Faculty of Sciences, Department of Chemistry, University Abdelmalek Essaadi, B.P. 2121 Mhannech II, 93002 Tétouan, Morocco.
Talanta. 2013 Apr 15;108:92-102. doi: 10.1016/j.talanta.2013.02.072. Epub 2013 Mar 13.
A monolithic flow conduit was especially designed and coupled to a multisyringe unit (MSFIA) in order to develop a kinetic analytical method. The new device, denoted CHIP, integrates different functions in a reduced size including confluent mixing, reaction coil, and thermostating, which allowed minimizing the dimensions of the entire analyzer system. The CHIP-MSFIA was satisfactorily applied to the determination of iodide using the Sandell-Kolthoff reaction. The resulting system allows fast, simple and automatic analysis in seawater samples and a pharmaceutical preparation. By the use of an additional syringe, reagent blank, sample blank, unspecific interferences, and sample analyte concentration was evaluated by simply changing the mode of operation. The instrumentation and analytical procedures were optimized in respect of sensitivity. A limit of detection of 4.7 μg L(-1) and linear working range of 4.3-70 μg L(-1) were achieved. Two new modes of air bubble elimination were developed and employed in this work, leading to improved reproducibility (RSD %=1.5%) and method robustness. The accuracy of analysis for seawater samples was evaluated by an Add-Recovery test obtaining recoveries between 97 and 106%. For the quantification of iodide in the pharmaceutical sample, standard addition calibration was required. No significant differences between the found and the certified value were found. The entire analytical procedure lasted about 150 s enabling a measuring frequency of 23 h(-1).
特别设计并耦合了一个多注射器单元（MSFIA）以开发一种动力学分析方法。该新设备被命名为 CHIP，集成了不同的功能，尺寸缩小，包括汇合混合、反应盘管和恒温控制，这使得整个分析系统的尺寸最小化。CHIP-MSFIA 成功地应用于使用 Sandell-Kolthoff 反应测定碘化物。该系统允许在海水中进行快速、简单和自动的分析，以及在药物制剂中进行分析。通过使用附加的注射器，可以通过简单地改变操作模式来评估试剂空白、样品空白、非特异性干扰和样品分析物浓度。仪器和分析程序在灵敏度方面进行了优化。检测限为 4.7 μg L(-1)，线性工作范围为 4.3-70 μg L(-1)。本文开发并采用了两种新的气泡消除模式，提高了重现性（RSD %=1.5%）和方法稳健性。通过添加-回收测试评估海水样品分析的准确性，回收率在 97%至 106%之间。对于药物样品中碘化物的定量，需要进行标准添加校准。未发现发现值与认证值之间存在显著差异。整个分析过程持续约 150 秒，测量频率为 23 h(-1)。
