Application of the hollow cathode discharge emission source to the determination of nonmetals in microsamples

Abstract

The use of the hollow cathode discharge source for the excitation of nonmetals In volume-limited samples is discussed. The effects of breakdown voltage, fill-gas composition, electrode composition, hollow size, sample deposition mode, current, and fill-gas pressure on the emission signal from phosphorus and chlorine are reported. Instrumentation, operation, and sample preparation procedures are described. Temporal profiles of the emission signal from very small samples deposited in the hollow are given for P, Cl, and Se. Detection limits of 9 and 20 pg are reported for P and Cl, respectively.

Pulsed glow discharge in thin-walled metallic hollow cathode. Analytical possibilities in atomic and mass spectrometry

“…As an alternative, a number of researchers used GD devices for indirect analysis of liquid samples by the sputter atomization of solution residues. [24][25][26][27][28][29][30] The solution under investigation (1-100 ml) is placed on a planar cathode or inside the hollow cathode surface and dried directly or by infrared heating. This procedure can be applied in atomic absorption, 24,25 emission, 26,27 fluorescence, 28 resonance-ionization spectroscopy, 29 or mass spectrometry.…”

“…[24][25][26][27][28][29][30] The solution under investigation (1-100 ml) is placed on a planar cathode or inside the hollow cathode surface and dried directly or by infrared heating. This procedure can be applied in atomic absorption, 24,25 emission, 26,27 fluorescence, 28 resonance-ionization spectroscopy, 29 or mass spectrometry. 30,31 In the case of solution analysis, however, the presence of water in ''dry residue'' may lead to essential deterioration of the analytical signal, especially in mass spectrometry.…”

Investigation of the role of hollow cathode (vaporization) temperature on the performance of particle beam-hollow cathode atomic emission spectrometry (PB-HC-AES)

“…The use of glow discharge devices for indirect analysis of solution samples by the sputter atomization of solution residues has been investigated by several researchers. 13±19 In these applications, dried residues from liquid samples are changed into the gas phase using cathodic sputtering, with the atomic population sampled by atomic absorption, 13,14 emission, 15,16 ¯uorescence, 17 or mass spectrometries. 18,19 Although this fairly simple method is capable of giving impressive levels of detection, the processes of sample deposition and solvent evaporation can be labor intensive and time consuming.…”

Analysis of Organic Compounds by Particle Beam/Hollow Cathode Atomic Emission Spectroscopy: Determinations of Carbon and Hydrogen in Amino Acids

“…While the glow discharge has been developed and proven as a powerful spectrochemical source for various solid samples, the analysis of liquid samples has found only limited interest. A few publications have reported the use of hollow cathode glow discharges to sputter atomize solution residues. , In these applications, an aliquot (<200 μL) of the liquid sample is placed in the base of the hollow cathode, dried to a solid (residue) by direct or IR heating, and converted into gas-phase atoms through cathodic sputtering. Very impressive levels of detectability have been achieved by hollow cathode atomic emission spectrometry (HC-AES), with Chen and Williams 4 reporting limits of detection of 9 and 20 pg of P and Cl, respectively, in renal fluids.…”