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Frans_M_Everaerts_Isotachophoresis_378342.pdf

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120 DETECTION SYSTEMS<br />

TABLE 6.1<br />

SURVEY OF SPECIFIC PROPERTIES THAT CAN BE RECOGNIZED IN ISOTACHOPHORETIC ANALYS:<br />

Type of electrolyte Initial conditions Steady state<br />

Leading electrolyte (L.E.)<br />

Sample zone(s)<br />

Conductivity<br />

Determined by the choice of the<br />

operational system in which<br />

the analysis is carried out.<br />

Unknown, but generally adjusted<br />

to the conditions of the L.E.<br />

with respect to pH and the<br />

concentration of the ionic<br />

species (roughly).<br />

Terminating electrolyte (T.E.) Chosen to be of approximately<br />

the same order of magnitude<br />

as the leading anion (anion<br />

separation) or cation (cation<br />

separation), to minimize the<br />

effect of fast-moving<br />

impurities.<br />

(pH is adjusted approximately to<br />

the pH of the leading elec-<br />

trolyte to prevent sample<br />

ions being 'missed'.)<br />

Conductivity<br />

Determined by the initial choice of<br />

the operational system.<br />

AU zones adjusted to the concen-<br />

tration of the leading anion<br />

(anion separation) or cation<br />

(cation separation).<br />

The concentration is adjusted to the<br />

concentration of the leading<br />

anion (anion separation) or<br />

cation (cation separation).<br />

The conductivity decreases from the<br />

L.E. towards the T.E. (except<br />

for 'enforced' isotachophoretic<br />

systems).<br />

An easy method of making these thin thermocouples is as follows. Copper (30 pm) and<br />

constantan (25 pm) wires are twisted symmetrically together, after the ends of each have<br />

been fixed in a small piece of shellac placed on a rod [ 1 ] .<br />

The difference in the diameters of the wires is necessary because otherwise, owing to<br />

their very different flexibilities, the twisting of the two wires of identical diameter results<br />

in an asymmetrically wound thermocouple, the copper wire being wound around the<br />

constantan wire. The procedure for mounting a thermocouple that is not symmetrically<br />

wound around the narrow-bore tube is very difficult and the thermocouple easily breaks<br />

on the copper side, especially if both diameters are 30 pm. Copper wires of 25 pm diameter<br />

easily breaks during the twisting procedure, especially if the wires are corroded.<br />

The tightly twisted part is cut so that a length of about 1 mm remains twisted. This<br />

twisted end is silver soldered by inserting it into molten silver solder, protected with a<br />

small amount of flux. This silver solder is kept molten by utilizing the heat capacity of<br />

a thick-walled Pyrex glass tube (Fig. 6.1). Other methods of making thin thermocouples<br />

are given in ref. 1.

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