Analytical Chemistry Laboratory, Department of Chemistry, Shivaji University, Maharashtra, India.
Talanta. 2010 May 15;81(3):1088-95. doi: 10.1016/j.talanta.2010.02.002. Epub 2010 Feb 6.
Synergistic liquid-liquid extractive spectrophotometric determination of gold(III) using 1-(2',4'-dinitro aminophenyl)-4,4,6-trimethyl-1,4-dihydro pyrimidine-2-thiol [2',4'-dinitro APTPT] has been described. Equal volumes (5cm(3)) of the 2',4'-dinitro APTPT (0.02molL(-1)) in the presence of pyridine (0.5molL(-1)) form an orange-red coloured ternary complex with gold(III) of molar ratio 1:1:1 at pH 1.8-2.4 with 5min of shaking. The absorbance of coloured organic layer in 1,2-dichloroethane is measured spectrophotometrically at 445nm against reagent blank. A pronounced synergism has been observed by the binary mixture of 2',4'-dinitro APTPT and pyridine, which shows that the enhancement in the absorbance is observed in the presence of pyridine by the adduct formation in the organic phase. Beer's law was obeyed in the concentration range 2.5-20.0microgmL(-1), with molar absorptivity and Sandell's sensitivity values of 8.7x10(3)dm(3)mol(-1)cm(-1) and 0.023microgcm(-2) respectively. A repetition of the method was checked by finding relative standard deviation (R.S.D.) (n=10) which was 0.17%. The composition of the gold(III)-2',4'-dinitro APTPT-pyridine adduct was established by slope analysis, molar ratio and Job's method. The ternary complex was stable for more than 48h. The influence of various factors such as pH, 2',4'-dinitro APTPT concentration, solvent and pyridine on the degree of complexation has been established. A number of foreign ions tested for their interferences and use of suitable masking agents wherever necessary are tabulated, which show that selectivity of the method has been enhanced. The method is successfully employed for the determination of gold(III) in binary, synthetic mixtures and ayurvedic samples. The reliability of the method is assured by inter-comparison of experimental values, using an atomic absorption spectrometer.
本文描述了一种利用 1-(2',4'-二硝基氨基苯基)-4,4,6-三甲基-1,4-二氢嘧啶-2-硫醇[2',4'-二硝基 APTPT]协同液-液萃取分光光度法测定金(III)的方法。在 pH 1.8-2.4 下,将 5cm³体积相等的 2',4'-二硝基 APTPT(0.02molL⁻¹)与吡啶(0.5molL⁻¹)混合 5 分钟,可形成摩尔比为 1:1:1 的橙色-红色三元配合物。在 1,2-二氯乙烷中测量有色有机层的吸光度,以试剂空白为参比,在 445nm 处进行分光光度法测定。通过 2',4'-二硝基 APTPT 和吡啶的二元混合物观察到明显的协同作用,这表明在吡啶存在下,通过有机相中的加合物形成观察到吸光度增强。在 2.5-20.0μgmL⁻¹的浓度范围内,比尔定律得到遵守,摩尔吸光率和桑德尔灵敏度值分别为 8.7x10³ dm³mol⁻¹cm⁻¹和 0.023μgcm⁻²。通过发现相对标准偏差(R.S.D.)(n=10)为 0.17%来检查方法的重复性。通过斜率分析、摩尔比和乔布法确定了金(III)-2',4'-二硝基 APTPT-吡啶加合物的组成。三元配合物在超过 48 小时内稳定。确定了 pH、2',4'-二硝基 APTPT 浓度、溶剂和吡啶等各种因素对配合程度的影响。列出了对各种外来离子的干扰测试以及在必要时使用适当掩蔽剂的情况,表明该方法的选择性得到了提高。该方法成功地用于二元、合成混合物和阿育吠陀样品中金(III)的测定。通过与原子吸收光谱仪进行实验值的比较,确保了方法的可靠性。