Determination of trace bismuth in selenium by hydride generation-atomic fluorescence spectrometry
Qin Li
Abstract
Qin Li
Abstract
After the selenium sample was dissolved with nitric acid and hydrochloric acid,hydroxylammonium chloride was added to reduce selenium(Ⅵ) to elementary selenium,realizing the separation of matrix from impurity elements.Then,the content of bismuth in sample was determined by hydride generation-atomic fluorescence spectrometry.The effects of medium and acidity in hydride generation,potassiun borohydride concentration,dosage of pre-reduction reagent,pre-reduction time,dosage of hydroxylammonium chloride and coexisting elements on the determination results were investigated.Under the optimum conditions,the concentration of bismuth in range of 0-100 ng/mL had good linearity to the fluorescence intensity with correlation coefficient higher than 0.9995.Detection limit of this method was 0.18ng/mL.The addition recovery is between 96%-106%.The results determinated by proposed method were consistent with those obtained by inductively coupled plasma atomic emission spectrometry(ICP-AES) with relative standard deviation(RSD,n=11) less than 10%.
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After the selenium sample was dissolved with nitric acid and hydrochloric acid,hydroxylammonium chloride was added to reduce selenium(Ⅵ) to elementary selenium,realizing the separation of matrix from impurity elements.Then,the content of bismuth in sample was determined by hydride generation-atomic fluorescence spectrometry.The effects of medium and acidity in hydride generation,potassiun borohydride concentration,dosage of pre-reduction reagent,pre-reduction time,dosage of hydroxylammonium chloride and coexisting elements on the determination results were investigated.Under the optimum conditions,the concentration of bismuth in range of 0-100 ng/mL had good linearity to the fluorescence intensity with correlation coefficient higher than 0.9995.Detection limit of this method was 0.18ng/mL.The addition recovery is between 96%-106%.The results determinated by proposed method were consistent with those obtained by inductively coupled plasma atomic emission spectrometry(ICP-AES) with relative standard deviation(RSD,n=11) less than 10%.
Key concepts: Hydride, Selenium, Hydrochloric acid, Chemistry, Bismuth, Reagent, Detection limit, Nitric acid