The cell is now fully connected and ready for experimentation. Turn on the potentiostat and ensure it’s connected to the computer.
To start the experiment open Framework. Go to the ‘Experiment’ tab > DC105-DC Corrosion > Polarization Resistance. A new window will open, seen in figure 5.
Figure 5: Entry screen for the experimental parameters used during the LPR experiment
The parameters you will use are highly dependent on the experimental setup, and are influenced by factors such as material type, type of electrolyte, and electrolyte concentration. A brief explanation of these parameters:
Initial E: The Initial E parameter defines the starting point for the potential sweep during data acquisition. The allowed range is ± 10 V with a resolution of 1/8th mV. Its accuracy depends on the setting. For LPR it is usually less than 20 mV negative ‘vs Eoc’ meaning referenced against the material’s Open Circuit Voltage.
Final E: The Final E parameter defines the ending point for the potential sweep during data acquisition. The allowed range is ± 10 V with a resolution of 1/8th mV. The Scan Range, defined as the absolute value of Final E minus Initial E, must be less than 8 V. Similar to the Initial E, it is usually less than 20 mV positive ‘vs Eoc’.
Scan Rate: The Scan Rate parameter defines the speed of the potential sweep during data acquisition. The Scan Rate is entered in units of mV/s. Typical scan rates are 0.1666 mV/s and 1 mV/s, as specified in select ASTM standards. A practical upper bound on the Scan Rate is 100 mV/s. Higher Scan Rates may run, but will yield unreliable data because the potentiostat's filtering is 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 volts, the slowest Scan Rate is 52.1 nV/s or 0.1875 mV/hr. Multiply these limits by four for scans longer than 2 V.
Sample Period: The Sample Period parameter determines the spacing between data points. It also helps determine the Step Size of the staircase ramp and the Number of Points in the data curve. The units used for the Sample Period are seconds (s). The shortest Sample Period we recommend is 0.2 s for DC corrosion experiments. The longest Sample Period allowed is 600 s.
Beta Anodic/Beta Cathodic: These are the Tafel constants, and are dependent on numerous factors such as electrode material, solution composition, and solution concentration. Values between 0.1 V/decade to 0.12 V/decade should be acceptable for most experiments. The exact values for these constants in a system can be determined through the DC105 technique known as ‘Tafel’ or non-destructively using electrochemical frequency modulation (EFM).
For this guide we will use the default parameters seen in figure 5. Press ‘OK’ on the setup box to begin the experiment. It will first measures the open circuit potential and then begin a linear voltage sweep that can be seen in figure 6. Measured current is seen on the x-axis, and applied potential is seen on the y-axis.
Figure 6: Active window during the polarization resistance experiment. The potentiostat is applying a linear voltage sweep to the working electrode and measuring the current response
When the experiment is done running, ‘Experiment done, press “F2-Skip” to continue” will appear in the bottom left status bar. Press this button, which can be seen in figure 6.
This section of the guide is designed to show how to get corrosion rate information, the most common reason to run polarization resistance. There is a full guide for Echem Analyst for a complete explanation of the tools and features available.
Once the experiment is done running go to the ‘Analysis’ menu in Framework and select the name of the file that was just run. In this case it will be named ‘polres.dta’. Selecting this will open the Echem Analyst program.
It is common to view polarization resistance data with current density on the x-axis. To change the axis from current to current density select the ‘Polarization Resistance’ menu in the upper left and click ‘Options’. In the Options window that appears select ‘Current Density’ under the ‘Units for Current’ section.
To get corrosion rate data take the following steps, which correspond to figure 7:
- Click the ‘Select Portion of the Curve using the mouse’ tool.
- Click twice on the data curve to define the starting and ending points of the selected region. Analysis will be performed on the selected region, and the zero current value should be roughly in the center of the region. This must be done so that the corrosion rate can be determined when the material is under no external load. The theory behind this can be found here.
- Select the ‘Polarization Resistance’ menu option, then click ‘Polarization Resistance’. A window will appear to confirm the Tafel constants. Click ‘Calculate’
- The corrosion rate, in mils per year, will be shown in the Quick View dock at the bottom left of the screen. The units of corrosion rate can be adjusted in the Polarization Resistance Options described earlier.