Here I provided a short-guide of experimental acquisition data. I summarized the main things you need to take into account but gcarrascohuertas is not responsible for the bad use of this guide and its consequences over materials and people involved. Please, be careful and document all steps you perform.
First you need following materials in order to perform experiments:
-
Three-electrode cell
- Platinum mesh as counter electrode (CE)). Here I used a Planium mesh from Goodfellow
- Ag/AgCl as reference electrode (RE). Here I used a Ag/AgCl/KCl (3 M)
- Your working electrode (WE). Here I used a a polished Glassy carbon electrode (GC, 3 mm diameter, BASI).
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Electrolyte
- K4[Fe(CN)6] 0.004 M (0.000004 mol/cm3) dissolved in 0.1 M KCl (D = 7.6E−6 cm2/s)
Electrochemical techniques performed is cyclic voltammograms with a staircase profile (CV). Parameters:
- Start potential : 0.69 V.
- Upper vertex potential: 0.7 V.
- Lower vertex potential: -0.1 V.
- Stop potential: 0.69 V.
- Number of scans: 4.
- Step: 0.002 V.
- Scan rates: 5 mV/seg , 10 mV/seg , 20 mV/seg , 40 mV/seg , 60 mV/seg ,80 mV/seg , 100 mV/seg , 125 mV/seg , 150 mV/seg , 200 mV/seg.
Before you obtain results from data read this website for undestand Randles–Ševčík analysis:
https://en.wikipedia.org/wiki/Randles%E2%80%93Sevcik_equation
Once you understand this analysis. Following parameters were applied as Randles–Ševčík equation parameters:
- Faraday constant: 96485.33289 mol-1
- Diffusion coeficient for K4[Fe(CN)6] 0.0000073 cm2/s
- Concentration of K4[Fe(CN)6] 0.000004 mol/cm3
- Gas constant 8.3144598 J mol-1 K-1
- Temperature 298 K
Once you finish setting-up all the electrochemical cell components. Create experimental sequence with the parameteres displayed in the screenshots attached in this project.
WARNING: Due to NOVA (Metrohm) software is licensed I can not upload sequence (.nox file). If you want NOVA (Metrohm) software sequence for ECSA measurements (.nox files) do no hesitate to contact me at : [email protected]