Universidade Federal Rural de Pernambuco, Departamento de Química, 52171-030, Recife, PE, Brazil.
Talanta. 2010 Apr 15;81(1-2):609-13. doi: 10.1016/j.talanta.2009.12.049. Epub 2010 Jan 11.
This study presents an automatic analysis system that does not require the use of standard solutions. The system uses an electrochemical flow cell for in line generation of the standards, and operates under the standard addition technique. The versatility of this system was demonstrated by the development of a one key touch fully automatic method for the determination of total available chlorine in real samples. The extremely simple, accurate and inexpensive method was based simply on the biamperometric monitoring of the well known redox reaction of chlorine with iodide ions in a flow-batch system, where the produced iodine (triiodide ions) generates an electrical current proportional to the chlorine concentration in the sample. The flow-batch parameters were optimized to maximize the sensitivity without losses on the precision of the analysis. An excellent linear dependence between the biamperometric signal and the chlorine concentration for the standard additions and a good agreement between the proposed approach and a reference method were obtained. The method was successfully applied to determine chlorine in several different bleach and chlorinated water samples (r=0.9995, LOD=8.261 x 10(-7) mol L(-1)) and could be easily extended to other oxidants and samples. Comparison to a reference method and recoveries close to 100% demonstrated the reliability of the proposed method. In addition, low residue disposal and reagent consumption, allied with high accuracy and precision, make it very promising for routine applications.
本研究提出了一种无需使用标准溶液的自动分析系统。该系统使用电化学流动池在线生成标准品,并采用标准添加技术进行操作。该系统的多功能性通过开发一种一键式全自动方法来测定实际样品中的总有效氯得到了证明。该方法极其简单、准确且廉价,仅基于在流动批处理系统中氯与碘离子的著名氧化还原反应的双安培监测,其中产生的碘(三碘离子)产生与样品中氯浓度成正比的电流。对流动批处理参数进行了优化,以在不损失分析精度的情况下最大限度地提高灵敏度。标准添加的双安培信号与氯浓度之间存在良好的线性关系,并且所提出的方法与参考方法之间具有良好的一致性。该方法成功应用于测定几种不同的漂白剂和氯化水样品中的氯(r=0.9995,LOD=8.261 x 10(-7) mol L(-1)),并且可以轻松扩展到其他氧化剂和样品。与参考方法的比较以及接近 100%的回收率证明了该方法的可靠性。此外,低残留处理和试剂消耗,以及高精度和高精准度,使其非常有前途用于常规应用。