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Figure
1
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While low
pressure reactor systems are useful for reactions run at pressures up
to about 100 psig (depending on the size of the reactor) they are not
adaptable for reactions run at atmospheric pressure. We have, however,
designed apparatus in which gas uptake can be automatically measured while
keeping the pressure in the reactor constant at atmospheric. This is diagramed
in Figure 1 with a picture shown in Figure 2. The
basic component in this system is a sensitive differential pressure transducer
(A) with one side measuring atmospheric pressure and the other the internal
reactor pressure. The computer monitors the transducer output and when
a slight pressure differential (about a half inch of water) is detected
because of the gas uptake in the reactor, the pulse valve (B) is opened
to introduce a known volume of gas into the reactor. The size of this
pulse is dependant on the gas pressure at the pulse valve and the time
it remains open. These factors are adjusted to provide calibrated pulses
of near one half cc of reactor gas. The selection valve (S) provides a
simple means of using different reaction gases. This apparatus can also
be used to study reactions in which a gas is produced.
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Figure
3
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Three of
these automated atmospheric pressure reactor systems are pictured in Figure
3. A reproduction of the computer screen showing the progress of all three
reactions is shown in Figure 4.
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Figure
4
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Each data
point represents the time of introduction of the calibrated pulse of reactant
gas. For room temperature reactions the standard low pressure reactors
shown in the Low Pressure Reactor section are also used with these systems.
When temperature control is needed, jacketed versions of these reactors
are used with the temperature maintained by a constant temperature recirculating
bath.
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