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一种用于阀上实验室中灵敏测定镉的微型光发射光谱系统。

A miniature optical emission spectrometric system in a lab-on-valve for sensitive determination of cadmium.

作者信息

Zhang Ya-Jie, Cai Yi, Yu Yong-Liang, Wang Jian-Hua

机构信息

Research Center for Analytical Sciences, College of Sciences, Northeastern University, Box 332, Shenyang 110819, China.

Research Center for Analytical Sciences, College of Sciences, Northeastern University, Box 332, Shenyang 110819, China.

出版信息

Anal Chim Acta. 2017 Jul 11;976:45-51. doi: 10.1016/j.aca.2017.04.055. Epub 2017 May 13.

Abstract

A miniature optical emission spectrometric (OES) system is developed by incorporating dielectric barrier discharge (DBD) microplasma as excitation source in a lab-on-valve (LOV) configuration for trace cadmium analysis. The entire system integrates bead injection (BI) sample pretreatment, post-column derivatization, in-situ nebulization and OES detection. Trace cadmium in sample solution is separated and preconcentrated by flowing through a 2-(5-Br-2-pyridylazo)-5-dethylaminophenol (5-Br-PADAP) loaded microcolumn in LOV, followed by elution with 20 μL of 0.1 M hydrochloric acid. The eluate after online derivatization with 5 μL of 0.2 M borate buffer solution containing 7.5% (v/v) ethanol is immediately transported into a pneumatic micronebulizer integrating DBD microplasma for cadmium excitation, and OES is recorded by using a charge coupled device (CCD) spectrometer. As a miniaturized analytical set-up, LOV provides an ideal sample-processing front-end with detection by DBD-OES, while introduction of DBD excitation source in LOV highly improves the analytical performances for trace metal species. With a sample volume of 1.0 mL, a detection limit of 0.06 μg L and a linear range of 0.2-50 μg L are achieved for cadmium, along with an enrichment factor of 38. The accuracy of the present system is confirmed by the determination of cadmium in certified reference materials, and further demonstrated by spiking recoveries of cadmium in real water samples.

摘要

通过将介质阻挡放电(DBD)微等离子体作为激发源整合到阀上实验室(LOV)配置中,开发了一种用于痕量镉分析的微型光发射光谱(OES)系统。整个系统集成了微珠进样(BI)样品预处理、柱后衍生、原位雾化和OES检测。样品溶液中的痕量镉通过在LOV中流经填充有2-(5-溴-2-吡啶偶氮)-5-二乙氨基苯酚(5-Br-PADAP)的微柱进行分离和预富集,然后用20 μL 0.1 M盐酸洗脱。用5 μL含7.5%(v/v)乙醇的0.2 M硼酸盐缓冲溶液进行在线衍生后的洗脱液立即被输送到集成DBD微等离子体的气动微型雾化器中进行镉激发,并用电荷耦合器件(CCD)光谱仪记录OES。作为一种小型化分析装置,LOV提供了一个理想的样品处理前端,并通过DBD-OES进行检测,而在LOV中引入DBD激发源极大地提高了痕量金属物种的分析性能。对于镉,在进样量为1.0 mL时,检测限为0.06 μg/L,线性范围为0.2 - 50 μg/L,富集因子为38。通过对标准参考物质中镉的测定证实了本系统的准确性,并通过对实际水样中镉的加标回收率进一步证明。

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