Method |
Reaction rates were measured at series of elevated temperatures,
following them to completion. The resulting Arrhenius
plot, if linear, can then be extrapolated to 25 °C. In much of this work, reaction mixtures were sealed in
quartz, heated over various intervals, and then opened for
analysis by proton NMR. The vapor pressure of water does
not change enough to affect reaction rates significantly,
but aqueous samples tend to burst at temperatures above
250 °C (40 atm). Explosions are avoided by placing
reaction tubes in water inside a steel bomb, equalizing
pressure across the wall of each tube. PTFE vessels must
be used for alkaline solutions which attack quartz. |