D. Helmig et Jp. Greenberg, AUTOMATED IN-SITU GAS-CHROMATOGRAPHIC MASS-SPECTROMETRIC ANALYSIS OF PPT LEVEL VOLATILE ORGANIC TRACE GASES USING MULTISTAGE SOLID-ADSORBENT TRAPPING, Journal of chromatography, 677(1), 1994, pp. 123-132
A fully automated sampling/injection system for the gas chromatographi
c-mass spectrometric (GC-MS) analysis of volatile organic compounds at
tropospheric background levels was developed. Organic trace gases fro
m air samples up to 100 l were trapped in temperature-controlled solid
-adsorbent traps. The instrument utilized a one stage sampling/desorpt
ion inlet system designed as a closed device that did not require any
replumbing steps between sampling and analysis. For analysis, the adso
rbent trap was thermally desorbed and backflushed onto the chromatogra
phic column where organic trace gases were directly cryofocused. Adsor
bents tested were Carbotrap, Carbotrap C, Carbosieve S III, Tenax TA,
Tenax GR and multistage combinations of these adsorbents. Interference
s from blanks and adsorbent artifacts were minimized by backflushing t
he adsorbent trap, switching valve and transfer line between sampling
sequences at temperatures above the levels used during trapping and sa
mple transfer. The high sample volumes that could be concentrated and
the low background levels allowed structural identification in GC-MS (
electron impact ionization scan mode) at minimum levels of ca. 100 pg
per peak (ca. 10-(12) mol) equivalent to atmospheric concentrations at
the lower parts per trillion (v/v) level. The volatility range of org
anic compounds that could be identified was approximately from pentane
to pentadecane. The system was completely computer controlled and cou
ld be operated continuously and unattended around the clock for in sit
u analysis. The instrument was successfully deployed at the Mauna Loa
Observatory, Hawaii, USA in July and August 1992.