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Frans_M_Everaerts_Isotachophoresis_378342.pdf

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COATING OF THE MICRO-SENSING ELECTRODES<br />

6.7. COATING OF THE MICRO-SENSING ELECTRODES<br />

6.7.1. Introduction<br />

The second means of preventing electrode processes is to apply a polymer coating to<br />

the micro-sensing electrodes. The main problem is to find a method of coating that gives<br />

a uniform layer. Two different methods were tested: (1) the electrophoretic coating<br />

process and (2) the electrolytic coating process. In the electrophoretic process for<br />

preparing coatings of polystyrene, acrylic and epoxy resins, both water and methanol<br />

were used as solvents. The platinum metal is probably not suitable for these coatings, and<br />

it is known that the metal plays a very important role in the coating process. In the<br />

electrolytic process, the electrode metal is less important, and therefore only electrolytic<br />

coatings are considered below.<br />

6.7.2. Experimental<br />

The anodic polymerization of aromatic amines was particularly successful. The more<br />

aromatic rings present in the compound, provided that a sufficient amount could be<br />

dissolved, the more stable the coatings were found to be. 1-Aminonaphthalene dissolved<br />

in ethanol (saturated solution at room temperature) was employed in several experiments.<br />

A few drops of this solution were added to 10 ml of 1 M potassium chloride solution and<br />

water was then added to give a total volume of 100 ml. The solution was filtered in order<br />

to remove undissolved 1-aminonaphthalene. The filtrate was approximately 0.01 Min<br />

the aromatic amine. During anodic oxidation at 700 mV, a violet-coloured layer was<br />

formed. The electric current was maintained at 0.1 mA for 5 min and an increase in the<br />

electrode potential up to 2000 mV was obtained; the cell constant increased from 0.68<br />

to 2.5 cm-' . The layer formed was cathodically very stable; even after drying and heating<br />

(lOO°C), the quality of the electrode improved. While the results with the coating of<br />

1-aminonaphthalene were satisfactory, the results with 1-aminoanthracene were even<br />

better. The colour of the coating layer was yellow, and the cell constant increased from<br />

0.68 to 3.5 cm-'.<br />

For these electrodes, current-voltage curves were obtained in order to characterize<br />

this quality. However, as it is difficult to estimate the thickness of the layers, experiments<br />

in the isotachophoretic equipment were still carried out. A conductivity measuring probe<br />

was used in which the micro-sensing electrodes were mounted axially as shown in Fig.6.12.<br />

In order to discriminate between electrodes, only a selection of thin and thick coatings<br />

was examined, depending mainly on the electric current applied during the coating<br />

procedure. The isotachopherograms obtained with the a.c. method of conductivity deter-<br />

mination were unusual for the separation of both anions and cations. In order to<br />

demonstrate the difference between the a.c. and d.c. methods, the influence of different<br />

coatings and the influence of changing the frequency of the measuring current and the<br />

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