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Trace determination of zinc in soil and vegetable samples by spectrophotometry using pyridoxal thiosemicarbazone and 2-acetyl pyridine thiosemicarbazone

机译:吡ido醛硫代氨基脲和2-乙酰基吡啶硫代氨基脲分光光度法痕量测定土壤和蔬菜中的锌

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The rapid and continuous progress in trace analysis of metals is associated with development of several new techniques such as spectrophotometry. Thiosemicarbazones have been used as chromogenic reagents in spectrophotometric determination of metals. In this study the synthesis and characterization of pyridoxal thiosemicarbazone (PDT) and 2-acetyl pyridine thiosemicarbazone (2-APT) using IR, MS, and ~(1)HNMR were conducted. Zn(II) forms yellow colored complex with PDT and 2-APT in the pH range of 5–7 at 430?nm, and 8–10 at 360?nm, respectively. The Zn(II)-PDT and Zn(II)-2-APT complexes obeys Beer’s law in the concentration range of 0.26–2.62 and 0.25–2.56?μg/mL, respectively. The molar absorptivity and Sandell’s sensitivity of Zn(II)-PDT and Zn(II)-2-APT complexes are 1.8?×?10~(4) L/mol.cm and 0.0035?μg/cm~(2), 2.9?×?10~(4) L/mol.cm and 0.0167?μg/cm~(2), respectively. A first derivative spectrophotometry method is proposed for the determination of Zn(II) in the range 0.06–2.94 and 0.05–2.72?μg/mL of Zn(II) using PDT and 2-APT, respectively. The first derivative spectrum of Zn(II)-PDT and Zn(II)-2-APT complexes exhibits maximum amplitude at 400 and 385?nm, respectively The method was tested for Zn(II) determination in soil and vegetable samples. Using paired sample t -test at 0.05 level, the results were in good agreement with those obtained using flame atomic absorption spectrophotometer.
机译:金属痕量分析的快速和连续进展与分光光度法等几种新技术的发展有关。硫代氨基甲唑酮已用作分光光度法测定金属的显色剂。在这项研究中,使用IR,MS和〜(1)HNMR进行了吡ido醛硫代半碳酮(PDT)和2-乙酰基吡啶硫代半碳酮(2-APT)的合成和表征。 Zn(II)与PDT和2-APT形成黄色的络合物,在430?nm的pH范围为5-7,在360?nm的pH范围为8-10。 Zn(II)-PDT和Zn(II)-2-APT配合物的浓度分别在0.26-2.62和0.25-2.56?g / mL范围内符合比尔定律。 Zn(II)-PDT和Zn(II)-2-APT配合物的摩尔吸光度和Sandell敏感性为1.8?×?10〜(4)L / mol.cm和0.0035?μg/ cm〜(2),2.9 Δ×Δ10〜(4)L / mol·cm和0.0167μg/ cm〜(2)。提出了一种使用PDT和2-APT分别测定0.06-2.94和0.05-2.72?g / mL Zn(II)范围内的Zn(II)的一阶导数分光光度法。 Zn(II)-PDT和Zn(II)-2-APT配合物的一阶导数光谱分别在400和385?nm处显示最大振幅。该方法用于土壤和蔬菜样品中Zn(II)的测定。使用成对样品在0.05水平下的t-检验,结果与使用火焰原子吸收分光光度计获得的结果非常吻合。

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