Details

Autor(en) / Beteiligte

• BEYER, JOHN OLIVER

Titel

HIGH RESOLUTION GAS CHROMATOGRAPHIC STUDIES OF VOLATILE INORGANIC COMPOUNDS (CHELATES, ARGON PLASMA)

Ort / Verlag

ProQuest Dissertations & Theses

Erscheinungsjahr

1984

Quelle

ProQuest Dissertations & Theses A&I

Beschreibungen/Notizen

• As knowledge has expanded concerning natural and synthenic chemical systems, and as society has manifested an increasing concern over substances occuring at very low levels in complicated matrices, gas chromatographic detectors have been developed in the complementary directions of increased sensitivity and selectivity. The complexity of real samples when analyzed at high sensitivity has caused chromatographic interference by excipients to become a major problem in many instances. The need has been clear for detectors which possess the needed sensitivity and a selectivity which will enable satisfactory discrimination of the analyte signal from that of the matrix and which exhibit a wide linear dynamic range to permit easy quantitation. In addition, application to complex samples requires that the detector be capable of use with modern high resolution (capillary) gas chromatographic systems without significant loss of chromatographic efficiency. The initial work reported in Chapter I of this dissertation describes the development and optimization of a high resolution element-selective gas chromatographic detector utilizing the commercially available Spectraspan IV('TM) direct current argon plasma emission spectrometer (Spectrametrics, Inc., Andover, MA). Fused silica open tubular technology was employed to minimize degradation of labile analytes. The element-specific gas chromatographic system was subsequently applied to brief studies of some silicon- and boron-containing derivatives of organic compounds (Chapter II) and of some alkyls and alkyl chlorides of Group IV-A elements (Chapter III). Chapter IV describes studies of the chromatographic performance of selected metal (beta)-diketonates and tetradentate (beta)-ketoamine complexes using fused silica columns. Finally, the system was characterized for element-specific analysis of compounds containing a wide range of elements. Detection limits, molar selectivities with respect to carbon and linear ranges for twenty-one elements are reported in Chapter V.