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本文叙述了对甲氧基苯甲醛-4苯基-3缩氨基硫脲(APT)的合成、光谱特征及其在分析上的应用。基于金属离子与APT的显色反应原理拟定出一套简易迅速、选择性好、灵敏度高的分光光度法测定微量金的方法。该法适用于在只有金或其他金属离子与之共存的情况下做微量金的测定。形成的黄棕色络合物(λmax=365nm)置人乙基醋酸盐中萃取。在pH4-7范围内,金与试剂按1:1进行反应(金属对配位体)。金浓度在0.1—12.3微克/毫升范围内符合比尔定律。该方法的摩尔吸收和桑德尔灵敏度分别为2.12×10~4l·mol~(-1)·cm~(-1)和0.0092μg·Cm~(-2)。对于45微克金(Ⅲ),经十次重复测定,其相对标准偏差为1.71%。通过对各种离子干扰的研究,从而进一步确定了测定某些合成样品中金的条件。
This paper describes the synthesis of p-methoxybenzaldehyde-4-phenyl-3-thiosemicarbazone (APT), its spectral characteristics and its analytical application. Based on the color reaction principle between metal ions and APT, a set of simple, rapid, selective, and sensitive spectrophotometric method for the determination of trace gold was developed. This method is applicable to the determination of trace gold in the presence of gold or other metal ions alone. The resulting yellow-brown complex (λmax = 365 nm) was taken in ethylacetate and extracted. In the pH range of 4 to 7, gold reacts with the reagent at 1: 1 (metal-to-ligand). Beer’s law is consistent with gold concentrations ranging from 0.1 to 12.3 μg / ml. The molar absorptivity and Sander sensitivity of this method were 2.12 × 10 -4 l · mol -1 cm -1 and 0.0092 μg · cm -2, respectively. For 45 micrograms of gold (III), the relative standard deviation was 1.71% after ten replicates. Through a variety of ion interference studies, which further determined the determination of certain synthetic samples of gold conditions.