电感耦合等离子体原子发射光谱法测定化学合成反应液中铑含量

Determination of rhodium in chemical synthesis reaction solution by inductively coupled plasma atomic emission spectrometry

为了更加快速准确的测定化学合成反应液中铑含量,建立微波消解前处理与电感耦合等离子体原子发射光谱的组合监测方法。采用硝酸-硫酸混合酸体系对样品进行微波消解前处理,将有机铑络合物体系转化为无机酸体系。在相同的条件下分别选用铑元素233.477 nm、249.077 nm、343.489 nm三个波长进行样品的测定,铑元素的质量浓度在(0~1.0)mg·L^(-1)线性良好,线性相关系数r≥0.9997,方法检出限分别为0.01 mg·L^(-1)、0.03 mg·L^(-1)、0.10 mg·L^(-1)。波长343.489 nm具有更好的灵敏度,更适合铑元素的检测,样品回收率98.0%~102.5%,相对误差为2.8%~3.4%,相对标准偏差为0.2%~1.1%。该方法是在密闭空间进行样品前处理,避免了元素的损失,操作简便,耗时短,精密度高,适用于化学合成反应液中铑含量检测。

In order to determine the rhodium content in chemical synthesis reaction solution more quickly and accurately,a combined monitoring method of microwave digestion pretreatment and inductively coupled plasma atomic emission spectrometry was established.The sample was pretreated with nitric acid-sulfuric acid mixed acid system by microwave digestion,and the organic rhodium complex system was transformed into an inorganic acid system.Under the same conditions,the rhodium element of 233.477 nm,249.077 nm and 343.489 nm were selected for the determination of samples.The mass concentration of rhodium element was(0~1.0)mg·L^(-1),and the linear correlation coefficient was≥0.9997.The detection limits of the method were 0.01 mg·L^(-1),0.03 mg·L^(-1) and 0.10 mg·L^(-1),respectively.The wavelength of 343.489 nm has better sensitivity and is more suitable for the detection of rhodium.The sample recovery is 98.0%~102.5%,the relative error is 2.8%~3.4%,and the relative standard deviation is 0.2%~1.1%.Element loss was avoided due to experimental operating in closed space.This method is suitable for the determination of rhodium content in chemical synthesis reaction solution due to its simple operation,short time consumption and high precision.