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Liquid Chromatographic Arsenic Speciation with Gas-Phase Chemiluminescence Detection

机译:气相色谱化学发光检测液相色谱砷形态

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摘要

We present a newly developed gas-phase chemiluminescence (CL) detection method for the separation and quantification of inorganic and organic arsenic species. Arsenite, arsenate, dimethylarsinic acid (DMA), and monomethylarsonic acid (MMA) were separated by anion exchange using carbonate-bicarbonate and NaOH eluents with step-gradient elution. The separated species were passed through a UV photooxidation reactor which decomposed the organic species and converted them to inorganic As(V). Subsequent on-line hydride generation with acid and sodium borohydride produces ASH3 and H2, which are separated from the liquid in a gas—liquid separator. The produced ASH3, driven by H2, reacts with ozone in a small reflective cell located atop a photomul-tiplier tube, resulting in intense CL. In the present form, the limits of detection (LODs, signal-to-noise = 3), based on peak height, for arsenite, arsenate, MMA, and DMA are 0.4, 0.2, 0.5, and 0.3 mu g/L, respectively, for a 100 mu L injected sample. This analyzer demonstrates the robustness of the CL detection system for arsenic and provides an affordable alternative to atomic spectrometry for use as a detector after chromatographic speciation. We found no significant practical interferences.
机译:我们提出了一种新开发的气相化学发光(CL)检测方法,用于无机和有机砷物种的分离和定量。使用碳酸氢盐-碳酸氢盐和NaOH洗脱液通过逐步梯度洗脱进行阴离子交换,分离出亚砷酸盐,砷酸盐,二甲基砷酸(DMA)和一甲基砷酸(MMA)。分离出的物质通过紫外光氧化反应器,该反应器将有机物质分解并将其转化为无机As(V)。随后用酸和硼氢化钠在线生成氢化物,生成ASH3和H2,它们在气液分离器中与液体分离。由H2驱动的生成的ASH3与臭氧在光敏管顶部的小反射池中与臭氧反应,从而导致强烈的CL。在当前形式下,基于峰高的亚砷酸盐,砷酸盐,MMA和DMA的检出限(LOD,信噪比= 3)分别为0.4、0.2、0.5和0.3μg / L ,用于100 µL进样样品。该分析仪证明了CL检测系统对砷的耐用性,并为色谱分析后用作检测器的原子光谱法提供了一种经济实惠的替代方法。我们发现没有重大的实际干扰。

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