Separation of complex gaseous mixtures using gas chromatography (GC) is an important step in analytical systems for environmental monitoring, medical diagnosis, and forensic science. Due to its high resolving power, analysis speed, and small sample size, GC, has become the premier technique for separation and analysis of volatile and semi-volatile organic compounds. Miniaturization of analytical systems has become a major trend which is mainly driven by advancements in microfabrication techniques and a need for portable lab-on-a-chip systems for onsite monitoring. Microfabricated columns have been explored for applications in analytical processes like GC in several research studies. These microGC columns typically have open rectangular or open circular cross sections which is a result of the etching process utilized in the fabrication. This work reports the fabrication and performance of a new generation of silicon-on-glass micro-electro-mechanical systems (MEMS) based GC columns with microposts namely "semi-packed." These columns can be fabricated on a 2 cm2-die for a 1 m-long channel or a 1 cm2-die for a 25 cm-long channel. The semi-packed columns have a higher sample capacity as the overall surface area is larger than that of open rectangular columns of the same dimensions. The separation efficiency of these columns is also superior to that of open columns due to the presence of the microposts. As compared to conventional packed columns, the semi-packed columns show lower pressure drops and a more uniform flow profile, both of which contribute to, performance in terms of separation efficiency. / Master of Science

Microelectromechanical systems (MEMS) technology allows the realization of mechanical parts, sensors, actuators and electronics on silicon substrate. An attractive utilization of MEMS is to develop micro instruments for chemical analysis. An example is gas chromatography (GC) which is widely used in food, environmental, pharmaceutical, petroleum/refining, forensic/security, and flavors and fragrances industries. A MEMS-based micro GC (µGC) provides capabilities for quantitative analysis of complex chemical mixtures in the field with very short analysis time and small amounts of consumables. The aim of this research effort is to enhance the sensitivity and selectivity of µGC instruments by implementing chemical amplification method known as preconcentration. A micro preconcentrator (µPC) extracts the target analytes from the sample matrix, concentrates them, and injects them into the separation column for analysis. This work resulted in the development of silicon-glass bonded chips consisting of 7 mm x 7 mm x 0.38 mm multiport cavity with thousands of embedded 3D microstructures (to achieve high surface-to-volume ratio) coated with polymeric thin film adsorbents. Deep reactive ion etching (DRIE) was the enabling technology for the realization of µPCs. Several coating methods, such as inkjet printing of polymers and polymer precipitation from solution have been utilized to coat complex geometrical structures. One major outcome was the development of cobweb adsorbent structure. Moreover, the porous polymeric adsorbent Tenax TA in the film form was characterized, for the first time, for μPC application and shown to have similar properties to that of the granular form. Several μPC designs were experimentally evaluated for their performance in concentrating volatile organic compounds, including cancer biomarkers, Propofol (anesthetic agent), environmental pollutants, and chemical warfare simulants. The possibility of utilizing the μPCs in practical applications such breath analysis was also demonstrated. / Ph. D.