2012 Volume 52 Issue 9 Pages 1616-1621
An advanced detection method based on a modulation technique is described in radio-frequency-powered glow discharge plasma optical emission spectrometry (r.f. GD-OES). A frequency-sensitive separation using a fast Fourier transform (FFT) analyser, where a pulsated bias-current was introduced into an r.f. GD plasma, was available for improving the limit of determination for the atomic emission analysis. The FFT analyser has an ability to disperse signal components by frequency, and it is thus employed to select the component of a particular frequency. A dc bias current introduced into the GD plasma can enhance the emission intensities of analyte species greatly, and furthermore, it can be easily pulsated to modulate the emission intensities from the plasma. The modulated emission signal was selectively detected with the FFT analyser, with removing any noise components from the overall signal. The duty ratio of the pulsed bias current largely affected the amplitude of the FFT frequency components, because the pulse waveform comprised sine-function components having frequencies integral-times as much as the fundamental frequency, whose contribution coefficients depended on the duty ratio. This detection method was applied to the determination of vanadium and molybdenum in low-alloyed steel samples. The detection limits were obtained to be 6.2 × 10–3 mass% V and 2.0 × 10–3 mass% Mo in low-alloyed steel samples.