Sözgen Kevser, Tütem Esma
Faculty of Engineering, Istanbul University, Avcilar, 34320 Istanbul, Turkey.
Talanta. 2004 Apr 19;62(5):971-6. doi: 10.1016/j.talanta.2003.10.020.
A simple, sensitive and rapid derivative spectrophotometric method using 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) has been developed for simultaneous determination of Co(II), Ni(II) and Fe(II) which have very similar chemical behavior and appear together in many real samples. The complexes of all these metal ions with 5-Br-PADAP were formed immediately at pH 7.0 ammonium acetate buffered solution and were stable for at least 24h. Second derivative spectra were selected for evaluation, because working wavelength determination was more precise and spectral overlap was less than in the ordinary and first derivative spectra. Three wavelengths at which the complexes exhibit extremum (2)D values for Co(II), Ni(II) and Fe(II) were selected as analytical wavelengths, i.e., 640, 600 and 740nm, respectively. Calibration curves drawn with zero-to-peak values at mentioned wavelengths were linear between 80 and 2000ngml(-1) for each metal ion. Concentrations of Co(II) and Ni(II) were calculated from the total (2)D values and the sum of the linear equations for these three cations at 640 and 600nm, after Fe(II) assay by making use of the (2)D value at 740nm. Limits of detection (LOD) for Co(II), Ni(II) and Fe(II) were 2.7, 13.9 and 3.0ngml(-1), respectively. The method has been applied to tool steel and heater resistance wire samples successfully.
已开发出一种使用2-(5-溴-2-吡啶偶氮)-5-二乙氨基苯酚(5-Br-PADAP)的简单、灵敏且快速的导数分光光度法,用于同时测定化学行为非常相似且在许多实际样品中同时出现的Co(II)、Ni(II)和Fe(II)。所有这些金属离子与5-Br-PADAP的络合物在pH 7.0的醋酸铵缓冲溶液中立即形成,并且至少稳定24小时。选择二阶导数光谱进行评估,因为工作波长的测定更精确,且光谱重叠比普通光谱和一阶导数光谱要小。选择Co(II)、Ni(II)和Fe(II)的络合物表现出极值(2)D值的三个波长作为分析波长,即分别为640、600和740nm。在上述波长下以零到峰值绘制的校准曲线对于每种金属离子在80至2000ngml(-1)之间呈线性。利用740nm处的(2)D值测定Fe(II)后,根据总(2)D值以及这三种阳离子在640和600nm处线性方程的总和计算Co(II)和Ni(II)的浓度。Co(II)、Ni(II)和Fe(II)的检测限(LOD)分别为2.7、13.9和3.0ngml(-1)。该方法已成功应用于工具钢和加热电阻丝样品。