Center for Nuclear Energy in Agriculture, University of São Paulo, P.O. Box 96, 13400-970, Piracicaba, SP, Brazil.
Luiz de Queiroz College of Agriculture, University of São Paulo, Av. Pádua Dias 11, 13418-900, Piracicaba, SP, Brazil.
Talanta. 2020 Mar 1;209:120530. doi: 10.1016/j.talanta.2019.120530. Epub 2019 Nov 2.
An automatic titration setup exploiting flow analysis was proposed for the evaluation of the copper complexation capacity of highly opaque substances (milk and humic substances). The binary search approach was implemented in a flow-batch analyzer, in order to add the in-line selected titrant (e.g. copper ions) volumes to the sample. When the titration end-point was surpassed, the free metal ions catalyzed the reaction of luminol with hydrogen peroxide, yielding the chemiluminescence, which was quantified even in solutions of high opacity. Accuracy was assessed through addition/recovery tests involving classical complexing species (EDTA, DTPA and DTTC), and recoveries ranged from 96% to 115%. The proposed system requires low amounts of reagents and samples (0.42 mg of luminol, 82 μg HO, 1.10 mL of sample) per titration run, meaning ca. 12 mL of effluent per titration, and yields precise results (5% r.s.d.) at a sampling throughput of 43 h.
一种利用流动分析的自动滴定装置被提出,用于评估高度不透明物质(牛奶和腐殖质)的铜络合容量。二进制搜索方法被应用于流动批次分析仪中,以便向样品中添加在线选择的滴定剂(例如铜离子)体积。当超过滴定终点时,游离金属离子催化鲁米诺与过氧化氢的反应,产生化学发光,即使在高不透明度的溶液中也能定量检测。通过涉及经典络合物种(EDTA、DTPA 和 DTTC)的添加/回收测试来评估准确性,回收率在 96%至 115%之间。该系统每次滴定运行需要的试剂和样品量较少(每次滴定 0.42mg 鲁米诺、82μg HO、1.10mL 样品),每次滴定约消耗 12mL 流出液,在 43 小时的采样吞吐量下可获得精确的结果(5%r.s.d.)。