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利用甲酸产生的羰基化合物,通过原子荧光光谱法对镍进行灵敏测定。

UV-induced carbonyl generation with formic acid for sensitive determination of nickel by atomic fluorescence spectrometry.

机构信息

College of Chemistry, Sichuan University, Chengdu, Sichuan 610064, China.

出版信息

Talanta. 2010 Jan 15;80(3):1239-44. doi: 10.1016/j.talanta.2009.09.016.

Abstract

UV-induced carbonyl generation with formic acid is used for gaseous sample introduction into an atomic fluorescence spectrometer for the determination of ultra-trace nickel. Compared with conventional carbonyl generation, no toxic gas CO is involved in this work, and volatile Ni(CO)(4) is generated with a single reagent formic acid under the irradiation of UV light (253.7nm, 15W). The reaction conditions, including reaction medium, UV irradiation time and reaction temperature, are optimized for the best signal. Under the optimized conditions, a limit of detection of 10ngL(-1) for nickel is obtained without any analyte-pre-concentration, which is comparable to that using in situ trapping technique. Interferences from common transition metal ions, noble metal ions and mineral acids are also investigated. The proposed method is applied to the analysis of three certified reference materials and two organic acid samples for trace nickel, with analytical results in good agreement with certified values or those obtained by electrothermal atomic absorption spectrometry. This is a simple, fairly green and highly sensitive method for ultra-trace nickel determination.

摘要

利用甲酸诱导羰基生成,将其应用于原子荧光光谱仪中的气体进样技术,用于测定痕量镍。与传统的羰基生成法相比,本工作不涉及有毒气体 CO,而是在 253.7nm、15W 的紫外光照射下,仅使用单一试剂甲酸即可生成挥发性 Ni(CO)(4)。对反应条件(包括反应介质、UV 照射时间和反应温度)进行了优化,以获得最佳信号。在最佳条件下,无需任何预浓缩,镍的检出限可达 10ngL(-1),与使用原位捕集技术相当。还研究了常见过渡金属离子、贵金属离子和矿物酸的干扰。该方法用于三种认证参考物质和两种有机酸样品中痕量镍的分析,分析结果与认证值或电热原子吸收光谱法的结果吻合良好。这是一种简单、绿色、高灵敏度的痕量镍测定方法。

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