C. Leonard et al., HIGH-SPEED GAS EXTRACTION OF VOLATILE AND SEMIVOLATILE ORGANIC-COMPOUNDS FROM AQUEOUS SAMPLES, Analytical chemistry (Washington), 70(16), 1998, pp. 3498-3504
A device is described for high-speed gas extraction of volatile and se
mivolatile organic compounds from aqueous samples. High-speed extracti
on is achieved by the use of elevated temperatures. Large quantities o
f water vapor produced at elevated temperatures are managed with a ref
lux condenser, which efficiently removes water vapor without sample lo
ss by returning the condensed water along with any cocondensed organic
compounds to the extraction cell. The heated extraction cell uses a 1
-2-mL sample with an extraction gas now of typically 30 mL/min. Extrac
tion temperatures as high as 95 degrees C can be used while maintainin
g a dew point temperature of similar to 5 degrees C for the extraction
gas and sample vapor leaving the device. Extraction profiles are obta
ined by connecting the device directly to a name ionization detector.
Extraction profiles for benzene show that quantitative recovery can be
achieved in similar to 30 s at an extraction temperature of 90 degree
s C. Large increases in recovery at higher extraction temperatures are
also demonstrated for tridecane and ethyl alcohol. For analytical stu
dies, the device is interfaced to a commercial cryofocusing inlet syst
em for highspeed gas chromatography, if all the extraction gas is trap
ped and injected into the separation column, detection limits for vola
tile organic compounds typically are in the 50-200 parts-per-trillion
range.