Zaijun Li, Jiaomai Pan, Jian Tang
College of Chemical and Material Engineering, Southern Yangtze University, Wuxi 214036, China.
Anal Bioanal Chem. 2002 Nov;374(6):1125-31. doi: 10.1007/s00216-002-1574-6. Epub 2002 Oct 18.
A new highly sensitive and selective chromogenic reagent, p-carboxyphenylfluorone (p-CPF), was studied for spectrophotometric determination of trace molybdenum. In 0.36 mol L(-1)phosphoric acid medium, p-CPF reacts with molybdenum(VI) to form a 1:3 red complex, which has a sensitive absorption peak at 531 nm. Under optimal conditions, the reaction of molybdenum(VI) with p-CPF completed rapidly and absorbance remains almost constant for at least 24 h. Molybdenum(VI) obeyed Beer's law in the range 0-2.0 microg mL(-1); the apparent molar absorption coefficient, Sandell's sensitivity and the limit of detection were found to be 1.03 x 10(5) L mol(-1) cm(-1), 1.028 ng cm(-2)and 0.73 ng mL(-1) respectively; the effect of various foreign ions were examined in detail. It was found that most coexisting ions can be tolerated in considerable amounts, especially 800 mg of Mn(II), 200 mg of Mg(II), Fe(II), Co(III), Ni(II) and Cd(II), 50 mg of Ca(II) and Al(III), 25 mg of Cu(II) and Fe(III), 10 mg of Hg (II), La(III), Bi(III), Pb(II) and Zn(II) don't interfere with the determination of molybdenum(VI). The proposed method is very simple, sensitive and selective, it has been applied to determine molybdenum in vegetable and food samples with a very high precision and accuracy. Moreover, the synthesis of the reagent and the conditions of the colour reaction were also studied in detail.
研究了一种新型高灵敏度和高选择性的显色剂对羧基苯基荧光酮(p-CPF),用于分光光度法测定痕量钼。在0.36 mol L(-1)磷酸介质中,p-CPF与钼(VI)反应形成1:3的红色络合物,该络合物在531 nm处有一个灵敏的吸收峰。在最佳条件下,钼(VI)与p-CPF的反应迅速完成,吸光度至少在24 h内保持几乎恒定。钼(VI)在0 - 2.0 μg mL(-1)范围内符合比尔定律;其表观摩尔吸收系数、桑德尔灵敏度和检测限分别为1.03×10(5) L mol(-1) cm(-1)、1.028 ng cm(-2)和0.73 ng mL(-1);详细考察了各种外来离子的影响。结果表明,大多数共存离子能大量容忍,特别是800 mg的Mn(II)、200 mg的Mg(II)、Fe(II)、Co(III)、Ni(II)和Cd(II)、50 mg的Ca(II)和Al(III)、25 mg的Cu(II)和Fe(III)、10 mg的Hg (II)、La(III)、Bi(III)、Pb(II)和Zn(II)不干扰钼(VI)的测定。所提出的方法非常简单、灵敏且具有选择性,已用于测定蔬菜和食品样品中的钼,具有很高的精密度和准确度。此外,还详细研究了该试剂的合成及显色反应条件。