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用于环境水样中溴化物和溴酸盐筛查的微型介质阻挡放电-光发射光谱系统的研制。

Development of a miniature dielectric barrier discharge-optical emission spectrometric system for bromide and bromate screening in environmental water samples.

作者信息

Yu Yong-Liang, Cai Yi, Chen Ming-Li, Wang Jian-Hua

机构信息

Department of Chemistry, 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.

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

出版信息

Anal Chim Acta. 2014 Jan 27;809:30-6. doi: 10.1016/j.aca.2013.11.054. Epub 2013 Dec 6.

Abstract

Dielectric barrier discharge (DBD) at atmospheric pressure provides an efficient radiation source for the excitation of bromine and it is used for the first time for optical emission spectrometric (OES) detection of bromide and bromate. A portable DBD-OES system is developed for screening potential pollution from bromide and bromate in environmental waters. Bromide is on-line oxidized to bromine for in-situ generation of volatile bromine. Meanwhile, a helium stream carries bromine into the DBD micro-plasma for its excitation at a discharging voltage of 3.7 kV and optical emission spectrometric detection with a QE65000 charge-coupled device (CCD) spectrometer in the near-infrared spectral region. Similarly, the quantification of bromate is performed by its pre-reduction into bromide and then oxidized to bromine. The spectral characteristics and configuration of the DBD micro-plasma excitation source in addition to the oxidation vapor generation of bromine have been thoroughly investigated. With a sampling volume of 1 mL, a linear range of 0.05-10.0 mg L(-1) is obtained with a detection limit of 0.014 mg L(-1) by measuring the emission at 827 nm. A precision of 2.3% is achieved at 3 mg L(-1) bromide. The system is validated by bromine detection in certified reference material of laver (GBW10023) at mg L(-1) level, giving rise to satisfactory agreement. In addition, it is further demonstrated by screening trace bromide and bromate as well as spiking recoveries in a series of environmental water samples.

摘要

大气压下的介质阻挡放电(DBD)为溴的激发提供了一种高效的辐射源,并且首次用于溴化物和溴酸盐的光发射光谱(OES)检测。开发了一种便携式DBD-OES系统,用于筛查环境水体中溴化物和溴酸盐的潜在污染。溴化物在线氧化为溴,用于原位生成挥发性溴。同时,氦气流将溴带入DBD微等离子体中,在3.7 kV的放电电压下对其进行激发,并使用QE65000电荷耦合器件(CCD)光谱仪在近红外光谱区域进行光发射光谱检测。同样,通过将溴酸盐预还原为溴化物,然后再氧化为溴来进行定量分析。除了溴的氧化蒸气生成外,还对DBD微等离子体激发源的光谱特性和配置进行了深入研究。通过测量827 nm处的发射,在1 mL进样量下,获得了0.05-10.0 mg L⁻¹的线性范围,检测限为0.014 mg L⁻¹。在3 mg L⁻¹溴化物浓度下,精密度达到2.3%。该系统通过在紫菜(GBW10023)标准物质中mg L⁻¹水平的溴检测进行了验证,结果令人满意。此外,通过对一系列环境水样中痕量溴化物和溴酸盐的筛查以及加标回收率的测定,进一步证明了该系统的有效性。

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