A hybrid injection system composed of a closed-loop vaporization chamb
er with a gas sampling valve is described. The system allows liquid in
jection into the vaporization loop with subsequent multiple injections
of the vaporized solute(s) via the gas sampling valve (GSV). Very sma
ll amounts of probe solutes can be injected without a dilution solvent
, and the vaporization loop acts as a ''retention gap'' for capillary
columns. The use of a pneumatically controlled valve injector provides
very accurate and reproducible injection volumes at precise time inte
rvals. Combination of precisely timed injections with temperature prog
ramming of the column oven produces continuous chromatograms and reten
tion data at controlled temperature increments. The proposed injection
system eliminates the need for split injectors; it is cleaner than no
rmal in-line injectors because nonvolatile samples cannot reach the co
lumn; and the instrumentation is easily automated. The major disadvant
ages are the restriction that the samples must be volatile at temperat
ures lower than the upper temperature limit of the valve rotor; the GS
V is susceptible to both contamination and mechanical failure; the sam
ple can be exposed to metal components of the valve; and initial distr
ibution of the sample throughout the closed-loop vaporization chamber
may be slow.