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

Extraction and separation of phosphorus by tributyl phosphate for determination of iron,zinc,silicon and aluminum in high purity yellow phosphorus by inductively coupled plasma atomic emission spectrometry

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。

2 g of yellow phosphorus was digested in nitric acid by reflux condensation.The phosphoric acid in high-purity yellow phosphorus digestion solution was extracted and separated using tributyl phosphate(TBP)to reduce the complexation with iron,zinc,silicon and aluminum.Meanwhile,the viscosity of digestion solution for testing could be decreased.The content of iron,zinc,silicon and aluminum was determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).Consequently the determination method of iron,zinc,silicon and aluminum in high-purity yellow phosphorus by ICP-AES after extraction and separation with TBP was established.The extraction conditions of this method were obtained as below:the volume ratio of sample solution and TBP was 1∶1;the oscillation time was 1 min;the standing time was 30 min.The mass concentration of elements in range of 0.50-50μg/mL was linear to the corresponding emission intensity.The correlation coefficients(r)of calibration curves were higher than0.999 5.The detection limits of elements were lower than 0.093μg/g.The proposed method was applied for the determination of iron,zinc,silicon and aluminum in yellow phosphorus samples,and the found results were consistent with those obtained by flame atomic absorption spectrometry(FAAS).The relative standard deviations(RSD,n=5)were all less than 0.80%.