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Frans_M_Everaerts_Isotachophoresis_378342.pdf

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CONDUCTIVITY DETECTION 145<br />

contact the 0.4-mm hole opposite to it, because Cyanolite is applied again in a subsequent<br />

step and if it penetrates into the 0.4-mm hole, this hole will be rough.<br />

With alancet under a microscope, excess of the Pt- 10-30% Ir foil is cut away such that<br />

the profile shown in Fig.6.16b remains. A new piece of insulating material is now glued<br />

to the first one with Cyanolite, applying a high pressure for at least 5 min. The pieces<br />

are glued well if the entire piece is completely clear again, which can easily be checked<br />

by immersing the acrylic in kerosene; if TPX is used, immersion in glycerol is necessary<br />

because TPX dissolves in kerosene.<br />

If the two pieces are glued satisfactonly (Fig.6.16c), they are placed in alathe and,<br />

after turning the piece, the 0.4-mm hole can now be drilled through the entire piece. On<br />

both sides, collars are made for mounting the brass pieces with a screw-thread (Fig.6.16d).<br />

These pieces are also glued to the Perspex with aid of Cyanolite. Finally, the brass pieces<br />

are futed stably with a lock pin, which penetrates the brass cylinder that covers the whole<br />

piece (Fig.6.16e).<br />

The cables that provide the electrical contact are supplied with extra insulation;<br />

generally the PTFE narrowbore tube can be used so as to minimize the chance of<br />

contact of the brass housing with the cables. The cables are fixed to the micro-sensing<br />

electrodes with a suitable metal paint, which is covered with a small amount of Cyanolite<br />

for optimal solidity. The connection with the interrupted narrow-bore tube is made in a<br />

simple manner. A piece of Perspex is provided with a hole with an inside diameter equal<br />

to the outside diameter of the PTFE narrowbore tube. The narrow-bore tube is first<br />

drawn out over a certain distance and is then pulled through the piece of Perspex. After<br />

a few minutes, the narrow-bore tube is cut off straight with a lancet. These clamping pieces<br />

are pressed in the detector with a clamping screw. To prevent any leakage, on the top of<br />

the clamping piece of perspex, where the narrowbore tube is cut, a small O-ring of soft<br />

rubber is applied. A film of electrolyte between the clamping piece of Perspex and the<br />

Perspex of the detector may cause a leak current to pass through towards the brass<br />

detector housing, which may render the analysis useless*. The basic principle of the<br />

electronic circuit is shown in Fig.6.17.<br />

This conductimeter is the result of the latest research and gives a linear response as a<br />

function of the resistance to be measured. Some of the isotachopherograms, however,<br />

were obtained with conductimetric equipment in which this linear relationship did not<br />

hold. This will be discussed separately because the isotachopherograms obtained by the<br />

older electronic measuring circuits differ. Later, the linearities of various conductimeters<br />

are compared.<br />

If the electric resistance of both coils of the transformer can be neglected and the<br />

coupling of both coils is assumed to be unity, the transformer can be considered to be an<br />

ideal transformer with a resistance R, and a coil L in parallel (Fig.6.17). The losses in<br />

iron and copper are responsible for this resistance R,. If the material of the core is not<br />

saturated, then R, can be considered to be a constant. The capacitance C and the coil<br />

L together form a resonance circuit with a resonance frequency given by<br />

*According to this principle, also a probe for potential gradient measurements (d.c. method) has been<br />

made with the electrodes mounted axially.

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