s 0 05 Amplitude V 0 05 Pstat Gstat 2nd Pulse Width s 10 05 Pulse Periad 5 0 20 Fes Final E V 0 10 vs Reference Cell Axis Type EAI vs E Help OCP will display the actual open circuit potential of the cell updated per second If the instrument is turned off this value will display Not Available 8 7 1 Data File When the experiment is performed the data will be saved in the file specified by Data File The Dir button can be used to display list of all directories and files This 15 particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file has already existed 8 7 2 Scan Parameters In Differential Pulse Voltammetry DPV the base potential is incremented from Init E toward Final E A potential pulse is applied Current is sampled before the potential pulse and at the end of the pulse The difference between these two current samples is recorded as a function of potential Init E and Final E should be at least 0 01 V apart vs Reference is used to select an exact potential to be applied Incr E is the increment potential of each pulse it can be chosen from 0 001 V to 0 05V Amplitude can be chosen from 0 001 V to 0 5 V Ist Pulse Width can be chosen from 0 001 s to 108 2nd Pulse Width can be chosen from 0 001
4. the electrode cable and working galvanic Electrode is connected to the electrode cable ground end GND wire black sheath clip and the reference electrode is still connected to the yellow sheath clip See the right figure Run CorrTest software select electrochemical noise measurements and at this time the software window will appear junction potential mixed potential and galvanic current If the current value is positive it means the working galvanic electrode is anodic and the working galvanic 15 a cathode The current is flowing from electrode to electrode II A negative current is the opposite During measurement potentiostat automatically switches the range according to the magnitude of current 65 User s Manual Electrochemical Noise New Data File Fil ename E V 0 69224 Comments KmA 0 00003 Pstat Gstat Data Acquisition Recording Time Fea Interval BB 0 2 Total Time 200 Sec Cell Frequency Secon ds 5 Hz Cancel Help Axis Type E vws Time 14 1 1 Data File When the experiment 15 performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This 15 particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file already e
5. The Scan Rate determines how fast the potential is scanned between one potential and another 6 4 3 Experiment Termination When the Term box is checked the sweep will end if certain potential and current conditions are met When the Rev is checked if certain potential and current conditions are met the experiment will immediately start sweeping toward the Final Potential The Termination or Reversal will occur when the current 15 above the Current or below Current Either of these conditions must be met to trigger the Termination or Reversal Be aware that the Termination Reversal conditions in the Potentiodynamic experiment are quite different from those in the other types of experiments 6 4 4 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second 15 specified 6 4 5 Axis Type When the experiment 15 performed the data will be displayed as specified by the Axis Type CorrView can be later used to display the data in other formats 6 4 6 Pstat Gstat The Experiments Setup Pstat Gstat menu item 1s usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 6 4 7 Cell Setting See Cell Setting 9 1 The OK button exits the setup diabox saves all the changes you have made and runs the experiment Cancel exits the setup diabox Any changes made to
6. Final E V bs r lvs OCP z Pstat Gstat Cell m neemo Cancel Help OCP will display the actual open circuit potential of the electrolytic cell updated per second This is particularly useful for the user to determine whether the working electrode is stable for impedance test 12 3 1 Data File When the experiment is performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This 15 particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file already exists 12 3 2 Polarization DC potential is used to set the DC polarization potential of the working electrode during impedance test If the test runs around the open circuit potential OCP then you can enter 0 and select versus OCP in the drop down box This moment potentiostat will automatically give a total output of the pen circuit potential and the DC potential to the working electrode If you need to do the impedance test under 50mV DC potential of anodic polarization you can enter O 05V for DC potential AC amplitude value is the amplitude value of the excitation signal of electrochemical Impedance For example E 0 012 sin wt V means AC signal amplitude 15 12mV However under the state of high frequen
7. Staircase Stripping 44 User s Manual Staircase Stripping New Data File Filename Comments Pn OCP V 0 80168 Data Acquisition Staircase Stripping Parameters a 212 Conditioning Ev 0 10 15 i Deposition 10 E Reference M Do Hz Deposition Time s 15 Quiet Time s 15 Initial E v 0 5 Final E v 0 10 Pstat Gstat Inc E V 10 004 Step Feriod 5 10 025 Axis ise ox Cancel Help OCP will display the actual open circuit potential of the cell updated per second If the instrument is turned off this value will display Not Available 10 3 1 Data File When the experiment is performed the data will be saved in the file specified by Data File The Dir button can be used to display list of all directories and files This 15 particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file has already existed 10 3 2 Staircase Stripping Parameters Before the experiment the surface of working electrode needs cleaning by this conditioning step A constant potential deposition step 15 applied to accumulate species on the working electrode surface This potential can be specified to choose either vs Open Circuit or vs Reference The deposition time determines how long the potential will b
8. b 21 24Hr Interval Minutes 4 3 Reset Workstation Restore the default values of all parameters User s Manual Corrtest4 Restore the default settings No 5 Experiment Setup 5 1 Cell amp Electrode Setup In this diabox users can set information about the working electrode and the electrolytic cell m Cell amp Electrode Setting Channel Channel3 Channel4 Electrode Cell Reference electrode SCE Hg Hg2CI2 sat KCl Electrode Area cm JE NHE Density g cm 7 8 Temperature 25 Chemical Equiv 28 Stern Geary Coef mV Active Chan Help These parameters are mainly used to calculate corrosion rate After clicking the button all parameters will be saved in a registration file The Surface Area specifies the exposed surface area of the sample or electrode This parameter does not affect the measurements It will be used by CorShow to calculate current density and corrosion rate The Density Equivalent Weight and Stern Geary Coefficient are saved in the file to help calculate corrosion rates The Equivalent Weight is the Relative Atomic Mass divided by number of electrons transferred during a reaction Take the reaction Fe for example Iron has an atomic mass of 55 847 and transfers 2 electrons so the Equivalent Weight 15 55 847 2 27 92 Equivalent Weight can also be interpreted as mass loss electron transferred
9. Cell Axis vs Time Cancel Help OCP will display the actual open circuit potential of the cell updated per second If the instrument is turned off this value will display Not Available wr 7 4 1 Data File When the experiment is performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This is particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file already exists 7 4 2 Scan Parameters A current sweep between up to 3 separate current setpoints 15 applied and the potential 22 User s Manual response is measured The experiment starts at the Initial Current sweeps to Step 1 and then to Step 1 2 Click on the Use boxes to turn on or turn off Step 1 2 setpoints If a Vertex s Use box is not checked that segment of the sweep Step 1 2 will be skipped The Time determines how long the current will be held at each step 7 4 3 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second 15 specified 7 44 Axis Type When the experiment 15 performed the data will be displayed as specified by the Axis Type CorrView can be later used to display the data in other formats 7 4 5 Pstat Gstat The Experiments Setup Pst
10. CorrTest CS Series Electrochemical Workstation 5 User s Manual Wuhan CorrTest Instruments Co Ltd 1 1 1 2 1 3 1 4 2 1 2 2 3 1 3 2 4 1 4 2 4 3 5 1 5 2 5 3 6 1 6 2 6 3 6 4 6 5 7 1 7 2 7 3 7 4 8 1 8 2 8 3 8 4 8 5 8 6 Contents INTRODUCTION a S A 1 HARDWARE SPECIFICATIONS uestis active OT nieces estat ecient 1 ELECTROCHEMICAL SIGNAL GENERATOR sexe races Cogo niet nena nes a aara a Pase ore 2 FRONT PANE T 2 PO TEN IOS TAIC ODE ae aac E deu 3 INTRODUCTION E NAE EEE hate sac aia ONERE TE ns EAT TEE EEEE A ET TEET abate sac PUR 4 SYSTEM REQUIREMENTS a aaa et 4 SOFPWARE INSTALLATION Sante venice 5 IVE IN cvv ovs Ve iT wal eva Sae ONE Rue Vs Va ovs Uo va E a ved ota cane Vae s ou ewan eva Vs eR ved ova uoo Vado s os Volvo ova Ve VV a ue Ova US 5 ub cm 6 BT D E P WS 6 SYSTEM ETOUR eddie tensor uua ten eM MMC tM s IM adio E 7 COMUPORT SE PUP T 7 TMINGMEASURF MENT Sides Peete uo eate acutum da to Rar dom ettet aids 7 RESET WORKSTATION redde deve tace bud dades eiae Okie os
11. or time in seconds The integration time indicates time cost at each frequency point The longer the integration time the higher the measurement accuracy and the more time it takes Delay time is the waiting time between measurements of two frequencies Before the measurement of the next point the internal frequency analyzer will wait for a period of time allowing electrodes to keep balanced The delay time is usually not needed for the electrochemical system 12 1 7 The impedance spectrum fitting CorrTest uses Zview software as a tool to analyze impedance spectroscopy and graph Zview is powerful for impedance analysis and it can do complex plane diagram amp Bode diagram about data files It allows users to create a variety of equivalent circuit and do data fitting It has functions of graph s locally zooming in curve smoothing data correction and so on Zview can output the graphics to a printer or clipboard and you can also paste a graphic into a Word document Generated impedance data files of CorrTest Z 15 fully compatible with Zview Users can directly click on Zview Drawing menu after data collection and introduce one or more data files from the Documents Data File menu and then select a variety of graphics selection method in the Options activities graphics menu If you want to change the graphics coordinate text you can right click the menu select Settings to modify and
12. the abscissa is the time in second the vertical axis is current vs I the abscissa is the current the vertical axis is electrode potential I vs E the abscissa is electrode potential the vertical axis is current E vs Lg I the abscissa 15 the logarithm value of current the vertical axis is electrode potential I vs time there are two graphs The abscissa is time and the vertical axis separately is electrode potential and polarization current Q vs time the abscissa is time and the vertical axis is the Integral electric quantity This option only works under potentiostat mode If data logger and potentiostat are both at work then display varies according to user selected menu 15 1 2 Work Pass Click on the drop down box on the right side of the working channel under the mode of data logger then the corresponding data of the working channel will be displayed This option is available only in data logger mode recording external signals If the data logger and potentiostat are both at work then display varies according to user selected menu 15 1 3 Live Data Live data shows the latest collection of data From left to right it s time s potential mV and current uA When the users want to know the value of a point on the graph they can move the cursor onto the graph area then immediately there will be a synchronized display of the value on the right side of the c
13. and automatically update working electrode surface state Duration It is a separate time value that specifies the length of time when that conditioning potential is applied Deposition potential Deposition potential 15 generally lower than the standard redox potential by 0 3 0 5V Metal ions which will be measured are easily reduced Deposition time It is a separate time value that specifies the length of time when that deposition potential is applied Quiet time When stopping stirring potential is not applied on the working electrode 10 4 3 Square wave stripping Parameters Initial potential the minimum potential for dissolution process to begin Final potential Final potential is generally higher than the oxidation potential of analyte ions Increment potential the incremental potential of each step Amplitude square wave amplitude half peak to peak Frequency square wave pulse frequency A potential can be specified in several ways If vs Open Circuit is chosen the specified potential is added to the open circuit potential of the cell For example 0 1V vs Open Circuit means applying a potential 0 1 Volts above the open circuit potential vs Reference is used to select an exact potential 10 4 4 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second is specified 10 4 5 Axis Type When the experiment 15 performed data will be displayed as specified by the Axis T
14. high input impedance of reference circuit such as high impedance coating may be the cause resulting in relatively large current noise At this time it s needed to increase the bandwidth filter capacitance thus can increase the stability of the test system User s Manual Original Freq 3 33E 1Hz I range Figure2 7 The sine wave signal in normal 16 Date Analysis 16 1 Corshow Date Analysis Find the Corshow software in the installation CD After installation is completed open the software The Corshow software interface is as below I CorShow File Graph Tool Window Help Bo 2 Q E V Al Files Fit Active Data M ES 2 amp CorrTest uses Corshow to analyze test data It can display data by multiple coordinates with functions of graph locally zooming curve smoothing data correction etc Also it can do calculations such as linear fitting tafel fitting and so on However the calculating results by the software may be different from results of parameter fitting Graphs can be output to a printer or a clipboard by Corshow software and can be pasted into the Word document directly Data files cor generated from is fully compatible with Corshow software 7A User s Manual Users can directly click on Corshow Drawing menu after data acquisition and introduce one more data files from File Import Data menu and
15. 1 73 Potential Stair Step Experiment Transient Polarization Potential Stair Step Potential Stair Step VSTEP Hew Data File Flenam es Comments OCP V 0 77088 Data Acquisition Step Potential Parameters Frequency xime Initial v 0 Time 200 2000 Step E 1 V 0 005 Time 800 Petat Gstat Use StepE2 V 0 010 Time 1000 Potential vs OCP Cell Axis vs Time Help OCP will display the actual open circuit potential of the cell updated per second If the instrument is turned off this value will display Not Available ime Unit mSecs X 7 3 1 Data File When the experiment is performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This 15 particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file has already existed 7 3 2 Step Potential Parameters A potential sweep between up to 3 separate potential setpoints is applied and the current response is measured Unlike the Potentiodynamic experiment the potential will be changed in discrete steps rather than a smooth sweep The experiment starts at the Initial Potential sweeps to Step EI and then to Step E2 Click on the Use boxes to tu
16. 5 Hz Experiment Termination Quiet time s 1 00 Pstat Gstat JUS Z Disabled Current sampling intv ms 0 1 When i mA 25 i Based on current Cell Or i mA 41 Based 01 01 When DI Dt Als 0 01 Axis Type Time ox Cancel Help 14 3 1 Data File When the experiment is performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This 15 particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file already exists 14 3 2 Deposition Parameters Polarization Potential V 1s the potential imposed on the test system For CS Series electrochemical workstation if the polarization potential 15 relative to the open circuit potential the negative value indicates cathodic polarization while positive value indicates anodic polarization Clicking on the drop down box users can also choose the applying way of polarization potential Polarization time you can specify the length of potentiostatic polarization time time unit can be second minute and hour Experiment Terminationlf you select Based on the current checkbox and set the silent time and current sampling interval CorrTest will automatically terminate potentiostatic polarization tests when the polarizat
17. DP Eo De ds Dir bna cede TOC Des UP DP eS DUBVI 23 LINEAR SWEEP V OLTAIVIVIE TRY anaietan a o ub e Eo cu Fus ree nue ea lcs lae dedu Ee va ea rie 23 GYCLIC VOLTAMIMETRY T TT 24 STAIRCASE VOLTAMNIETRY eimetel varese evaes 27 SQUARE WAVE VOLTAMMETRY ceive istasttancseciwenicceidevssadinetedeuiiarcvedusatadansbauseaeineustawsbavebedinenidearteucuaaess 28 DIFFERENTIAE PULSE VOLTAMMETRY isi reo be 29 NORMALE PUESEVOLTAMIMETRY chea 31 9 10 11 12 13 14 15 16 17 8 7 DIFFERENTIAL NORMAL PULSE VOLTAMMETRY cceccccecccceccccecccecccccccsceececeececencecenceeencecenceceaceseaseneas 8 8 WOETAMIMETIRY A 0 ceste etes eoo to 8 9 2ND HARMONICA VOETAMMETRY 55 vice t ado E iua ge ey RE cel CHRONO TECHNIGUES iie pe ek P ea ERU ERE CRAT E UME RE PEIBNERRU SEE SER Neu EAE SA E ME RN REUS a 9 1 CHRONOPOTENTIOMETRY 22 5 ctae ideni a ades Debs 9 2 CHRONOAMPEROMETRY ARTT 9 3 CHRONGCOULIOMEEIRY tas mda cure n uen eU c eU TM O STRIPPING VOLTAMMETRY RUE EUR TD Se ea Vel VES MEUS EVA ERE SUR VS 10 1 POTENTIOMETRIC STRIPPING ora e E ORE E ca ERU Ea vae RERO NES EE A KE pO VE se e RASSE TIMES 10 2
18. Data Acquisition Scan Parameters REN Initial E V 050 vs Reference 2 rim Inc E v 10 004 Amplitude V 0 025 D Pulse Width s 0 05 Pulse Period 5 0 20 Pstat Gstat Final E 0 05 vs Reference E Axis Type BA vs E m Help OCP will display the actual open circuit potential of the cell updated per second If the instrument is turned off this value will display Not Available 8 5 1 Data File When the experiment is performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This 15 particularly useful in case you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file has already existed 8 5 2 Scan Parameters In Differential Pulse Voltammetry DPV the base potential is incremented from Init E toward Final E A potential pulse is applied Current is sampled before and at the end of the potential pulse The difference between these two current samples is recorded as a function of potential Init E and Final E should be at least 0 01 V apart A potential can be specified in several ways If vs Open Circuit is chosen the specified potential is added to the open circuit potential of the cell vs Reference is used to select an exact potential
19. EE EN 14 3 ELECTROCHEMICAL STRIPPING DEPOSITION scs acri ee testes etta expe we vert ertet DATA VIEW ERR IEEE 15 1 VIEUX oet dure eR ae ca cc 15 2 EIS DATA VIEW cenean boue dotar tt d pore or tope tul feta medo M Sors AG DILE I DLL CU OT A E DU EE uae oU coude cou ud OP 16 1 CORSHOWXDATE ANALISIS do cdanacies seu eed ed nM Eo ode edad COR aM EET 16 2 CORROSION RATE CAECUERATION escis on Gier var etate a aret e ova ebat e a e Ee a CONTACT US User s Manual Part 1 CS Electrochemical Workstation 1 Introduction CorrTest electrochemical suite consists of a CS series electrochemical workstation potentiostat galvanostat and a set of Corrtest software CS workstations are dedicated to the cutting edge research areas from batteries electroplating electrolysis electroanalysis corrosion to the synthesis of nanomaterial etc 1 1 Hardware Specifications Potential control range 10V Current control range 2 0A Potential control accuracy 0 1 x full range 1mV Current control accuracy 0 1 x full range Potential resolution gt 100Hz 3uV 10Hz Current sensitivity Rise time lus 10mA lt 10us lt 2A Reference electrode input impedance gt 10 7Q 20pF Current range 2A 200nA 8 ranges
20. Final E should be at least 0 01 V apart vs is used to select an exact potential Incr E is the increment potential of each pulse it can be chosen from 0 001 V to 0 05V Step Period can be chosen from 0 01 s to 50 s No of Cycles specifies how many times potential are cycled between Initial E and Final E 8 3 3 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second is specified 8 3 4 Axis Type When the experiment 15 performed data will be displayed as specified by the Axis Type Corr View can be later used to display data in other formats 8 3 5 Pstat Gstat The Experiments Setup Pstat Gstat menu item 1s usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 8 3 6 Setting See Cell Setting 9 1 8 4 Square Wave Voltammetry Experiment Voltammetry Square Wave Voltammetry The potentiostat applies a series of forward and reverse pulses both equal in duration and defined as a frequency superimposed on a linear staircase scan The resulting currents can be subtracted from one another to plot the difference current which is helpful for improving the sensitivity of analytical measurements Technique is also referred to as SWV Square Wave Voltammetry SWV Hew Data File Filename Comments OC
21. Incr E is the increment potential of each pulse it can be chosen from 0 001 V to 0 05 V Amplitude can be chosen from 0 001 V to 0 5 V Pulse Width can be chosen from 0 001 5 to 10 5 Pulse Period can be chosen from 0 01 s to 50 8 30 User s Manual 8 5 3 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second is specified 8 5 4 Axis Type When the experiment 15 performed data will be displayed as specified by the Axis Type CorrView can be later used to display the data in any of the other formats 8 5 5 Pstat Gstat The Experiments Setup Pstat Gstat menu item 15 usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 8 5 6 Cell Setting See Cell Setting 9 1 8 6 Normal Pulse Voltammetry Experiment Voltammetry Normal Pulse Voltammetry The potentiostat applies a series of potential pulses from a constant baseline equal to the initial potential each pulse increasing by a defined increment step height to a final potential The resulting currents can be subtracted from one another to plot the difference current which 15 useful for improving the sensitivity of analytical measurements Technique 15 also referred to as NPV Normal Pulse Voltammetry NPV Hew Data File Fil ename Comments OCP V 0 80615 Data Acquisit
22. LINEAR STRIPPING ne MEE 10 3 STAIRCASE STRIPPING s et lieto utpote e ic Le ED D Lo M 10 4 SOUARE WAVE STRIPPING scie oen a peto E tor euet eov ento Debe Oud sev Pee ero e duree adis BI POTENTIOSTALT o a ER s PRO SURU E QUA Ens VAN SUR re Qua Pus Vau ed cedo a RU 11 1 HYDROGEN DIFFUSION MEASUREMENTS cececceccccacccccceccccsceaceceacsceaceceacscencecsacecencecenceeeaceeeaceueas 11 2 ROTATING DISK EEECTRODEARDE assescin ie dee hebr ottima eiae uu d oL Ee Ip vont que Lave eoe od cepi e buta IMPEDANGCE vt EXE Pbi eX re e eo vm ee edu ciat ha eco EA a EPI d 12 1 EISAWS FREQUENCY audi 12 2 ie TASA PE E EE EEE dies 12 3 EIS POTENTIA chooses susiea ts A E RD CE I rem CHARGING DISCHARGING ccccccsccsccecccsccscccsccscceccccccscceccecccecceccecccecceccecccecceccecccecceccence 13 1 BATTERY CHARGING DISCHARGING oaa trans vn eee vet P pb vau tota Eve Va UR a PER vi 13 2 GALVANNOSTATIC CHARGING DISCHARGING eene enne nennen enters sense stesse sesso res MISC TECHNIQUES ii oe UR Boi asia ie o Aaa sodas ao R 14 1 EFECTROCHEMICAIS NOISE sexa eot at a uut Di eov uut 14 2 DATE OG GER
23. Setting 9 1 8 2 Cyclic Voltammetry Experiment Voltammetry Cyclic Voltammetry Cyclic Voltammetry is a technique devoted to the theoretical study of redox couples Cyclic Voltammetry 15 a particular LSV that performs a triangular shaped scanning at the working electrode In this way a redox couple in solution 1s exposed to an oxidation and afterwards to a reduction The plot of a cyclic voltammetry consists on a closed curve reversible redox couples 24 User s Manual show both cathodic and anodic peak while irreversible redox systems show only one peak The following formulas can be useful to establish the standard potential of a reversible redox couple and figure out the number of electrons involved in the discharge process 28 25 HE Bus T n Where anodic peak potential 28 25 n 0 FE Epc cathodic peak potential 56 5 n High E 2 G 4 5 Scan Rate V s A Init E N Low E Segment 1 Segment 2 Segment 3 Time 5 two stage voltage ramp is programmed from an initial potential to a vertex potential and then from the first vertex potential to a second one at a defined scan rate The scan can be repeated for many times cycles between the two vertex potentials To keep the step size on an analog like level the maximum scan rate should be10000V s To control the number of points acquired the data acquisition should be separated from any particular p
24. This definition is particularly helpful when using alloys The values are also used by the Polarization Resistance experiment to calculate corrosion rates The Reference electrode Type saves information on the reference electrode for later use by CorrTest This parameter is not used during measurements CorrTest always displays and stores the actual cell potential Most common reference types are predefined If your reference electrode is not in the list you can enter the User Defined Once the reference electrode type is selected CorrTest will be able to translate the potential data from one reference type to another User s Manual 5 2 Pstat Gstat Setup Setting C 350 Pstat Gstat Current Range Manual f Auto W Only Inc SENE Min Range 20uA Pot Range IR Compensation Ground Mode Auto Off v Virtual f Feedback 100 0 Real Quiet time Polarity Convention r Low Pass filter Potential Current 5 Sec 6 02 fe Dos 10 g2 C oz v Digital Smoothing Hotch filter 50Hz Notch Cancel Help The Current Range parameter selects a full scale current range to be applied during the experiments Selecting allows the instrument to select the current range based on the measured current The Potential Range parameter selects a maximum cell potential which can be applied and measured Generally speaking Auto is the best choice unless the signal changes
25. already existed 10 1 2 Deposition Parameters Before the experiment the surface of working electrode needs cleaning by this conditioning step A constant potential deposition step 15 applied to accumulate species on the working electrode surface This potential can be specified to choose either vs Open Circuit or vs Reference The deposition time determines how long the potential will be held at this step After deposition the experiment can be quiet for some time 10 1 3 Potentiometric Stripping Parameters After the constant potential deposition step 15 applied the species accumulated on the electrode surface are stripped out by applying a constant potential This stripping potential can be specified in several ways If vs Open Circuit is chosen the specified potential is added to the open circuit potential of the cell vs Reference is used to select an exact potential 42 User s Manual 10 1 4 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second is specified 10 1 5 Axis Type When the experiment 15 performed data will be displayed as specified by the Axis Type CorrView can be later used to display the data in other formats 10 1 6 Pstat Gstat The Experiments Setup Pstat Gstat menu item 1s usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Setting
26. can be measured and displayed by the auxiliary channel potentiostat UR User s Manual F3 Rotating Disk Electrode RDE Hew Data File Filename Comments OCP V 0 79998 Data Acquisition Disk electrode scan parameters Frequency Initial E V 10 2 Use Vertex E st1 V 0 10 Interval Use VetexEs2 0 10 05 FimaE 010 PstatiGstat Scan Rate 0 5 Imus gt Main unit Ring electrode polarization Potential 0 4 Ref electrode Cell Axis Evs Logi Help For disk ring electrode test disk electrode is the main working electrode while the ring electrode is mainly used to monitor the intermediate product on the disk electrode So disk electrode generally still uses potentiodynamic scan testing and the potential difference between ring electrode and disk electrode 15 set to be a constant potential value as 2 47 in the ring electrode polarization parameter settings There are two sets of test data records One is the polarization potential Ed and polarization current Id on the main unit potentiostat 1 e disk electrode the other 15 polarization potential the set value for the fixed Er and polarization current Ir on the slave unit potentiostat i e ring electrode 11 2 1 Data File When the experiment is performed the data will be saved in the file specified by Data File
27. concrete resistance Rs Moreover CorrTest provides as a dual channel data logger for pH temperature or some physical quantities records The software can be widely applied in the following areas 1 Electrochemical mechanism studies qualitative quantitative chemical analysis 2 General electrochemical preparation including electro synthesis electro deposition electroplating performance evaluation 3 Research functional and or energy materials batteries super capacitor nanometer material biological sensors etc 4 Evaluation of corrosion inhibitor water stabilizer coating and cathodic protection efficiency and measurement of hydrogen permeability 5 Electrochemical corrosion measurement of materials in a conductive medium such as water concrete and soil 2 1 System Requirements 1 Operating System Windows XP Vista 7 8 2 Communication between PC and instrument USB or RS 232 serial port 3 Output device any printer or plotter supported by Windows _4 User s Manual 2 2 Software Installation 1 USB Driver Installation For the first time the workstation connects to the host PC and is powered on Windows will display a Found New Hardware message and require driver installation Upon this request insert the CD into the CD ROM drive and then select Automatic to install the CP2102USBdriverWinx exe file 2 In the CD folder choose CSW x32 exe or CSW_x64 exe ac
28. display a list of all directories and files This is particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file has already existed 8 1 2 Scan Parameters Up to 2 separate potentials can be applied during the experiment The experiment Starts at the Initial Potential and then to the Final Potential A potential can be specified in several ways If vs Open Circuit is chosen the specified potential is added to the open circuit potential of the cell For example 0 1 V vs Open Circuit means applying a potential of 0 1 Volts above the measured open circuit potential vs Reference 15 used to select an exact potential to be applied The Scan Rate determines how fast the potential 15 scanned between one potential and another 8 1 3 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second is specified 8 1 4 Axis Type When the experiment 15 performed data will be displayed as specified by the Axis Type CorrView can be later used to display the data in other formats 8 1 5 Pstat Gstat The Experiments Setup Pstat Gstat menu item 1s usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 8 1 6 Setting See Cell
29. easy to use flexible and versatile electrochemical tool and can be applied in many research fields from corrosion voltammetry electroanalysis to battery test etc The main electrochemical techniques include Open circle potential OCP potentiostatic galvanostatic polarization potentiodynamic galvanodynamic polarization Multi potential current potential current stair step Chronopotentiometry CP Chronoamperometry CA Chronocoulometry CC Cyclic Voltammetry CV Linear Sweep Voltammetry LSV Staircase Cyclic Voltammetry SCV Square Wave Voltammetry SWV Differential Pulse Voltammetry DPV Normal Pulse Voltammetry NPV Differential Normal Pulse Voltammetry DNPV A C Voltammetry ACV Second Harmonic A C Voltammetry SHACV Potentiostatic Stripping Volammetry Linear Sweep Stripping Volammetry Staircase Stripping Volammetry Square Stripping Volammetry Differential Pulse Stripping Volammetry AC Impedance Battery Test Electrochemical Noise etc CorrTest software is also equipped with powerful corrosion analysis module it can calculate the corrosion rate of the material by linear polarization and weak polarization as well as the polarization resistance Rp Tafel slope ba and corrosion current density icor through the non linear fitting of Tafel curves In addition via the inherent electrochemical impedance spectroscopy EIS technique it can measure the double layer capacitance and the solution
30. if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you may be warned if the file has already existed 6 5 2 Galvanodynamic Parameters Up to 4 separate currents can be applied during the experiment The experiment starts at the Initial Current sweeps to Vertex 11 to Vertex 1 2 and then to the Final Current Click on the Used boxes to turn on or turn off the Vertex 1 1 and Vertex 142 setpoints If a Vertex s Used box 1s not checked that segment of the sweep will be skipped For example if only Vertex 171 is checked the sweep Initial Vertex 1 1 gt is performed If neither Vertex 1 1 nor Vertex 1 2 is checked Initial Final is performed 6 5 3 Experiment Stop When the Scan Rev box 15 checked the experiment will immediately start sweeping toward the Final Current if certain potential conditions are met _17 User s Manual When the Scan Stop box is checked the sweep will end if certain potential conditions occur Note The Current values specify the total current applied rather than the current density The Scan Rate determines how fast the current 1s scanned between one current and another 6 5 4 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second is specified 6 5 5 Axis Type When the experiment 15 performed data will be displayed as specified by the Axis Type CorrView can be late
31. less than this value due to rate limitation of the amplifier and the high frequency transmission loss of the conducting wires 12 2 3 Time Scan Perform EIS at a single frequency over several points by setting the high and low frequency and setting point spacing to linear and the desired number of points _ 59 User s Manual 12 2 4 Pstat Gstat The Experiments Setup Pstat Gstat menu item is usually used to configure the Pstat Gstat for all experiments in the Experiment List These settings apply to all experiments where the Default Settings are selected See Pstat Gstat Setting 12 2 5 Cell Setting See Cell Setting 9 1 12 3 EIS vs Potential Experiment Impedance EIS vs Potential The method is used to measure characteristics of single frequency impedance under different DC polarization potential The potential 1s stepped from the initial potential to terminate potential It is mainly used for Mott Schottky M S diagram curve test M S diagram has been extensively used to study the semiconductor passivation film on the surface of metals It can determine carrier s type and concentration and the flat band potential thereby contributing to the study of semiconductor function of a passivation film When the passivation film is in contact with the solution medium and the space charge of the semiconductor passivation film is in the depletion state remove majority carriers from the space charge region and minority carriers is
32. opposite sign The charge and discharge portions of the loop are separated by a Constant Potential action allowing the cell to be maintained at a fixed potential which 1s terminated based either on a set time or until a current or capacity limit 1s reached as set by the user The fixed potential used for this intermediate step is often the potential at which the charging step terminated Additional actions can be added to or removed from this sequence as desired m Battery Charging Discharging EE Hew Data File Filename a Comments OCP V 0 01 548 Data Acquisition r Experiment Interval Charge 1200 threshold for Conv V 1 36 0 Frequency Trickle current mA 20 HH Charging Time TEN Hours l PstatGstat Discharge Current mA HOD Discharge Threshold Voltage 1 1 Quiet time s 100 Cell as Discharge Time 10 Cycles 5 Cancel Help 62 User s Manual 13 1 1 Data File When the experiment 1s performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This is particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file already exists 13 1 2 Experiment Charge Current with different connecting ways of the electrode the cha
33. s to 108 Pulse Period can be chosen from 0 05 s to 50 s 8 7 3 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second is specified 8 7 4 Axis Type When the experiment 15 performed data will be displayed as specified by the Axis User s Manual Type CorrView can be later used to display the data in other formats 8 7 5 Pstat Gstat The Experiments Setup Pstat Gstat menu item is usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 8 7 6 Cell Setting See Cell Setting 9 1 8 8 A C Voltammetry Experiment Voltammetry A C Voltammetry In A C Voltammetry the base potential 15 incremented from Init to Final and a sequential sine waveform is superimposed Current is sampled when the AC signal is applied and it is analyzed by using a software lock in amplifier During the experiment only the absolute AC current is displayed After the experiment the phase selective current at any phase angle will also be available for display 5 A C Voltammetry ACV General Analyzer New Data File Filename Comments OCP V 0 80751 Pstat Gstat Scan Parameters Eg Initial E V 0 5 Inc E V 004 Cell Amplitude mV 25 v 0 05 Reference AC Frequency Hz 100 Axis Type Sample Per
34. the parameters will be lost Help accesses the on line help information on the setup of this experiment 6 4 Potentiodynamic Experiment Stable Polarization Potentiodynamic A potential sweep between up to 4 separate potential setpoints is applied and the current response is measured The sweep will be terminated or the sweep s direction will be reversed if a particular current is reached This can be configured to obtain either Polarization Resistance or Tafel data F4 Potentiodynamic New Data File Filename Comments OCP V 0 83432 Data Acquisition Scanning Parameters C Frequency Initial E V 0 10 vs Hz Use VertexE 1 0 40 Interval Use Vertex E 2 V 0 10 0 5 I mv Final E v 0 10 vs OCP Pstat Gstat D M zs Scan Rate 0 5 mVis Experiment Termination cell Stop scan When anodic i 2 Misi Reverse scan or cathodic i mA lt 2 Cancel Help OCP V will display the actual open circuit potential of the cell updated per second Axis E vs Logi 6 4 1 Data File When the experiment is performed the data will be saved in the file specified by Filename The Dir button can be used to display a list of all directories and files This is particularly useful if you forget the file names you have already used However before CorrTest begins performing the firs
35. then select various graphic coordinates such as vs time vs I vs loglI etc from Standaxis menu When graph 15 displayed disproportionately you can right click the mouse button to get Menu in the graph area and select Auto Zoom to support full graph Standaxis b Graph Setting Add Annotate Delete Annotate Edit Annotate Auto Zoom Zoom To Cursors Zoom Previous Zoom Next Export Graph Copy To Clipboard Resore Graph Export Active Data Auto E Volts Time Sec I amp mps cm2 Time Sec C Coulombs cm2 Time Sec E Volts If amp mps cm2 I amp mps cm2 EtVolts E Volts log I amp mps cm2 logd Amps cm2 E Volts CiCoulombs cm2 Efvolts E Volts C Coulombs cm2 1 0 Corshow software also has strong data calculation power It can calculate anodic and cathodic Tafel slope as well as the corrosion rate You can use the Auto Tafel fit or Auto Tafel Fit between cursors and other methods to calculate the electrochemical parameters and corrosion rate If fitting curve blue 1s well matched with the original data curve it means the results have high reliability Fitting results can be pasted onto the drawing via Auto Insert as shown in Figure 2 8 04 100mgLHTinhibitore Ba 0 046205 Be 0 152806 533006 Vols qa 7 3 21062e 5 Amps crr 1000mz L HC Ba 0 104266 Be 0 178142 05
36. will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This is particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file has already existed 7 2 2 Multi Current Steps Parameters A current sweep between up to 12 separate current setpoints 15 applied and the potential response is measured The experiment starts from the Initial Current and sweeps to Step 1 to Step 2 to Step 3 and Final 1 the step time box is filled with zero this segment of the sweep will be skipped No of Cycles specifies the cycles of the current sweep from the Initial 1 to the Final The Time determines how long the current will be held at each step 7 2 3 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate is set as Points Second 7 2 4 Axis Type When the experiment is performed the data will be displayed as specified by the Axis Type CorrView can be later used to display the data in other formats 7 2 5 Pstat Gstat The Experiments Setup Pstat Gstat menu item is usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all 20 User s Manual experiments where the Default Settings are selected See Pstat Gstat Setting 7 2 6 Cell Setting See Cell Setting 9
37. 0 x 10 Hz 10 x 10 7Hz 10 x 10 Hz 10 x 10 Hz 10 x 10 Hz 10 x 10 9 This mode 15 usually selected 12 1 4 Pstat Gstat The Experiments Setup Pstat Gstat menu item 1s usually used to configure the Pstat Gstat for all experiments in the Experiment List These settings apply to all experiments where the Default Settings are selected See Pstat Gstat Setting 12 1 5 Cell Setting See Cell Setting 9 1 12 1 6 Analyzer Settings E EIS vs Frequency IMP TTT Current Ranges Bandwidth Auto Min High FreqRange 2mA iffefc Use 22pF Transition Freq 10 Hz Transition Freq Hz OF High Freq ff 5000 High Freq bla Mid Freg Mid Freq if between Attenuator LowFreq 200ua LowFreq 001 1 C Intergration Intergration lon zl DC Bias Rejection Integration Time t 2 DC Removal Delay 2 Cancel Help Current range Users can choose current range automatically or manually If you select auto range you need to set up a high frequency current range threshold which can limit the minimum current range potentiostat can use during high frequency measurements The figure above indicates when the measuring frequency is above 1000Hz the automatic range will be no less than 2mA High frequency range is defined by the user The set value in the 56 User s Manual figure shows that fH 1000Hz is high fre
38. 685 V x Seconds Cancel Help 14 2 1 Data File When the experiment 15 performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This 15 particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if file already exists 14 2 2 Date Record Total Time recording the total time Sampling Data allowing to select the group signal channel 14 2 3 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second 15 specified 14 3 Electrochemical Stripping Deposition Experiment Misc Techniques Electrochemical Stripping Deposition In this test method a constant polarization potential 15 imposed onto the working electrode and at the same time the user should monitor the change of polarization current with time The polarization time may be specified by the user and it can also be specified when the current reaches a certain polarization value letting CorrTest automatically terminate the testing process 67 User s Manual LI Electrochemical Stripping Deposition Hew Data File Filename 27 Comments OCP V LO 58113 Data Acquisition Deposition Parameters Interval Applied Potential 020 5 0 4 Sec Total Time 200 Seconds f Frequency
39. 71097 Vols 12845625 E nidi p 1000 mz HT m asm mr m a rate 0 151092 mmPFY 1l 1 lt 10 10 104 I A mps cnz Figure 2 8 Polarization curve of A3 steel T User s Manual 16 2 Corrosion Rate Calculation 16 2 1 Polarization Resistance Polarization curves for the data processing module polarization curves for each segment to adopt different methods for linear and Tafel region using a linear regression calculation The polarization resistance Rp is calculated as the inverse of the slope of the I vs E data near the Open Circuit potential Rp Ohms 15 the inverse of slope of the I vs data Ecorr Volts is the potential at which the current changed polarities This usually corresponds to the open circuit potential of the system Estimated Icorr Amps cm is based on the Stern Geary relationship Stern and Geary J Electrochem Soc 104 56 1957 Icorr A cm 2 Ba x Bc 2 3x Ba Bc x Rp Since the Tafel slopes Ba and Bc cannot be calculated from this data 0 12 V decade are often used resulting in the approximation Mansfeld Advances in Corrosion Science and Tech 6 Ed Fontana and Staehle Plenum Press p 163 1976 Stern Geary Coef x Bc 2 3x Ba Bc 0 026 Icorr A cm 2 0 026 The Stern Geary Coefficient 1s specified in the Setup Cell window Corrosion Rat
40. Compliance voltage 21V Maximum current output 2 0A CV and LSV scan rate 0 01 mV 10 000V s CA and CC pulse width 0 0001 65 0005 Current increment during scan ImA A mS Potential increment during scan 0 076mV V ms SWV frequency 0 001 100K Hz DPV and NPV pulse width 0 0001 1000s AD data acquisition 16bit IM Hz 20bit 1K Hz DA Resolution 16bit Setup time I us Minimum potential increment in CV 0 075mV IMP frequency 10u Hz 115K Hz Low pass filters Covering 8 decade Potential and current range switch Automatic _ User s Manual 1 2 Electrochemical Signal generator Waveform generator Frequency range 10u Hz 115K Hz AC amplitude 0 2 500mV DC Bias 10 10V Output impedance 50Q Waveform Sine wave triangular wave and Sine wave Wave distortion lt 1 Scanning mode Logarithmic linear increase decrease Signal analyzer Integral time minimum 10ms or the longest time of a cycle Maximum 10 cycles or 10 s Measurement delay 0 10 s DC offset compensation Potential automatic compensation range 10V 10V Current compensation range Bandwidth 8 decade Frequency range Automatic and manual setting 1 3 Front Panel The front panel of CS series instrument is shown in Figure 1 1 Fig 1 1 Front panel of CS Electrochemical Workstation Electrode Cable The electrode cable provides a means for connecting an electrode to the electrochemical workstation The cell cable is describe
41. P V 0 80558 Data Acquisition r Scan Parameters Interval Initial E v 0 5 vs Reference 0 1 Sec Inc E 0 00 EE nc E V p o04 20 Amplitude V 10 025 Frequency Hz 15 E Final E V 0 10 vs Reference Cell Axis Type TA ox Cancel Help _ 28 User s Manual OCP will display the actual open circuit potential of the cell updated per second If the instrument is turned off this value will display Not Available 8 4 1 Data File When the experiment 1s performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This 15 particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file has already existed 8 4 2 Scan Parameters In Square Wave Voltammetry SWV the base potential is incremented from Init E towards Final E A square wave potential is superimposed onto the base potential which increments after each cycle of the square wave Current is sampled at the end of the forward and reverse steps and recorded as a function of the base potential During the experiment only the difference between the two current samples is displayed After the experiment the forward and reverse currents will also be available for display Init E and Final E should be at least 0 01
42. Rak it Mete E 7 EXPERIMENT SETUP 5 ens seuteeuss 8 CELES ELECTRODE e Siu eir iL scs eec 8 PSTAT SETUP o DOLO nci ones 9 WAITING BEFORE RUN RETE 10 STABLE POLARIZATION S Deu DX Ex Cody e Dua boa Qua A eis EQ VER UN 10 OPEN CIRCUIT POTENTIAL caeso tonno de ups e tlawalte tete eni idera e me Dev QUE a da 10 PPOTENTIOSTPATICS secius duet erede ue doeet cote ped oA ME cro d Suas 11 GAL AIO TATIC e c CMM E EM I DM LSU C MD TERM eo DUCUM AM S CE 13 odd REIS bru ame NT 15 GALV ANG DY NAMIC vinwindecs a aa A 17 TRANSIENT POLARIZATION 5 55vssbsceuuseeEhoeea oe na a Toa eoa FEE ee bYE ae EAT e ea Pe a E TP e SR T eee br E ae E AT e 18 MIWETIE re d S E Pd ee dd SAEPE ET E S 18 MUETIEGURRENT STEP Sic c 19 POTENTIAL i SI ER fect S 21 GAIWANIG S TAIR dese sentar odes instote o Mic Poor sate 22 VOLTAMMIETR Y Us SEEN VDE
43. The Dir button can be used to display a list of all directories and files This 15 particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file has already existed 11 2 2 Disk electrode scanning parameters Similar with potentiodynamic scanning disk electrode can have a maximum of 4 independent polarization potential setpoints Please see the potentiodynamic scanning 11 2 3 Ring electrode polarization parameters Polarization potential ring electrode relative to the disk electrode polarization potential with unit of V s 11 2 4 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second is specified 53 User s Manual 11 2 5 Axis Type When the experiment is performed the data will be displayed as specified by the Axis Type CorrView can be later used to display the data in other formats 11 2 6 Pstat Gstat For bipotentiostat users need to do settings for the main amp slave unit respectively Parameters of them can be the same or different With buttons of main unit and slave unit users can set the current range switching signal gain low pass filter switches digital smoothing scan polarization delay time and so on Please note real ground must be chosen for earthing mode 11 2 7 Cell Setting See Cell Setting 9 1 12 Impedance CS350 series us
44. V apart vs Reference is used to select an exact potential to be applied Incr E is the increment potential of each pulse it can be chosen from 0 001 V to 0 05 V Amplitude can be chosen from 0 001 V to 0 5 V Frequency can be chosen from 1 to 100000 Hz 8 4 3 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second 15 specified 8 4 4 Axis Type When the experiment 15 performed data will be displayed as specified by the Axis Type CorrView can be later used to display the data in other formats 6 4 5 Pstat Gstat The Experiments Setup Pstat Gstat menu item 1s usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 8 4 6 Setting See Cell Setting 9 1 8 5 Differential Pulse Voltammetry Experiment Voltammetry Differential Pulse Voltammetry 29 User s Manual The potentiostat applies a series of forward and reverse pulses defined as a forward pulse and a reverse step superimposed on a linear staircase scan The resulting currents can be subtracted from one another to plot the difference current which is helpful for improving the sensitivity of analytical measurements Technique 15 also referred to as DPV e Differential Pulse Voltammetry DPV Hew Data File Filename Comments OCP V 0 80494
45. already used However before CorrTest begins performing the first experiment in the Experiment List you may be warned if the file has already existed 9 2 2 Scan Parameters The experiment starts at the Initial Potential sweeps to High E and then to Low E A potential can be specified in several ways If vs Open Circuit is chosen the specified potential 15 added to the open circuit potential of the cell vs Reference is used to select an exact potential to be applied Pulse Width specifies how long the potential is sustaining Number of Steps specifies how many potential cycles are formed between High E and Low E 9 2 3 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second is specified 9 2 4 Axis Type When the experiment 15 performed data will be displayed as specified by the Axis Type CorrView can be later used to display the data in other formats 9 2 5 Pstat Gstat The Experiments Setup Pstat Gstat menu item 1s usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all _ 39 User s Manual experiments where the Default Settings are selected See Pstat Gstat Setting 9 2 6 Cell Setting See Cell Setting 9 1 9 3 Chronocoulometry Experiment Chrono Techniques Chronocoulometry A fast rising potential pulse is enforced on the working sense electrode of an electrochemical cell The current flo
46. and anodic currents correspond to reduction and oxidation respectively The 24 User s Manual time can be different for switching between cathodic and anodic However the Initial Polarity parameter specifies the initial current polarity Number of Segments specifies how many times the current is cycled between Cathodic and anodic currents When the number of current polarity switches Segments is reached the experiment stops 9 1 3 Current Switching Polarity When the Low E limit is reached during reduction the current polarity will automatically be switched to be anodic Similarly when the High E limit is reached during oxidation current will automatically be switched to be cathodic The current switching polarity can be checked when either the specified potential or the specified time has been reached If the limiting potential is reached the current polarity will still be reversed in order to protect the electrode 9 1 4 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second is specified 9 1 5 Axis Type When the experiment 15 performed data will be displayed as specified by the Axis Type CorrView can be later used to display the data in other formats 9 1 6 Pstat Gstat The Experiments Setup Pstat Gstat menu item is usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Settings
47. are selected See Pstat Gstat Setting 9 1 7 Cell Setting See Cell Setting 9 1 9 2 Chronoamperometry Experiment Chrono Techniques Chronoamperometry A fast rising potential pulse is enforced on the working sense electrode of an electrochemical cell the current flowing through this electrode is measured as a function of time Technique is also referred to as CA For a Two Step Chronoamperometry experiment either insert two CA actions into the same sequence each set at the desired Potential step and with the cell remaining ON at the end of the first step or preferably run a two step Fast Potential Pulse action if that is available _ 38 User s Manual Chronoamperometry CA New Data File Filename Comments OCP V 0 81 280 Data Acquisition Scan Parameters Interval Initial E V 0 5 vs Reference 0 01 Sec High E V 5 vs Reference Frequency 00 Hz Low E V 1 vs Reference Pstat Gstat Pulse Width s 0 25 E Number of Steps Axis Help OCP will display the actual open circuit potential of the cell updated per second If the instrument is turned off this value will display Not Available 9 2 1 Data File When the experiment is performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This 15 particularly useful if you forget the file names you have
48. at Gstat menu item 1s usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 7 4 6 Cell Setting See Cell Setting 9 1 8 Voltammetry 8 1 Linear Sweep Voltammetry Experiment Voltammetry Linear Sweep Voltammetry A single voltage ramp programs from an initial potential to a final potential that progresses at a defined scan rate To keep the step size on an analog like level the maximum scan rate should be 1000V s To control the number of points acquired the data acquisition should be separated from any particular point and spread out over the entire scan range to a maximum of 1000 points per scan Linear Sweep Voltammetry LSV New Data File Filename 50 zm Commens OCP 0 82164 Data Acquisition Scan Parameters t Frequency Initial E V 0 2 vs Reference 100 Hz Interval Final E V 0 60 vs Reference 0 5 mV Scan Rate mV s 100 Pstat Gstat zz Axis Type vs E Cell Help 23 User s Manual OCP will display the actual open circuit potential of the cell updated per second If the instrument 15 turned off this value will display Not Available 8 1 1 Data File When the experiment 1s performed the data will be saved in the file specified by Data File The Dir button can be used to
49. capacitance values To check if a shock appears you can observe the amplitude of signal and the form of wave in waveform diagram After the measured frequencies are below fc you should select the second grade capacitance and its value should be no less than that of the first grade The instrument has a relatively low bandwidth When fc 10Hz bandwidth setting capacitance is 22pF when fc lt 10Hz it is 470pF in order to improve the signal stability For the filter settings see 9 5 filter settings within the instrument settings DC Bias Compensation DC Bias Compensation is used to eliminate DC level which is superimposed on the potentiostat or the current output signal It is used to increase the AC magnification of potential or current signals and increase impedance measurement accuracy CS350 instrument automatically uses internal bias elimination of potential and current and thus impedance measurement accuracy is improved During impedance measurement you are recommended to at least open the bias compensation option If the amplitude of AC excitation signal is less than 100 you can open signal enhancement option Integration Time Integration can be divided into automatic and manual integration Increasing the integration time can improve the impedance measurement accuracy and reduce the impact of noise on the measurement results Integration time can be set to be the number of cycles 57 User s Manual
50. cording to your computer s operating system Double click on the setup file and follow the instructions to complete installation 3 Open the software shortcut on the Desktop When CorrTest is opened for the very first time a software interface similar to the following picture will appear CorrTest Electrochemical Workstation lt Model CS350 in 4 gt SN CS350081134 File Edit Setup Experiments Data Analysis Window Help Gr ki i OR er CorrTest Instruments http Copyright 2000 2013 Fig 2 1 Interface of CorrTest software for CS Electrochemical Workstation 3 Menu There are keyboard shortcuts for experiment methods on the right such as F2 for Open Circuit Potential Either by clicking on the Open Circuit Potential or pressing F2 key can users open the OCP test dialog box There is a toolbar under the main menu and it can achieve the same function as the main menu and there will be a text message alert when users hover the mouse over a button Users can also right click the mouse on the main window it will pop up the Experiments menu User s Manual The button will be activated when a test is running Users can click on it to stop the testing process This button will be grayed out when the test is finished 3 1 File The File menu offers the following commands 3 1 1 Open Open an existing data file and 1t can be edited and rena
51. ctrode surface This potential can be specified to choose either vs Open Circuit or vs Reference The deposition time determines how long the potential will be held at this step After deposition the experiment can be quiet for some time 10 2 3 Linear Stripping Parameters In Linear Stripping a constant potential deposition step 1s first applied After that the species accumulated on the electrode surface are stripped out by applying a linear potential which is scanned from an initial potential to a final potential that progresses at a defined scan rate A potential can be specified in several ways If vs Open Circuit is chosen the specified potential is added to the open circuit potential of the cell vs Reference is used to select an exact potential 10 2 4 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second is specified 10 2 5 Axis Type When the experiment is performed the data will be displayed as specified by the Axis Type CorrView can be later used to display the data in other formats 10 2 6 Pstat Gstat The Experiments Setup Pstat Gstat menu item is usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 10 2 7 Cell Setting See Cell Setting 9 1 10 3 Staircase Stripping Experiment Stripping Voltammetry
52. cy the actual polarization amplitude of the working electrode may be less than this value due to rate limitation of the amplifier and the high frequency transmission loss of the conducting wires 12 3 3 Potential Parameters Initial potential it is the initial DC electrical level of the working electrode set in impedance potential sweep polarization potential drop down box you can choose potential applying means thereby changing the reference potential of all the set points of 61 User s Manual polarization potential Termination potential it is the stop potential set in impedance potential sweep Potential incremental it is increased with the form of steps users can do single frequency impedance measurement at each step potential point 12 3 4 Pstat Gstat The Experiments Setup Pstat Gstat menu item 1s usually used to configure the Pstat Gstat for all experiments in the experiment list These settings apply to all experiments where the Default Settings are selected See Pstat Gstat Setting 12 3 5 Cell Setting See Cell Setting 9 1 13 Charging Discharging 13 1 Battery Charging Discharging Experiment Charging Discharging Battery Charging Discharging A sequence of Constant Current and Constant Potential actions within a loop to define the number of desired cycles to create a cyclic charge discharge sequence with charging and discharging performed by constantly applied current with
53. d below for more details Green Working electrode WE lead This lead connects to the electrode of interest at which the desired reactions will occur The electrical signal is measured through WE lead Red Counter electrode CE lead This lead connects to the electrode opposite the WE and controls the power output of the instrument 29 User s Manual Yellow Reference electrode RE lead This lead connects to the reference electrode a component of the differential amplifier that measures controls the potential between itself and the sense electrode Black Ground lead The use of this lead depends on the application fields It 15 mainly used to supply a ground point on a Faraday shield for the experimental cell and can also be used in some open circuit experiments to form a zero resistance ammeter ZRA 1 4 Potentiostatic mode The mode of CS instrument is computerized general purpose potentiostat galvanostat The Figure below shows the electric schematic diagram of the instrument Analog digit converter 4 monitor Applied potential Voltage follower Digit analog converter Power amp Reference electrode 4 Counter electrode Analog digit converter binis I monitor didtur Fig 1 2 Schematic diagram of CS instrument User s Manual Part 2 CorrTest Software 2 Introduction CorrTest software shipped with the CS electrochemical workstation is an
54. d connect the double electrolytic cell in the way as shown below add 0 1 mol L of NaOH into the anode chamber on the right and link the anodic chamber electrode cable onto the main unit of the front panel and cathode chamber electrode cable onto the slave unit Firstly set the anodic polarization potential of the potentiostat on main unit to be 0 2V vs Hg HgO start the polarization the anode current will sharply decline at the beginning then slowly tends to retain a constant value that is anode residual current It is produced by hydrogen left inside the steel or some oxidated impurities in the diffusion surface solution When the residual current 15 lower than the setting value users can add experimental media such as dilute Hydrochloric Acid into the cathode chamber and then start galvanostatic polarization of the slave unit The initial current 1s in the peak See the below figure 10mA for instance And on C face of cathode chamber the hydrogen ions will be reduced to hydrogen atoms some of which will permeate into and across metallic disk reaching A face of the anodic chamber Upon potentiostatic anodic polarization on the main unit these hydrogen atoms will be oxidated and become 1015 forming oxidation currents 48 User s Manual CS2350 Workstation RE CEI p p p Ni plated face Sample Figure 2 3 Connection diagram for Hydrogen diffusion coefficient test device T M 3
55. e dual signal correlation integral system to improve the impedance measurement accuracy The test frequency ranges from 115KHz 10uHz and you can automatically proceed electrochemical impedance test under open circuit potential or any DC bias Built in DC offset cancellation circuit can effectively improve the measurement accuracy of the AC signal Excitation amplitude of the sine wave from 0 2 5V can be set arbitrarily For AC impedance measurement it includes the following three methods D impedance frequency sweep curve It measures the system s impedance spectroscopy at different frequencies It s the most commonly used method to measure impedance with the common form of Nyquist and Bode plots 2 impedance time scanning curve It measures the characteristics of impedance with time s change at a single frequency It is used to track the dynamic processes of some systems such as conductivity 3 impedance potential sweep curves It measures at a single frequency characteristics of impedance of the system with the change of DC polarization potential It can be used to measure the differential capacitance curve and zero charge potential and 50 on 12 1 EIS vs Frequency Experiment Impedance EIS vs Frequency 54 User s Manual x EIS vs Frequency IMP General Analyzer New Data File Filename EN c Comments OCP V 6 8931 1 Polarization Frequency Sweep DC Potential v 0 vw oce mt
56. e held at this step After deposition the experiment can be quiet for some time In Staircase Stripping a constant potential deposition step is applied After that the species accumulated on the electrode surface are stripped out by applying a staircase potential which is incremented from Initial E toward Final E that progresses at a defined increment 10 3 3 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second is specified 10 3 4 Axis Type When the experiment is performed the data will be displayed as specified by the Axis 45 User s Manual Type CorrView can be later used to display the data in other formats 10 3 5 Pstat Gstat The Experiments Setup Pstat Gstat menu item is usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 10 3 6 Cell Setting See Cell Setting 9 1 10 4 Square wave stripping Experiment Stripping Voltammetry Square wave Stripping The waveform can be viewed as a special case of that used for DPV in which the preelectrolysis period and the pulse are of equal duration and the pulse is opposite from the scan direction However the interpretation of results is facilitated by considering the waveform as something consisting of a staircase scan each tread of which 15 superimposed by a symmetrical double pulse one in t
57. e is calculated from MPY Icorr A cm 2 xEquiv Weight g equivalent x393 7 mils cm Density g cm x 96500 coulomb equivalent mmPY Icorr A cm 2 xEquivWeight g equivalent x 10 mm cm Density g cm x 96500 coulomb equivalent The Corrosion Rate calculations are only possible if Density and Equivalent Weight values were entered in the Setup Cell window Note The calculated values depend on the proper selection of data to be used by this function In addition data artifacts or improper experimental technique may cause large discrepancies in the results So the users must depend on their own knowledge of electrochemistry or corrosion to determine if the values are valid 16 2 2 Corrosion Rate Calculation Date Analysis Corrosion Calculation This dialog box 15 used for corrosion calculation according to the electrode kinetic equations The cell parameters need to fill well 76 User s Manual 2 Fast Corrosion Calculation uw Cell Parameters Electrode Area cm 1 Temperature 25 Density g cm 7 8 Stem Ceary B mV Equivalent Weight q 28 3 Methods Results x Accuracy LRR Fit Tafel ba mV dec Tafel Fit 3 Parameters Tafel bc mV dec C Tafel Fit 4 Parameters Icorr mA cm Corr Rate mma Exit Help 16 2 3 Three calculation methods LRR Fi t it is used to do linear regression calculations of data in the range of 1 5mv on the cathode or anode polarizatio
58. ed in the file specified by Filename The Dir button can be used to display a list of all directories and files This is particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you may be warned if the file has already existed CorrTest will automatically append the suffix to a data file if you do not enter one Therefore if you specify tutorl the tutorl cor will be used In the same say if you specify tutor abc the file tutorl abc cor will be used The Comments text 1s saved in the data file The time date and all measurement parameters are automatically saved in the data file so you don t need to write these information into the comment area 6 2 20 Experiment Parameters The Initial E specifies the potential applied during the experiment A potential can be specified in several ways If vs Open Circuit is chosen the specified potential will be added to the open circuit potential of the cell For example 0 1 vs Open Circuit Potential means applying a potential of 0 1 Volts above the measured open circuit potential vs Reference is used to select an exact potential to be applied The Total Time determines the total length of the experiment 6 2 3 Experiment Termination If the Use I box 15 checked the experiment will be automatically terminated as long as the current goes below the Current A val
59. efore starting the test the Start button 15 inactive Only when the user specifies a valid file name can the start button be activated All subsequent data will be saved in the created file 13 2 1 Data File When the experiment is performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This 15 particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file already exists 13 2 2 Charging Discharging Current Charge Current if the battery positive is connected to the working electrode then enter a positive number indicating the charging Discharge current if the battery positive 1s connected to the working electrode then enter a negative number indicating the discharging 13 2 3 Condition for switch of Charging Discharging Charge and discharge time set the stage charging and discharging time When the potential V Ec relative to the reference electrode Ec for the user settings that material has been fully discharged the instrument will switch to the charging state when the constant current charging process after potential than Ed relative reference electrode it indicates that the material charge has been completed to complete a measurement cycle and re enter the discharge state Cycles one c
60. elp OCP will display the open circuit potential of the current electrolytic cell updated per second This is particularly useful for the user to determine whether the working electrode is stable for impedance test 12 2 1 Data File When the experiment 1s performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This is particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file already exists 12 2 2 Polarization DC potential is the set DC polarization potential of the working electrode during impedance test If the test needs to proceed under the open circuit potential OCP then you can enter O and select relatively open circuit potential in the drop down box This moment the potentiostat will automatically give a total output of the pen circuit potential and the DC potential to the working electrode If you need to do the impedance test under 50mV DC potential of anodic polarization you can enter 0 05 for DC potential AC amplitude value is the amplitude value of the excitation signal of electrochemical Impedance For example E 0 012 sin wt V means AC signal amplitude 15 12mV However under the state of high frequency the actual polarization amplitude of the working electrode may be
61. ents in the experiment list These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 8 8 6 Cell Setting See Cell Setting 9 1 8 9 2nd Harmonic A C Voltammetry Experiment Voltammetry 2nd Harmonic A C Voltammetry In Second Harmonic AC Voltammetry the base potential is incremented from Init E toward Final and a sequential sine waveform 15 superimposed Current is sampled when the AC signal is applied and a second harmonic component is analyzed by using a software lock in amplifier During the experiment only the absolute second harmonic AC current is displayed After the experiment the phase selective second harmonic current at any phase angle will also be available for display 245 User s Manual 2nd Harmonic A C Voltammetry SHACV General Analyzer New Data File Filen ame Comments OCP V 0 80629 PstatiGstat Scan Parameters Initial E V 10 5 vs Reference Inc E V 004 Cell Amplitude mV 25 EA Final V 0 05 vs Reference Frequency Hz 100 Axis Type Sampling Period 1 Bias DC Current lof OCP will display the actual open circuit potential of the cell updated per second If the instrument is turned off this value will display Not Available 8 9 1 Data File When the experiment is performed the data will be saved in the file specified by Data File The Dir button can be used to displa
62. es will be displayed in the title bar of the window and the adopted test methods e g constant potential polarization potentiodynamic scanning etc the working parameters such as scan rate measurement time work state the total amount of data etc as well as the progress and completion percentage will all be displayed at the bottom of the window Graphing Filename C Program Files x86 CorrTest4 tafel cor ELS Amt mo Chan 1 Chan 2 Chan 4 Axis Pts 396 Time 5 396 00 Potential V 9 9286E 2 Current A 9 0299E 5 1 100E 1 6 800E 2 7 2 600E 2 4 1 600E 2 4 5 800E 2 4 1 000E 1 T T TTTTT T T T T T T 1 8 1 7 1 6 1 5 1 4 I A Potentiodynamic Scan Ranael V 0 1 0 1 Scan Rate m s 0 5 Freq Hz 1 00 Run Time s Progress PRONOUN Nox 69 User s Manual CorrTest software will automatically select the best starting and ending point in the coordinate and dynamically refresh the graph 15 1 1 Graph Coordinate By clicking on the drop down box in the right side of graph options you can change the dynamic graph display Users can select 7 kinds of graph coordinates and they can also select coordinate units mV V mA A according to the value of potential and current vs time the abscissa 15 the time in second the vertical axis is electrode potential I vs time
63. gress 86 Lefttime 00 12 35 341333 x 145 68 940 90 254 2 497 5 709 5 937 2 Z 7 Ampim 10 Potential 00008 Int 5 Final 1E 2 Current Range ze 15 2 1 Data When the users want to know the value of a point on the graph they can move the cursor onto the graph area then immediately there will be a synchronized display on the right side of the cursor 15 2 2 Zoom In When users need to observe graphs or data of a local position during the test they can left press the mouse button on the upper left side of the certain area and drag to the lower right side and then release the button This local graph will immediately be zoomed in and fill the entire diabox The graph will not be updated but this time test system of CorrTest is still scanning and collecting data signals If you want to go back to the original status just click the mouse on the graph Note Due to a large amount of data processing in the test users are recommended to use this function after testing 15 2 3 Stop Click onl Dlo terminate the ongoing test Click M to pause the test 15 2 4 Real time Waveform Show The waveform acquisition window is used to display the acquired potential and current waveforms in the process of EIS measurements guiding the user to set the appropriate parameter of minimal high frequency range and bandwidth response in the impedance test window If the potential a
64. he forward direction and the other in the reverse Over many cycles the waveform is a bipolar square wave superimposed on the staircase This view gives rise to the name of the method m Square Wave Stripping New Data File Flnam Comments Data Acquisition Deposition Parameters Interval Conditioning Efo t0 Time s 15 NN Deposition 0 10 vs Reference 0 Hz Deposition Time s 15 Quiet Time s 15 PstatiGstat Square Wave Stripping Parameters Initial E V 0 5 Final E V 0 10 E4 Inc E WV lo oo4 Cell Amplitude V 0 025 Frequency Hz 15 as Axis Type vs E ok Cancel Help OCP will display the actual open circuit potential of the cell updated per second If the instrument is turned off this value will display Not Available 10 4 1 Data File When the experiment 1s performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files Corrtest automatically appends the suffix to data files The Comments text is saved in the data file The time date and all measurement parameters are automatically saved in the data file so you don t need to write these information into the comment area 46 User s Manual 10 4 2 Deposition Parameters Conditioning potential Before deposition the conditioning potential is applied on working electrode in order to remove impurities
65. her formats 7 1 5 Pstat Gstat The Experiments Setup Pstat Gstat menu item is usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 7 1 6 Cell Setting See Cell Setting 9 1 7 2 Miulti Current Steps Experiment Transient Polarization Multi Current Steps In the Multi Current Steps technique twelve Current steps can be applied and cycled Potential 1s recorded as a function of time 19 User s Manual A 5 Multi Current Steps New Data File Filename 27 Comments OCP V 0 83563 Data Acquisition Multi Current Steps Parameters C Interval Ii ali 1 Time 100 6 4 0 001 Sec Stepi 1 Time 100 7 4 Frequency Step2 Steps 5 me oo 100 Hz Step 32 T me Hoo Step9 T 100 M Recording Step 4 m Hoo p T x efo Pstat Gstat Steps 3 rime io Finali 1 00 89 Current Unit mA Time Unit Msec v Cycles 10 Cell Ml 2 OCP will display actual open circuit potential of cell updated per second If the instrument is turned off this value will display Not Available 7 2 1 Data File When the experiment 15 performed the data
66. ical cell and the potential of this electrode is measured against a reference electrode as a function of time Technique is also referred to as CP For a Two Step Chronopotentiometry experiment two CP actions are inserted into the same sequence each set at the desired current step and with the cell remaining ON at the end of the first step m Chronopotentiometry CP Hew Data File Filename Comments OCP V 0 82990 Data Acquisition Scan Parameters f Interval Cathadic Current 0 1 0 01 EE Anadic Current 0 2 Frequenc in m Hi Cathodic Time 10 Seconds Anodic Time 10 Seconds Pstat Gstat esl Initial Polarity Anode Cell Number of Segments 10 TAI Current Switching Priority High 1 vs Reference Axis Type MEM ve Time Low E V vs Reference Help OCP will display the actual open circuit potential of the cell updated per second If the instrument is turned off this value will display Not Available 9 1 1 Data File When the experiment is performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This 15 particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file has already existed 9 1 2 Scan Parameters Cathodic
67. ick on the Use boxes to turn on or turn off the Initial and Final setpoints If the Initial or Final setpoint is unchecked this segment of the sweep will be skipped For example if only the Initial is checked the sweep Initial High E Low E will be performed If neither the Initial nor Final is checked High E Low E will be performed A potential can be specified in several ways If vs Open Circuit is chosen the specified potential is added to the open circuit potential of the cell For example 0 1V vs Open Circuit means applying a potential of 0 1 Volts above the measured open circuit potential vs Reference is used to select an exact potential to be applied The Scan Rate selects how fast the potential is scanned between one potential and another No of Cycles specifies how many times potentials are cycled between High E and Low E 8 2 3 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second 15 specified 8 2 4 Axis Type When the experiment 15 performed data will be displayed as specified by the Axis Type CorrView can be later used to display the data in other formats 8 2 5 Pstat Gstat The Experiments Setup Pstat Gstat menu item is usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 8 2 6 Cell Setting See Cell Sett
68. imum charge and the longest discharge time after a period of time of battery charging or discharging if the specified critical voltage hasn t yet been reached the charging or discharging will stop and turn to discharging or charging Cycles one complete cycle includes a charging and a discharging process This parameter specifies the total number of cycles performed throughout the experiment When the number is achieved the experiment will be stopped Time unit drop down box it lets you specify the time unit of charging and 99 66 discharging You can select seconds minute and hour Based on the current value set by the user the Software will automatically select an appropriate current range without user settings 63 User s Manual 13 1 3 Pstat Gstat The Experiments Setup Pstat Gstat menu item is usually used to configure the Pstat Gstat for all experiments in the experiment list These settings apply to all experiments where the Default Settings are selected See Pstat Gstat Setting 13 1 4 Cell Setting See Cell Setting 9 1 13 2 Galvannostatic Charging Discharging Experiment Charging Discharging Galvannostatic Charging Discharging It is used to measure characteristics of cyclic charge discharge of the electrode material such as a secondary battery or super capacitor electrode material under a constant current and test the cycle life of the electrode material B
69. ing 9 1 26 User s Manual 0 0003 0 0002 2 0 0001 0 0002 0 0003 0 5 0 0 5 1 0 16 Volts Figure 2 1 CV of Pt electrode in IM 504 8 3 Staircase Voltammetry Experiment Voltammetry Staircase Voltammetry In Staircase Voltammetry SCV the potential 15 incremented from Initial toward Final E and it may be scanned back Current is sampled after every potential increment and recorded as a function of potential Staircase Voltammetry SCV New Data File Fil ename Comments OCP V Data Acquisition Scan Parameters 2 initialE v 0 20 Reference Uz Sec Doa C Frequency 222 Ead 5 T Step Period 5 0 05 Pstat Gstat Final E V 0 60 vs Reference Cycles 5 Axis ir ox Cancel Help OCP will display the actual open circuit potential of the cell updated per second If the instrument is turned off this value will display Not Available 8 3 1 Data File When the experiment is performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This 15 particularly useful in case you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file already exists 27 User s Manual 8 3 2 Scan Parameters Init E and
70. iod 5 1 Ex Bias DC Current lor Cancel Help OCP will display the actual open circuit potential of the cell updated per second If the instrument is turned off this value will display Not Available 8 8 1 Data File When the experiment is performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This is particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you may be warned if the file has already existed 8 8 2 Scan Parameters Init E and Final E should be at least 0 01 V apart _ 34 User s Manual Incr E is the increment potential of each pulse it can be chosen from 0 001 V to 0 05 V Amplitude can be chosen from 0 001 V to 0 5 V When the AC frequency is 2 Hz or lower the Sample Period parameter should be at least 2 seconds Bias DC Current check off or on enables DC current bias during run 8 8 3 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second is specified 8 8 4 Axis Type When the experiment is performed the data will be displayed as specified by the Axis Type CorrView can be later used to display the data in other formats 8 8 5 Pstat Gstat The Experiments Setup Pstat Gstat menu item is usually used to configure the Pstat Gstat for all experim
71. ion Scan Parameters 9 LEE Initial E V 0 50 vs Reference 0 02 Sec Frequency Inc E V 10 004 50 Hz PstatiGstat Pulse Width s 0 05 Pulse Period s 0 20 E Final V 0 05 vs Reference Cell Axis Type OCP will display the actual open circuit potential of the cell updated per second If the instrument is turned off this value will display Not Available 8 6 1 Data File When the experiment 1s performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This 15 particularly useful in case you forget the file names you have already used However 3 User s Manual before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file has already existed 8 6 2 Scan Parameters In Normal Pulse Voltammetry NPV the base potential is held at Init E and a sequence of potential pulses with increasing amplitude is applied The current at the end of each potential pulse is sampled and recorded as a function of the pulse potential Init E and Final E should be at least 0 01 V apart 5 Reference is used to select an exact potential to be applied Incr E is the increment potential of each pulse it can be chosen from 0 001 V to 0 05 V Pulse Width can be chosen from 0 001 s to 10 s Pulse Period can be chosen from 0 01 s to 50 s 8 6 3 Data Acquisition If Sampl Freq H
72. ion current value 15 higher than specified maximum anode current or lower than the specified minimum cathode current If you choose Based on DI Dt Stop checkbox CorrTest will automatically terminate potentiostatic polarization tests when the DI Dt is greater than a certain set value If you choose the Disabled checkbox the above two test termination conditions are both discarded 68 User s Manual 14 3 3 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second 15 specified 14 3 4 Axis Type When the experiment 15 performed data will be displayed as specified by the Axis Type CorrView can be later used to display the data in other formats 14 3 5 Pstat Gstat The Experiments Setup Pstat Gstat menu item 1s usually used to configure the Pstat Gstat for all experiments in the experiment list These settings apply to all experiments where the Default Settings are selected See Pstat Gstat Setting 14 3 6 Cell Setting See Cell Setting 9 1 15 Data View 15 1 CV Data View In the potentiostat mode including those test methods based on constant potential constant current and galvanic current etc this Data View window graphically shows data in real time and has Stop Reverse Pause and other graphical buttons In the mode of data logger it shows the outside signal path at work and recorded data and graphs at present Name of the data fil
73. lled the main channel potentiostat and the slave unit 1s also called the auxiliary channel potentiostat whose function is to control the potential difference between DW and RW Rotating driver Disk electrode Bi potentiostat ve i Slave Unit Ring electrode P ify E Main FE E Counter aheference Figure 2 5 Rotating disk electrode left and its connection with Bi Potentiostat right The main unit adopts the common three electrode mode sheath clip of the auxiliary electrode 15 connected to counter electrode CE sheath clip of the reference electrode 1s connected to reference electrode RE and that of the working electrode 1s connected to the output wire of disk electrode Disk Electrode The slave unit uses two electrode potentiostatic mode sheath clip of auxiliary electrode and the reference electrode are connected to the ring electrode and sheath clip of the working electrode 15 connected to the disk electrode This two electrode potentiostatic mode 15 to control the potential difference between the ring electrode the disk electrode Note the potentiostats of the main unit and the slave unit both use field work mode In the process of disk electrode polarization the generated intermediate reaches the ring electrode Due to the potential difference between disk electrode and ring electrode it will be further oxidated or reduced And current on ring electrode
74. med 3 1 2 Close Close an open file If the file has been modified CorrTest software will prompt you to save the changes 3 1 3 Save Save an open file with the same name 3 1 4 Save As Save As saves the current File with a different name 3 1 5 Print Setup A dialog box to set the print format 3 1 6 Print Print experiment results by using a default template created and selected in Print Setup 3 1 7 Exit Close the software 3 2 Edit The Edit menu include the following functions 3 2 1 Cut Cut allows the user to select the desired data from a Data Cut window to the clipboard 3 2 2 Copy Copy allows the user to select the desired data from a Data Copy window and paste into another program 3 2 3 Paste Paste allows the user to select the data and paste into another program 3 2 4 Delete Delete permits the permanent deletion of data 6 User s Manual 4 System Setup 4 1 Com Port Setup The software will automatically search for the Com Port when the instrument 15 connected to the PC s USB port fuse USB interface please Baud Rate 115200 select virtual part Handshaking Hone Cancel Parity hal ty None B C RTS Help stop bit 1 Zon RTS 4 2 Timing Measurement Timing measurement mode is convenient for users to run unattended experiments Timing Measurement New Data File Filename Open Circuit Potential Run from
75. n curve selected by the user and thus to calculate the linear polarization resistance Rp value of the system It is also used to calculate the corrosion rate according to the formula Vcorr B Rp where Stern B value is given by the user For linear polarization the polarization resistance of the cathode and the anode segment may be somewhat different so both results of Rp value will be displayed simultaneously But the corrosion rate will be calculated according to the average of the two Tafel Fit 3 parameters by fitting the weakly polarized area it will calculate the anode cathode Tafel slope ba bc the corrosion current density 1 and corrosion rate These calculations are dependent on the present electrode parameters Tafel Fit 4 parameters using 4 parameters method it can calculate Tafel slopes ba and limiting diffusion current density corrosion current density icon and corrosion rate vcor by fitting anodic and cathodic weak polarization curves 17 Contact us If you have any suggestions or comments about this product please contact us Wuhan Corrtest Instruments Co Ltd Our address 501 Block B Dingye building International Enterprise Center Guanggu Avenue Donghu Development District Wuhan China URL http www corrtest com cn E mail service corrtest com cn Tel 86 27 67849450 86 27 67849890 86 13971066778 Fax 86 27 67849890 39 Nm
76. nd slave unit users can set the current range switching signal gain low pass filter switches digital smoothing scan polarization delay time and so on Please note real ground must be chosen for earthing mode 11 1 7 Cell Setting See Cell Setting 9 1 11 2 Rotating Disk Electrode RDE Experiment Bi Potentiostat Rotating disk electrode Compared with the stationary electrode rotating disk electrode has the following advantages stable concentration polarization good stability of polarization curves capable of measuring relatively rapid electrochemical reactions So polarization curves of the rotating disk electrode have wide applications especially in the aspects of calculating diffusion coefficients electron gains amp losses in reactions the concentration of reactants leveling effect of electroplating additives and the electrode kinetic parameters etc With the help of ring electrode users can also detect reaction intermediates on the disk electrode DW is disk electrode See left in the figure below while RW is the ring electrode They are two separate concentric working electrodes According to the experimental requirements DW and RW should be at different polarization potential so that electrochemical product on DW can reach ring electrode for further oxidation reduction 5 User s Manual reaction and be detected Disk and ring electrodes are connected to potentiostat with dual units The main unit is also ca
77. nd current waveforms have much noise the capacitance of the bandwidth filter needs to be increased for preventing shock User s Manual In impedance test of high resistance system if the bandwidth response capacitance doesn t open in Impedance test Analyzer window it may cause shock phenomenon during the test As shown in the graph below there is no sine wave signal in the waveform signals of the current and potential and the amplitude is not the same for the two signals It indicates the test system does not correctly follow the sinusoidal signal and that a shock occurs Original Freq 6 28 4 Figure2 6 The current and potential waveform in shock After changing the bandwidth capacitance in the Analyzer window to 22 normal sine wave signal can be seen indicating that the instrument works well and can respond with the imposed sine wave signals The acquired waveform is shown in Figure below The amplitude of the potential signal 15 1OmV which is in accordance with that of the imposed signal The current is in the range of 35uA conforming to the selected current range 200uA If the current amplitude 15 too large in a square wave or too small signal noise ratio 15 too low the measured 1mpedance will have big errors In this case the minimum high frequency current range in the analyzer needs to be re adjusted If it s just the noise of current signal being relatively large
78. nd enter 0 5 The potentiostat will make the polarization potential of work electrode to be 0 5 V rather than 0 5 V OCP test potentials AC amplitude value 15 the amplitude value of the excitation signal of electrochemical Impedance For example E 0 012 sin wt V means AC signal amplitude is 12mV However under the state of high frequency the actual polarization amplitude of the working electrode may be less than this value due to rate limitation of the amplifier and the high frequency transmission loss of the conducting wires 2 9 s User s Manual 12 1 3 Frequency Sweep Users should determine the frequency scanning method Frequency scanning starts from the initial frequency to the stop frequency and the mode can be linear or logarithmic If you choose linear mode the frequency test points will be evenly distributed between start frequency and stop frequency If the frequency range is Ik to I HZ and you set 10 test points the measuring frequencies will be 1Hz 99 9Hz 2 x 99 0 Hz Generally users don t select this mode except for special requirements If the selected mode 15 logarithmic the sampled frequency data points will be evenly distributed in Bode diagram It is particularly useful for frequency scanning with frequency range of 2 to 5 logarithmic orders of magnitude If the frequency range is lk to IOHZ and you set 5 test points for every 10 octave the measuring frequencies will be 1
79. not present for the space charge capacitance Csc and the measured potential measured voltage Vm there is the following linear relationship 2 N type semiconductor 1 9 4 kT F Vn Vrt P type semiconductor 2 Where is flat band potential Na and Na are donor and acceptor carrier concentration is the relative permittivity is the permittivity of vacuum A electrode surface area k 15 Boltaman constant T 15 absolute temperature is the electric charge Passivation film has a double structure Since the composition and the crystal structure of the inner and outer layer of the passivation film is different semiconductor type of the inner and outer layers is different either And thus two space charge layers are formed inside the passivation film that is the solution passivation film interface space charge layer and the passivation film inner layer outer layer interface pn junction capacitance Because both pn and passivation film capacitance are small in the impedance potential sweep high frequency sine wave is generally used for measurement 60 User s Manual is EIS vs Potential IMPE General New Data File Filename E Commens ocP v r4rsa9 EIS Parameters Potential Parameters Frequency Hz 100000 Init E V 0 5 vs OCP T 10 AC Amplitude mV
80. nts in the experiment list These parameters are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 6 1 7 Cell Setup See Cell Setup 9 1 The OK button exits the setup diabox saves all the changes you have made and runs the experiment Cancel exits the setup diabox Any changes made to the parameters will be lost Help accesses the on line help information on the setup of this experiment 6 2 Potentiostatic Experiment Stable Polarization Potentiostatic This experiment applies a constant potential and monitors the current as a function of time The experiment can be performed for a fixed duration or until a particular current 15 reached A Galvanic corrosion can be performed by setting the applied potential to zero vs Reference electrode 11 User s Manual Potentiostatic New Data File Comments OCP V 0 83034 Data Acquisition Experiment Parameters s sec Applied Potential 20 OCP ee Total Time 200 Seconds 5 Hz Experiment Termination Cutoff when i mA 10 D Usel aoe Pstat Gstat or i mA 10 Disabled Cutoff when Q 0 UseQ Q lt 10 Cell BAI Axis type Time ox Cancel Help OCP V will display actual open circuit potential of cell updated per second 6 2 1 Data File When the experiment is performed the data will be sav
81. oints and spread out over the entire scan range to a maximum of 1000 points per cycle Cyclic Voltammetry CV gt New Data File Filename Comments OCP V 0 77874 Data Acquisition Scan Frequency Use Initial E V 100 Hz Low E V 2 vs Reference Interval High E V l6 vs Reference 5 id B Final E V vs Reference Pstat Gstat een a E ScanRate mVis 100 10 Cell Axis Type we This experiment applies a potential sweep between up to 4 separate potential setpoints 25 User s Manual If only 2 setpoints are used multiple cycles will be performed OCP will display the actual open circuit potential of the cell updated per second If the instrument 15 turned off this value will display Not Available 8 2 1 Data File When the experiment 15 performed the data will be saved in the file specified by Data File The Dir button can be used to display list of all directories and files This 15 particularly useful in case you forget the file name you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file has already existed 8 2 2 Scan Parameters The potential may be swept between up to 4 separate setpoints in this experiment The experiment starts at the Initial Potential sweeps to High E to Low E and then to the Final Potential Cl
82. omplete cycle includes one charge and one discharge process this parameter specifies the total number of cycles performed throughout the experiment this number is reached the experiment will be stopped Time unit drop down box Lets you specify the charge and discharge time unit 99 66 you can select seconds minute and hour 64 User s Manual For charge discharge potential value users can select relative reference or relatively open 13 2 4 Pstat Gstat The Experiments Setup Pstat Gstat menu item 1s usually used to configure the Pstat Gstat for all experiments in the experiment list These settings apply to all experiments where the Default Settings are selected See Pstat Gstat Setting 13 2 5 Cell Setting See Cell Setting 9 1 14 Misc Techniques 14 1 Electrochemical Noise Experiment Misc Techniques Electrochemical Noise This test method is mainly used for monitoring changes of the noise potential and the noise current zero resistance current or galvanic current with time Length of monitoring time can be set accordingly For CS series workstations the noise signal or the galvanic current measurements 15 different from other methods because it does not require polarization state In the noise galvanic current measurements the working galvanic electrode 1 15 connected to the green sheath clip of To RE cli Ref electrode To WE clip Black Yellow
83. ot Available 18 User s Manual 7 1 1 Data File When the experiment 1s performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This is particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you may be warned if the file has already existed 7 1 2 Multi Potential Steps Parameters A potential sweep between up to 12 separate potential setpoints is applied and the current response is measured The experiment starts at the Initial Potential sweeps to Step 1E to Step 2E to Step 3E and Final E If the step time box is filled with zero this segment of the sweep Step will be skipped A potential can be specified in several ways If vs Open Circuit is chosen the specified potential 15 added to the open circuit potential of the cell vs Reference is used to select an exact potential to be applied No of Cycles specifies how many times the potential 1s cycled between Initial E and Final E The Time determines how long the potential will be held at each step 7 1 3 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second 15 specified 7 1 4 Axis Type When the experiment is performed the data will be displayed as specified by the Axis Type CorrView can be later used to display the data in ot
84. quencies fL 10Hz is relatively low frequency and 10 1000Hz 1s in the middle range The impedance of the working electrode is different in face of high frequency signal and low frequency signal If accuracy improvement is needed for measurement results the setting for current range is varied The user can select different current range based on frequency band Generally current range under low frequency band should be smaller than that under high frequency band If the users set range inappropriately the measured impedance spectrum curve may have large noise Or if they frequently change the range there will be obvious turning point in the curve In such cases the users should re set By observing signal amplitude in the waveform display users can check if the current range setting 15 appropriate Bandwidth Settings Bandwidth Setting 15 used to change the frequency response bandwidth of potentiosta When the capacitance value increases the bandwidth of the potentiostat will be narrower the high frequency performance will decrease but stability will enhance Bandwidth switching is set based on the critical frequency fc When measuring frequencies are above fc generally you should choose a smaller capacitance or turn it off The instrument has high bandwidth so there will not be false impedance spectra in high frequency area But for impedance test of the high impedance system it may result in shock You may have to increase the
85. r button can be used to display a list of all directories and files This is particularly useful if you forget the file names you have already used However before CorrTest starts performing the first experiment in the Experiment List you may be warned if the file has already existed 10 User s Manual CorrTest will automatically append the suffix COR to a data file if you do not enter one Therefore if you specify tutor the file tutorl cor will be used In the same way if you specify tutorl abc the file tutorl abc cor will be used The Comments text 1s saved in the data file The time date and all measurement parameters are automatically saved in the data file so you don t need to write these information into the comment area 6 1 2 Experiment The Total Time determines the total length of the experiment 6 1 3 Experiment Termination If the Use E box 15 checked the experiment will be automatically terminated as long as the potential goes below the Potential V value or above the Potential V gt value 6 1 4 Data Acquisition The acquisition rate in Points Second is specified by the Sampl Freq Hz value 6 1 5 Axis Type When the experiment 15 performed data will be displayed as specified by the Axis Type CorrView can be later used to display the data in other formats 6 1 6 Pstat Gstat The Experiments Setup Pstat Gstat menu item 15 usually used to configure the Pstat Gstat for all experime
86. r potential 1s reached Galvanostatic x New Data File Filename zx Comments OCP V 0 83994 Data Acquisition Experiment Interval Applied Current 0 20 mA 1 Sec Total Time 200 Seconds Frequency Experiment Termination 5 Hz When potential V 2 C UseE or potential V 2 Disabled Potential vs OCP EA E h 3 gt 110 UseQ or Q Coub 10 Joel Axis E vs Time Help OCP V will display the actual open circuit potential of the cell updated per second 13 User s Manual 6 3 1 Data File When the experiment is performed the data will be saved in the file specified by Filename The Dir button can be used to display a list of all directories and files This 15 particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file has already existed CorrTest will automatically append the suffix to data files if you do not enter one Therefore if you specify tutorl the tutorl cor will be used In the same way if you specify tutorl abc the file tutorl abc cor will be used The Comments text 1s saved in the data file The time date and all measurement parameters are automatically saved in the data file so you don t need to write these information into the comment area 6 3 2 Experiment Applied Cu
87. r used to display the data in other formats 6 5 6 Pstat Gstat The Experiments Setup Pstat Gstat menu item is usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 6 5 7 Cell Setting See Cell Setting 9 1 7 Transient Polarization 7 1 Miulti Potential Steps Experiment Transient Polarization Multi Potential Steps In the Multi Potential Steps technique twelve potential steps can be applied and cycled Current 1s recorded as a function of time Multi Potential Steps New Data File Filename ta Commens O QcP y 0281530 Data Acquisition _ Multi Potential Steps Parameters f Interval Initial E V 01 Time 100 Step amp E v o4 Time 100 10 001 Sec Stepi Eo Time Ho0 Step E V 04 Time Step2 02 Time Ho0 Step8 05 Time 100 Step3 00 02 Time Ho0 Step9 E V 05 Time 100 stepaE o3 00 Et oe 100 PstatGstat steps E v 02 Time foo FinarE o oe Time 100 un Potential vs Time Unit Msec Cell ost Axis Time 100 Hz wW Recording OCP will display the actual open circuit potential of the cell updated per second If the instrument is turned off this value will display N
88. rging current symbol will be different If the working electrode is connected to battery positive and the reference amp auxiliary electrodes are connected to the battery negative the displayed open circuit potential will be positive Then enter a positive value and it indicates charging Constant current constant voltage conversion it s the critical voltage when charging process is changed from constant current mode to constant voltage mode According to the charging rules generally constant current charging mode is adopted in the early stage of charging When the battery voltage is higher than the critical voltage the charging will turn into constant voltage mode and this moment the charging current will gradually decrease with time When it decreases to the cutoff current of the constant voltage charging usually 10 to 20 of the charging current the software will automatically disconnect the charging circuit Discharge current if the working electrode 15 connected to battery positive and the reference amp auxiliary electrode are jointly connected with battery negative then enter a negative value in the discharge current input box it indicates the discharge Discharge critical voltage in discharging process when the voltage drops to the critical voltage it will stop the discharge in order to avoid excessive discharge Charge discharge interval during this time interval the battery is in the open circuit Max
89. rn on and turn off Step E2 setpoints If a Vertex s Use box is not checked that segment of the sweep Step E2 will be skipped The Time determines how long the potential will be held at each step A potential can be specified in several ways If vs Open Circuit is chosen the specified potential is added to the open circuit potential of the cell vs Reference is used to select an exact potential to be applied User s Manual 7 3 3 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second is specified 7 3 4 Axis Type When the experiment is performed the data will be displayed as specified by the Axis Type CorrView can be later used to display the data in other formats 7 3 5 Pstat Gstat The Experiments Setup Pstat Gstat menu item is usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 7 3 6 Cell Setting See Cell Setting 9 1 7 4 Galvanic Stair Step Experiment Transient Polarization Galvanic Stair Step Galvanic Stair Step ISTEP New Data File Filename Comments OCP V 0 82952 Data Acquisition Scan Parameters Frequency Initial Current 0 Time 200 2000 Hz Step Current 1 0 05 Time 800 Pstat Gstat Use Step Current 210 Time 1000 89 Current Unit ime Unit mSecs
90. rrent specifies the amount of current applied during the experiment This is the total current applied rather than the current density The Total Time determines the total length of the experiment 6 3 3 Experiment Termination When Use E box 15 checked the experiment will be automatically terminated if the potential goes below the Potential V value or above the Potential V value When the Use Q box is checked the experiment will be automatically terminated if the total charge in Coulombs goes below the Charge C value or above the Charge C value If the not enabled box 15 checked the experiment 15 not terminated until the total time is reached 6 3 4 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second 15 specified 6 3 5 Axis Type When the experiment 15 performed the data will be displayed as specified by the Axis Type Corr View can be later used to display the data in other formats 6 3 6 Pstat Gstat The Experiments Setup Pstat Gstat menu item 1s usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 6 3 7 Cell Setting See Cell Setting 9 1 14 User s Manual The OK button exits the setup window saves all changes you have made and runs the experiment Cancel exits the setup diabox Any changes made to
91. s are selected See Pstat Gstat Setting 10 1 7 Cell Setting See Cell Setting 9 1 10 2 Linear Stripping Experiment Stripping Voltammetry Linear Stripping l 5 Linear Stripping New Data File Filename oe Comments OCP V 0 801 38 Data Acquisition Deposition Parameters f Frequency Conditioning 0 10 Time 5 15 2 Deposition E V 10 10 vs OCP Interval 0 5 mv Deposition Time s 15 Quiet Time s 15 Linear Stripping Parameters Pstat Gstat Init E V 0 10 vs Final E V 0 10 vs Cell Scan Rate 05 ImVis Axis vs E Cancel Help OCP will display the actual open circuit potential of the cell updated per second If the instrument is turned off this value will display Not Available 10 2 1 Data File When the experiment is performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This 15 particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file has already existed 43 User s Manual 10 2 2 Deposition Parameters Before the experiment the surface of working electrode needs cleaning by this conditioning step A constant potential deposition step 1s applied to accumulate species on the working ele
92. s experiment The experiment starts at the Initial Potential and then to the Final Potential A potential can be specified in several ways If vs Open Circuit is chosen the specified potential 15 added 40 User s Manual to the open circuit potential of the cell vs Reference is used to select an exact potential to be applied Pulse Width specifies how long the potential 1s sustaining Number of Steps specifies how many times the potential is cycled between Initial Potential and Final Potential 9 3 3 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second 15 specified 9 3 4 Axis Type When the experiment 15 performed data will be displayed as specified by the Axis Type Corr View can be later used to display the data in other formats 9 3 5 Pstat Gstat The Experiments Setup Pstat Gstat menu item 1s usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 9 3 6 Cell Setting See Cell Setting 9 1 10 Stripping Voltammetry 10 1 Potentiometric Stripping Experiment Stripping Voltammetry Potentiometric Stripping In stripping voltammetry the usual working electrode is a dropping or a film mercury and the most common technique is the anodic stripping meaning that a negative potential is applied to the electrode and the ca
93. select Text to insert whatever text in the graphics If you want to change the color line pattern or mark etc you can do settings in the pop up diabox of File Data File menu Equivalent circuit fitting From the Tools menu select Equivalent Circuit then you can make a strong analysis of impedance spectroscopy Users can set up equivalent circuit of their own or just choose the classic equivalent circuit In the equivalent circuit window select Model equivalent circuit then you can start the simulation or fitting Graph copy Right click the mouse button from the pop up menu select copy graphics to the clipboard then the graphics can be copied to the Windows clipboard And then in Word via the Edit Paste menu graphics will be directly inserted 1nto Word document Details about Zview and usage please refer to its Help files 12 2 EIS vs Time Experiment Impedance EIS vs Time It measures the characteristics of impedance with time s change at a single frequency and 15 used to track the dynamic processes of some system such as conductivity S8 User s Manual E EIS vs Time IMPT General Analyzer New Data File Filename Comments OCP V 7 4931 6 Polarization Time Scan DC Potential v 0 vs OCP Frequency Hz 100000 AC Amplitude mV 10 Interval Sec Step 1 Pstat Gstat Cell Total Time s 1000 H
94. t experiment in the Experiment List you will be warned if the file has already existed 11 1 2 Hydrogen ion reduction Slave unit Users should set peak and trough current of the hydrogen charging current square wave as well as the corresponding duration Hydrogen charging current can only flow to the cathode so that hydrogen atoms become ions via reduction and diffuse through the working electrode metal disk in the center Number of cycles of hydrogen charging current is equal to the number of square wave 11 1 3 Hydrogen ion oxidation main unit Polarization potential V in the electrolytic cell the hydrogen is applied to the working end of the current detecting electrode polarization potential Generally speaking this potential enables the working electrode metal thin disk to stay in anodic polarization That is to say a positive polarization potential should be entered to allow hydrogen atoms from the opposite side of the medal disk to be oxidated and turn into ions Oxidation of residual current With the continuing of potentiostatic polarization residual hydrogen current in the metal will gradually reduce When it is lower than the set value the software can be start galvanostatic polarization of hydrogen charging and hydrogen charging begins Upon the start of the measurement firstly the main unit will open potentiostatic polarization so that the hydrogen atoms in the metal foil can sufficiently diffuse out onto the o
95. t experiment in the Experiment List you will be warned if the file has already existed CorrTest will automatically append the suffix COR to data files if you do not enter one Therefore if you specify tutorl the file tutorl cor will be used In the same way if you specify tutorl abc the file tutorl abc cor will be used The Comments text is saved in the data file The time date and all measurement parameters are automatically saved in the data file so you don t need to write these information into the comment area 6 4 2 Scanning Parameters Up to 4 separate potentials can be applied during the experiment The experiment 15 User s Manual starts at the Initial Potential sweeps to Vertex 1 to Vertex 2 and then to the Final Potential Click on the Used boxes to turn on or turn off the Vertex 1 and Vertex 2 setpoints If a Vertex s Used box is not checked that segment of the sweep will be skipped For example if only Vertex 1 is checked the sweep Initial Vertex 1 Final is performed If neither Vertex 1 nor Vertex 2 1s checked Initial Final 15 performed A potential can be specified in several ways If vs Open Circuit is chosen the specified potential 15 added to the open circuit potential of the cell For example 0 1 V vs Open Circuit means applying a potential of 0 1 Volts above the measured open circuit potential vs Reference is used to select an exact potential to be applied
96. the parameters will be lost Help accesses the on line help information on the setup of this experiment 16 User s Manual 6 5 Galvanodynamic Experiment Stable Polarization Galvanodynamic Corrosion technique that uses a single current scan or ramp programs from an initial current to a final current plotting the resulting potential vs time A typical use of this technique is to measure the relative susceptibility to localized corrosion m Galvanodynamic New Data File Filename Comments OCP V 0 83452 Data Acquisition Galvanodynamic Parameters t Interval Initial Current 0 50 Scan Rate Sec Use Vertex Current 1 0 10 0 01 mAs Frequency Use Vertex Current 2 0 5 Final Current 0 50 Current Unit Expeirment Stop Scan Stop When Potential 2 2 Scan Potential vs OCP S Axis Type Evs Logi ok Cancel Help This experiment applies a current sweep between up to 4 separate setpoints The Sweep can be terminated if a particular potential is reached OCP will display the actual open circuit potential of the cell updated per second If the instrument 15 turned off this value will display Not Available 6 5 1 Data File When the experiment is performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This 15 particularly useful
97. tions are discharged as metallic atoms into the mercury amalgam Successively the metal atoms are oxidised again during an anodic scanning of potential During the scanning of the potential the current 1s measured and plotted so the resulting voltammogram is a peak shaped graphic L 5 User s Manual Figure 2 2 Stripping voltammetry in a solution containing Pb Cd Cu Potentiostatic Stripping ES New Data File Filename Comments OCP V 0 8021 6 Data Acquisition Deposition Parameters Interval Conditioning E V 0 10 Time s 15 0 5 Sec DepositionE v 010 vs ocP Frequenc 7 Deposition Time s 15 Quiet Time s 15 Pstat Gstat Potentiostatic Stripping Parameters EEE Stripping 10 20 OCP Stripping Time 200 Seconds Cell Imi Axis Type vs E Cancel Help OCP will display the actual open circuit potential of the cell updated per second If the instrument is turned off this value will display Available 10 1 1 Data File When the experiment 15 performed the data will be saved in the file specified by Data File The Dir button can be used to display a list of all directories and files This 15 particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you may warned if the file has
98. ue or above the Current A value If the Use Q box is checked the experiment will be automatically terminated as long as the total charge in Coulombs goes below the Charge C value or above the Charge 12 User s Manual C gt value If the not enabled box is checked the experiment will not be terminated until the total time is reached 6 2 4 Data Acquisition If Sampl Freq Hz 15 chosen the acquisition rate in Points Second is specified 6 2 5 Axis Type When the experiment 15 performed the data will be displayed as specified by the Axis Type CorrView can be later used to display the data in other formats 6 2 6 Pstat Gstat The Experiments Setup Pstat Gstat menu item 1s usually used to configure the Pstat Gstat for all experiments 1n the Experiment List These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 6 2 7 Cell Setting See Cell Setting 9 1 The OK button exits the setup diabox and saves all changes you may have made and runs the experiment Cancel exits the setup diabox Any changes you may have made to the parameters will be lost Help accesses the on line help information on the setting up of this experiment 6 3 Galvanostatic Experiment Stable Polarization Galvanostatic A constant current 15 applied and the potential is monitored as a function of time The experiment can be performed for a fixed duration or until a particula
99. ursor For example if you select E vs time the text is the time s and potential mV And when you switch to the E vs the content is the current mA and the potential mV 15 1 4 Zoom in When users need to observe graphs or data in a local position during the test they can left press the mouse button on the upper left side of the certain area and drag to the lower right side and then release the button This local graph will immediately be zoomed in 70 User s Manual and fill up the entire diabox The graph will not be updated but this time test system of CorrTest is still scanning and collecting data signals If you want to go back to the original status just click the mouse on the graph 15 1 5 Stop and Pause Click on o to terminate the ongoing test Click on to pause test 15 1 6 Reverse Scan A click on can reverse scanning But this is just applicable for potentiodynamic sweep and cyclic voltammetry test Click on this button then the scanning direction will immediately be reverse but the scan rate remains the same If click again the scan will go back to the original direction This button allows users to change the scan direction at any time in order to study the cyclic characteristics of the electrochemical reaction 15 1 7 Polarization Nature Switch pera Click on then you can change the polarization natural state of electrode 15 1 8 Print graph Click on the print b
100. utton then you can immediately output the displayed real time graph to the printer 15 1 9 Lock Graph A click on allows users to lock the graph diabox You can watch the progress of testing while doing other operations such as parameter fitting document editing If you want to unlock it just click on it again 15 2 EIS Data View CorrTest is able to display the test data of the impedance spectroscopy Users can read test data by moving the mouse onto the graph area on the screen that displays the real part imaginary part complex modulus phase angle and frequency The measured data is automatically saved After selecting the box of locked the data point the user can read the coordinate of the data points in Nyquist or Bode graph including the real part the imaginary part frequency impedance modulus and phase angle by locking the mouse In the title bar of the diabox the data file names are displayed At the bottom of the diabox there are displays of the operating parameters such as the polarization amplitude DC level scanning range current range and so on CorrTest software will automatically select the best starting and ending coordinates and make adjustments for display mode of the coordinate 7 User s Manual m EIS vs Frequency IMP Graphing 7 z60 24 u 8 1 6 2 Chan 3 Chan 4 Pts 60 Z Oy1 080E 3 Z 0y 5823E 1 2007 1 082E 3 Freq Hzy 1 034E 1 Pro
101. ve current is for an anodic oxidation reaction User s Manual The Low Pass Filter can be used to reduce high frequency noise 5 3 Waiting before run 7 ai Wait Work Mode status Galyanodynami Active Channel 1 e V Range Potential V 0 64554 ema I Range Current ma 0 5005 8 seconds later the experiment will run When switching from the natural state to the polarization of potentiostat it takes time before starting to scan because the electrode itself 1s unstable in the beginning This can be adjusted according to the specific requirements of the system 6 Stable Polarization 6 1 Open Circuit Potential Experiment Stable Polarization Open Circuit Potential This experiment aims at monitoring the Open Circuit Potential or Free Corrosion Potential as a function of time The experiment can be performed for a fixed duration or until a particular potential 15 reached Er Open Circuit Potential New Data File Comments OCP V 0 83236 Data Acquisition Experiment Experiment Termination Interva uod TetalTime 200 Use SEC PORA Potential 2 Frequency Seconds 5 or Potential V 2 Pstat Gstat Cell Axis Type E vs Time OCP will display actual open circuit potential of cell updated per second 6 1 1 Data File When the experiment is performed the data will be saved in the file specified by Filename The Di
102. very fast In this case data points will be lost IR Compensation Correction refers to methods requiring compensation for unwanted medium resistances in an electrochemical system Without correction these unwanted resistances may distort data or make it impossible to perform the desired experiments The resistance of the electrolyte between the working electrode and the reference electrode is the most common cause of errors Moreover contact resistance and long electrode leads can cause errors too The Feedback compensation method may be used to boost the cell potential to compensate potential drops caused by the cell geometry and solution resistivity Feedback may only be used with a fixed not Auto Current Range Polarity Convention defines how positive and negative potentials and currents are interpreted When the potential polarity is set to 02 a more positive potential produces a larger driving force for an anodic oxidation reaction and a more negative potential produces a cathodic reduction reaction When the potential polarity 1s set to O2 a more negative potential produces a larger driving force for an anodic oxidation reaction and a more positive potential produces cathodic reduction reaction If the Current polarity is set to 02 positive current is for an anodic oxidation reaction and negative current 15 for a cathodic reduction reaction When using O2 positive current is for a cathodic reduction reaction and negati
103. wing through this electrode is measured and integrated reporting coulombs as a function of time Technique is also referred to as CC For bulk electrolysis measurements a Pre Electrolysis parameter is provided to electrolyze and subtract out solvent background currents with the sample of interest added after the Pre Elect s stage to measure the total charge associated with the sample minus the background current contributions Chronocoulometry CC New Data File Filename Comments OCP V 0 76145 Data Acquisition Scan Parameters cB Initial E v 05 vs Reference 0 01 Sec Frequency Final E V 0 1 vs Reference 100 Hz Pulse Width 5 25 Pstat Gstat a Number of Steps Axis Cell EAI Q vs Time Cancel Help OCP will display the actual open circuit potential of the cell updated per second If the instrument 1s turned off this value will display Not Available 9 3 1 Data File When the experiment is performed the data will be saved in the file specified by Data File The Dir button can be used to display list of all directories and files This 15 particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you may be warned if the file has already existed 9 3 2 Scan Parameters The potential may be swept between up to 2 separate setpoints in thi
104. xidation surface and finish the process of oxidation It takes a relatively long time According to ISO standards generally speaking only when the residual oxidation current 50 User s Manual is lower than 1 2uA em threshold value of residual current can the users consider hydrogen atoms in the metal foil being completely oxidized away Once the oxidation current is lower than the threshold the slave unit will start the process of constant current hydrogen charging Hydrogen charging current varies between the peak and the trough value In general 10 20 minutes later based on the material and thickness of the metal the anode current detected by the main unit will gradually increase and eventually keep stable because hydrogen atoms diffuse out to the opposite side of the metal disk and are oxidized to form anode current Polarization time Users can specify the potentiostatic polarization time They can choose unit among second minute and hour 11 1 4 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second 15 specified 11 1 5 Axis Type When the experiment 15 performed the data will be displayed as specified by the Axis Type CorrView can be later used to display the data in other formats 11 1 6 BiStat Config For bipotentiostat users need to do settings for the main amp slave units respectively Parameters of them can be the same or different With buttons of main unit a
105. xists 14 1 2 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second 15 specified 14 1 3 Axis Type When the experiment 15 performed data will be displayed as specified by the Axis Type CorrView can be later used to display the data in other formats 14 1 4 Pstat Gstat The Experiments Setup Pstat Gstat menu item 15 usually used to configure the Pstat Gstat for all experiments in the Experiment List These settings apply to all experiments where the Default Settings are selected See Pstat Gstat Setting 14 1 5 Cell Setting See Cell Setting 9 1 14 2 Data logger Experiment Misc Techniques Data logger The data logger is used to record sync external signal A maximum of six external signals can be recorded simultaneously Two channels have already been used for internal electrochemical measurement This test method 15 completely independent from other electrochemical tests 1 e there will be no interaction between potentiostat s work and external signal recording Before the test the Start button is inactive Only when the user specifies a valid file name will it be activated All subsequent data will be saved in the created file 66 User s Manual Parameter Setup New Data File Filename Comments 2 Data Acquisition Sampling Data Data Record t Interval Channel Ext Gain Total Time 11 Sec 3 33588 V x 1 00 f Frequency Channel Ext Gain 3 33
106. y a list of all directories and files This 15 particularly useful if you forget the file names you have already used However before CorrTest begins performing the first experiment in the Experiment List you will be warned if the file has already existed 8 9 2 Scan Parameters Init E and Final E should be at least 0 01 V apart Incr E is the increment potential of each pulse it can be chosen from 0 001 V to 0 05 V Amplitude can be chosen from 0 001 V to 0 5 V When the AC frequency is 2 Hz or lower the Sample Period parameter should be at least 2 seconds Bias DC Current check off or on enables DC current bias during run 8 9 3 Data Acquisition If Sampl Freq Hz is chosen the acquisition rate in Points Second is specified 8 9 4 Axis Type When the experiment 15 performed the data will be displayed as specified by the Axis Type CorrView can be later used to display the data in other formats 8 9 5 Pstat Gstat The Experiments Setup Pstat Gstat menu item 1s usually used to configure the 36 User s Manual Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 8 9 6 Cell Setting See Cell Setting 9 1 9 Chrono Techniques 9 1 Chronopotentiometry Experiment Chrono Techniques Chronopotentiometry A fastrising current pulse is enforced on the working sense electrode of electrochem
107. ype CorrView can be later used to display the data in other formats 10 4 6 Pstat Gstat The Experiments Setup Pstat Gstat menu item 1s usually used to configure the Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 10 4 7 Cell Setting See Cell Setting 9 1 47 User s Manual 11 Bi Potentiostat 11 1 Hydrogen diffusion measurements Experiment Bi Potentiostat Hydrogen diffusion measurements Hydrogen permeation measurements require a special set of electrolytic cells where two electrolytic cells one for the constant current charging hydrogen the other for hydrogen current detection In each electrolytic cell there is an independent set of reference electrode and the auxiliary electrode sharing a common working electrode This working electrode is composed of a metallic thin plate clipped between the two electrolytic cells See the right Figure When hydrogen charging surface of the working electrode is impose with square wave cathode current by changing the hydrogen charging current via alternating the atoms will diffuse into the metal and gradually arrive at the detection surface 1 e opposite surface of the working electrode By measuring the value of the hydroxide current and delay time users can calculated the hydrogen diffusion rate and the diffusion coefficient Users shoul
108. z is chosen the acquisition rate in Points Second 15 specified 8 6 4 Axis Type When the experiment 15 performed the data will be displayed as specified by the Axis Type CorrView can be later used to display the data in any of the other formats 8 6 5 Pstat Gstat The Experiments Setup Pstat Gstat menu item is usually used to configure Pstat Gstat for all experiments in the experiment list These settings are applicable to all experiments where the Default Settings are selected See Pstat Gstat Setting 8 6 6 Setting See Cell Setting 9 1 8 7 Differential Normal Pulse Voltammetry Experiment Voltammetry Differential Normal Pulse Voltammetry This 15 a hybrid of differential pulse and normal pulse voltammetry Similar to the normal pulse method in this case a pulse will be superimposed on a base potential On top of this pulse a modulation step with definable amplitude and duration 15 applied The current just before and at the end of the modulation step will be measured and the difference will be stored In this manner the advantages of normal pulse short electrolysis time are combined with those of differential pulse pronounced faraday currents Nom User s Manual Differential Normal Pulse Voltammetry DNPV New Data File Filename Comments Pn OCP v Lo 80707 Data Acquisition r Scan Parameters 92 2 Initial E V 0 50 vs Reference 02 re Inc E V 10 004

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