磷锑钼杂多酸-孔雀绿-聚乙烯醇体系分光光度法测定压延磷铜板中微量磷

Spectrophotometric determination of trace phosphorus in calendared phosphorus copper plate with phosphorus antimony molybdenum heteropoly acid-malachite green-PVA system

在硫酸介质中,钼酸铵和酒石酸锑钾与磷形成的杂多酸阴离子再与孔雀绿形成离子缔合物,在聚乙烯醇的作用下,测定磷的灵敏度明显提高,据此提出了在水相中测定压延磷铜板中微量磷的分光光度法。探讨了显色剂、表面活性剂、缓冲溶液的用量以及显色时间等对吸光度的影响,着重考察了不同的表面活性剂对体系的增溶增敏作用。实验测得离子缔合物的最大吸收波长为650 nm,表观摩尔吸光系数为1.52×10^5L mol^-1·cm^-1,磷含量在0～0.40μg/mL内符合比尔定律。样品中大量铜的干扰采用硼氢化钾还原沉积,使基体中大量铜与微量磷分离而消除。该方法用于压延磷铜板中微量磷的测定,加标回收率为96.0%～102.5%,相对标准偏差为2.9%（n=8）。

In media of sulfuric acid, the heteropoly acid anion formed by ammonium molybdate, antimony potassium tartrate with phosphorus reacts with malachite green to form an ionic associated complex. Under the action of polyvinly alcohol, the sensitivity of detecting phosphorus is improved obviously. According to this, A spectrophotometric method for determination of trace phosphorus in calendared phosphocopper plate in aqueous phase is proposed. Influence of chromogenic agent, surfactant, buffer soulution amount, chromogenic time etc on the absorbance are examined, with emphasis on the function of enhancing sencitivity and solubility of different surfactants in the system. It shows expermentally that the maximum absorbance wavelength of the ionic associated complex is 650 nm and apparent molar absorptivity is 1.52 × 10^5 L·mol^-1·cm^-1. Bee＇s law is obeyed in the range of 0- 0.40 μg/mL for phosphorus. Interference from large amounts of copper can be eliminated by reducing and depositing copper＇with BKH4. The method is used to detect trace phosphorus in calendared phosphours copper plate with the standard addition recovery of 96.0%-102.5% and the relatively standard deviation of 2.9% （n=8）.