26.12.2012 Views

Frans_M_Everaerts_Isotachophoresis_378342.pdf

Frans_M_Everaerts_Isotachophoresis_378342.pdf

Frans_M_Everaerts_Isotachophoresis_378342.pdf

SHOW MORE
SHOW LESS

You also want an ePaper? Increase the reach of your titles

YUMPU automatically turns print PDFs into web optimized ePapers that Google loves.

228 INSTRUMENTATION<br />

The W light is generated by a microwave-powered low-pressure mercury lamp. This<br />

W light is transported by an optical quartz rod and fed into a cylindrical slit of width<br />

0.05-0.3 mm. As already mentioned, the PTFE narrow-bore tube is not interrupted and is<br />

clamped by the slit, which is made of brass, and the W light passes through the narrow-<br />

bore tube and is again transported via an optical quartz rod to a set of filters (an<br />

interference filter in combination with an end filter). The UV quanta then illuminate a<br />

UV light-sensitive photodiode (S330; Hamamatsu, Hamamatsu City, Japan). The quality<br />

of the PTFE narrow-bore tube is not sufficiently constant for the UV detector, because<br />

the PTFE material itself has a high W absorption. On mounting a particular narrow-bore<br />

tube, the amount of light that passes through it and finally reaches the detector may<br />

vary by a factor of up to three compared with a previously used narrow-bore tube owing<br />

to the difference in the thickness of the two tubes, if they are filled with a non-UV-<br />

absorbing liquid. On one hand the high absorptivity of the PTFE material in the UV<br />

range is a disadvantage, while on the other hand the dark current, i.e., the current that is<br />

transported by the PTFE wall and reaches the detector without passing through the<br />

narrow-bore tube, is reduced to a minimum.<br />

The signals are handled electronically and result in a trace on a potentiometric recorder.<br />

The trace does not have a continuous stepwise character if the isotachophoretic zones pass<br />

the detector.<br />

At the position where the conductimeter is mounted, the narrow-bore tube is inter-<br />

rupted by a piece of insulating material (Perspex or TPX) in which the micro-sensing<br />

electrodes are mounted (Chapter 6). As a result, there is always a slight difference in cell<br />

volume between the conductimeter and the UV detector. The sequence of mounting<br />

these two detectors was tested and it proved to be of no importance; experiments were<br />

carried out to prove this only with components that were stable in the UV region, and<br />

possible deleterious effects due to W light were not studied.<br />

The conductivity detector can be applied for measurements of the conductivity<br />

(a.c. method) or for measurements of the potential gradient (d.c. method) via two micro-<br />

sensing electrodes (10-pm Pt-Ir foil) mounted axially and in direct contact with the<br />

electrolytes inside the narrow-bore tube. In Fig. 7.16 can be seen the position where<br />

the coil is mounted in order to give good galvanic separation of the high potential on<br />

the micro-sensing electrodes from the circuit for measuring the conductivity (potential<br />

gradient) at low potential. As discussed in Chapter 6, a leak current towards earth (even<br />

lo-” A) must be prevented. For this reason the conductivity probe is surrounded by<br />

PTFE insulation. Even the wires connecting the micro-sensing electrodes with the<br />

electronic measuring circuit are provided with extra insulation by means of a PTFE<br />

narrow-bore tube.<br />

The signals derived from the conductivity probe are fed to a field effect transistor<br />

(potential gradient measurement) or directly to a well insulated transformer for good<br />

galvanic insulation. If the measuring electrodes are mounted equiplanar, only the<br />

conductivity can be determined of course.<br />

For the measurement of the conductivity (a.c. method) with axially mounted elec-<br />

trodes, these electrodes must be separated from each other via a capacitor, otherwise an<br />

electric current will flow, due to the potential gradient, and electrode reactions will<br />

result, e.g. , coating or gas production. Even when the micro-sensing electrodes were

Hooray! Your file is uploaded and ready to be published.

Saved successfully!

Ooh no, something went wrong!