WuhanCorrtestInstrumentsCorp.,Ltd....MANUAL-4-electrodestotheelectrochemicalworkstationfromthe“Cell”port:...

Wuhan Corrtest Instruments Corp., Ltd.

Contents

NOTICE............................................................................................................................................... - 1 -

PART 1 CS SERIES POTENTIOSTAT / ELECTROCHEMICALWORKSTATION.............................................- 2 -

1. INTRODUCTION........................................................................................................................ - 2 -

1.1 SPECIFICATIONS........................................................................................................................ - 2 -1.2 ELECTROCHEMICAL SIGNAL GENERATOR..........................................................................................- 3 -1.3 FRONT PANEL AND REAR PANEL................................................................................................... - 3 -1.4 SCHEMATIC DIAGRAM................................................................................................................ - 5 -

PART 2 CORRTEST® SOFTWARE...........................................................................................................- 6 -

1. INTRODUCTION........................................................................................................................ - 6 -

1.1 SYSTEM REQUIREMENTS..............................................................................................................- 6 -1.2 SOFTWARE INSTALLATION........................................................................................................... - 6 -

2. MENU.......................................................................................................................................- 7 -

2.1 FILE....................................................................................................................................... - 8 -2.2 EDIT...................................................................................................................................... - 8 -

3. SYSTEM SETUP.......................................................................................................................... - 9 -

3.1 COM PORT SETUP.....................................................................................................................- 9 -3.2 TIMING MEASUREMENT............................................................................................................. - 9 -3.3 RESETWORKSTATION................................................................................................................ - 9 -

4. EXPERIMENT SETUP............................................................................................................... - 10 -

4.1 CELL& ELECTRODE SETUP......................................................................................................... - 10 -4.2 PSTAT/GSTAT SETUP................................................................................................................ - 11 -4.3 WAITING BEFORE RUN............................................................................................................. - 12 -

5. STABLE POLARIZATION........................................................................................................... - 12 -

5.1 OPEN CIRCUIT POTENTIAL.........................................................................................................- 12 -5.2 POTENTIOSTATIC..................................................................................................................... - 13 -5.3 GALVANOSTATIC..................................................................................................................... - 15 -5.4 POTENTIODYNAMIC................................................................................................................. - 17 -5.5 GALVANODYNAMIC..................................................................................................................- 18 -

6. TRANSIENT POLARIZATION.................................................................................................... - 20 -

6.1 MULTI-POTENTIAL STEPS.......................................................................................................... - 20 -6.2 MULTI-CURRENT STEPS............................................................................................................ - 21 -6.3 POTENTIAL STAIR-STEP............................................................................................................. - 23 -6.4 GALVANIC STAIR-STEP.............................................................................................................. - 24 -

7. VOLTAMMETRY...................................................................................................................... - 25 -

7.1 LINEAR SWEEP VOLTAMMETRY................................................................................................... - 25 -7.2 CYCLIC VOLTAMMETRY..............................................................................................................- 26 -7.3 STAIRCASE VOLTAMMETRY.........................................................................................................- 29 -7.4 SQUARE WAVE VOLTAMMETRY...................................................................................................- 30 -7.5 DIFFERENTIAL PULSE VOLTAMMETRY........................................................................................... - 32 -7.6 NORMAL PULSE VOLTAMMETRY................................................................................................. - 33 -7.7 DIFFERENTIAL NORMAL PULSE VOLTAMMETRY.............................................................................. - 35 -7.8 A.C. VOLTAMMETRY................................................................................................................ - 36 -

7.9 2ND HARMONIC A.C. VOLTAMMETRY......................................................................................... - 38 -

8. CHRONO TECHNIQUES............................................................................................................- 39 -

8.1 CHRONOPOTENTIOMETRY..........................................................................................................- 39 -8.2 CHRONOAMPEROMETRY........................................................................................................... - 41 -8.3 CHRONOCOULOMETRY............................................................................................................. - 42 -

9. STRIPPING VOLTAMMETRY.....................................................................................................- 44 -

9.1 POTENTIOSTATIC STRIPPING....................................................................................................... - 44 -9.2 LINEAR STRIPPING................................................................................................................... - 45 -9.3 STAIRCASE STRIPPING...............................................................................................................- 47 -9.4 SQUARE-WAVE STRIPPING......................................................................................................... - 48 -

10. BIPOTENTIOSTAT.................................................................................................................... - 50 -

10.1 HYDROGEN DIFFUSION TEST (HDT)....................................................................................... - 50 -10.2 ROTATING DISK ELECTRODE (RDE).........................................................................................- 54 -

11. EIS (ELECTROCHEMICAL IMPEDANCE SPECTROSCOPY)...........................................................- 56 -

11.1 EIS VS FREQUENCY............................................................................................................. - 56 -11.2 EIS VS TIME......................................................................................................................- 60 -11.3 EIS VS POTENTIAL.............................................................................................................. - 62 -

12. CHARGING/DISCHARGING..................................................................................................... - 64 -

12.1 BATTERY CHARGING/DISCHARGING........................................................................................ - 64 -12.2 GALVANOSTATIC CHARGING/DISCHARGING.............................................................................. - 65 -

13. MISC.TECHNIQUES..................................................................................................................- 67 -

13.1 ELECTROCHEMICAL NOISE.................................................................................................... - 67 -13.2 DATA LOGGER................................................................................................................... - 68 -13.3 ELECTROCHEMICAL STRIPPING/DEPOSITION..............................................................................- 69 -

14. DATA VIEW............................................................................................................................. - 70 -

14.1 CV DATA VIEW..................................................................................................................- 70 -14.2 EIS DATA VIEW................................................................................................................. - 73 -

15. DATA ANALYSIS...................................................................................................................... - 75 -

15.1 CORSHOW DATA ANALYSIS................................................................................................... - 75 -15.2 CORROSION RATE CALCULATION............................................................................................ - 77 -

16. FAQS.......................................................................................................................................- 78 -

16.1 HOW TO INSTALL THE CS POTENTIOSTAT / GALVANOSTAT?.......................................................... - 78 -16.2 HOW TO CHECK IF THE WORKSTATION IS FUNCTIONAL?............................................................... - 80 -16.3 HOW TO UNDERSTAND 3-ELECTRODE SYSTEM............................................................................ - 80 -16.4 WHAT CAUSE CURRENT OVERLOAD?....................................................................................... - 81 -16.5 WHAT CAUSE POTENTIAL OVERLOAD?..................................................................................... - 81 -16.6 HOW TO CHECK THE RE?..................................................................................................... - 81 -16.7 HOW TO REDUCE THE NOISE IN ELECTROCHEMICAL EXPERIMENT?.................................................. - 82 -16.8 COMMON PROBLEM AND SOLUTION.......................................................................................- 82 -

17. CONTACT US...........................................................................................................................- 83 -

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NOTICE

GroundingThe electrochemical workstation must be well connected to the ground. It is the basic

requirement in terms of security, and also the important way to increase the anti-interferenceof the instrument. There is a “Ground” port at the rear panel, it is the grounding point for thepotentiostat.

SecurityThe connection or replacement of any cable leads or accessories must be proceeded after

the potentiostat is powered off. To make sure the instrument can be used normally and achievethe specifications as design, the user should pay attention to the following details regardingthe environment factors:This instrument belongs to the indoor installation equipment. It should be protected from

rain, other water sources, corrosive gas or direct sunlight.

The user should make sure that there is ground wire in the power supply socket. Goodgrounding can not only improve the abilities of electromagnetic shielding andanti-interference, but also guarantee the security. The instrument is powered by AC 220Vwhich is must be stable in voltage. The user should also make sure that there is no electricequipment of high power or transient high current near the instrument sharing the samepower supply to prevent big interference resulting from the power supply coupling.

！

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Part 1 CS series Potentiostat / ElectrochemicalWorkstation

1. IntroductionCS Potentiostat / Galvanostat(electrochemical workstation) contains a fastdigital function generator, high-speed dataacquisition circuitry, a potentiostat and agalvanostat. With high performance instability and accuracy with advancedhardware and well-functioned software, it is acomprehensive research platform forcorrosion, batteries, electrochemical analysis,sensor, life science and environmentalchemistry etc.

1.1 Specifications

Potential control range: ±10VCurrent control range: ±2.0APotential control accuracy: 0.1%× full range±1mVCurrent control accuracy: 0.1%× full rangePotential resolution: 10μV (>100Hz), 3μV (<10Hz)Current sensitivity: 10pARise time: <1μs (<10mA), <10μs (<2A)Reference electrode input impedance: >1012Ω||20pFCurrent range: 200nA~ 2A, 8 rangesCompliance voltage: ±21VMaximum current output: 2.0ACV and LSV scan rate: 0.001mV~ 10,000V/sCA and CC pulse width: 0.0001~ 65,000sCurrent increment during scan: 1mA@1A/msPotential increment during scan: 0.076mV@1V/msSWV frequency: 0.001~100K HzDPV and NPV pulse width: 0.0001~1000sAD data acquisition: 16bit@1M Hz, 20bit@1K HzDAResolution: 16bit, setup time: 1μsMinimum potential increment in CV: 0.075mV

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IMP frequency: 10μHz~ 1MHzLow-pass filters: Covering 8-decadePotential and current range switch: Automatic

1.2 Electrochemical Signal generator

Waveform generatorFrequency range: 10μHz~ 1MHzAC amplitude: 0~ 2500mVDC Bias: -10~ +10VOutput impedance: 50ΩWaveform: Sine wave, triangular wave and square waveWave distortion: <1%Scanning mode: Logarithmic/linear, increase/decreaseSignal analyser:Integral time: minimum: 10ms or the longest time of a cycleMaximum: 106 cycles or 105sMeasurement delay: 0~ 105sDC offset compensation:Potential automatic compensation range: -10V~ +10VCurrent compensation range: -1A~ +1ABandwidth: 8-decade Frequency range, Automatic and manual setting

Dimensions (cm):36 (width) ×30(depth) ×14(height); weight: 6.5kgEnvironment :temperature -10℃～40℃， relative humidity <=75%, no high corrosive

gas in the air. ‘

1.3 Front Panel and rear 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 (with crocodile clamp): The electrode cable is used to connect the

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electrodes to the electrochemical workstation from the “Cell” port:Green clamp –This clamp connects to the working electrode. The electrical signal is

measured through WE lead. The green lead consists of 2 cables: WE and SENS cable. Wedesign like this to avoid potential measurement and control error resulting from cable voltagedrop.

Red clamp –This clamp connects to the electrode opposite to the WE and controls thepower output of the instrument.

Yellow clamp –This clamp connects to the reference electrode, a component of thedifferential amplifier that measures/controls the potential between itself and the senseelectrode.

Black clamp– it connects to the Faraday cage or Galvanic electrode.Ov/L light – output current is higher than120% of the set range.Pol (Polarization) indicator light – it means the electrode is on the status of polarization whenthe light is on.Current range – the indicator light shows the present current range.Pstat/Gstat light – working mode of potentiostat / galvanostatLPF light– low pass filter is open if light is on. It can reduce the bandwidth and increase thestability.Power switch – ON and OFF to power on and power off.

Fig.1-2. Rear panel of CS Potentiostat

AC 220Vpower supply port –AC 220V power supply socket with 1A fuse.

Ground option - switch to “floating earth”, then the WE lead is completely insulated withthe shell of the instrument, which can be applied in the electrochemical system where WE isconnected to the ground such as autoclave electrochemical test. If plug to “GND”, then theWE is connect to the shell of the instrument. The anti-interference ability is high in thiscase.

Interface port – this port is to control the external stirrer, electric machine span rate, or as afrequency meter to test the frequency of the external signals (can externally connectEQCM).

USB port– communication port to connect PC and instrument.

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Signal I/O – expansion port for analog input/output. PI pin can achieve analog waveformoutput, such as sawtooth wave, sine wave；P2&P3 pin is to record the external analog signal,such as the temperature, and pH sensor etc.

1.4 Schematic diagram

The mode of a CS electrochemical workstation is a computerized general-purposepotentiostat/galvanostat.

Fig.1-2. Schematic diagram of CS potentiostat

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Part 2 CorrTest® Software1. Introduction

CorrTest® software shipped with the CS electrochemical workstation is an easy-to-use,flexible, and versatile electrochemical tool and can be applied in many research fields fromcorrosion, voltammetry, electroanalysis to battery test, etc. The main electrochemicaltechniques include: Open circle potential (OCP), potentiostatic/galvanostatic polarization,potentiodynamic/galvanodynamic polarization, Multi-potential/current, potential/currentstair-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), NormalPulse Voltammetry (NPV), Differential Normal Pulse Voltammetry (DNPV), A.C.Voltammetry (ACV), Second Harmonic A.C. Voltammetry (SHACV), Potentiostatic StrippingVolammetry, Linear Sweep Stripping Volammetry, Staircase Stripping Volammetry, SquareStripping Volammetry, Differential Pulse Stripping Volammetry, AC Impedance, Battery Test,Electrochemical Noise, etc.

CorrTest® software is also equipped with powerful corrosion analysis module. Iit cancalculate the corrosion rate of the material by linear polarization and weak polarization, aswell as polarization resistance (Rp), Tafel slope (ba, bc), and corrosion current density (icorr)through the non-linear fitting of Tafel plots. In addition, by the inherent electrochemicalimpedance spectroscopy (EIS) technique, it can measure the double layer capacitance (Cdl)and the solution (concrete) resistance (Rs). Moreover, CorrTest® provides as a dual-channeldata logger for pH, temperature or some physical quantities records.

With these techniques, the CS Potentiostat /Galvanostat can be applied in the followingfields:

(1) electro-synthesis, electro-deposition (electroplating), anodic oxidation, etc.(2) electrochemical analysis and sensor;

(3) Battery (Li-ion battery, solar cell, fuel cell, supercapacitor), new materials,

optoelectronic materials;

(4) Corrosion mechanism of the metal in water, concrete and soil;(5) Fast evaluation of corrosion inhibitor, water stabilizer, coating and cathodic

protection.

1.1 System Requirements

(1) Operating System: Windows XP / Vista /7/ 8/10.(2) Communication between PC and instrument: USB or RS-232 serial port.(3) Output device: any printer or plotter supported by Windows.

1.2 Software Installation

(1) USB Driver Installation. For the first time the workstation connects to the host PC and

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is powered on, Windows® will display a “Found New Hardware” message, and require driverinstallation. Upon this request, insert the CD into the CD-ROM drive, and then select“Automatic” to install the CP2102USBdriverWin×.exe file.

(2) In the CD folder, choose “CSW_x32.exe”, or “CSW_x64.exe” according to thecomputer’s operating system. Double click the setup file and follow the instructions tocomplete installation.

(3) Open the software shortcut on the desktop. When CorrTest is opened for thefirst time, a software interface similar to the following picture will appear:

Fig.2-1. Interface of CorrTest software for CS Electrochemical Workstation

2. MenuThere are keyboard shortcuts for experiment techniques on the right side, such as “F2”

for “Open Circuit Potential”. Either by clicking the “Open Circuit Potential” or pressing “F2”key can the users open the OCP test dialog box.

There is a toolbar under the main menu, and it can achieve the same function as the mainmenu, 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; the “Experiments” menu willappear.

The button will be activated when a test is running. The users can click it to stop thetest. This button will gray out when the test is completed.

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2.1 File

The File menu offers the following commands:

2.1.1 Open

Open an existed data file, and it can be edited and renamed.

2.1.2 Close

Close an open file. If the file has been modified, CorrTest software will prompt you tosave the changes.

2.1.3 Save

Save an open file with the same name.

2.1.4 Save As

Save As saves the current File with a different name.

2.1.5 Print Setup

A dialog box to set the print format.

2.1.6 Print

Print experiment results by using a default template created and selected in Print Setup.

2.1.7 Exit

Close the software.

2.2 Edit

The Edit menu include the following functions:

2.2.1 Cut

Cut allows the user to select the data from a Data Cut window to the clipboard.

2.2.2 Copy

Copy allows the user to select the data from a Data Copy window and paste it intoanother program.

2.2.3 Paste

Paste allows the user to paste the selected data by cutting or copying into anotherprogram.

3.2.4 DeleteDelete permits the permanent deletion of data.

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3. System Setup

3.1 Com Port Setup

The software will automatically search for the Com Port when the instrument isconnected to the PC’s USB port

3.2 Timing Measurement

Timing measurement mode is used for users to run unattended experiments.

3.3 Reset Workstation

Restore the default values of all parameters.

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4. Experiment Setup

4.1 Cell& Electrode Setup

In this diabox, the user can enter information on the working electrode and theelectrolytic cell.

The parameters are mainly used to calculate corrosion rate. Clicking the “OK” button,then all parameters will be saved in a registration file.

The Electrode Area specifies the exposed surface area of the sample or electrode. Itdoesn’t affect the measurement results. It will be proceeded by CorShow afterwards tocalculate current density and corrosion rate.

The Density, Chemical Equivalent Weight, and Stern-Geary Coefficient are saved inthe file to help calculate the corrosion rate. The Chemical Equiv.is the relative atomic massdivided by number of electrons transferred during a reaction. Take the reaction Fe→ Fe2+

for example, Fe has an atomic mass of 55.847 and transfers 2 electrons so the EquivalentWeight is 55.847/2=27.92. Equivalent Weight can also be interpreted as mass loss perelectron transferred. This definition is particularly helpful when it comes to alloys.The Reference electrode Type saves reference electrode information for later use. This

parameter is not used during measurements (CorrTest always displays and saves the actualcell potential). Most common reference types are predefined (SCE, , AgCl, Cu/SO4, Hg/HgO,

etc). If your reference electrode is not in the list, you can enter the “User Defined”. Once thereference electrode type is selected, CorrTest will be able to translate the potential data fromone reference type to another.

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4.2 Pstat/Gstat Setup

The Current Range parameter selects a full-scale current range to be applied during theexperiments. Selecting “Auto” allows the instrument to select the current range based on themeasured current.

The Potential Range parameter selects a maximum cell potential which can be appliedand measured. Generally speaking, “Auto” is the best choice unless the signal changes veryfast. In this case, data points will be lost.

IR Compensation Correction refers to methods requiring compensation for unwantedmedium resistances in an electrochemical system. Without correction, these unwantedresistances may distort data or make it impossible to perform the desired experiments.

The resistance of the electrolyte between the working electrode and the referenceelectrode is the most common cause of errors. Moreover, contact resistance and long electrodeleads can cause errors too.

The Feedback compensation method may be used to boost the cell potential tocompensate potential drops caused by the cell geometry and solution resistivity. Feedbackmay only be used with a fixed (not “Auto”) Current Range.

Polarity Convention defines how positive and negative potentials and currents areinterpreted. When the potential polarity is set to (O2+), a more positive potential produces alarger driving force for an anodic/oxidation reaction and a more negative potential produces acathodic/reduction reaction. When the potential polarity is set to (O2-), a more negativepotential produces a larger driving force for an anodic/oxidation reaction and a more positivepotential produces cathodic/reduction reaction.

If the Current polarity is set to (O2+), positive current is for an anodic/oxidation reactionand negative current is for a cathodic/reduction reaction. When using (O2-), positive current isfor a cathodic/reduction reaction and negative current is for an anodic/oxidation reaction.

The Low Pass Filter can be used to reduce high frequency noise.

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4.3 Waiting before run

When switching from the natural state to the polarization of potentiostat, it takes timebefore starting to scan because the electrode itself is unstable in the beginning. This can beadjusted according to the specific requirements of the system.

5. Stable Polarization

5.1 Open Circuit Potential

Experiment→Stable Polarization→Open Circuit PotentialThis 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 untila particular potential is reached.

OCP (V) will display the actual open circuit potential of the cell (updated per second).

5.1.1 Data FileWhen 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 isparticularly useful if you forget the file names you have already used. However, beforeCorrTest starts performing the first experiment in the Experiment List, you may be warned if

app:ds:adjust

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the file has already existed.CorrTest will automatically append the suffix “.COR” to a data file if you do not enter

one. Therefore, if you specify tutor1, the file tutor1.cor will be used. In the same way, if youspecify tutor1.abc, the file tutor1.abc.cor will be used.

The Comments text is saved in the data file. The time, date, and all measurementparameters are automatically saved in the data file so you don’t need to write theseinformation into the comment area.

5.1.2 ExperimentThe Total Time determines the total length of the experiment.

5.1.3 Experiment TerminationIf the Use box is checked, the experiment will be automatically terminated as long as the

potential goes below the Potential (V) < value or above the Potential (V) > value.

5.1.4 Data AcquisitionThe acquisition rate in Points/Second is specified by the Sampl Freq(Hz) value.

5.1.5 Axis TypeWhen 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.

5.1.6 Pstat/GstatThe Experiments | Setup Pstat/Gstat... menu item is usually used to configure the

Pstat/Gstat for all experiments in the experiment list. These parameters are applicable to allexperiments where the Default Settings are selected. (See Pstat/Gstat Setting)

5.1.7 Cell SetupSee 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.

5.2 Potentiostatic

Experiment→Stable Polarization→PotentiostaticThis 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 isreached. A galvanic corrosion can be performed by setting the applied potential to zero vs.Reference electrode.

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Filename. The Dir button can be used to display a list of all directories and files. This isparticularly useful if you forget the file names you have already used. However, beforeCorrTest begins performing the first experiment in the Experiment List, you may be warned ifthe file has already existed.

CorrTest will automatically append the suffix ‘.COR’ to a data file if you do not enter one.Therefore, if you specify tutor1, the file tutor1.cor will be used. In the same say, if you specifytutor1.abc, the file tutor1.abc.cor will be used.


5.2.2 Experiment ParametersThe 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 addedto the open circuit potential of the cell. For example, 0.1 vs. Open Circuit Potential meansapplying a potential of 0.1 Volts above the measured open circuit potential. ‘vs. Reference’ isused to select an exact potential to be applied.

The Total Time determines the total length of the experiment.

5.2.3 Experiment TerminationIf the Use I box is checked, the experiment will be automatically terminated as long as

the current goes below the Current (A) < value 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 Q (Coulomb) < value or above the Q

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(Coulomb) > value.If the not enabled box is checked, the experiment will not be terminated until the total

time is reached.

5.2.4 Data AcquisitionIf Sampl Freq(Hz) is chosen, the acquisition rate in Points/Second is specified.




Pstat/Gstat for all experiments in the Experiment List. These settings are applicable to allexperiments where the Default Settings are selected.(See Pstat/Gstat Setting)

5.2.7 Cell SettingSee Cell Setting 5.1.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.

5.3 Galvanostatic

Experiment→Stable Polarization→GalvanostaticA constant current is applied and the potential is monitored as a function of time. The

experiment can be performed for a fixed duration or until a particular potential is reached.

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Filename. The Dir button can be used to display a list of all directories and files. This isparticularly useful if you forget the file names you have already used. However, beforeCorrTest begins performing the first experiment in the Experiment List, you will be warned ifthe file has already existed

CorrTest will automatically append the suffix ‘.COR’ to data files if you do not enter one.Therefore if you specify tutor1, the file tutor1.cor will be used. In the same way, if youspecify tutor1.abc the file tutor1.abc.cor will be used.


5.3.2 ExperimentApplied Current 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.

5.3.3 Experiment TerminationWhen the Use E box is 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 is checked, the experiment is not terminated until the total time isreached.





Pstat/Gstat for all experiments in the experiment list. These settings are applicable to allexperiments where the Default Settings are selected.(See Pstat/Gstat Setting)

5.3.7 Cell SettingSee Cell Setting 5.1.

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The OK button exits the setup window, saves all changes you have made, and runs theexperiment.

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.

5.4 Potentiodynamic

Experiment→Stable Polarization→PotentiodynamicA 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 reversedif a particular current is reached. This can be configured to obtain either PolarizationResistance or Tafel data.



Filename. The Dir button can be used to display a list of all directories and files. This isparticularly useful if you forget the file names you have already used. However, beforeCorrTest begins performing the first experiment in the Experiment List, you will be warned ifthe file has already existed.

CorrTest will automatically append the suffix ‘.COR’ to data files if you do not enter one.Therefore if you specify tutor1, the file tutor1.cor will be used. In the same way, if youspecify tutor1.abc the file tutor1.abc.cor will be used.


5.4.2 Scanning ParametersUp to 4 separate potentials can be applied during the experiment. The experiment starts at

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the Initial Potential, sweeps to Vertex #1, to Vertex #2, and then to the Final Potential. Clickon 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 onlyVertex #1 is checked the sweep Initial →Vertex #1→Final is performed. If neither Vertex #1nor Vertex #2 is checked, Initial → Final is performed.

A potential can be specified in several ways. If ‘vs. Open Circuit’ is chosen, the specifiedpotential is added to the open circuit potential of the cell. For example 0.1 V vs Open Circuitmeans 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 determines how fast the potential is scanned between one potential andanother.

5.4.3 Experiment TerminationWhen 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 aremet, the experiment will immediately start sweeping toward the Initial Potential.

The Termination or Reversal will occur when the current is above the Current> or belowCurrent<. Either of these conditions must be met to trigger the Termination or Reversal. Beaware that the Termination/Reversal conditions in the Potentiodynamic experiment are quitedifferent from those in the other types of experiments.

5.4.4 Data AcquisitionIf Sampl Freq (Hz) is chosen, the acquisition rate in Points/Second is specified.





5.4.7 Cell SettingSee Cell Setting 5.1.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.

5.5 Galvanodynamic

Experiment→Stable Polarization→Galvanodynamic

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Corrosion technique that uses a single current scan or ramp programs from an initialcurrent to a final current, plotting the resulting potential vs. time. A typical use of thistechnique is to measure the relative susceptibility to localized corrosion.

This experiment applies a current sweep between up to 4 separate setpoints. The sweepcan be terminated if a particular potential is reached.

OCP will display the actual open circuit potential of the cell (updated per second). If theinstrument is turned off, this value will display ‘Not Available’.

5.5.1 Data FileWhen 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 particularlyuseful if you forget the file names you have already used. However, before CorrTest beginsperforming the first experiment in the Experiment List, you may be warned if the file hasalready existed.

5.5.2 Galvanodynamic ParametersUp to 4 separate currents can be applied during the experiment. The experiment starts at

the Initial Current, sweeps to Vertex i#1, to Vertex i #2, and then to the Final Current. Click onthe Used boxes to turn on or turn off the Vertex i #1 and Vertex i#2 setpoints. If a Vertex’sUsed box is not checked, that segment of the sweep will be skipped. For example, if onlyVertex i#1 is checked the sweep Initial→Vertex i#1→Final is performed. If neither Vertex i#1nor Vertex i #2 is checked, Initial→Final is performed.

5.5.3 Experiment StopWhen the Scan Rev. box is checked, the experiment will immediately start sweeping

toward the Initial Current if certain potential conditions are met.When the Scan Stop box is checked, the sweep will end if certain potential conditions

occur.

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Note: The Current values specify the total current applied, rather than the current density.The Scan Rate determines how fast the current is scanned between one current and

another.







6. Transient Polarization

6.1 Multi-Potential Steps

Experiment→Transient Polarization→Multi-Potential StepsIn the Multi-Potential Steps technique, twelve potential steps can be applied and cycled.

Current is recorded as a function of time.



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6.1.2 Multi-Potential Steps ParametersA 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 willbe skipped.

A potential can be specified in several ways. If ‘vs. Open Circuit’ is chosen, the specifiedpotential is added to the open circuit potential of the cell. ‘vs. Reference’ is used to select anexact potential to be applied.

No. of Cycles specifies how many times the potential is cycled between Initial E andFinal E.

The Time determines how long the potential will be held at each step.







6.2 Multi-Current Steps

Experiment→Transient Polarization→Multi-Current StepsIn the Multi-Current Steps technique, twelve Current steps can be applied and cycled.

Potential is recorded as a function of time.

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OCP will display the actual open circuit potential of the cell (updated per second). If theinstrument is turned off, this value will be ‘Not Available’.


File. The Dir button can be used to display a list of all directories and files. This is particularlyuseful if you forget the file names you have already used. However, before CorrTest beginsperforming the first experiment in the Experiment List, you will be warned if the file hasalready existed.

6.2.2 Multi-Current Steps ParametersA current sweep between up to 12 separate current setpoints is 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 i. If the step time box is filled with zero, this segment of the sweep will beskipped.

No. of Cycles: specifies the cycles of the current sweep from the Initial i to the Final i.The Time determines how long the current will be held at each step.

6.2.3 Data AcquisitionIf Sampl Freq.(Hz) is chosen, the acquisition rate is set as Points/Second.




Pstat/Gstat for all experiments in the experiment list. These settings are applicable to all

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experiments where the Default Settings are selected.(See Pstat/Gstat Setting)


6.3 Potential Stair-Step

Experiment→Transient Polarization→Potential Stair-Step




6.3.2 Step Potential ParametersA 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 changedin discrete steps rather than a smooth sweep.

The experiment starts at the Initial Potential, sweeps to Step E1, and then to Step E2.Click on the “Use” boxes to turn on and turn off Step E2 setpoints. If “Use” box is notchecked, 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 anexact potential to be applied.

mk:@MSITStore:C:\SAI\Programs\CorrWare.chm::/setup_experiment_m_potentiodynamic.htm

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6.4 Galvanic Stair-Step

Experiment→Transient Polarization→Galvanic Stair-Step



File. The Dir button can be used to display a list of all directories and files. This is particularlyuseful if you forget the file names you have already used. However, before CorrTest beginsperforming the first experiment in the Experiment List, you will be warned if the file alreadyexists.

6.4.2 Scan ParametersA current sweep between up to 3 separate current setpoints is applied and the potential

response is measured.

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The experiment starts at the Initial Current, sweeps to Step i#1, and then to Step i#2.Click on the “Use” boxes to turn on or turn off Step i #2 setpoints. If a Vertex’s “Use” box isnot checked, that segment of the sweep Step i #2 will be skipped.

The Time determines how long the current will be held at each step.







7. Voltammetry

7.1 Linear Sweep Voltammetry

Experiment→Voltammetry→Linear Sweep VoltammetryA 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, themaximum scan rate should be 1000V/s. To control the number of points acquired, the dataacquisition should be separated from any particular point, and spread out over the entire scanrange to a maximum of 1000 points per scan.

OCP will display the actual open circuit potential of the cell (updated per second). If the

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instrument is turned off, this value will be ‘Not Available’.



7.1.2 Scan ParametersUp to 2 separate potentials can be applied during the experiment. The experiment starts at

the Initial Potential, and then to the Final Potential.The 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 vsOpen Circuit means applying a potential of 0.1 Volts above the measured open circuitpotential. ‘vs. Reference’ is used to select an exact potential to be applied.

The Scan Rate determines how fast the potential is scanned between one potential andanother.







7.2 Cyclic Voltammetry

Experiment→Voltammetry→Cyclic VoltammetryCyclic Voltammetry is a technique used for the theoretical study of redox couples. Cyclic

Voltammetry is a particular LSV that performs a triangular-shaped scanning at the workingelectrode. In this way, a redox couple in solution is exposed to an oxidation and afterwards toa reduction.

The plot of a cyclic voltammetry consists on a closed curve: reversible redox couplesshow 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

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redox couple and figure out the number of electrons involved in the discharge process:

1/228.25

paE En

Where Epa = anodic peak potential

nEE pc

25.282/1

Epc= cathodic peak potential.

nEEE PCpap

5.56

A two-stage voltage ramp is programmed from an initial potential to a vertex potential,and then from the first vertex potential to the second one at a defined scan rate. The scan canbe repeated for many times (cycles) between the two vertex potentials. To keep the step sizeon an “analog-like” level, the maximum scan rate should be 10,000V/s. To control the numberof points acquired, the data acquisition should be separated from any particular points, andspread out over the entire scan range to a maximum of 1000 points per cycle.

This experiment applies a potential sweep between up to 4 separate potential setpoints. If2 setpoints are used, multiple cycles will be performed.

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File. The Dir button can be used to display a list of all directories and files. This is particularlyuseful in case you forget the file name you have already used. However, before CorrTestbegins performing the first experiment in the Experiment List, you will be warned if the filehas already existed.

7.2.2 Scan ParametersThe 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 FinalPotential. Click on the “Use” boxes to turn on or turn off the Initial and Final setpoints. If theInitial 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 neitherthe 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 specifiedpotential is added to the open circuit potential of the cell. For example, “0.1V vs. OCP”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 andanother.

No. of Cycles specifies how many times potentials are cycled between High E and LowE.

-0.5 0 0.5 1.0 1.5-0.0003

-0.0002

-0.0001

0

0.0001

0.0002

0.0003

E (Volts)

I (Am

ps/c

m2 )

Figure 2-2. CV of Pt electrode in 1M H2SO4

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7.2.4 Axis Type:When the experiment is performed, the data will be displayed as specified by the Axis



Pstat/Gstat for all experiments in the experiment list. These settings are applicable to allexperiments where the Default Settings are selected. (See Pstat/Gstat Setting)


7.3 Staircase Voltammetry

Experiment→Voltammetry→Staircase VoltammetryIn Staircase Voltammetry (SCV), the potential is incremented from Initial E toward Final

E, and it may be scanned back. Current is sampled after every potential increment andrecorded as a function of potential.



File. The Dir button can be used to display a list of all directories and files. This is particularlyuseful in case you forget the file names you have already used. However, before CorrTest

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begins performing the first experiment in the Experiment List, you will be warned if the filealready exists.

7.3.2 Scan ParametersInit E and Final E should be at least 0.01 V apart. ‘vs. Referenc’ is used to select an exact

potential.Incr E is the increment potential of each pulse; it can be chosen from 0.001V to 0.05V.Step Period can be chosen from 0.01s to 50s.No. of Cycles specifies how many times potential are cycled between Initial E and Final

E.







7.4 Square Wave Voltammetry

Experiment→Voltammetry→Square Wave VoltammetryThe 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 currentscan be subtracted from one another to plot the current difference, which is helpful forimproving the sensitivity of analytical measurements. Technique is also referred to as SWV.

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7.4.2 Scan ParametersIn 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, whichincrements after each cycle of the square wave. Current is sampled at the end of the forwardand reverse steps and recorded as a function of the base potential. During the experiment, onlythe difference between the two current samples is displayed.

Init E and Final E should be at least 0.01V apart. ‘vs. Reference’ is used to select an exactpotential to be applied.

Incr E is the increment potential of each pulse; it can be chosen from 0.001V to 0.05V.Amplitude can be chosen from 0.001V to 0.5V.Frequency can be chosen from 1Hz to 100,000Hz.




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7.5 Differential Pulse Voltammetry

Experiment→Voltammetry→Differential Pulse VoltammetryDPV is very useful for analytical determination (for example, metal ion quantification in a

sample). The differential measurements discriminate a faradic current from a capacitive one. In thistechnique, the applied waveform is the sum of a pulse train and a staircase from the initial potentialto a limit potential, or to the final potential if the scan is reversed. The current is sampled just beforethe pulse and near the end of the pulse. The resulting current is the difference between these twocurrents. It has a relatively flat baseline. The current peak height is directly related to theconcentration of the electroactive species in the electrochemical cell.



File. The Dir button can be used to display a list of all directories and files. This is particularlyuseful in case you forget the file names you have already used. However, before CorrTestbegins performing the first experiment in the Experiment List, you will be warned if the file

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has already existed.

7.5.2 Scan ParametersIn 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 thepotential pulse. The difference between these two current samples is recorded as a function ofpotential.

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 anexact potential.

Incr E is the increment potential of each pulse; it can be chosen from 0.001V to 0.05V.Amplitude can be chosen from 0.001V to 0.5V.Pulse Width can be chosen from 0.001s to 10s.Pulse Period can be chosen from 0.01s to 50s.



Type. CorrView can be later used to display the data in any of the other formats.




7.6 Normal Pulse Voltammetry

Experiment→Voltammetry→Normal Pulse VoltammetryIn Normal pulse voltammetry (NPV) pulses of increasing amplitude are applied. The

pulses always start from the initial potential. The current response is usually sampled at theend of the pulse and then plotted versus pulse potential. In such a way a discrete, digitizedcurve is obtained. The initial potential is a very important parameter. It determines theelectrode surface state before the faradaic current starts to flow. The measurement of thecurrent at the end of the pulse allows for a substantial elimination of the charging current andleads to exposition of the faradaic current of interest.

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File. The Dir button can be used to display a list of all directories and files. This is particularlyuseful in case you forget the file names you have already used. However, before CorrTestbegins performing the first experiment in the Experiment List, you will be warned if the filehas already existed.

7.6.2 Scan ParametersIn 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 eachpotential pulse is sampled and recorded as a function of the pulse potential.


Incr E is the increment potential of each pulse; it can be chosen from 0.001V to 0.05V.Pulse Width can be chosen from 0.001s to 10s.Pulse Period can be chosen from 0.01s to 50s.



Type. CorrView can be later used to display the data in any of the other formats.


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7.7 Differential Normal Pulse Voltammetry

Experiment→Voltammetry→Differential Normal Pulse VoltammetryThis is 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 thispulse a modulation step with definable amplitude and duration is applied. The current justbefore and at the end of the modulation step will be measured and the difference will bestored. In this manner, the advantages of normal pulse (short electrolysis time) are combinedwith those of differential pulse (pronounced faraday currents).




7.7.2 Scan ParametersIn Differential Normal Pulse Voltammetry (DNPV), the base potential is held at Init E,

and a sequence of dual potential pulses is applied. The magnitude of the first pulse incrementsafter every iteration, and the second pulse has a constant amplitude relative to the first.

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Current is sampled at the end of both potential pulses, and the difference of these two valuesis recorded as a function of the first pulse potential.


Incr E is the increment potential of each pulse; it can be chosen from 0.001V to 0.05V.Amplitude can be chosen from 0.001V to 0.5V.1st Pulse Width can be chosen from 0.001s to 10s.2nd Pulse Width can be chosen from 0.001s to 10s.Pulse Period can be chosen from 0.05s to 50s.







7.8 A.C. Voltammetry

Experiment→Voltammetry→A.C. VoltammetryIn A.C. Voltammetry, the base potential is incremented from Init E to Final E, 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 theabsolute AC current is displayed. After the experiment, the phase-selective current at anyphase angle will also be available for display.

MANUAL

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7.8.2 Scan ParametersInit 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.






MANUAL

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7.9 2nd Harmonic A.C. Voltammetry

Experiment→Voltammetry→2nd Harmonic A.C. VoltammetryIn Second Harmonic AC Voltammetry, the base potential is incremented from Init E

toward Final E, and a sequential sine waveform is superimposed. Current is sampled when theAC signal is applied, and its second harmonic component is analyzed by using a softwarelock-in amplifier. During the experiment, only the absolute second harmonic AC current isdisplayed. After the experiment, the second harmonic current at any phase angle will also beavailable for display.




7.9.2 Scan ParametersInit 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.

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When the AC frequency is 2 Hz or lower, the Sample Period parameter should be at least2 seconds.

Bias DC Current, check off or on, enables DC current bias during run.







8. Chrono Techniques

8.1 Chronopotentiometry

Experiment→Chrono Techniques→ChronopotentiometryA fast-rising current pulse is enforced on the working-sense electrode of an

electrochemical cell and the potential of this electrode is measured against a referenceelectrode as a function of time. Technique is also referred to as CP.

For a Two-Step Chronopotentiometry experiment, two CP actions are inserted into thesame sequence, each set at the desired current step, and with the cell remaining ON at the endof the first step.

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8.1.2 Scan ParametersCathodic and anodic currents correspond to reduction and oxidation respectively. The

time can be different for switching between cathodic and anodic. However, the Initial Polarityparameter specifies the initial current polarity.

Number of Segments specifies how many times the current is cycled between Cathodicand anodic currents. When the number of current polarity switches (Segments) is reached, theexperiment stops.

8.1.3 Current Polarity SwitchWhen 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 thespecified time has been reached. If the limiting potential is reached, the current polarity willstill be reversed in order to protect the electrode.

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8.2 Chronoamperometry

Experiment→Chrono Techniques→ChronoamperometryA 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 oftime. Technique is also referred to as CA.

For a Two-Step Chronoamperometry experiment, either insert two CA actions into thesame sequence (each set at the desired Potential step and with the cell remaining ON at theend of the first step) or preferably, run a two-step Fast Potential Pulse action if that isavailable.


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8.2.2 Scan ParametersThe 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 specifiedpotential is added to the open circuit potential of the cell. ‘vs. Reference’ is used to select anexact 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.





Pstat/Gstat for all experiments in the experiment list. These settings are applicable to allexperiments where the Default Settings are selected.(See Pstat/Gstat Setting).


8.3 Chronocoulometry

Experiment→Chrono Techniques→ChronocoulometryA fast-rising potential pulse is enforced on the working-sense electrode of an

electrochemical cell. The current flowing 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 toelectrolyze and subtract out solvent background currents, with the sample of interest addedafter the Pre-Elect (s) stage to measure the total charge associated with the sample, minus thebackground current contributions.

MANUAL

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8.3.2 Scan ParametersThe potential may be swept between up to 2 separate setpoints in this experiment. The

experiment starts at the Initial Potential, and then to the Final Potential. A potential can bespecified in several ways. If ‘vs. Open Circuit’ is chosen, the specified potential is added tothe open circuit potential of the cell. ‘vs. Reference’ is used to select an exact potential to beapplied.

Pulse Width specifies how long the potential is sustaining.Number of Steps specifies how many times the potential is cycled between Initial

Potential and Final Potential.






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9. Stripping Voltammetry

9.1 Potentiostatic Stripping

Experiment→Stripping Voltammetry→Potentiostatic StrippingIn 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 isapplied to the electrode and the cations are discharged as metallic atoms into the mercury(amalgam). Successively, the metal atoms are oxidised again during an anodic scanning ofpotential. During the scanning of the potential, the current is measured and plotted, so theresulting voltammogram is a peak shaped graphic.

Figure 2-3.Stripping voltammetry in a solution containing Pb2+, Cd2+, Cu2+

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9.1.2 Deposition ParametersBefore the experiment, the surface of working electrode needs cleaning by this

conditioning step.A constant potential deposition step is 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. Afterdeposition, the experiment can be quiet for some time.

9.1.3 Potentiostatic Stripping ParametersAfter the constant potential deposition step is 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 usedto select an exact potential.


9.1.5 Axis Type:When the experiment is performed, the data will be displayed as specified by the Axis





9.2 Linear Stripping

Experiment→Stripping Voltammetry→Linear Stripping

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9.2.2 Deposition ParametersBefore the experiment, the surface of working electrode needs cleaning by this


electrode surface. This potential can be specified to choose either ‘vs. OCP’ or ‘vs.Reference’.


9.2.3 Linear Stripping ParametersIn Linear Stripping, a constant potential deposition step is 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 scanrate.

A potential can be specified in several ways. If ‘vs. Open Circuit’ is chosen, the specifiedpotential is added to the open circuit potential of the cell. ‘vs. Reference’ is used to select anexact potential.

MANUAL

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9.3 Staircase Stripping

Experiment→Stripping Voltammetry→Staircase Stripping




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9.3.2 Staircase Stripping ParametersBefore the experiment, the surface of working electrode needs cleaning by this


electrode surface. This potential can be specified to choose either ‘vs. Open Circuit’ or ‘vs.Reference’.


In Staircase Stripping, a constant potential deposition step is applied. After that thespecies 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.







9.4 Square-wave stripping

Experiment→Stripping Voltammetry→Square wave StrippingThe waveform can be viewed as a special case of that used for DPV, in which the

pre-electrolysis period and the pulse are of equal duration, and the pulse is opposite from thescan direction. However, the interpretation of results is facilitated by considering thewaveform as something consisting of a staircase scan, each tread of which is superimposed bya symmetrical double pulse, one in the forward direction and the other in the reverse. Overmany cycles, the waveform is a bipolar square wave superimposed on the staircase. This viewgives rise to the name of the method.

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File. The Dir button can be used to display a list of all directories and files. Corrtestautomatically appends the suffix ‘.COR’ to data files. The Comments text is saved in the datafile. The time, date, and all measurement parameters are automatically saved in the data file soyou don’t need to write these information into the comment area.

9.4.2 Deposition ParametersConditioning potential: Before deposition, the conditioning potential is applied on

working electrode in order to remove impurities, and automatically update working electrodesurface state.

Duration: It is a separate time value that specifies the length of time when thatconditioning potential is applied.

Deposition potential: deposition potential is generally lower than the standard redoxpotential 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 thatdeposition potential is applied.

Quiet time: When stopping stirring, potential is not applied on the working electrode.

9.4.3 Square wave stripping ParametersInitial 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.

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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. OpenCircuit ’means applying a potential 0.1 Volts above the open circuit potential. ‘vs. Reference’is used to select an exact potential.







10. Bipotentiostat

10.1 Hydrogen Diffusion Test (HDT)

Experiment→Bi-Potentiostat→Hydrogen diffusion measurementThis part is for CS2350 bipotentiostat.Hydrogen Diffusion Test requires a

special set of electrolytic cell(Devnathan-Stachurski Cell) where twocells (one is for galvanostatic hydrogencharging, the other is for hydrogen currentdetection). In each cell there is anindependent set of reference electrode andcounter electrode, sharing a commonworking electrode. This working electrodeis a thin metal plate which is clippedbetween the two cells. (See the rightpicture).

When hydrogen charging surface of the working electrode is imposed with square wavecathodic current, by alternatively changing the hydrogen charging current, the atoms willdiffuse into the metal, and gradually arrive at the detection surface (i.e. opposite surface) of

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the working electrode. By measuring the amplitude of the waveform of hydroxide current andthe delay time, the user can calculate the hydrogen diffusion rate and the diffusion coefficient.

Connect the double electrolytic cells in the way as shown in figure 2-4, add 0.1mol/L ofNaOH into the anodic cell , then connect the testing cable of anodic cell to the main unit andtesting cable of cathodic cell to the slave unit. Firstly set the anodic polarization potential ofthe potentiostat of main channel to be 0.2V vs. Hg/HgO, then start the polarization, the anodiccurrent will decline sharply at the beginning, then slowly incline to be a constant value,namely anodic residual current. It is generated by hydrogen left inside the steel or someimpurities that can be oxidized in the solution of diffusion surface. When the residual currentis lower than the setting value, the user can add experimental media (such as dilutehydrochloric acid) into the cathodic cell, and then start galvanostatic polarization of the slavechannel. The initial current is at the peak (see figure 2-5), 10mA for instance. At this momenthydrogen ions on surface C of cathodic cell will be reduced to hydrogen atoms, some ofwhich will permeate into and across metallic disk and reach surface A of the anodic cell.Under anodic polarization on the main unit, these hydrogen atoms will be oxidized into ions,forming oxidation currents.

Figure 2-4. Connection diagram for Hydrogen diffusion coefficient test device

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http://cn.bing.com/dict/clientsearch?mkt=zh-CN&setLang=zh&form=BDVEHC&ClientVer=BDDTV3.5.0.4311&q=%E7%A8%80%E7%9B%90%E9%85%B8

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Figure 2-5. Hydrogen charging current curve under control of square wave

Owing to diffusion rate limitation of the hydrogen atoms in metal, current on thehydrogen detection side delays, taking the form that anodic current gradually increases (riseedge) or decreases (fall edge) with time. According to delay time of the hydrogen detectioncurrent and its value, the user can calculate the concentration of hydrogen in the metal and thediffusion rate, and further, evaluate corrosion inhibitors’ inhibiting effect on hydrogendiffusion.



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10.1.2 Hydrogen Atoms Oxidation (main channel)Polarization potential (V) — it is the polarization potential applied to the working

electrode on the hydrogen current detection end in the electrolytic cell. This potential shouldenable the working electrode (thin metal disk) to stay at anodic polarization. That is, apositive value should be entered to allow hydrogen atoms diffused from the opposite side ofthe metal disk to be oxidized into ions.

10.1.3 Hydrogen Ions Reduction (slave channel)Users should set peak and valley of the square wave of hydrogen charging current as well

as their time duration. Hydrogen charging current can only flow towards the cathodicdirection so that hydrogen atoms become ions through reduction and diffuse through theworking electrode (metal disk in the center). Number of cycles of hydrogen charging currentequals to number of square wave.

residual current — With the continuation of potentiostatic polarization, residualhydrogen current in the metal will gradually decrease. When it is lower than this setting value,the software can start hydrogen charging galvanostatic polarization, and hydrogen chargingbegins.

Upon the start of the measurement, the main channel will firstly start potentiostaticpolarization so that the hydrogen atoms in the metal foil can completely diffuse onto theoxidation surface and be oxidized. It takes a long time. According to ISO standard, when theresidual current is lower than 1 ~ 2μA/cm ² (threshold of residual current) , the user canconsider hydrogen atoms in the metal foil being completely oxidized. Once it is lower thanthe threshold, the slave channel will start the process of galvanostatic hydrogen charging.Hydrogen charging current varies between the peak and the valley. In general, 10~20 minuteslater (depends on the material and thickness of the metal), because hydrogen atoms diffuseonto the opposite side of the metal disk and are oxidized to form anodic current, the anodiccurrent detected by the main unit will gradually increase and eventually keep stable.

Polarization time — the user can choose unit as “second”, “minute” or “hour.”




10.1.6 BiStat ConfigFor bipotentiostat the user needs to do setting for the main & slave channel respectively.

Parameters can be both same and different. With buttons of “main channel” and “slavechannel”, the user can set the current range switching, signal gain, low-pass filter turn on orturn off, data smoothing, scan (polarization) delay time and so on. Please note that groundmode must be chosen.

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10.2 Rotating Disk Electrode (RDE)

Experiment→Bi-potentiostat→Rotating disk electrodeThis part is for CS2350 bipotentiostat.Compared with the stationary electrode, rotating disk electrode has the following

advantages: stable concentration polarization; good stability of polarization curves; beingcapable of measuring rapid reactions. So polarization curves of the rotating disk electrodehave wide applications, especially in the aspects of diffusion coefficients calculation, electrongains &losses in reactions, the concentration of reactants, leveling action of electroplatingadditives, and the kinetic parameters of electrode reactions, etc. With the help of ringelectrode, the user can also detect reaction intermediates on the disk electrode.

DW is disk electrode (See figure 2-6), while RW is the ring electrode. They are twoseparate concentric working electrodes. According to the experimental requirements, DW andRW should be controlled at different polarization potential to ensure that electrochemicalproduct on DW can arrive at ring electrode for further redox reaction and be detected.

Disk and ring electrodes are connected to potentiostat with dual channels, the mainchannel potentiostat and the slave channel potentiostat whose function is to control thepotential difference between DW and RW.

Figure 2-6. Rotating disk electrode (left) and its connection with Bi-Potentiostat (right)

The main channel uses the common three-electrode mode: clamp of the counter electrodeconnects to CE; clamp of the reference electrode connects to RE; and clamp of the workingelectrode connects to the output wire of disk electrode. The slave channel uses two-electrode

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potentiostatic mode: the clamp of counter electrode and the reference electrode are bothconnected to the ring electrode, and clamp of the working electrode is connected to the diskelectrode. This mode is to control the potential difference between RW and DW.

Note: Both the main channel and the slave channel work in field mode.In the process of disk electrode polarization, the generated intermediate arrives at the ring

electrode. Due to the potential difference between RW and DW, it will be further oxidized orreduced. Current on ring electrode can be measured and displayed by the slave channel.

Figure 2-7 parameters setting for rotating ring-disk electrode test

For disk-ring electrode test, disk electrode is the main working electrode, while ringelectrode is mainly used to monitor the intermediate product on the disk electrode. Sogenerally potentiodynamic scan is still used for disk electrode, and the potential difference isset to be a constant value, as parameter setting in figure 2-7. .

There are two sets of data recorded. One is the polarization potential (Ed) and current (Id)on the main channel potentiostat (i.e. disk electrode); the other is the polarization potential Er(the set value) and current Ir on the slave channel potentiostat (i.e. ring electrode).



10.2.2 Disk electrode scanning parametersSimilar to potentiodynamic scan, a maximum of 4 independent polarization potentials can

be set on disk electrode.

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10.2.3 Ring electrode polarization parameterPolarization potential —polarization potential of ring electrode vs. the disk electrode,

with unit of V/s.




10.2.6 Pstat/GstatFor bipotentiostat, users need to do settings for the main & slave channel respectively

(refer to contents of 5.2 in this manual). Please note real filed / ground mode must be chosen.


11. EIS (Electrochemical Impedance Spectroscopy)CS350 series use dual signal correlation integral system to improve accuracy. The

frequency range is 10μHz~1MHz. The user can automatically do impedance measurementunder open circuit potential or any DC bias. Built-in DC offset eliminating circuit caneffectively improve measurement accuracy of the AC signal. The amplitude of the excitationsine wave can be set arbitrarily from 0 ~ 2.5V.

AC impedance measurement includes the following three methods:① EIS ~ frequency sweep curve: it measures impedance spectroscopy of the system atdifferent frequencies. It’s the most commonly used method to measure impedance withNyquist and Bode plots.② EIS ~ time scan curve: it measures impedance of the system as a function of time at asingle frequency. It is used to track the dynamic process of some systems such asconductivity.③ EIS ~ potential sweep curve: it measures impedance of the system with the change of DCpolarization potential at a single frequency. It can be used to measure the differentialcapacitance curve and zero charge potential, etc.

11.1 EIS vs Frequency

Experiment→Impedance→EIS vs Frequency

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OCP will display the actual open circuit potential of the electrolytic cell (updated persecond). It is particularly useful for the users to judge whether the working electrode is stablefor impedance test.

11.1.1 Data FileWhen the experiment is conducted, the data will be saved in the file specified by Data


11.1.2 Polarization“DC potential” is the set DC polarization potential of the working electrode during

impedance test. If the test needs to proceed under open circuit potential (OCP), then the usercan enter “0” and select “vs open circuit potential” in the drop-down box. At this moment thepotentiostat will automatically give an output of the sum of OCP and the DC potential to theworking electrode. If you need to do the impedance test under 50mV DC potential of anodicpolarization, you can enter “0.05V” here.

If the test needs to be carried out at a certain potential (such as-0.5V vs. SCE), you canselect “vs. reference electrode” in the drop-down box and enter “-0.5V”. The potentiostat willpolarize the working electrode to be “-0.5V”.

AC amplitude is the amplitude of the excitation signal of electrochemical impedance. Forexample, E = 0.012 sin (wt) V means AC signal amplitude is 12mV. Under high frequency,the actual polarization amplitude of the working electrode may be lower than this value due torate limitation of the amplifier and high-frequency transmission loss of the conducting wires.

11.1.3 Frequency SweepUsers should decide the mode of frequency sweep. Frequency sweep starts from the

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initial frequency to the final frequency, and the mode can be both linear and logarithmic. Ifyou choose linear mode, the frequency measured points will be evenly distributed between theinitial frequency and final frequency. If the frequency range is from “1k to 1Hz”, and you set10 measured points, the measured frequencies will be “1Hz, 99.9Hz, 2×99.9 Hz ...” Generallyspeaking, users don’t use this mode except for special requirements.

If the mode is logarithmic, the sampled frequency data points will be evenly distributed infrequency logarithmic axis (Bode plot). It is particularly useful when frequency range isbetween 2 to 5 orders of magnitude. If the frequency range is from“1k to 10Hz”, and youset 5 measured points for every 10 octaves, the measured frequencies will be 10 × 100Hz, 10× 100.2Hz, 10 × 100.4Hz, 10 × 100.6Hz, 10 × 100.8Hz, 10 × 101.0Hz. This mode is usuallyselected.

11.1.4 Pstat/GstatClick on this button, and open the window for instrument setting. You can choose the

instrument model, set the switching way of current range, signal gain/loss, ground mode, filterbandwidth, digital smoothing, quiet time (scan delay). For regular electrochemical impedancemeasurement system, real ground mode is recommended, and 2.2pF~1μF is OK for filterbandwidth.

11.1.5 Cell SettingIt allows the user to enter related information regarding work electrode and electrolytic

cell, such as surface area of the electrode, material, and temperature etc. These parametersdon’t affect the raw data and will be automatically saved in the data file so that the user canrecognize the measuring conditions in the future. Meanwhile, this information is needed forcorrosion rate computation.

11.1.6 Analyzer Setting

Current range

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The user can choose current range automatically or manually. If select “auto”, you needto set a threshold for high-frequency current range to limit the minimum current range thepotentiostat can use during high frequency measurements. The figure above shows that whenthe measured frequency is higher than 1000Hz, the automatic range will be no less than 2mA.The definition of high frequency is made by the user. The figure above shows that fH>5000Hz is high frequencies, fL <5Hz is low frequency, and 5 ~ 5000Hz is middle range.

The impedance of the working electrode is different at high and low frequency signal. Ifit needs to improve accuracy for measurement results, the setting for current range is varied.The user can select different “current range” according to frequency band. In general, currentrange at low frequency should be lower than that at high frequency. If the user sets currentrange inappropriately, the impedance spectroscopy curve may have large noise. Or if thecurrent range is too frequently changed, there will be obvious turning points in the curve. Insuch cases, the user should re-set. By observing signal amplitude of the waveform displayed,users can judge if the current range setting is appropriate.

Bandwidth SettingBandwidth is set to change the frequency response bandwidth of potentiostat. When the

capacitance value is higher, the bandwidth of the potentiostat will be narrower, and thehigh-frequency performance will weaken, but stability will be improved. Bandwidth is setbased on the critical frequency fc. If measured frequency is higher than fc, you should choosea smaller capacitance (or turn it off), then there will not be false impedance spectra at highfrequency area. But for high impedance system, it may result in shock. You may have toincrease the capacitance. To check if a shock appears, you can observe the amplitude of signaland the wave form.

When the measured frequency is lower than fc, you should select the second-gradecapacitance, and its value should be no less than that of the first grade and the instrument hasa low bandwidth.

When f> 10Hz, bandwidth setting capacitance is 22pF; when f <= 10Hz, it is 100pF.DC Bias CompensationDC bias compensation is used to eliminate DC level which is superimposed on the

potentiostat or the current output signal and increase the AC magnification of potential orcurrent signals, and thus increase impedance measurement accuracy. CS350 instrumentautomatically uses internal bias elimination of potential and current, and therefore impedancemeasurement accuracy is improved. During impedance measurement, you are recommendedto at least choose the “bias compensation” option. If the amplitude of AC excitation signal isless than 100mV, you can choose “AC enhancement” option.

Integration TimeIncreasing the integration time can improve the impedance measurement accuracy, and

reduce the impact of noise on the result. Integration time can be set to be the number of cyclesor time (in second). The integration time represents time cost at each frequency point. Thelonger the integration time is, the higher the measurement accuracy will be, and the more timeit takes.

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Delay time is the waiting time between measurements of two frequency points. Beforethe measurement of the next point, the internal frequency analyzer will wait for a period oftime, allowing electrode to come to the state of balance. The delay time is usually not neededfor electrochemical system.

11.1.7 The impedance spectroscopy fittingCorrTest uses Zview software as a tool to analyze impedance spectroscopy and draw

graphics. Zview is powerful for impedance analysis, and it can make complex plane diagram&Bode plot about data. It allows users to create a variety of equivalent circuits and do datafitting. It has functions of graphic’s local zooming in, curve smoothing, data correction and soon. Zview can output the graphics to a printer or clipboard, and you can also paste a graphicinto a Word document.

Generated impedance data files (. Z) from CorrTest is fully compatible with Zview. Userscan directly click on “Zview Drawing” menu after data acquisition, and import one or moredata files from the “Documents” → “Data File” menu, and then select from a variety ofgraphics methods in the “Options” → “activities graphics” menu.

If you want to change the graphics’ coordinate text, you can right-click the menu, select“Setting” to modify, and select “Text” to write whatever in the graphics. If you want to changethe color, line pattern, or mark, etc., you can set in the pop-up diabox of “File” → “Data File”menu.

Equivalent circuit fittingSelecting “Equivalent Circuit” from the tool bar, users can set up equivalent circuit of

their own or just choose the classic equivalent circuit. In the equivalent circuit window, select“Model” → “Edit equivalent circuit”, then you can start simulating or fitting.

Graph copyRight-click the mouse, from the pop-up diabox, select “copy graphics to the clipboard”,

then in Word, through “Edit” → “Paste”, graphics will be directly pasted into Word document.

11.2 EIS vs Time

Experiment→Impedance→EIS vs TimeIt measures the characteristics of impedance with time at a single frequency. This method

is used to track the dynamic processes of some systems, such as conductivity.

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OCP will display the current open circuit potential of the electrolytic cell (updated persecond). This is particularly useful for the user to judge whether the working electrode isstable for impedance test.



11.2.2 Polarization“DC potential” is the set DC polarization potential of the working electrode during

impedance test. If the test needs to proceed under open circuit potential (OCP), then the usercan enter “0” and select “vs open circuit potential” in the drop-down box. At this moment thepotentiostat will automatically give an output of the sum of OCP and the DC potential to theworking electrode. If you need to do the impedance test under 50mV DC potential of anodicpolarization, you can enter “0.05V” here.

If the test needs to be carried out at a certain potential (such as-0.5V vs. SCE), you canselect “vs. reference electrode” in the drop-down box and enter “-0.5V”. The potentiostat willpolarize the working electrode to be “-0.5V”.

AC amplitude is the amplitude of the excitation signal of electrochemical impedance. Forexample, E = 0.012 sin (wt) V means AC signal amplitude is 12mV. Under high frequency,the actual polarization amplitude of the working electrode may be lower than this value due torate limitation of the amplifier and high-frequency transmission loss of the conducting wires.

11.2.3 Time ScanIn impedance~time scan, frequency of sine wave is constant. It measures the impedance

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of some electrochemical systems at a frequency point as a function of time.Interval - time interval for measurement at each frequency point.Total time - the total time of measurement.


instrument model, set the switching way of current range, signal gain/loss, ground mode, filterbandwidth, digital smoothing, quiet time (scan delay). For regular electrochemical impedancemeasurement system, real ground mode is recommended, and 2.2pF~1μF is OK for filterbandwidth.



11.3 EIS vs Potential

Experiment→Impedance→EIS vs PotentialThe method is used to measure single-frequency impedance at different DC polarization

potential. The potential is stepped from the “initial potential” to “final potential”. It is mainlyused for Mott-Schottky (M-S) curve. M-S curve has been widely used to study thesemiconductor of passivation film on the surface of the metal. It can determine the carrier’stype, concentration and the flat band potential.

When the passivation film is in contact with the solution and the space charge of thesemiconductor passivation film is in the state of depletion (remove majority carriers from thespace charge region and minority carriers don’t exist), for the space charge capacitance (Csc)and the measured voltage (Vm), there is the following linear equation:

Where, Vfb is flat band potential, Nd and Na are donor and accepter carrier concentration,ε is the relative permittivity, ε0 is the permittivity of vacuum, A the electrode surface area, k isBoltaman constant, T is absolute temperature, e is the electric charge.

Passivation film has a double layer structure. Because the composition and the crystalstructure are different for the inner and outer layer of the passivation film, semiconductor typeis also different for the two layers. Two space charge layers are thus formed inside thepassivation film, that is, the solution /passivation film interface space charge layer and the

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inner layer /outer layer interface pn junction capacitance. Because both pn and passivationfilm capacitance are small, in the impedance ~ potential sweep, high-frequency sine wave isgenerally used for measurement.

OCP will display the actual open circuit potential of the electrolytic cell (updated persecond). This is particularly useful for the user to determine whether the working electrode isstable for impedance test.



11.3.2 EIS ParametersFrequency and AC Amplitude specify the frequency and amplitude of sine wave during

the impedance measurement.

11.3.3 Potential ParametersInitial potential - it is set as the initial DC level of the working electrode in impedance ~

potential sweep. You can choose potential applying means, thereby changing the referencepotential of all the polarization potential set points.

Final 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.


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instrument model, set the switching way of current range, signal gain/loss, ground mode, filterbandwidth, digital smoothing, quiet time (scan delay). For regular electrochemical impedancemeasurement system, real ground mode is recommended, and 10pF~100pF is OK for filterbandwidth.



12. Charging/Discharging

12.1 Battery Charging/Discharging

Experiment→Charging/Discharging→Battery Charging/DischargingIt is used to test the charge and discharge characteristics of rechargeable battery and its

lifetime.



12.1.2 ExperimentCharge Current - because of different connecting ways of the electrodes, the charge

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current sign will be different. If the working electrode is connected to battery positive, and thereference & counter electrodes are connected to the battery negative, the displayed opencircuit potential will be positive. Then enter a positive value and it indicates charge.

Constant current-voltage conversion voltage - it’s the critical voltage when chargeprocess is changed from constant current mode to constant voltage mode. According to thecharge rules, constant current charge mode is generally adopted in the early stage of charge.When the battery voltage is higher than the critical voltage, it will turn into constant voltagemode. At this moment the charge current will gradually decrease with time. When it falls tothe trickle current (usually 10 to 20% of the charge current), the software will automaticallydisconnect the charge circuit.

Discharge current - if the working electrode is connected to battery positive end, and thereference & counter electrode are connected to battery negative end, then enter a negativevalue in this input box, it represents the discharge.

Discharge threshold voltage - in discharge process when the voltage drops to thisthreshold voltage, the battery will stop discharge so as not to excessively discharge.

Quiet time - it specifies the interval time from the state of charge to the state of discharge.During this time, the battery is in the open circuit.

Maximum charge and discharge time - after a period of time of battery charge (ordischarge), if the specified critical voltage hasn’t been reached yet, the charge (or discharge)process will stop, and turn to discharge (or charge).

Cycles - a complete cycle includes a charging and a discharging process. This parameterspecifies the total number of cycles performed throughout the experiment. When the numberis achieved, the experiment will be stopped.

“Time unit” drop-down box - it lets you specify the time unit of charging anddischarging. You can select “second”, “minute” and “hour.”

Based on the current value set by the user, the software will automatically select anappropriate current range without users’ setting.


Pstat/Gstat for all experiments in the experiment list. These settings apply to all experimentswhere the Default Settings are selected.(See Pstat/Gstat Setting)


12.2 Galvanostatic Charging/Discharging

Experiment→Charging/Discharging→Galvanostatic Charging/DischargingIt is used to measure cyclic charge-discharge characteristics of the electrode material

(such as secondary battery or supercapacitor electrode material) under a constant current andtest the cycle life of the electrode material. Before starting the test, the “Start” button isinactive. Only when the user specifies a valid file name can the “Start” button be activated.

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All data afterwards will be saved in the created file.



12.2.2 Charge/Discharge CurrentCharge Current - if the battery positive is connected to the working electrode, then enter a

positive number, indicating charge.Discharge Current - if the battery positive is connected to the working electrode, then

enter a negative number, indicating discharge.

12.2.3 Condition for switch of Charging/DischargingIf “based on time” is chosen:Charge and discharge time - it specifies the time duration of the process of charge and

discharge. Process of charge will stop and turn to discharge if the time duration reaches the setcharging time, and vice versa.

If “based on potential” is chosen:If the potential (V) <Ec (vs reference electrode), Ec is set by the user, it means the

material has been fully discharged, the instrument will switch to the charging state. If thepotential during constant current charging process is higher than Ed (vs reference electrode),it indicates that for the material charge process has been completed. Thus it completes ameasurement cycle, and will re-enter the discharge state.

Cycles - a complete cycle includes a charge and a discharge process. It specifies the totalnumber of cycles performed throughout the experiment. When this number is reached, theexperiment will be stopped.

“Time unit” drop-down box - it lets you specify the charge and discharge time unit, youcan select “seconds”, “minute” and “hour.”

For charge-discharge potential, users can select “vs reference electrode” or “vs OCP.”




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13. Misc.Techniques

13.1 Electrochemical Noise

Experiment→Misc.Techniques→Electrochemical NoiseThis method is mainly used to monitor

noise potential and the noise current (zeroresistance current or galvanic current) as afunction of time. Monitoring duration can beset as you wish.

For CS series electrochemicalworkstation, the noise signal (or the galvaniccurrent) measurement is different from othermethods because it does not requirepolarization state. In the noise / galvaniccurrent measurement, the working (galvanic)electrodeⅠ is connected to the green clip ofthe electrode cable, and working (galvanic)ElectrodeⅡ is connected to the black clip of GND cable, and the reference electrode isconnected to the yellow clip. (See the figure.)

Run the CorrTest software, select electrochemical noise measurement, and at this time thesoftware window will appear coupling potential (mixed potential) and galvanic current. If thecurrent value is positive, it means the working /galvanic electrodeⅠis anodic and the working(galvanic)Ⅱ is cathodic. The current is flowing from electrodeⅠto electrodeⅡ. A negativecurrent is the opposite.

During measurement, the potentiostat will automatically switch the range according to thecurrent.


File. The Dir button can be used to display a list of all directories and files. This is particularlyuseful if you forget the file names you have already used. However, before CorrTest begins

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performing the first experiment in the Experiment List, you will be warned if the file alreadyexists.




13.1.4 Pstat/GstatPlease pay especial attention that you should choose “virtual” for the ground mode.

Otherwise ZRA cannot be used to measure galvanic current.


13.2 Data logger

Experiment→Misc.Techniques→Data loggerThe data logger is used to synchronously record external signal. A maximum of six

external signals can be recorded simultaneously. (Two channels have already been used forinternal electrochemical measurement). This method is completely independent from otherelectrochemical tests. That is to say there is no interaction between potentiostat’s work andexternal signal recording. Before the test, the “Start” button is inactive. Only when the userspecifies a valid file name will it be activated. All data afterwards will be saved in the createdfile.



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13.2.2 Data AcquisitionInterval - it specifies the time it takes to acquire 1 sampling point.Frequency - it specifies sampling rate. 1Hz means 1 sampling point is acquired per

second. 10Hz means 10 sampling points is acquired per second.

13.2.3 Sampling DataExternal gain - It shows the value of channels at present. The external Gain is the

amplification of external signals. For example, if the external signal is expected to amplify 5times, then enter “5” here.

All external signals are recorded in the form of potential. The user has to convert thepotential value to magnitude of the original signal. Please note that external gain cannot belower than 0.

13.3 Electrochemical Stripping/Deposition

Experiment→Misc.Techniques→Electrochemical Stripping/DepositionA constant polarization potential is imposed onto the working electrode, and monitor the

polarization current as a function of time. The polarization total time can be specified by theuser, and it can also be specified when the polarization current reaches a certain value, lettingCorrTest automatically terminate the test.



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13.3.2 Deposition ParametersPolarization potential (V) - it is the potential applied to the measured system. For CS

series electrochemical workstation, if the polarization potential is “vs OCP”, the negativevalue indicates cathodic polarization, while positive value indicates anodic polarization. Byclicking on the drop-down box, users can choose the applying way of polarization potential.

Polarization total time - you can specify the length of potentiostatic polarization time;time unit can be “second”, “minute” and “hour”.

13.3.3 Experiment TerminationIf you select “Based on the current” and set the quiet time and current sampling interval,

CorrTest will automatically terminate potentiostatic polarization test once the polarizationcurrent is higher than the specified maximum value (anodic current) or lower than thespecified minimum value (cathodic current).

If you choose “Based on DI / Dt”, CorrTest will automatically terminate potentiostaticpolarization test once the DI / Dt is greater than the set value.

If you choose “Disabled”, the above two conditions to terminate test are both inoperative.







14. Data View

14.1 CV Data View

In the “potentiostat” mode (including all the methods based on constant potential,constant current and galvanic current, etc.), this Data View window displays data in the formof graphic in real time, and has graphical buttons such as “Stop”, “Reverse”, “Pause”.

In the mode of data logger, it displays the external signal channel at work and therecorded data and graphs at present.

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The name of the data files will be displayed in the title bar, and the methods (e.g.potentiostatic polarization, potentiodynamic scan), the parameters (such as scan rate,measurement time, working state, the total amount of data, etc.), as well as the progress andcompletion percentage will all be displayed at the bottom of the window.

CorrTest software will automatically select the best starting and ending point in thecoordinate, and dynamically refresh the graph.

14.1.1 Graph CoordinateBy clicking on the drop-down box of graph options at the right side, you can change the

way to display dynamic graphics. Users can select 7 types of graph coordinates, and they canalso select coordinate unit (mV, V, mA, μA) according to potential and current.

“E vs. time” - the abscissa is time in “second”; the Y- axis is electrode’s potential.“I vs. time” - the abscissa is time in “second”; the Y- axis is current.“E vs. I” - the abscissa is current; the Y- axis is electrode’s potential.“I vs. E”- the abscissa is electrode’s potential; the Y- axis is current.“E vs. Lg I” - the abscissa is the logarithm of current; the Y- axis is electrode’s potential.“E + I vs. time” - there are two graphs. The abscissa is time, and the Y- axis is electrode’s

potential and polarization (galvanic) current.“Q vs. time” - the abscissa is time and the Y- axis is the integral quantity of electricity.This option only works under potentiostat mode. If data logger and potentiostat work

simultaneously, then display varies according to users’ selected menu.

14.1.2 Working ChannelClick on the drop-down box of the working channel at the right side, in the mode of data

logger, the corresponding data of the working channel will be displayed.

app:ds:coordinates

app:ds:quantity

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This option is available only in data logger mode (recording external signals). If the datalogger and potentiostat are both at work, then display varies based on users’ selected menu.

14.1.3 Live DataLive data shows the real-time acquired data. From left to right it’s time (s), potential

(mV), and current (μA).When the user wants to know the value of a point on the graph, they can move the cursor

on the graph area, then immediately there will be a synchronized display of the value on theright side of the cursor. For example if you select “E vs. time”, the text is the time (s) andpotential (mV). When you switch to “E vs. I”, the text is current (μA) and potential (mV).

14.1.4 Zoom inWhen the user needs to observe graphic or data of a local position during the test, he/she

can left-press the mouse button on the upper left side of the target area, and drag it to thelower right side, and then release the button. This local graph will be immediately zoomed inand fill up the entire diabox. The graph will not be updated, but CorrTest test system is stillscanning and acquiring data signals. If the user wants to go back to the original state of autoupdating, just click the mouse on the graph.

14.1.5 Stop and Pause

Click on to terminate the ongoing test. Click on to pause the test.

14.1.6 Reverse Scan

A click on can reverse scanning. It is just applicable for potentiodynamic sweepand cyclic voltammetry test. Clicking on this button, the scan direction will immediatelyreverse, but the scan rate remains the same. If click again, the scan will reverse and turn to bethe original direction again. This button allows users to change the scan direction at any timeto study the cyclic characteristics of the electrochemical reaction.

14.1.7 Polarization /Nature Switch

Click on then you can change the polarization/natural state of electrode.

14.1.8 Print graphClick on the print button then you can immediately output the displayed real-time graph

to the printer.

14.1.9 Lock Graph

A click on allows the user to lock the graph diabox on the top of the desktop. Youcan watch the progress of the test while doing other operations (such as parameter fitting,document editing, etc.). If you want to unlock it, just click on it again.

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14.2 EIS Data View

CorrTest is able to display real-time impedance spectroscopy data. The user can read thedata point in current test by moving the mouse onto the graph area .The real part, imaginarypart, complex modulus, phase angle and frequency are shown at the same time. The measureddata will be automatically saved.

By selecting the box of “lock to the data point”, the user can lock and read the coordinateof the data points in “Nyquist” or “Bode” plot (including the real part, the imaginary part,frequency, impedance modulus and phase angle).

In the title bar of the diabox the data file name will be displayed. At the bottom of thediabox it shows the parameters, such as the polarization amplitude, DC potential, scan range,and current range. CorrTest software will automatically select the best initial and finalcoordinates and make adjustments for the display mode of the coordinates.

14.2.1 DataWhen the user wants to know the value of a point on the graph, he / she can move the

cursor onto the graph area, then immediately there will be a synchronized display of value onthe right side of the cursor.

14.2.2 Zoom InWhen the user needs to observe graphs or data of a local position during the test, he / she

can left-press the mouse button on the upper left side of the specific area, and drag it to thelower right side, and then release the button. This local graph will immediately be zoomed inand fill the entire diabox. The graph will not be updated, but the test system of CorrTest is stillscanning and acquiring data signals. If the user wants to go back to the original state of autoupdating, just right-click the mouse on the graph.

Note: Due to a large amount of data processing in the test, users are recommended to use

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this function after testing.

14.2.3 Stop

Click on to terminate the ongoing test. Click to pause the test.

14.2.4 Real-time Waveform ShowThe waveform acquisition window is to display the acquired potential and current

waveforms in the process of EIS measurement, guiding the user to set appropriate parametersof “minimal high frequency range” and “bandwidth response” in analyzer setting. If thepotential and current waveforms have big noise, the user may need to increase the capacitanceof the bandwidth filter to prevent shock.

For impedance test of high resistance system, if the user doesn’t open bandwidth responsecapacitance from “Impedance test” → “Analyzer” window, it may cause shock during thetest. As shown in figure 2-8, there is no sine wave signal in current and potential waveformsand the amplitude is not the same. It indicates the test system does not correctly follow theapplied sine wave signal, and that a shock occurs.

Figure 2-8. The current and potential waveform in shock

After changing the bandwidth capacitance in the “Analyzer” window to “22pf”, normalsine wave signal can be seen, indicating that the instrument works well and can respond to theapplied sine wave signal. The acquired waveform is shown in Figure 2-9 below. Theamplitude of the potential signal is 10mV, which is the same as applied signal amplitude. Thecurrent amplitude is about 35μA, conforming to the selected current range 200μA. If thecurrent amplitude is too large or too small (signal-noise ratio is too low), the measuredimpedance spectroscopy will have big errors. In this case, the minimum high-frequencycurrent range in the analyzer setting needs to be re-adjusted.

If the noise of current signal is big, it may be caused by high input impedance ofreference circuit (such as high-impedance coating). In this case the user should increase thebandwidth filter capacitance, thus improve the stability of the test system.

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Figure 2-9. The sine wave signal in normal

15. Data Analysis

15.1 Corshow Data Analysis

Please find the Corshow software in the installation CD. After installation is completed,open the software. The Corshow software interface is as below:

Corshow is used to analyze test data. It can display data by multiple coordinates withfunctions of graph locally zooming in, curve smoothing, data correction, etc. It can also dolinear fitting, tafel fitting. However the result by the software may be slightly different fromresult of “parameter fitting”. Graphs can be output to a printer or a clipboard by Corshowsoftware, and can be pasted into Word directly.

Data files (.cor) generated from CorrTest are completely compatible with Corshowsoftware. Users can directly click on “Corshow Drawing” menu after data acquisition, andimport one or more data files from “File”→ “Import Data” menu and then select from various

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graphic coordinates (such as “E vs. time”, “E vs. I”, “E vs. logI”, etc.) from “Standaxis” menu.When the graph is displayed disproportionately, you can right-click the mouse button to getMenu in the graph area, and select “Auto Zoom” to support full graph.

Corshow software is also strong in data computing. It can calculate anodic and cathodicTafel slope as well as the corrosion rate. You can choose “Auto Tafel fitting” or “Auto TafelFitting (between cursors)” or some other methods to calculate the electrochemical parametersand corrosion rate. If fitting curve is well matched with the original data curve, it means theresults have high reliability. Fitting result can be pasted onto the drawing via “Auto Insert”, asshown in Figure 2-10.

Figure 2-10. Polarization curve of A3 steel

app:ds:coordinates

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15.2 Corrosion Rate Calculation

15.2.1 Polarization ResistanceThe data processing module adopts different method for each segment of a polarization

curve. For linear and Tafel areas it uses unitary linear regression calculation.The polarization resistance (Rp) is calculated as the inverse of the slope of the I vs. E data

near the OCP.Ecorr (Volts) is the potential at which the current changed polarity. This usually

corresponds to the OCP of the system.Icorr (A/cm2) is based on the Stern-Geary Equation (Stern and Geary, J. Electrochem. Soc.

104 56, 1957):Icorr (A/cm2) =(ba × bc) / (2.3×(ba+ bc) × Rp)Since the Tafel slopes (ba and bc) cannot be calculated directly in linear polarization area,

CorrTest assumes this value to be 0.12 V/dec. Tafel slopes (ba and bc) can also be calculatedby polarization curve. (Mansfeld, Advances in Corrosion Science and Tech., 6 Ed. Fontanaand Staehle, Plenum Press, p. 163, 1976):

Stern Geary Coef. = (ba× bc) / (2.3× (ba+ bc)) = 0.026Icorr (A/cm2) = 0.026 /RpThe Stern-Geary Coefficient is specified in the Setup | Cell... window.Corrosion rate is calculated from:MPY=Icorr(A/cm2)×EquivWeight(g/equivalent)×393.7(mils/cm))/Density(g/cm3)×365×24

×3600 (seconds/year) / 96500(coulomb/mol))mmPY=Icorr(A/cm2)×EquivWeight(g/equivalent)×10(mm/cm))/Density(g/cm3)×365×24×

3600 (seconds/year) / 96500(coulomb/mol))The Corrosion rate calculation is only possible if density and equivalent weight values

were entered in the Setup | Cell... window.Note: The calculated value depends on the proper selection of data to be used by this

function. In addition, data artifacts or improper experimental technique may cause largediscrepancies in the results. So the user must depend on their own knowledge ofelectrochemistry or corrosion to determine if the value is valid.

15.2.2 Corrosion Rate CalculationDate Analysis→Corrosion CalculationThis dialog box is used for corrosion calculation according to the electrode kinetic

equations. The cell parameters need to fill in well.

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15.2.3 Three calculation methodsLRR Fit — it is used to do linear regression calculation of data in the range of ±15mv of

the cathodic or anodic polarization curve selected by the user, and thus to calculate the linearpolarization resistance Rp value of the system. It is also used to calculate the corrosion rateaccording to the equation Vcorr = B/Rp where Stern B value is set by the user. For linearpolarization, the polarization resistance of the cathodic and the anodic segment may bedifferent, so both of the results of Rp value will be displayed. But the corrosion rate willbe calculated according to the average of the two.

Tafel Fit (3 parameters) — for the weak polarization area, it will calculate the anodic andcathodic Tafel slope (ba, bc), the corrosion current density icorr, and corrosion rate vcorr. Thesecalculations are dependent on the present electrode parameters.

Tafel Fit (4 parameters) — using 4 parameters method, it can calculate Tafel slopes (baand bc), limiting diffusion current density iL, corrosion current density icorr and corrosion ratevcorr by fitting anodic and cathodic weak polarization curves.

16. FAQs

16.1 How to install the CS Potentiostat / Galvanostat?

1. Connecting PC and the potentiostat with the USB.2. Power on the potentiostat, the windows OS will display finding USB device

information, put the installation CD, specify the Windows OS from the CD USB driversdirectory to install the appropriate driver, click to install “CP210xVCP Installer_**.exe”depending on your Windows OS; Don't let Windows OS automatically looking for drivers, asshown below:

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3. After finishing the driver installation, in the device manager "port (COM and LPT)"will appear the project "CP210X USB to UART Bridge Controller (COM X), X=1~6, COM Xis the virtual COM port number of CP210X, as shown below, the X is 3.

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4. In the root directory of CD，run the “CSW_win7_x64.exe”, “CSW_win7_x86.exe” or“CSW_win8_x64.exe” folder depending on your Windows OS. Double click the“CSW_**.exe” file and follow the instructions to complete the installation. Finally create an"Corrtest electrochemical test" shortcut on the desktop.

5. Run the “Electrochemical Test”, Corrtest software will automatically search availableUSB port. Note: for Win7/win8/win10 OS, when run the software for the first time, pleasechoose “Run as the administrator”. To ensure instrument stability, please make sure that theAC power supply is connecting ground.

6. In some cases, you may need to reinstall the driver. Please start with "control panel"→"add/remove programs" remove CP2102 driver installed, then repeat step 2).

16.2 How to check if the workstation is functional?

The instrument should be put in dry, clean andcorrosive-gas-free environment. During use, thepower supply of both the potentiostat and PC mustbe connected to the ground well.

If there is malfunction or something abnormal,please use the dummy cell to check following thesteps as below:

1) Power on the electrochemical workstation2）connect the green clamp to the WE, the yellow clamp to the RE, and the red clamp to

the CE. Based on the principles of the potentiostat, when altering the imposed potential, theRE potential should eternally be the imposed value. The output current should obey the Ohmlaw I= Voltage (imposed on RE) / R(R= resistance between WE and RE)

3）Start the Corrtest software, and do the potentiodynamic test: impose 0～1V scanning,then the V-I curve should be a slant going through the dot (0,0). The slant ratio should be R×(10.1%). If it is the case, it means that potentiostat is OK.4） If the slant ratio or the value of potential/current is completely wrong, please checkwhether the crocodile clamp is broken, or whether there is poor connection betweenterminals on the dummy cell (the user can use the multimeter to measure the resistancebetween two terminals.). If these possible causes are ruled out, then it is deemed to bebroken. The user should contact us (the manufacturer) for repair;

5）If the result is correct using dummy cell, obvious malfunction still appears when measuringthe real system, please check carefully of the following:

① the actual test system/design of the experiment ② environmental interference ③

Reference Electrode ④GND wire

16.3 How to understand 3-electrode system

3-electrode system: the potentiostat measures and controls the voltage difference betweena WE and a RE. Current flow between the WE and CE is measured. CS series Potentiostat

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works with three electrodes immersed in a conductive electrolyte.Working Electrode (WE): a sample of the corroding metal being tested.Reference Electrode (RE): an electrode with a constant electrochemical potential.WE and RE constitute measuring circuit. There is no current flow on RE.Counter Electrode (CE): a current-carrying electrode that completes the cell circuit.WE and CE constitute polarization circuit. Current flows fromWE to CE.2-electrode system: there is no separate RE involved in the experiment in 2-electrode

system. When using the CS potentiostat/galvanostat for 2-electrode system, the CE can beused as RE to provide reference potential. During the measurements, the user simply need toconnect the RE&CE clamp to a same electrode.

16.4 What cause current overload?

1) Current flow in I/E converter is higher than current range

2) When choosing “auto” range, when the measured current is higher than the autorange, the current overload can happen during the process of the electronicalcircuit’s switching to higher range.

3) The Ov/L light blinking frequently shows that there is high-frequency noiseinterference.

4) RE in poor condition, high capacitance system or bad connection of electrodes canall cause current overload.

16.5 What cause potential overload?

1) Max. voltage is higher that 10V between the RE and WE.2) WE is unconnected.3) Low resistance system (fuel cell, battery) in the galvanostat mode.4) Compliance voltage of the potentiostat: imposed max. voltage on the WE and CE

(power amplifier’s max. output voltage) is higher than 21~25V.5) Broken RE or poor connection of RE.6) High-resistance organic system where the IR drop should be overcome.

16.6 How to check the RE?

Take a newly refilled RE (same as the RE to be measured), and soak the microporousceramic at the bottom of the RE into the deionized water. Assume the potential of it is correct,and then put it with the RE to be measured into a cup holding saturated KCl solution, measurethe voltage difference between them by the electrochemical workstation or digital voltmeter.If the difference is bigger than 10mV, the RE to be measured should be refilled or replaced.

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16.7 How to reduce the noise in electrochemical experiment?

1. Make sure the solution in salt bridge is conductive, and that the tip of the RE is drownin the agar and connected well with the WE solution. To make sure the microporous ceramicis well socked, so as to reduce the RE impedance.

2. Open the filter of the system to improve stability.

3. Give a serial capacitor (100nF) between the RE and CE if the noise resulted from thesolution resistance is unavoidable.

4. For corrosion test, add a 1uF capacitor between WE and machine shell of thepotentiostat (or the outer shell of the high frequency socket on the front panel of theinstrument.)

5. For impedance test, make a parallel connection of a Pt wire and RE. Dip one end of thePt wire into solution and connect the other end to RE output port by a 100nF capacitor.

6. All of the equipment in the experiment incl. the PC must be connected to the groundusing a separate ground wire. If there is no suitable ground wire, the user should use a thickcopper wire to connect the PC with a nearby water tap.

7. Shut down all the possible environmental interference source such as high-powerpower supply, computer monitor, stirrer, and fluorescence light etc.

8. Use the Faraday cage, and connect it to the ground.

16.8 Common problem and solution

Phenomenon Cause Solution

No displayafter bootingup.

failure of connecting to the powersupply

Switch on power

the 1A fuse in the socket of the rearpanel is broken

reinstall or replace the fuse

no currentoutput

open circuit or bad contact of theelectrode cable

Check the electrode leads

Dry joint inside the WE or CE Check resistance between theelectrode lead and the workingface by a multimeter

communicationfailuresappears afterusing the USBinterface

1) poor repair stitching of the USBcablepower supply shortage for USB port

no connection to the ground forpower supply cable

replace the USB cable for abetter quality one.re-plug the USB cableConnect the PC casing to theground

Software run-time error‘339’

lack of some control for theWindows system

contact our technical support toask for VBessential controlresister package

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17. Contact usWuhan Corrtest Instruments Corp., Ltd.Address: Room 501, Dingye Hall B, International Enterprise Center, Optics valley Ave.,

East lake high-tech Development Zone, Wuhan, 430074, China.http://www.corrtest.com.cn/enTechnical Service e-mail: [email protected]: +86-27-67849450，+86-27-67849890，+86-13971066778Fax: +86-27-67849890-39

http://corrtest.nease.net

mailto:[email protected]

Wuhan Corrtest Instrument Corp., Ltd.Room 501, Dingye Hall B, International Enterprise Center, Optics

valley Ave., East lake high-tech Development Zone, Wuhan, China.http://www.corrtest.com.cn/en

http://www.corrtest.com.cn

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