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Preparation of Polypyrrole QRE

Preparation of Polypyrrole QRE. Ref: Jalal Ghilane, Philippe Hapiot, and Allen J. Bard, Anal. Chem. 2006, 78, 6868-6872. Experimental Conditions used in Liverpool. Solution: 10 -2 M Pyrrole 0.1 M TetraButyl Ammonium Perchlorate (!!!) Acetonitrile as solvent.

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Preparation of Polypyrrole QRE

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  1. Preparation of Polypyrrole QRE Ref: Jalal Ghilane, Philippe Hapiot, and Allen J. Bard, Anal. Chem. 2006, 78, 6868-6872 Experimental Conditions used in Liverpool Solution: 10-2 M Pyrrole 0.1 M TetraButyl Ammonium Perchlorate (!!!) Acetonitrile as solvent Electrodes: WE Pt wire 0.25 mm diameter CE Pt grid RE Saturated Calomel Electrode Sweeping between -0.6 and +1.1 V, at 100 mV.s-1, for 50 cycles

  2. Results The Figure represents the first, 10th, 20th and 50th scans. One should see the current regularly increasing during the first scans.

  3. Results The growing of the polymer layer is clearly seen on the Figure. Of special interest is the increase of the "peaks" around +0.3 V. These peaks correspond to the oxidation (reduction) of the polypyrrole. As for the rise of current around the positive limit, it reflects the electropolymerisation process.

  4. Remarks 1- For safety purposes, it is advised to change the supporting electrolyte from TetraButyl Ammonium Perchlorate - (CH3)4NClO4 - to TetraButyl Ammonium HexaFluoroPhoshate -(CH3)4NPF6- 2- The actual potential of the quasi-reference electrode depends on two factors: - the potential at which it is removed from the preparation solution. We suggest, at the end of the 50 scans, to apply a potential of +0.4 V for ~ 10s, and to remove the electrode from the solution while applying the potential - the nature of the anion present in the subsequent experiment. We suggest, prior to any use of the QRE, to immerse it in a solution similar to that to be used in the STM experiments. Allow enough time to reach the equilibrium; it can be useful to replace the solution from time to time. It is advised to check the actual potential (vs a known Ref) just before the use of the QRE. 3- It is possible that the positive limit, +1.1 V, should be slightly changed (±50 mV). Looking at the evolution of the CV gives an idea on the effectiveness of the process.

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