光谱学与光谱分析, 2012, 32 (5): 1397, 网络出版: 2012-06-14  

纳米二氧化钛胶体分离富集-氢化物原子荧光光谱法测定水中超痕量锗

Preconcentration of Ultra-Trace Germanium in Water Samples with Nano-Sized TiO2 Colloid and Determination by HGAFS with Colloid Sampling
作者单位
武汉大学资源与环境科学学院, 生物质资源化学与环境生物技术湖北省重点实验室, 湖北 武汉430079
摘要
提出了用纳米TiO2胶体富集, 氢化物原子荧光光谱法测定水样中超痕量锗的新方法。 当溶液的pH为6.0~8.0时, 纳米TiO2胶体对Ge((Ⅳ)吸附率为97.0~99.0%, 并且吸附速度快。 利用纳米TiO2胶体良好的吸附性能对水样中超痕量Ge((Ⅳ)进行富集, 离心后, 弃去上清液, 用少量盐酸将富集了Ge((Ⅳ)的沉积物(纳米二氧化钛)转化成胶体, 用氢化物原子荧光光谱法直接测定胶体中的锗。 该法检出限(3σ)低(0.060 μg·L-1), 精密度好(相对标准偏差(RSD)为2.0%), 简单、 快速(省去了繁琐的过滤和脱附过程), 用于实际水样中超痕量锗的测定, 结果满意。
Abstract
A novel method for preconcentration of ultra-trace germanium and determination by hydride generation atomic fluorescence spectrometry (HGAFS) was presented in this work. When the pH values of solution were 6.0~8.0, the adsorption efficiency of nano-sized TiO2 colloid for germanium was 97.0%~99.0% in a short time. Nano-sized TiO2 colloid was used to concentrate the ultra-trace germanium in water sample due to its high absorption capacity. After centrifugation, the supernatant fluid was removed. The sediment which contained the concentrated Ge(Ⅳ) was inverted to colloid by adding HCl of certain concentration. Ge(Ⅳ) in colloid was directly determined by HGAFS. The proposed method possesses low detection limit (3σ) (0.060 μg·L-1) and good precision (the relative standard deviation (RSD) is 2.0%, n=6). The method is was also quite simple and time saving (without any filtration and desorption process). Satisfactory results were obtained when applying this method to the determination of ultra-trace germanium in water samples.

钱沙华, 鲁敏, 张旭. 纳米二氧化钛胶体分离富集-氢化物原子荧光光谱法测定水中超痕量锗[J]. 光谱学与光谱分析, 2012, 32(5): 1397. QIAN Sha-hua, LU Min, ZHANG Xu. Preconcentration of Ultra-Trace Germanium in Water Samples with Nano-Sized TiO2 Colloid and Determination by HGAFS with Colloid Sampling[J]. Spectroscopy and Spectral Analysis, 2012, 32(5): 1397.

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