Charge injection device array detection for atomic spectroscopy with applications in gas chromatography.
AuthorLamoureux, Burton Richard.
Chromatographic analysis -- Equipment and supplies
Atomic emission spectroscopy Electrochemical sensor.
AdvisorDenton, M. Bonner
MetadataShow full item record
PublisherThe University of Arizona.
RightsCopyright © is held by the author. Digital access to this material is made possible by the University Libraries, University of Arizona. Further transmission, reproduction or presentation (such as public display or performance) of protected items is prohibited except with permission of the author.
AbstractVery early in the history of atomic emission spectroscopy (AES) it was understood to be a powerful analytical tool. Until the 1930's the usefulness of atomic spectroscopy was not utilized very extensively even though its fundamental power was understood. The breakthrough that placed it in the standard chemistry laboratory was the discovery and implementation of the photoelectric effect. Since this discovery there has been a revolution in atomic spectroscopy which has brought it from the role of a humble servant used for primary elemental screening to an outstanding leader in applications of elemental analysis. Atomic emission spectroscopy of complex samples has long suffered from matrix effects which result in overlapping of spectral lines, fluctuating backgrounds and changing conditions in the source. Investigations employing an echelle polychromator with a two dimensional solid state array detector show great promise in minimizing the effects of these interferences on multielement analyses of complex samples. The Charge Injection Device (CID) detector used exhibits many characteristics which make it uniquely qualified for simultaneous, multielement detection in AES. With only slight modifications to the optics of a commercial spectrometer and the employment of a CID detector, detection limits for a number of elements are quite favorable. Dynamic ranges of over seven orders of magnitude are obtainable with this experimental system. The reduction of matrix effects by utilizing the huge wealth of information available from over 60,000 individual detector elements are demonstrated through results from several complex matrix standards. This CID-polychromator system was also employed for the element selective detection of gas chromatographic (GC) effluents. A microwave-induced plasma (MIP) based on the Surfatron design was built. A helium plasma from this device has shown to have resilience to organic samples and give good emission response to non-metallic atoms. A number of studies with this GC-AES-polychromator system are presented. This system is capable of monitoring atomic emissions from C, H, F, Cl, Br, I, O, N and S all simultaneously, and the selectivity of this system is unsurpassed. Elemental ratios for separated compounds are also presented as a precursor to empirical formula prediction.