A practical approach to non-spectral interferences elimination in inductively coupled plasma optical emission spectrometry

2016 ◽  
Vol 70 (6) ◽  
Author(s):  
Anna Krejčová ◽  
Tomáš Černohorský ◽  
Lenka Bendakovská

AbstractMatrix effects and practical possibilities of reducing accompanying non-spectral interferences in inductively coupled plasma optical emission spectrometry (ICP-OES) were studied for microconcentric Micromist, concentric and V-groove nebulizers (VGN) coupled with two cyclonic spray chambers of different sizes. The effect of a wide scale of interferents and mixtures thereof in the concentration range of up to 2 mass % (Na, Ca, Ba, La, urea) or up to 20 vol. % (nitric acid) on the analysis of Cd, Cu, K, Mg, Mn, Pb and Zn was investigated in terms of their analytical recovery and Mg(II) 280.27 nm/Mg(I) 285.29 nm line intensity ratio. Recoveries of ionic lines were lower than those of atomic lines (37–102 %) depending on the matrix concentration. The Mg(II)/Mg(I) ratios were found to be 12–15 and they slightly decreased as the matrix load increased. Exceptional behavior of pure La matrix, steeply lowering the recoveries and Mg(II)/Mg(I) ratios was observed. A Micromist nebulizer coupled with a small inner volume spray chamber provided the highest recoveries (94–102 %), lowest matrix effects across the matrix loads and, compared to others, the least significant dependence without worsening of the analytical characteristics (recoveries, signal background ratios and the Mg(II)/Mg(I) ratios) across the studied matrices.

2017 ◽  
Vol 46 (2) ◽  
pp. 22
Author(s):  
Nikolaya Velitchkova ◽  
Metody Karadjov ◽  
Olga Veleva ◽  
Serafim Velichkov ◽  
Nonka Daskalova

The possibilities of 40.68 MHz radial-viewing inductively coupled plasma optical emission spectrometry equipped with a high-resolution spectrometer (spectral bandwidth = 5 pm) (HR-ICP-OES) were studied in the determination of rhenium in molybdenum and copper concentrates. By using equipment with a high spectral resolution, a hyperfine structure (HFS) of the most prominent lines of rhenium (i.e., Re II 197.248 nm, Re II 221.426 nm and Re II 227.525 nm) were registered. The HFS components, under high-resolution conditions, were used as separate prominent lines in order to circumvent spectral interferences in the presence of complex matrix containing Mo, Al, Ti, Fe, Mg, Ca and Cu. The Q-concept was applied for quantification of the spectral interferences and optimum line selection. Microwave acid digestion method was used as a sample dissolution procedure. The feasibility, accuracy and precision of the analytical results were experimentally demonstrated by certified reference materials from molybdenum and copper concentrates. Comparative data for true detection limits by using HR-ICP-OES 40.68 MHz ICP and Slurry sampling total reflection X-RAY fluorescence were presented in the determination of rhenium in CRM Molybdenum concentrate “CGL-202”.


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