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Elemental analysis of silicon based minerals by ultrasonic slurry sampling electrothermal vaporisation ICP-MS
Authors:Rodríguez Pablo Fernández  Marchante-Gayón Juan Manuel  Sanz-Medel Alfredo
Institution:a Departamento de Prevención Técnica, Instituto Nacional de Silicosis, c/Doctor Bellmunt s/n, 33006 Oviedo, Spain
b Departamento de Química Física y Analítica, Universidad de Oviedo, c/Julián Clavería 8, 33006 Oviedo, Spain
Abstract:Ultrasonic slurry sampling electrothermal vaporisation inductively coupled plasma mass spectrometry (USS-ETV-ICP-MS) was applied to the elemental analysis of silicate based minerals, such as talc or quartz, without any pre-treatment except the grinding of the sample. The electrothermal vaporisation device consists of a tungsten coil connected to a home-made power supply. The voltage program, carrier gas flow rate and sonication time were optimised in order to obtain the best sensitivity for elements determined. The relationship between the amount of sample in the slurry and the signal intensity was also evaluated. Unfortunately, in all cases, quantification had to be carried out by the standard additions method owing to the strong matrix interferences. The global precision of the proposed method was always better than 12%. The limits of detection, calculated as three times the standard deviation of the blank value divided by the slope of the calibration curve, were between 0.5 ng/g for As and 3.5 ng/g for Ba. The method was validated by comparing the concentrations found for Cu, Mn, Cr, V, Li, Pb, Sn, Mg, U, Ba, Sr, Zn, Sb, Rb and Ce using the proposed methodology with those obtained by conventional nebulisation ICP-MS after acid digestion of the samples in a microwave oven. The concentration range in the solid samples was between 0.2 μg/g for Cr and 60 μg/g for Ba. All results were statistically in agreement with those found by conventional nebulisation.
Keywords:Ultrasonic slurry sampling  Electrothermal vaporisation  ICP-MS  Silicate based minerals
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