Volatile and semi-volatile organic compounds are ubiquitous, and some of them are hazardous. The ability to rapidly detect and identify trace levels of them in air has become increasingly important. The conventional device used today for sampling and concentrating them in air is thermal desorption tubes filled with specific sorbents, which can only collect air samples at flow rates of 100-200 mL/min. In order to detect low concentration (ppt level) VOC compounds, long sampling time (>2 h) and sensitive detection are required. At the same time, portable instrumentation for on-site analysis has been developing rapidly. The somewhat lower performance of portable instruments compared to benchtop systems requires the sampling of even greater sample volume in order to reach the same detection limits. In this study, two high flow rate air sampling devices, i.e., a multi-capillary trap and a concentric packed trap, were developed to sample a large volume of air in a short time period. The multi-capillary trap was constructed by bundling analytical capillary gas chromatography columns together in parallel. As low as single digit ppt detection limits were reached in less than 25 min with this trap, and as high as 8.0 L/min flow rate was sampled. The simple and compact multi-capillary trap could be easily used with a conventional thermal desorption system to perform high flow rate sampling. A concentric packed high flow rate trap was also developed by packing sorbent layers concentrically around an empty tube. The concentric packed trap achieved a high flow rate (>10 L/min) because it had a high surface area and short sorbent bed. Also, its large sorbent amount (>1 g) provided large breakthrough volume (>100 L) required to achieve low detection limits. An equilibrium distribution sampling system was developed by absorbing selected analytes in granular PDMS to provide calibration for on-site instrumentation. Furthermore, a needle trap device was coupled in tandem to both high flow rate air samplers to perform second-stage concentration of VOCs down to the ppt level. Concentration factors of 104 to 105 were achieved within 30 min using both systems, i.e., over 10 to 100 times more sample was collected compared to conventional TD systems.

The ability to rapidly detect and identify hazardous analytes in the field has become increasingly important. One of the most important analytical detection methods in the field is gas chromatography-mass spectrometry (GC-MS). In this work, a hand-portable GC-MS system is described that contains a miniature toroidal ion trap mass analyzer and a low thermal mass GC. The system is self-contained within the dimensions of 47 x 36 x 18 cm and weighs less than 13 kg. Because the instrument has a small footprint, it was used as the detector for an automated near-real-time permeation testing system. In permeation testing, materials that are used to make individual protective equipment such as gloves, masks, boots, and suits are exposed to hazardous analytes to determine how long the equipment can be worn safely. The system described herein could test five samples simultaneously. A multi-position valve rotated among the various sample streams and delivered time aliquots into the MS for quantitation. Current field air sampling techniques suffer from long desorption times, high pressure drops, artifact formation and water retention. These disadvantages can be avoided by concentrating the analytes in short open tubular traps containing thick films. There are several advantages to using polymer coated capillaries as traps, including fast desorption, inertness and low flow restriction. An air sampling trap was constructed utilizing open tubular traps for the concentration of semi-volatile organic compounds. The system consisted of multiple capillary traps bundled together, providing high sample flow rates. The analytes were desorbed from the multi-capillary bundle and refocused in a secondary trap. The simultaneous focusing and separation effect of a trap subjected to a negative temperature gradient was also explored. In this configuration, analytes were focused because the front of the peak was at a lower temperature than the rear of the peak and, hence, moved slower. In addition to the focusing effect, analytes with different volatilities focused at different temperatures within the gradient, allowing for separation.