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On-line coupling of capillary electrophoresis to hydride generation atomic fluorescence spectrometry for arsenic speciation analysis

机译:毛细管电泳与氢化物发生原子荧光光谱的在线耦合,用于砷形态分析

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A novel hyphenated technique, on-line coupling of capillary electrophoresis (CE) to atomic fluorescence spectrometry (AFS), was developed for speciation analysis of four environmentally significant and toxic forms of arsenic: arsenite, arsenate, monomethylarsenic acid, and dimethylarsenic acid. Baseline separation of the four arsenic species was achieved by capillary electrophoresis in a 50 cm x 100 mum W. fused-silica capillary at 20 kV and using a 20 mmol L-1 phosphate buffer (pH 6.5). A hydride generation (HG) technique was employed to convert the arsenic species from the CE effluent into their respective hydrides. The CE-AFS interface was constructed on the basis of a cross design for introducing a sheath flow around the CE capillary and a Pt electrode, which provided an electrical connection for stable electrophoretic separations and allowed on-line volatile hydride formation. A laboratory-made gas-liquid separator was used to isolate the generated volatile species from the reaction mixture solution, and an argon flow was used to transport the volatile hydrides into the atomizer of AFS for on-line detection. The precision (RSD, n = 7) ranged from 2.1 to 3.1% for migration time, from 2.8 to 4.2% for peak area response, and from 2.0 to 4.1% for peak height response for the arsenic species at the 1 mg L-1 (as As) level. The detection limits were in the range of 9-18 mug L-1 (as As). The recoveries of the four arsenic species in locally collected water samples and urine sample ranged from 91 to 115%. The developed technique was successfully applied to the speciation of the water-methanol extractable arsenic in a sediment sample. [References: 42]
机译:开发了一种新的联用技术,将毛细管电泳(CE)与原子荧光光谱(AFS)在线耦合,用于对四种对环境具有重大影响和毒性的砷形态进行形态分析:亚砷酸盐,砷酸盐,一甲基砷酸和二甲基砷酸。通过在20 kV的50 cm x 100 m W. W.熔融石英毛细管中进行毛细管电泳,并使用20 mmol L-1磷酸盐缓冲液(pH 6.5)进行四种砷的基线分离。采用氢化物发生(HG)技术将CE废水中的砷物质转化为它们各自的氢化物。 CE-AFS接口是基于用于在CE毛细管和Pt电极周围引入鞘流的交叉设计而构建的,该交叉设计为稳定的电泳分离提供了电连接,并允许在线形成挥发性氢化物。使用实验室制造的气液分离器从反应混合物溶液中分离出生成的挥发性物质,并使用氩气流将挥发性氢化物传输到AFS雾化器中以进行在线检测。对于1 mg L-1的砷,迁移时间的精度(RSD,n = 7)为2.1至3.1%,峰面积响应为2.8至4.2%,峰高响应为2.0至4.1%。 (以As级别)。检出限在9-18马克杯L-1(以As计)范围内。当地收集的水样和尿样中四种砷的回收率在91%至115%之间。这项开发的技术已成功应用于沉积物样品中水-甲醇可萃取砷的形态分析。 [参考:42]

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