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Needle Trap Device and Solid Phase Microextraction Combined with Portable GC-MS for On-Site Applications

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Warren_Jamie.pdf (1.53 MB)

Date

2011-06-21T17:54:55Z

Authors

Warren, Jamie

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Publisher

University of Waterloo

Abstract

Needle trap device (NTD) is a technique that is useful for a wide variety of applications involving the sample preparation of compounds with a wide range of chemico-physico properties, and varying volatilities. A newly designed NTD that improves the performance relative to previous NTD designs is simple to produce is developed. The NTD utilizes a side-hole needle with a modified tip to improve the sealing between the NTD and narrow neck liner of the GC injector, thereby increasing the desorption efficiency. The slurry packing method was applied, evaluated, and NTDs prepared by this method were compared to NTDs prepared using the vacuum aspiration method. NTD geometries including blunt tip with a side-hole needle, tapered tip with side-hole needle, dome tapered tip with side-hole, sliding tip with side-hole and blunt tip with no side-hole needle (expanded desorptive flow) were prepared and evaluated. Sampling performance and desorption efficiency were investigated using automated headspace extraction of benzene, toluene, ethylbenzene, p¬-xylene (BTEX), anthracene and pyrene. The tapered tip and sliding tip NTDs were found to have increased desorption efficiency. SPME and NTDs are valuable sample preparation tools for on-site analysis. Combining both extraction techniques allows for the differentiation of free and particle-bound compounds in a sample matrix. Portable GC/MS instrumentation can achieve fast separation, identification, and quantitation of samples prepared by the above techniques on-site without the need for transport to the laboratory. This minimizes the effects of volatiles lost and sample degradation during storage time. Here, SPME and tapered tip NTDs combined with portable GC/MS are used to investigate free and total emissions of BTEX and select PAHs from gasoline and diesel exhaust. Using the above optimized technologies, cigarette smoke in a smoking area where people were actively smoking and inside a smoker’s car were also investigated. Target contaminants were found in the investigated matrices at ng/mL levels.

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Keywords

SPME, needle trap device, on-site, portable GC/MS

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URI

http://hdl.handle.net/10012/6014

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Chemistry