Determination of trace antimony in selenium by hydride generation-atomic fluorescence spectrometry

After the selenium sample was dissolved with nitric acid and hydrochloric acid,hydroxylammonium chloride was added to reduce selenium to elementary selenium,realizing the separation of matrix from impurity elements.Then,the content of antimony in sample was determined by hydride generation-atomic fluorescence spectrometry.The effects of medium and acidity in hydride generation,potassium borohydride concentration,dosage of pre-reduction reagent,pre-reduction time and dosage of hydroxylammonium chloride on the determination results were investigated.The optimal determination conditions were obtained.The interference test showed that the coexisting elements in selenium sample had no interference with the determination.Under the optimal conditions,the concentration of antimony in range of 0-100 ng/mL had good linearity to the fluorescence intensity with correlation coefficient higher than 0.999 5.Detection limit of this method was 0.23 ng/mL.The proposed method has been applied to the analysis of actual samples.The determination results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry(ICP-AES) with relative standard deviation(RSD,n=11) less than 10 %.