Determination of antimony in fluorspar by hydride generation-atomic fluorescence spectrometry
JIN Yu2, LIU Shu*1, LI Chen1 , LIN Miao*2
1. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China; 2. College of Chemistry, Chemical Engineering and Biotechnology, Key Laboratory of Science and Technology of Eco-Textile, Ministry of Education, Donghua University, Shanghai 201620, China
Abstract：A new method was described for the determination of total antimony in fluorspar by hydride generation-atomic fluorescence spectrometry. The samples were dissolved in HNO3+HF+HClO4 mixed acid. Through heating until fumes of perchloric acid disappearing, system acidity was controlled and F- in the sample solution was removed. L-cysteine was added under 60 ℃ for 30 min to pre-reduce Sb from the pentavalent state to the trivalent state. The results indicated that F- could not interfere with the fluorescence signals of Sb but could significantly interfere with the fluorescence signals of Sb, i.e., it would interfere with the determination of total antimony. Even after the addition of L-cysteine or thiourea-ascorbic acid, the interference of F- in the determination of total antimony still could not be eliminated. The detection limit was 0.024 μg/L. Six different fluorspar samples were determined. The relative standard deviations (RSDs) were 3.3%-8.0% (n=6).
金宇, 刘曙, 李晨, 林苗. 氢化物发生-原子荧光光谱法测定氟石中锑[J]. 冶金分析, 2014, 34(5): 64-67.
JIN Yu, LIU Shu, LI Chen , LIN Miao. Determination of antimony in fluorspar by hydride generation-atomic fluorescence spectrometry. , 2014, 34(5): 64-67.
