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Principle of operation |
The mixture to be separated
are filled into standard Autosampler Vials which are placed into a Automatic
Sampler. The sample will be injected using the On-Column technique on
conditioned 0.32 mm i.d. capillary columns. Small glass tubes filled with an
adsorbent are used for sample enrichment. They are fixed in a special
designed revolving drum which is screwed on a additional detector base body
heated by the standard detector heating block. One branch of an exit
splitter leads through available PRES-FIT T-piece. During normal run
conditions the whole column effluent flows into the detector. On changing to
the switch condition the effluent can be directed completely or partially
into the adsorption tubes. This is accomplished by the following mechanism:
The adsorption tube placed directly above the splitter branch is connected
to vacuum. The vacuum is activated byswitching a solenoid valve opening the
circuit to the vacuum pump. On sucking, the whole effluent can be passed
through the adsorption tube, so efficiently that the flame of the FID can
even be extinguished. During normal operation the solenoid valve is closed.
Thus a standing gas volume, serving as a gas barrier, is obtained in the
splitter branch leading the adsorption tube. Therefore, the column effluent
is forced to flow through the splitter branch leading to the FID and does
not contaminate the adsorption tube. Changing over from one fraction to
another is performed by turning the pneumatically driven revolving fraction
collector. This procedure needs about 2 seconds. Any loss of sample during
this time can be neglected, particularly since it is preferable anyway to
collect neighbouring peaks in such a way that the overlapping zone, which is
generally larger than 2 seconds, is not collected. For resolved peaks, the
sample loss between the peak valleys is negligible. Generally, the ratio
between bleed and sample improves if the eluting sample is not collected at
the bottom of either slope. Furthermore, the information gained from a
spectrum of pure sample is more valuable than from a sample containing 10 to
20% impurities. Collected fractions can be stored or be desorbed with a
suitable solvent for subsequent analysis, e.g. NMR, UV, IR, micro chemical
reactions, and biological activity tests. |