Tecnológico de Monterrey, Campus Monterrey
NT2004B. Aplicación de nanodispositivos en soluciones integrales
February-June 2024
Experiment. Construction of a carbon paste working electrode and its
characterization by cyclic voltammetry
1. Objective
To fabricate a functional carbon paste electrode (CPE) that can be used as substrate for deposition
of nanoparticles.
To characterize the CPE using cyclic voltammetry
2. Introduction
The study of electrocatalytic reactions is of great importance for energy applications (fuel cells,
batteries) environmental remediation (electrochemical capture of CO2, electrochemical oxidation
of drugs in water bodies), and clinical applications (sensors).
To determination of electrocatalytic activity of materials can be achieved via a plethora of
electrochemical techniques e.g. cyclic voltammetry, chronoamperometry, electrochemical
impedance spectroscopy, and others. Regardless of the chosen technique, the first step of the
study must be the incorporation of the catalyst to a working electrode. The selection of the
working electrode, that acts as a substrate for the catalyst, is crucial. The substrate must be an
electric conductor, with negligible catalytic activity, chemically stable in the reaction medium, and
the regeneration of the surface must be simple.
Carbon paste electrodes are a popular choice for working electrodes, carbon is an electronic
conductor with low catalytic activity for many electrochemical reactions. The electrode can be
easily regenerated by removing the tip and refilling it with more carbon paste.
3. Materials and reagents
3.1 Materials
▪ Potentiostat/galvanostat
▪ Laptop (personal)
▪ Multimeter
▪ Copper wire
▪ Glass tubbing
▪ Crucible
▪ Microspatula
▪ 50 ml Volumetric flask (2)
▪ 50 ml beakers (2)
▪ Reference electrode
▪ Graphite counter electrode
▪ Electrochemical cell cap
▪ Heating plate
▪ Air gun
▪ Silicone gun
3.2 Reagents
▪ Graphite
▪ Paraffin
▪ Potassium ferrocyanide
▪ Potassium ferricyanide
▪ Sodium nitrate
4. Methodology
4.1 CPE construction
Make a mixture of 70 % graphite, 30 % paraffin and place it the crucible. Use the beating plate to
melt the mixture. Polish the copper wire with sandpaper and for a coil on one of its ends.
Impregnate the coil with the carbon paste and insert it inside the glass tube, fix the wire to the
tube using the silicone gun. Use the microspatula to fill the tube with the carbon paste, be sure to
press the paste, this will help to guarantee electrical conduction. Once the past is cool polish the
electrode by drawing 8s in a paper sheet. To verify that the construction was successful, measure
the resistance from the copper wire to the tip of the carbon paste, you need the value to be
bellow 100 ohms.
4.2 Electrochemical measurements
Prepare a 1 M KNO3 solution and a 1 M KNO3+5 mM K4Fe(CN)6+5 mM K3Fe(CN)6. Assemble
your cell using the CPE as working electrode, graphite as counter electrode, and the Ag|AgCl as
reference electrode. Connect the electrodes to the potentiostat and measure the open circuit
potential (OCP) for 5 minutes.
Perform a cyclic voltammetry at 50 mV s-1 form -500 mV vs. OCP to +500 mV vs. OCP, adjust the
current range as needed. Once the parameters have been optimized perform 10 cycles at the
same scan rate. Repeat the measurement with at least four more scan rates.
5. Results
Compare the OCP measurements with the expected values from Nernst equation
Make a plot with the most stables voltammograms recorded at the different scan rates.
Verify that the Randles-Sevcik equation applies to your experimental results
Estimate the diffusion coefficient of ferricyanide.
