Determination of eighteen impurity elements in niobium pentoxide by full spectrum arc emission spectrometry
WU Dong-mei, ZHAO Yan-qiu, FU Guo-yu
Emission Spectrum Department of Beijing Beifen Rayleigh Analytical Instruments (Group) Co., Ltd., Beijing Material Component Analysis Instrument Engineering Research Center, Beijing Enterprise Technology Center, Beijing 100095, China
Abstract：According to the characteristic that the Nb2O5 sample is hardly dissolved and there are many impurity elements, the determination method of 18 impurity elements in niobium pentoxide sample using full spectrum arc emission spectrometer was studied. The influence of spectral buffer, electrode shape, sample loading method, analytical line and signal acquisition time on the determination was investigated. The results showed that the mixture of graphite powder, sodium fluoride and gallium oxide in mass ratio of 94∶5∶1 was used as the spectral buffer. The pass graphite electrode with pore size of 4mm and depth of 7mm was selected as the bottom electrode. After filling the electrode with sample, it was pressed downwards for 2mm and the sucrose solution was added. When the signal intensity was collected for each optimal analytical line of elements within corresponding characteristic evaporation time, the determination results were best. Under the selected working conditions, the limit of detection were all lower than 1.5μg/g. The recoveries were between 86% and 118%. The synthetic calibration sample was determined and the found results were basically consistent with the theoretical values. The relative standard deviations (RSD, n=10) of determination results for elements were all less than 10%.
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