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Feasibility of measuring Cr(III) and Cr(VI) in water by laser-induced breakdown spectroscopy using ceramics as the solid support
Microchemical Journal ( IF 4.8 ) Pub Date : 2019-01-01 , DOI: 10.1016/j.microc.2018.08.031
Alexandrina A.C. Carvalho , Daniel M. Silvestre , Flávio O. Leme , Juliana Naozuka , Danielle P. Intima , Cassiana S. Nomura

Abstract Laser-induced breakdown spectroscopy (LIBS) is a multi-elemental technique with multiple advantages. However, direct determination in liquid samples is not an easy task since laser water interaction can affect the precision and accuracy of the method and cause loss of sensitivity. To enable LIBS application in liquid sample analysis, some strategies such as liquid-to-solid transfer have been used. This work proposes the quantification of chromium in water samples by LIBS using ceramic as the solid support. Results showed that the ceramic selectively adsorbs Cr(III) species at pH 7 and quantification of Cr(VI) species by LIBS was also possible after reduction of this species to Cr(III) using Fe(II) as the reducing agent. Instrumental parameters were optimized, and the best conditions found included a 65 μm spot size, 430 accumulated pulses with 20 mJ pulse−1, and 0.75 ms of delay time. Calibration was carried out with synthetic calibration standards prepared by adsorption of increasing concentrations of chromium in ceramic. Tap water samples spiked with 0.9 mg L−1 of Cr(III) and 0.1 mg L−1 of Cr(VI) were analysed by the proposed method and recoveries of 105 ± 2% and 103 ± 3% were obtained for Cr(III) and Cr(VI), respectively.

中文翻译:

以陶瓷为固体载体,通过激光诱导击穿光谱法测量水中 Cr(III) 和 Cr(VI) 的可行性

摘要 激光诱导击穿光谱(LIBS)是一种具有多种优势的多元素技术。然而,直接测定液体样品并非易事,因为激光水相互作用会影响方法的精密度和准确度并导致灵敏度损失。为了在液体样品分析中实现 LIBS 应用,已经使用了一些策略,例如液体到固体的转移。这项工作提出了使用陶瓷作为固体载体通过 LIBS 对水样中的铬进行定量。结果表明,陶瓷在 pH 值为 7 时选择性吸附 Cr(III) 物质,并且在使用 Fe(II) 作为还原剂将该物质还原为 Cr(III) 后,还可以通过 LIBS 对 Cr(VI) 物质进行定量。仪器参数得到优化,发现的最佳条件包括 65 μm 光斑尺寸,430 个累积脉冲,20 mJ 脉冲-1,延迟时间为 0.75 毫秒。使用合成校准标准进行校准,该标准通过在陶瓷中吸附增加浓度的铬而制备。通过建议的方法分析了添加 0.9 mg L-1 Cr(III) 和 0.1 mg L-1 Cr(VI) 的自来水样品,获得了 105 ± 2% 和 103 ± 3% 的 Cr(III) 回收率) 和 Cr(VI)。
更新日期:2019-01-01
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