A detailed evaluation of the analytical characteristics of a particle beam/hollow cathode glow discharge atomic emission spectroscopy (PB/HC-AES) system is described for applications in the area of organic sample analysis. The optimization of sample introduction, nebulization parameters, and glow discharge conditions was performed for the elemental analysis (focusing on C and H) of a group of amino acids. By use of a high-efficiency thermoconcentric nebulizer, analyte particles are introduced into a heated hollow cathode glow discharge source, in either flow injection or continuous-flow mode, for subsequent vaporization/atomization and excitation. Nebulization temperature, solvent composition, and liquid flow rate were studied to elucidate their roles in the ultimate analyte emission characteristics for organic compound analysis. The hollow cathode operating discharge current and gas pressure were optimized, with the general responses found to be similar to those for the case of metal analysis. Background interferences from solvent and additive media on carbon and hydrogen determinations were studied and substantially reduced. The analytical response curves for carbon and hydrogen present in amino acids were obtained using 200 μL injection volumes, showing less than 10% RSD for replicate injections over a concentration range of 10-250 ppm, with detection limits of 3 and 1 ppm, respectively, for C (I) and H (I) emission. Subsequent studies of the response of carbon and hydrogen emission signal intensities to differences in amino acid stoichiometries suggest a capability of the PB/HC-AES system for the determination of empirical formulas based on H (I)/C (I) intensity ratios.
Capillary-channeled polymer (C-CP) fibers are demonstrated as a potential stationary phase for liquid chromatography separation of protein mixtures. Separation of a synthetic mixture of four proteins is accomplished within a 45-second window using a conventional revered-phase (RP) gradient, at a mobile phase flow rate of 7 mL/min (10,200 mm/min).
A parametric study has been conducted on a radio frequency glow discharge atomic emission spectrometry (rf-GD-AES) source to evaluate the sputtering characteristics and resultant crater shapes for both metallic and nonconducting samples. These studies include a determination of how the operating parameters, namely, power and pressure, influence the sputtered crater's depth, the degree of convexity and/or concavity, and the crater bottom roughness. The results imply that many similarities exist between the rf mode of powering and the well-characterized dc powered devices. Some differences are noted, namely, differing crater shapes at low operating pressures and a lesser dependence of crater flatness on the applied voltage, i.e., dc-bias voltage. A new method of quantifying the degree of concavity/convexity is introduced which involves comparison of the calculated (ideal) cross-sectional area to the resultant crater area as measured by a diamond stylus profilometer. The studies indicate that the rf-GD is well suited for depth-resolved analysis under correctly chosen operating conditions, which fortuitously correspond to those used for optimum bulk elemental analyses.
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