原子荧光光谱法测定三苯基膦羰基铑催化剂中的砷含量  

Determination of arsenic in triphenylphosphine rhodium carbonyl catalyst by atomic fluorescence spectrometry

作　　者：张岩 荣丽丽 陈斯佳 ZHANG Yan;RONG Lili;CHEN Sijia(Daqing Chemical Engineering Research Center,PetroChina Petrochemical Research Institute,Daqing 163714,China)

机构地区：[1]中国石油石油化工研究院大庆化工研究中心,黑龙江大庆163714

出　　处：《石油化工》2024年第10期1461-1465,共5页Petrochemical Technology

摘　　要：采用原子荧光光谱法测定三苯基膦羰基铑催化剂中的砷含量,考察了消解酸的种类和用量、共存元素铑的干扰及消除方法,验证了测定方法的准确度和精密度。实验结果表明,在5.0 mL硝酸+2.0 mL高氯酸的混合酸体系中,催化剂可消解完全,采用共沉淀的方法,pH在9~10时,可完全消除铑对砷含量测定的影响。当砷含量在1.0~10.0μg/L范围内时,砷含量与荧光强度的关系曲线呈线性,相关系数大于0.999。测定结果的相对标准偏差小于5%,加标回收率在92%~106%之间,满足分析测试要求。Arsenic in triphenylphosphine rhodium carbonyl rhodium catalyst was determined by atomic fluorescence spectrometry.The type and amount of dissolved acid,interference and elimination method of rhodium,a co-existing element,were investigated.The accuracy and precision of the method was demonstrated.The experimental result shows that the catalyst is completely dissolved in the mixed acid system of 5.0 mL nitric acid and 2.0 mL perchloric acid.The interference of rhodium on arsenic is eliminated outright by the co-precipitation method when the pH value reaches 9-10.When the concentration of arsenic is in the linear range of 1.0-10.0μg/L,the relation curve between the concentration of arsenic and fluorescence intensity is linear,with a correlation coefficient higher than 0.999.The relative standard deviation of the measured result is less than 5%,and the recovery rate is 92%-106%,which meets the requirement of analysis and test.

关 键 词：原子荧光光谱 三苯基膦羰基铑催化剂 砷 消除 干扰 

分 类 号：TQ213[化学工程—有机化工]