The work described herein focuses on FT-IR and quantum cascade laser (QCL) based studies towards the development of compact and portable trace gas sensor for benzene, toluene, and xylenes (BTX). FT-IR broadband radiation was used to probe the mid-infrared fingerprint region for quantitatively detecting trace gas levels of BTX. Using direct absorption through a hollow waveguide, parts-per-million (ppm) detection limits for BTX with a response time of 39 seconds was demonstrated. Univariate calibration provided limits of detection (3σ) for benzene, toluene, and meta-xylene at 5, 17, and 11 ppm, respectively. Multivariate calibration using partial least squares regression algorithms were used to simulate real-world conditions with multiple analytes present within a complex sample. A calibration model was built with 110 training set standards enabled by using a customized gas mixing system. Furthermore, a preconcentration/thermal desorption (TD) step was added to the FT-IR HWG trace gas sensor enabling parts-per-billion detection of BTX. A univariate calibration was established in the laboratory with certified gas standards over a dynamic range of 1000 - 100 ppb for benzene, toluene, and the xylenes. The sensor was then taken to an industrial site during a field measurement campaign for the quantitative determination of BTX in field air samples. The laboratory calibration was used to predict unknown concentrations which were in close agreement with industrial hygiene standard techniques, and industrial prototype analyzers, that were simultaneously operated in the field environment.
In addition to FT-IR, quantum cascade laser spectroscopy was also investigated due to enhanced spectral density and efforts to precisely overlap emission with analyte absorption. Particular efforts were dedicated on a novel principle for consistent and deliberate QCL emission wavelength selection by varying the QCL cavity length. These studies experimentally confirmed that using this straight-forward post-processing technique, emission wavelength tuning across a range of one hundred wavenumbers range may be achieved. This tuning range was experimentally demonstrated for a QCL emitting across an entire absorption feature of carbon dioxide by tailoring the length of the cavity. Additionally, using an external cavity (EC) - QCL combined with a HWG gas sensor module for the first time enabled the quantitative and simultaneous determination of ethyl chloride, trichloromethane, and dichloromethane within exponential dilution experiments at ppb limits of detection. Multianalyte detection was demonstrated utilizing partial least squares regression for quantitative discrimination of individual constituents within a mixture, yet applying a single broadly tunable QCL light source.
| Identifer | oai:union.ndltd.org:GATECH/oai:smartech.gatech.edu:1853/31702 |
| Date | 16 November 2009 |
| Creators | Young, Christina Rachel |
| Publisher | Georgia Institute of Technology |
| Source Sets | Georgia Tech Electronic Thesis and Dissertation Archive |
| Detected Language | English |
| Type | Dissertation |
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