Akl M A, Khalifa M E, Ghazy S E, Hassanien M M
Chemistry Department, Faculty of Science, Mansoura University 35516, PO. Box 70, Mansoura, Egypt.
Anal Sci. 2002 Nov;18(11):1235-40. doi: 10.2116/analsci.18.1235.
A simple, selective and sensitive procedure is described for the preconcentration by flotation followed by spectrophotometric determination of trace amounts of Cd(II). Cadmium forms an intense red 1:2 complex with phenanthraquinone monophenylthiosemicarbazone (PPT) at pH > or = 6. The colored Cd-PPT complex was floated quantitatively with oleic acid (HOL) surfactant at pH 6.5, exhibiting maximum absorbance at 520 nm and having a molar absorptivity of 2.4 x 10(5) L mol(-1) cm(-1). The stability constant of the formed complex is 1.5 x 10(12); log K = 12.2. Beer's law was obeyed over the concentration range 0.01-0.34 mg/L. The Sandell sensitivity and relative standard deviation are 0.4 ng/cm2 and 2.6%, respectively. The results obtained spectrophotometrically were compared to those obtained by AAS analysis. The analytical parameters affecting flotation and hence determination have been thoroughly investigated. The proposed procedure was successfully applied to the determination of Cd(II) traces in certified and real human hair samples as well as in natural waters. The structure of the complex formed and the mechanism of flotation were proposed.
描述了一种简单、选择性好且灵敏的方法,用于通过浮选预富集,随后分光光度法测定痕量镉(II)。镉在pH≥6时与菲醌单苯基硫代半卡巴腙(PPT)形成强烈的红色1:2络合物。在pH 6.5时,有色的Cd-PPT络合物与油酸(HOL)表面活性剂定量浮选,在520 nm处呈现最大吸光度,摩尔吸光系数为2.4×10⁵ L mol⁻¹ cm⁻¹。形成的络合物的稳定常数为1.5×10¹²;log K = 12.2。在0.01 - 0.34 mg/L的浓度范围内符合比尔定律。桑德尔灵敏度和相对标准偏差分别为0.4 ng/cm²和2.6%。将分光光度法获得的结果与原子吸收光谱(AAS)分析获得的结果进行了比较。对影响浮选进而影响测定的分析参数进行了全面研究。所提出的方法成功应用于认证的和实际的人发样品以及天然水中痕量镉(II)的测定。提出了形成的络合物的结构和浮选机理。