Santos Felisberto G, Reis Boaventura F
Centro de Energia Nuclear na Agricultura, Universidade de São Paulo, Av. Centenário, 303 São Dimas, 13400 970 Piracicaba, SP, Brazil.
J Anal Methods Chem. 2017;2017:9361460. doi: 10.1155/2017/9361460. Epub 2017 Mar 5.
A highly sensitive analytical procedure for photometric determination of molybdenum in plant materials was developed and validated. This procedure is based on the reaction of Mo(V) with thiocyanate ions (SCN) in acidic medium to form a compound that can be monitored at 474 nm and was implemented employing a multicommuted flow analysis setup. Photometric detection was performed using an LED-based photometer coupled to a flow cell with a long optical path length (200 mm) to achieve high sensitivity, allowing Mo(V) determination at a level of g L without the use of an organic solvent extraction step. After optimization of operational conditions, samples of digested plant materials were analyzed employing the proposed procedure. The accuracy was assessed by comparing the obtained results with those of a reference method, with an agreement observed at 95% confidence level. In addition, a detection limit of 9.1 g L, a linear response ( = 0.9969) over the concentration range of 50-500 g L, generation of only 3.75 mL of waste per determination, and a sampling rate of 51 determinations per hour were achieved.
开发并验证了一种用于光度法测定植物材料中钼的高灵敏度分析方法。该方法基于在酸性介质中Mo(V)与硫氰酸根离子(SCN)反应形成一种可在474nm处监测的化合物,并采用多通道流动分析装置来实施。使用基于发光二极管的光度计与具有长光程(200mm)的流通池进行光度检测以实现高灵敏度,无需使用有机溶剂萃取步骤即可测定g L水平的Mo(V)。在优化操作条件后,采用所提出的方法对消化后的植物材料样品进行分析。通过将所得结果与参考方法的结果进行比较来评估准确性,在95%置信水平下观察到一致性。此外,实现了9.1g L的检测限、50 - 500g L浓度范围内的线性响应( = 0.9969)、每次测定仅产生3.75mL废物以及每小时51次测定的采样率。