Herrero M A, Atienza J, Maquieira A, Puchades R
Department of Chemistry, Polytechnic University of Valencia, Spain.
Analyst. 1992 Jun;117(6):1019-24. doi: 10.1039/an9921701019.
Flow injection procedures for the determination of calcium, phosphate and chloride ions in milk samples are described. The reactions are based on the formation of coloured complexes and their spectrophotometric monitoring. A sample pre-treatment with acetate buffer was carried out owing to the complexity of the sample matrix. For chloride, a rapid and reliable automated procedure for direct measurement of its content in milk (using a dialyser to eliminate interferences) is also described. After optimizing the sample pre-treatment and flow injection variables, the procedures were applied to commercial milk; the results obtained agreed satisfactorily with those of the reference methods. With 50 mm3 samples, a working range of 0-15 ppm for calcium, 50-150 ppm for phosphate and 5-100 ppm for chloride is covered with a precision of better than 1.1%. The sample throughput was higher than 50 samples h-1. These preliminary experiments are the basis for the automation of the determination of calcium, phosphate and chloride ions using a computer-controlled, self-designed and laboratory-built autoanalyser.
本文描述了用于测定牛奶样品中钙、磷和氯离子的流动注射程序。这些反应基于有色络合物的形成及其分光光度监测。由于样品基质的复杂性,采用醋酸盐缓冲液进行了样品预处理。对于氯离子,还描述了一种快速可靠的直接测定牛奶中氯离子含量的自动化程序(使用透析器消除干扰)。在优化样品预处理和流动注射变量后,将这些程序应用于市售牛奶;所得结果与参考方法的结果令人满意地一致。对于50立方毫米的样品,钙的工作范围为0 - 15 ppm,磷为50 - 150 ppm,氯为5 - 100 ppm,精密度优于1.1%。样品通量高于50个样品/小时。这些初步实验是使用计算机控制、自行设计并在实验室构建的自动分析仪实现钙、磷和氯离子测定自动化的基础。