Spectrophotometric determination of phosphite in fertilizers in a flow injection system with online sample preparation

José Anchieta Gomes Neto, Helenice Akemi Ito, Kelly das Graças Fernandes, Mercedes de Moraes, Arnaldo Alves Cardoso
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引用次数: 8

Abstract

A flow injection system with online sample preparation is proposed for the determination of phosphite in liquid fertilizers by spectrophotometry. After loop-based injection, phosphite is oxidized by an acidic permanganate solution (1.0 10−2 mol L−1 KMnO4 + 1.0 mol L−1 H2SO4) in a heated reactor (50 °C). The phosphate generated is then determined by the molybdenum blue method. Influence of flow rates, temperature, and concentration and order of addition of reagents, sample volume, and reactor configuration for the blue complex formation on recorded signals were investigated. The flow system was applied to phosphite determination in commercial samples of liquid fertilizers. The proposed system handles about 80 samples per hour [0.05–0.40% (w/v) H3PO3; R = 0,9998), consuming about 80 μL sample, 1 mg KMnO4, 25 mg (NH4)6Mo7O24, and 10 mg ascorbic acid per determination. Results are precise [relative standard deviation ≤ 3.5% for 0.1% (w/v) H3PO3, n = 12] and in agreement with those obtained by gravimetry at 95% confidence level. © 2000 John Wiley & Sons, Inc. Lab Robotics and Automation 12:286–290, 2000

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流动注射系统在线制样分光光度法测定肥料中的亚硝酸盐
提出了一种在线制样的流动注射系统,用于分光光度法测定液体肥料中的亚磷酸盐。循环注入后,在加热反应器(50℃)中,用酸性高锰酸盐溶液(1.0 mol L L−1 KMnO4 + 1.0 mol L−1 H2SO4)氧化亚磷酸酯。然后用钼蓝法测定生成的磷酸盐。研究了蓝色络合物形成的流速、温度、浓度和添加试剂的顺序、样本量和反应器配置对记录信号的影响。将该流动系统应用于液体肥料中亚磷酸盐的测定。该系统每小时处理约80个样品[0.05-0.40% (w/v) H3PO3;R = 0,9998),每次测定消耗约80 μL样品,KMnO4 1 mg, (NH4)6Mo7O24 25 mg,抗坏血酸10 mg。结果精确[0.1% (w/v) H3PO3, n = 12的相对标准偏差≤3.5%],在95%置信水平上与重力法得到的结果一致。©2000 John Wiley &儿子,Inc。实验室机器人与自动化,2000:286 - 290
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