2410
Anal. Chem. 1989, 61, 2410-2416
Registry No. Hydrogen, 1333-74-0;2,4-dimethylaniline, 9568-1; n-hexylbenzene, 1077-16-3;n-octylbenzene, 2189-60-8; ndecylbenzene, 104-72-3;n-dodecylbenzene, 123-01-3;acenaphthylene, 208-96-8; tetradecane, 629-59-4.
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(16) Hail, M. E.; Yost, R. A. Proc. ASMS Conf. Mass Spectrom. Allied Top., 36th 1988, 803-804. (17) Hail, M. E.; Berberich, D. W.; Yost, R. A. Anal. Chem. 1989, 67, 1874- 1879. (18) Hail, M. E.; Yost, R. A. Anal. Chem., following paper in this issue. (19) McClennen, W. H.; Richards, J. M.; Meuzelaar, H. L. C. Roc. ASMS Conf. Mass Spectrom. Allied Top ., 36th 1988, 403-404. (20) Richards, J. M.; McClennen, W. H.; Bunger, J. A,; Meuzehar, H. L. C. Roc. ASMS Conf. Mass SpeCtrM. Allied Top., 36th 198& 547-548. (21) Hatch, F. W.; Parrish, M. E. Anal. Chem. 1978, 50, 1164-1168. (22) Goiay, M. J. E. Nature 1958, 782, 1146-1 147. (23) Gddings, J. C.; Seager, S. L.; Stucki, L. R.; Stewart, G. H. Anal. Chem. 1960, 32,867-870. (24) Guiochon, G. Anal. Chem. 1978, 50, 1612-1821. (25) Ettre, L. S.Inhoduction to open Tubular Columns; PerkinIlmer Corp.: Norwaik, CT, 1979; pp 52-57. (26) Omega Engineering, Inc., Stamford, CT, 1987. (27) Kelley, J. D.; Walker, J. Q. Anal. Chem. 1989. 41, 1340-1342. (28) Scott, R. P. W.; Hazeldean, G. S. F. Gas Chromatography 1960; Scott, R. P. W., Ed.; Butterworth: London, 1960; p 144. (29) Jennings, W. J. Analytical Gas Chromatography; Academic Press: Orlando, FL, 1987; pp 77-78. (30) Hail, M. E. Ph.D. Thesis, University of Florida, Gainesvllle, FL, 1989. (31) Harrison, A. G. Chemical Ionkation Mass Spectrometry; CRC Press, Inc.: Boca Raton, FL, 1983; Chapter 2.
RECEIVED for review January 27, 1989. Accepted August 4, 1989. This research was sponsored in part by the U S . Air Force Engineering and Services Center, Environics Division (HQ-AFESC/RDVS) at Tyndall Air Force Base and by the U.S. Army Chemical Research Development and Engineering Center (CRDEC) a t Aberdeen 1 roving Grounds.
Compact Gas Chromatograph Probe for Gas Chromatography/Mass Spectrometry Utilizing Res stively Heated Aluminum-Clad Capillary Columns Mark E. Hail' and Richard A. Yost* Department of Chemistry, University of Florida, Gainesuille, Florida 32611 A compact gas chromatograph (GC) probe for use In gas chromatography/mass spectrometry (GCIMS) Is described. The GC probe Is similar in size and operation to a conventional direct insertion solids probe and utilizes open tubular aiuminum-ciad capillary columns that are heated resistively. The temperature of the column is varied by a computer-programmable dc power supply. The temperature of the column Is sensed by measuring the resistance of the column itself, obviating the need for additional thermocouples or temperature sensors, and Simplifying the electrical circuitry for readback and control of the temperature. The low thermal mass of the Ai-clad columns allows the probe to be heated and cooled at faster rates aml wtth less electrical power than that used by conventional GC ovens. The GC probe Is particularly attractive when used with short (typically 3 m) open tubular columns. Samples are injected directly onto wide-bore coiumns with the injection port at subambient pressures. The GC probe can be Inserted or removed from the mass spectrometer inlet port in a matter of seconds without venting the system. The GC probe exhlbits considerable promise as a rapld sample introduction tool for GC/MS and GC/MS/MS. Resistive heating of metal-clad caplliary columns should be widely appUcabk for portable, iow-cost, and high-performance GC instrumentation.
* Author to whom correspondence should be addressed.
Current address: Finnigan MAT, 355 River Oaks Parkway, San
Jose, CA 95134.
Short-column gas chromatography (GC) has become a popular analytical method for the rapid analysis of mixtures (1-13). Short-column GC applications employing nonselective detection systems (e.g., flame ionization detection) have been reported utilizing small diameter open tubular columns (
