气态进样电感耦合等离子体原子发射光谱法测定.doc

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Email:xuchuan_duan@ 摘要：使用电感耦合等离子原子发射光谱（ICP-AES）） Tianjin Normal University, Tianjin Key Laboratory of Cyto-Genetical and Molecular Regulation,Tianjin300387) By using inductively coupled plasma atomic emission spectrometry(ICP-AES), The conditions of chemical vapour generation(CVG) between sodium borohydride and acid solution containing rhodium metals were investigated and the method was applied for determination of rhodium in waste catalyst for organic synthesis. Under experimental conditions that rate of sample and sodium borohydride solution was 2mL·min-1, waste rate was 6mL·min-1, the optimum conditions obtained were found to be as follows: : 0.4 L/min of carrier rate、1.0 M acidity of nitric acid for vapor generation and concentration of sodium borohydride 1.2(（m/v）a two-fold increase in the efficiency of CVG of rhodium was achieved as compared to nebulization. The detection limit was 6.89μg.L-1 ,which is slight better than that with nebulization. The linear range for rhodium was found to be up at least 6.98 to 1500μg.L-1 with a coefficient of correlation(r)0.9986. The mean recovery of sample analysis was 95.5%. Excellent agreement was found between experimental and FAAS. Keyword: Chemical Vapour generation, inductively coupled plasma atomic emission spectrometry, rhodium, waste catalyst 1 引言 铑是一种贵金属，常被应用在汽车尾气转化和有机合成催化剂1，2）表1　ICP-AES仪器及蒸汽发生操作条件 Table1 Operating conditions of inductively coupled plasma atomic emission spectrometry ( ICP-AES) and vapour generation ICP-AES 工作条件(Condition of ICP-AES) 蒸气发生条件(Condition of vapour generation) RF发生器功率 Radio frequency power 1.3kW 样品流速 Sample flow rate 2. 0 mL /min 冷却气流量 Coolant gas flow rate 15L/min 还原剂流速 Reductant flow rate 2. 0 mL /min 辅助气流量 Auxiliary gas flow rate 0.5 L/min 还原剂浓度 Reductant flow rate 1.2%(m/V) NaBH4 载气流量 Nebulizer gas flow rate 0.4 L/min 废液流速 Waste flow rate 5.0 mL /min ICP观测方式 Plasma view type 水平 Axial 酸的类型 Acid type 硝酸 Nitric acid 1000mg/L)购自国家标准物质储