磷酸三丁酯萃取分离磷-电感耦合等离子体原子发射光谱法测定高纯黄磷中铁锌硅铝

发布时间：2018-04-08 07:29

本文选题：磷酸三丁酯(TBP)　切入点：萃取分离　出处：《冶金分析》2017年11期

【摘要】：将2g黄磷经硝酸回流冷凝消解后,采用磷酸三丁酯(TBP)萃取分离高纯黄磷消解液中的磷酸,从而降低磷酸与铁、锌、硅和铝的络合作用,同时降低待测消解液的黏度,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定其中的铁、锌、硅和铝,从而建立了磷酸三丁酯萃取分离磷-电感耦合等离子体原子发射光谱法测定高纯黄磷中铁、锌、硅和铝的方法。方法以样品溶液和TBP的体积比为1∶1、振荡时间为1min、静置时间30min为萃取条件。各元素质量浓度为0.50~50μg/mL范围内与其发射强度呈线性,校准曲线相关系数r均大于0.999 5,方法中各元素检出限均低于0.093μg/g。按照实验方法测定黄磷样品中铁、锌、硅和铝,结果的相对标准偏差(RSD,n=5)均小于0.80%,结果与火焰原子吸收光谱法(FAAS)测定铁、锌、铝,重量法测定硅的结果相吻合。
[Abstract]:After 2 g yellow phosphorus was refluxed and condensed by nitric acid, the phosphoric acid in high purity yellow phosphorus solution was extracted and separated by TBP. The complexation of phosphoric acid with iron, zinc, silicon and aluminum was reduced, and the viscosity of the solution was reduced.The determination of iron, zinc, silicon and aluminum in high purity yellow phosphorus by inductively coupled plasma atomic emission spectrometry (ICP-AES-) was established.Methods of silicon and aluminum.Methods the extraction conditions were as follows: the volume ratio of sample solution to TBP was 1: 1, the oscillating time was 1 min, and the static time was 30min.The calibration curve correlation coefficient r is greater than 0.999, and the detection limit of each element in the method is lower than 0.093 渭 g / g.The relative standard deviation of the determination of iron, zinc, silicon and aluminum in yellow phosphorus samples was less than 0.80. The results were in agreement with the results obtained by Faas (Flame Atomic absorption Spectrometry) for the determination of iron, zinc, aluminum and silicon by gravimetric method.
【作者单位】：江西省安全生产科学技术研究中心安全科研标准所江西省工业安全工程技术研究中心;江西省化学工业设计院工艺设计所;
【分类号】：O657.31;TQ126.317

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