Electrochemical Reactivation - Setup Parameters

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Electrochemical Reactivation - Setup Parameters

Description

 

5 - Electrochemical Reactivation

 

Parameter

Description

Units

Pstat

Select the potentiostat/galvanostat to perform the experiment. Each radio button corresponds to an installed potentiostat. You can select only one potentiostat at a time. Potentiostats that are already in use are marked with an asterisk. They can be selected but cannot be used.

 

Test Identifier

A string that is used as a name. It is written to the data file, so it can be used to identify the data in database or data manipulation programs. The Identifier string defaults to a name derived from the technique's name. While this makes an acceptable curve label, it does not generate a unique descriptive label for a data set. The Identifier string is limited to 80 characters. It can include almost any normally printable character. Numbers, upper- and lower-case letters, and the most common punctuation characters including spaces are valid.

 

Output File

The name of the file in which the output data are written. By default, it is saved in the default file directory.

 

The input can be a simple file name with no path information. In this case the output file is located in the default file directory. The default file directory is specified in the Gamry.INI file under the [Framework] section with a Key named DataDir. The default path can be changed using the Path command in the Options menu. It can also include path information, such as C:\MY GAMRY DATA\YOURDATA.DTA. In this example, the data are written to the YOURDATA.DTA file in the MY GAMRY DATA directory on drive C. The default value of the Output File parameter is an abbreviation of the technique name with a *.DTA filename extension. We recommend that you use a *.DTA file name extension for your data file names. The data analysis package assumes that all data files have *.DTA extensions.

 

If the script is unable to open the file, an error message box, Unable to Open File, is generated. Common causes for this type of problem include:

•Invalid file name.

•The file is already open under a different Windows® application.

•The disk is full.

 

After you click the OK button in the error box, the script returns to the Setup where you can re-enter the file name.

 

Notes...

Enter several lines of text that describe the experiment. A typical use of Notes is to record the experimental conditions for a data set.

 

Notes defaults to an empty string and is limited to 400 characters. It can include all printable characters including numbers, upper- and lower-case letters, and the most common punctuation including spaces. Tab characters are not allowed in the Notes string. Press the Notes button on the right-hand side to open a separate Notes dialog box.

 

Sample Area

The surface area of the sample that is exposed to the solution. The software uses the sample area to calculate the current density and corrosion rate (if applicable). If you do not want to enter an area, we recommend that you leave it at the default value of 1.00 cm².

 

Gamry tip bulb

Do not enter a value of zero!

cm2

Density

The density of the metal sample, used in calculating the corrosion rate. You may disregard this parameter if absolute corrosion rates are not required for analysis.

g/cm3

Equiv. Wt

Theoretical mass of metal lost from the sample after one Faraday of anodic charge is passed. One Faraday of charge is equivalent to an Avogadro's number of electrons. The Equivalent Weight can be used to calculate the corrosion rate. You may disregard this parameter if absolute corrosion rates are not required.

 

To calculate the equivalent weight for an alloy, you need to know:

•The composition of the metal sample, expressed in mole fractions.

•The atomic weight AW of each alloy constituent.

•The number of electrons n, lost by each component of the sample as it oxidizes.

 

Suppose we have a 40:60 mole-percent Cu:Ni alloy dissolving in an acidic Cl–-solution. Ni forms Ni2+ as it dissolves and Cu forms a Cu+ complex. The equivalent weight is

 

 

 

The above discussion assumes that the sample oxidizes without changing the composition. This is not always the case. The de-zincification of brass is a well-known problem, where under special conditions brass becomes enriched in Cu as it corrodes. If selective dissolution occurs in your system, the best way to find the equivalent weight may be to measure the concentration of your corrosion products in the solution.

g/equivalent

Initial Delay

Use the Initial Delay parameter to tell the system your definition of a stable potential and when to begin the actual measurement. If the absolute value of the Eoc drift-rate falls below the Stability parameter, the Initial Delay phase ends immediately and the experiment begins, disregarding the Time parameter. The drift rate can never fall below zero, so entering a Stability value of zero ensures that the Initial Delay will not end prematurely. A typical value is 0.05 mV/s. The lower limit of the Stability parameter is set by your patience. For example, a stability of 0.01 mV/s indicates a drift of less than 1 mV within 100 seconds.

 

Activation Time

The duration for which the sample remains activated. The resolution is determined by the Sample Period.

seconds (s)

Activation E

The potential during electrode activation. The allowed range is ±10 V with a resolution of 0.125 mV. The accuracy depends on the setting.

volts (V)

Passivation Time

The duration for which the sample is passivated. The resolution is determined by the Sample Period.

seconds (s)

Passivation E

The potential during electrode passivation. The allowed range is ±10 V with a resolution of 0.125 mV. Its accuracy depends on the setting.

volts (V)

Scan Rate

The speed of the potential sweep during data acquisition. The sweep is actually a staircase waveform, not a linear ramp.

 

Changing the Scan Rate invalidates Passivation Time analysis when using the "standard" techniques.

 

A practical bound on the Scan Rate is 5 mV/s. Higher Scan Rates may run but will yield unreliable data because the potentiostat's compensation and filtering are set for long time constants. A lower bound on the Scan Rate is given by the minimum Step Size divided by the longest Sample Period. For scans shorter than 2 V, the slowest Scan Rate is 52.1 nV/s or 0.1875 mV/hour. Multiply these limits by four for scans longer than 2 V.

mV/s

Sample Period

The spacing between data points. The shortest Sample Period we recommend is 0.25 s (25 ms). The longest Sample Period allowed is 715 s for Reference potentiostats and 750 s for Interface potentiostats.

 

Use Sample Period to determine the Step Size of the staircase ramp and the Number of Points in the data curve. Sample Period specifies the length of a step. The height of a step depends on both the Scan Rate and the Sample Period. You can calculate the Step Size nd the Number of Points in the scan from:

 

 

 

The Step Size is rounded to the resolution of the D/A converter making the steps. The resolution of the D/A converter is dependent on the type of potentiostat you are using. Consult your potentiostat manual for more information. The default Step Size for a Reactivation scan is 1 mV/step. If the Step Size has to be rounded to fit the resolution of the D/A converter, the Sample Period is also adjusted so that the Scan Rate is correct. The Number of Points must be less than 262 143 (218 - 1). If you have more points, the experiment aborts just before the scan phase of the sequence.

seconds (s)

IR Comp

Choose to turn iR-compensation either On or Off. Turning on IR Comp causes the applied potential to be adjusted for the estimated iR-drop.

 

Gamry potentiostats are able to estimate uncompensated voltage-drop caused by cell resistance. They do so by performing a current-interrupt experiment after every data point.