中空纤维液相微萃取结合全反射 X 射线荧光光谱法测定水中痕量无机砷形态。
Hollow fiber liquid phase microextraction combined with total reflection X-ray fluorescence spectrometry for the determination of trace level inorganic arsenic species in waters.
机构信息
Department of Chemistry, University of Girona, Campus Montilivi, s/n. 17071, Girona, Spain; Department of Geology & Geophysics, Texas A&M University, College Station, TX, 77843-3115, USA; Departmental of Environmental Management, International Centre for Ecological Engineering, University of Kalyani, Kalyani, 741 235, West Bengal, India; Department of Chemistry, University of Kalyani, Kalyani, 741 235, West Bengal, India.
Department of Chemistry, University of Girona, Campus Montilivi, s/n. 17071, Girona, Spain.
出版信息
Talanta. 2020 Sep 1;217:121005. doi: 10.1016/j.talanta.2020.121005. Epub 2020 Apr 13.
In the present study, we investigated the possibilities and drawbacks of hollow fiber liquid phase microextraction (HF-LPME) combined with total reflection X-ray fluorescence (TXRF) spectrometry for the determination of low amounts of inorganic arsenic (As) species in water samples. The obtained results showed that a three-phase HF-LPME system was more suitable to be used in combination with TXRF than the two phase configuration, since lower detection limit and better precision for As determination can be attained. Relevant experimental parameters affecting As extraction (i.e. types of extractant, organic solvent, agitation speed, pH and extraction time) and TXRF analysis (deposition volume and drying mode) were systematically evaluated. It was found that As(III) was more efficiently extracted at pH 13, whereas, optimum pH for As(V) extraction was at pH 8.5. Limits of detection (LOD) achieved using the best analytical conditions meet the requirements of current legislation and allow the determination of inorganic As(V) and As(III) in water. The proposed method was also applied to different spiked environmental water samples for the preconcentration and subsequent determination of trace inorganic As species.
在本研究中，我们研究了中空纤维液相微萃取（HF-LPME）与全反射 X 射线荧光光谱法（TXRF）相结合测定水样中低浓度无机砷（As）形态的可能性和缺点。结果表明，三相 HF-LPME 系统比两相配置更适合与 TXRF 结合使用，因为可以获得更低的检测限和更好的 As 测定精密度。系统评估了影响 As 萃取（即萃取剂类型、有机溶剂、搅拌速度、pH 值和萃取时间）和 TXRF 分析（沉积量和干燥模式）的相关实验参数。结果发现，在 pH 13 下，As(III)的萃取效率更高，而 As(V)的最佳萃取 pH 值为 8.5。使用最佳分析条件可达到的检测限（LOD）符合当前法规的要求，可用于测定水中的无机 As(V)和 As(III)。该方法还应用于不同加标环境水样中痕量无机 As 形态的预浓缩和随后测定。
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