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(I) Start-up Procedure
Please allow 30 minutes for the potentiostat to warm up after turning on. Once warmed up, start the Ossila
Cyclic Voltammetry software. Ensure that the potentiostat is detected by the software. If it is, the “Connected
Systems” drop-down box will be populated, and the “Measure” button will be green. If there is nothing
in the “Connected Systems” drop-down box and the “Measure” button is greyed out, please refer to the
troubleshooting guide in Section 10.
9.4.2 Taking a Measurement
(III) Prepare the Electrolyte Solution
We use a 0.1 M solution of tetrabutylammonium hexafluorophosphate (TBAPF6) 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 0.775 g of dry tetrabutylammonium hexafluorophosphate (387.4 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.
(V) Degas the Solution
Gently bubble inert gas through the solution using a thin tube or needle for approximately 10 minutes to
remove dissolved oxygen.
(VI) Connect the Potentiostat and Cell
Use the cable to connect the Potentiostat and electrodes. The connector colour corresponds to which
electrode it connects to:
•
Red -> Working electrode
•
Black -> Counter electrode
•
Blue -> Reference electrode
Содержание T2006A
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