Evaluation and Application of Microextraction Techniques Coupled with Portable Analytical Instrumentation for On-site Analysis
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In recent years, on-site analysis has garnered increased interest from the scientific community. The development of smaller, more sophisticated analytical instruments, and the establishment of new environmental regulations have encouraged the application of new methodologies for field analysis. Prominent advantages of on-site analysis include elimination of error sources due to sample transportation and matrix modification, considerable reduction in analysis time, and more accurate and precise analytical results. Several techniques suitable for on-site analysis, which integrate sampling and sample preparation in one step, have demonstrated high versatility and throughput in field applications. This research was focused on the application and evaluation of three microextraction techniques: solid phase microextraction (SPME), needle trap devices (NTD) and membrane extraction with sorbent interface (MESI), which were then coupled with various portable instruments for on-site analysis of different systems. Additionally, the conducted project involved the development of an approach using ion mobility spectrometry detection (IMS) coupled with a miniaturized gas chromatograph (GC) as a powerful system for field analysis. This proposed GC-IMS exhibited satisfactory performance in terms of retention time (inter-day variation < 3%) and response stability (intra and inter-day relative standard deviations (RSDs) < 10 %). Moreover, when coupled with NTD, it showed limits of detection comparable to those provided by conventional benchtop instruments. Other portable GC instruments employed in this project included flame ionization and mass spectrometry detection. Three different sample systems were investigated using SPME and NTD together with these portable instruments: emissions of a pine branch, breath samples, and indoor pollutants in a polymer synthesis laboratory. Consequently, the feasibility of using SPME and NTD for determination of free and total concentrations was investigated. Finally, MESI was successfully coupled with the newly proposed GC-IMS system, and its functionality was evaluated by analyzing acetone in breath samples.