Graduate Thesis Or Dissertation
 

Fundamental studies of a gas-jet enhanced sputtering system and its applications

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  • The use of gas jets in a sputtering cell makes this direct sampling method practical for atomic absorption and mass spectrometry determinations. With a commercial six-jet sputtering source, the Atomsource (Analyte Corp., Grants Pass, Oregon), that directly atomizes solid samples for conventional atomic absorption spectrophotometers, the sample loss rate for a Cu sample is 400 μg/min with a 0.2 L/min gas flow rate, and 170 μg/min with no gas flow. With a single-jet glow discharge source, the gas jet increases the absorbance by a factor of 40. Studies of the electrical and spectral characteristics of this six-jet Atomsource and a similar single-jet glow discharge source have been made to help determine the mechanisms responsible for the increased absorbance and the increased sampling rate. A scanning electron microscope is used to investigate the effect of experimental parameters such as current density, sputter time, gas flow rate, and cathode base material on the microstructure of the cathode surface. The Atomsource is interfaced to the mass spectrometer of a VG PlasmaQuad ICP-MS, replacing the ICP. The pressure, current, anode voltage, sampling distance, and sampling cone hole size are optimized to obtain improved performance for analytical applications. With an optimized source, it is possible to determine elements at low concentrations that would be difficult to determine with ICP-MS. Three zirconium standards, one zircaloy standard, and one zircaloy sample were analyzed and the presence of 15 elements was determined. The average relative precision of measurement for 10 elements was better than 4 percent. In a multielement analysis the detection limits for 13 elements were lower than 0.5 ppm, while single element determination improved the detection limits by an order of magnitude. Concentrations determined with an internal stsandard were in agreement within 10 % of the certified values for most of the elements in the Zircaloy sample.
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