Jv. Hinshaw, THE EFFECTS OF INLET LINER CONFIGURATION AND SEPTUM PURGE FLOW-RATE ON DISCRIMINATION IN SPLITLESS INJECTION, HRC. Journal of high resolution chromatography, 16(4), 1993, pp. 247-253
An unmodified split/splitless inlet system using forward-pressure cont
rolled pneumatics was operated in splitless injection mode with severa
l inlet liners under a range of septum purge flow rates. The relative
recovery (discrimination) of hydrocarbons ranging from n-C-8 to n-C20
depended strongly upon the injected sample volume with open-ended line
rs at high septum purge flow rates of e.g. 50 mL/min. Little or no dis
crimination was observed at septum purge flows of 2-3 mL/min.The same
inlet was also operated in a back-pressure regulated configuration tha
t produced mass discrimination similar to that observed with the highe
r septum purge flows in the forward-pressure configuration. An inlet l
iner with a restricted inlet and outlet gave mass-discrimination level
s independent of septum purge flow rate, but in the reverse sense of t
hat observed with open-ended liners. Preferential volatile-component l
osses out of the inlet liner to the septum purge vent are principally
responsible for the observed mass discrimination with open-ended liner
s, while mass-dependent losses with doubly-restricted liners seem due
to slow sample evaporation.