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ANALYTICAL CHEMISTRY, VOL. 50, NO. 12, OCTOBER 1978 1705 retention time vs. temperature plots, indicate that while
 

Summary: ANALYTICAL CHEMISTRY, VOL. 50, NO. 12, OCTOBER 1978 1705
retention time vs. temperature plots, indicate that while
solubilities would be smaller, separations would be increased
by operation at a slightly higher temperature. The linear flow
rate through this column at 90 atm ethane is observed to be
7 cm/s-slightly slower than the optimum 20 cm/s for a
standard capillary column and within the range of acceptable
values.
The major problem encountered thus far has been plugging
of the nozzle orifice caused both by foreign particles and by
sample deposition. Even with carefully filtered (multiple-
stage, 5 pm) solvent gas and a dual 512 bm filter placed
directly between the final zero-dead-volume shut-off valve and
the nozzle orifice, we have observed slow closure (after 1to
10 h of operation) of the nozzle orifice from particle accu-
mulation correlated with actuation of the preceding valve, the
packing of which is graphite-filled fluorocarbon polymer.
Inspection of the orifice once showed a symmetrical black
deposit about the entire circumference with a long, thin
particle ( - 2 pm by 15 pm) centered along a diameter. In-

  

Source: Aneja, Viney P. - Department of Marine, Earth and Atmospheric Sciences, North Carolina State University

 

Collections: Environmental Sciences and Ecology; Geosciences