Potentiostat
User Manual
Ossila.com
19
Ossila Limited © 2020
9.3
Performing Cyclic Voltammetry of Ferrocene
9.3.1
Preparing an Electrochemical Cell
Here we will give an example on how to prepare a simple electrochemical cell to take a
measurement of ferrocene (Fc), which is the standard reference used for cyclic voltammetry.
(I)
Before Starting
We recommend switching on the potentiostat 30 minutes prior to use. This allows it to warm up
and reach a stable temperature, ensuring a stable measurement.
Furthermore, ensure that all apparatus, solvents and electrolytes are dry. This is because the
presence of water and its redox by-products may reduce the solvent potential window or react
with the solvent or analyte.
(II)
Clean and Dry the Electrochemical Cell and Electrodes
The cell and electrodes should always be thoroughly rinsed immediately after each experiment
with the solvent that was used in your electrolyte. Always set the cell to dry, preferably in an oven,
before you prepare your electrolyte. This helps reduce contamination of your solution from water.
(III)
Prepare the Electrolyte Solution
We use a 0.1 M solution of tetraethylammonium hexafluorophosphate (TEAPF
6
) in acetonitrile as
our background electrolyte, but other electrolyte salts and solvents can be used. The solvent and
electrolyte choice are determined by the solvent potential window and the solubility of your
analyte. Most electrolytes are hygroscopic, so should be stored in a desiccator or inert
atmosphere.
Weigh out into a dry volumetric flask 0.550 g of dry tetraethylammonium hexafluorophosphate
(275.2 g/mol) necessary to make up 20 ml of 0.1 M solution. Add acetonitrile up to mark of the
volumetric flask and stir until the electrolyte has dissolved.
Secure the electrochemical cell with a clamp to ensure it is stable before adding the 20 ml of
electrolyte solution. Once dissolved, add approximately 10 mg of Fc to the solution and stir to
dissolve it.
(IV)
Set up the Electrodes
Place the cap on the electrochemical cell, then insert the working and counter electrodes into two
of the holes. We will now prepare the reference solution; a 0.01 M solution of silver nitrite in
acetonitrile. Prepare the solution in a volumetric flask and add it into the reference electrode tube
with the help of a syringe and needle until the tube is approximately 2/3 full. Insert this electrode
into the final hole in the cap.
