在线化学蒸气发生-电感耦合等离子体原子发射光谱法测定废催化剂中的微量铑  

Determination of Rhodium by Inductively Coupled Plasma Atomic Emission Spectrometry With Chemical Vapour Generation Sample Introduction Technique

作　　者：段旭川[1] 

机构地区：[1]天津师范大学化学与生命学院,天津市细胞遗传与分子调控重点实验室,天津300387

出　　处：《分析化学》2010年第3期421-424,共4页Chinese Journal of Analytical Chemistry

摘　　要：使用电感耦合等离子原子发射光谱(ICP-AES)研究了贵金属铑和NaBH4在酸性水溶液中的化学蒸气发生反应的条件,并测定了有机合成催化剂中的铑。研究结果表明:在NaBH4和样品溶液流速为2mL/min、废液排放流速为6mL/min的条件下的最佳蒸气发生条件为:载气流速0.4L/min、HNO3浓度为1.0mol/L、NaBH4浓度为1.2%(m/V)。研究中获得的铑化学蒸气进样效率是常规的气动雾化进样效率的2.7倍;检出限是6.9μg/L,略优于气动雾化法;线性范围20～1500μg/L;线性相关系数是0.9986;RSD是1.6%。样品分析加标回收率分别是94%和97%。用本法测得的样品值与原子吸收法的测得值吻合很好。An inductively coupled plasma atomic emission spectrometry（ ICP-AES） combined with a boron hydride vapour generation device was used for the determination of rhodium in waste catalyst. When the flow rate of sample and sodium borohydride solution was 2 mL/min,waste rate was 6 mL/min,the optimum conditions were as follows： 0. 4 L/min of carrier rate,1. 0 mol/L of acidity of nitric acid for vapor generation and concentration of sodium borohydride 1. 2（ m/V） . The study showed that a two-fold increase in the efficiency of rhodium was achieved as compared to nebulization. The detection limit was 6. 9 μg/L,which is slight better than that of with nebulization. The linear range for rhodium was 20-1500 μg/L with a correlation coefficient of 0. 9986. The mean recovery of sample analysis was 95. 5% . Excellent agreement was found between the present method and FAAS.

关 键 词：化学蒸气发生 电感耦合等离子体原子发射光谱 铑 

分 类 号：O657.31[理学—分析化学] O614.243[理学—化学]