Determination of silver in lead ash and lead mud by atomic absorption spectrometry after microwave digestion
ZUO Guo-qiang,LU Xin,LI Quan-min, Xu Yin-xia
1. Department of Metallurgy and Chemical Engineering, Jiyuan Vocational and Technical College,
Jiyuan 454650, China;2. Department of Chemistry, Henan Normal University, Xinxiang 453007, China
Abstract:A novel method for the determination of silver in lead ash and lead mud was established by flame atomic absorption spectrometry after microwave digestion with aqua regia and ammonium fluoride. Such experiment conditions were investigated as the influence of sample dissolution methods, digestion reagents, microwave digestion program, hydrochloric acid concentration and interfering ions on the determination. The results indicated that the digestion effect was optimum with three-step digestion program including 60 ℃ and 8 atm/1 min, 70℃ and 13 atm/2 min, 100 ℃ and 20 atm/3 min and aqua regia and ammonium fluoride as digestion reagents. Copper in lead ash and lead mud has no effect on the determination of silver. Experiment indicated that silver concentration within the range of 0.2-10 μg/mL had linear relationship with its absorbance. Detection limit of this method was 0.03 μg/mL. The proposed method was applied to the determination of lead ash and lead mud samples. The results were consistent with those obtained by conventional sample dissolution-atomic absorption spectrometry, and the relative standard deviations (RSDs, n=5) were 1.1%-1.3%.
左国强,卢 鑫,李全民,许银霞. 微波消解-火焰原子吸收光谱法测定铅烟灰和铅泥中银[J]. 冶金分析, 2012, 32(6): 43-46.
ZUO Guo-qiang,LU Xin,LI Quan-min, Xu Yin-xia. Determination of silver in lead ash and lead mud by atomic absorption spectrometry after microwave digestion. , 2012, 32(6): 43-46.