【摘要】 提出了一种流动注射在线离子交换分离富集-氢化物发生原子荧光光谱法测定铜合金中痕量铋的方法。在1 mol/L HCl介质中,Bi3+与Cl-生成稳定的络阴离子,被吸附于717强碱性阴离子树脂,用0.75 mol/L HNO3与0.05 mol/L柠檬酸的混合液洗脱,并在线引入石英炉以原子荧光光谱法测定。设计了流动注射在线离子交换分离富集及氢化物发生流路和操作程序,优化了各项化学条件及操作参数。方法的检出限为0.04 ng/mL,铋量在0.04~50ng/mL范围内有良好的线性关系。对5 ng/mL铋平行测定11次,所得相对标准偏差为2.02%。经过离子交换有效地消除了大量基体铜及其它共存元素的干扰,方法应用于铜合金标样中痕量铋的测定,结果与认定值相符。更多还原

【Abstract】 A method for determination of trace bismuth in copper alloy by flow injection system of on-line ion exchange combined with hydride generation-atomic fluorescence spectrometry was established.In the medium of 1 mol/L hydrochloric acid,Bi3+ reacts with Cl-to form a stable anion complex which was adsorbed on the column of strongly basic anion exchange resin 717.The anion complex is desorbed from the column with the mixture of 0.75 mol/L HNO3 and 0.05 mol/L citric acid and then determined by atomic fluorescence spectrometry.The manifold and operating program for on-line ion exchange and hydride generation were designed,and chemical conditions and operation parameters were optimized.The detection limit of the method was 0.04 ng/mL and the calibration curve was rectilinear over 0.04～50 ng/mL Bi3+.The relative standard deviation was 2.02 %(n=11) for determination of 5 ng/mL Bi3+ in the standard solution.Interferences from matrix copper and other concomitant elements were eliminated effectively.The proposed method has been applied to the determination of trace bismuth in standard copper alloy,and experimental results are in agreement with the certified values.更多还原