A method for the determination of trace antimony in copper by flow injection on-line ion-exchange separation and enrichment-hydride generation atomic fluorescence spectrometry is suggested. The manifolds and operating program for ftlow injection on-line ion-exchange were designed and chemical conditions were optimized. Antimony complex was absorbed on strongly basic anion exchange resin 717 with 1. 4 mol/L HC1 as absorbent medium and 2. 0 mol/L HNO_3 for elution. The interference of co-existent elements (i-ron, nickel, lead, etc) was eliminated while antimony was enriched and was determined by hydride generation-atomic fluorescence spectrometry. The method is easy to operate and fast, and has lesser pollution to environment. The linear range is 0. 2-120μg/L and the RSD is 3%～5% with detection limit of 0. 05 μg/L. The results for determination of antimony in standard samples of copper alloys are satisfactory.%提出了流动注射离子交换在线分离富集-氢化物发生原子荧光光谱法测定铜合金中痕量锑的分析方法.设计了流动注射在线离子交换的流路和操作程序,优化了各项化学条件.采用717强碱性阴离子交换树脂吸附锑,并能有效消除铁、镍、铅等元素的干扰,也使大量基体元素铜与待测元素分离,锑在1.4 mol/L的HCl介质中上柱,选用2.0 mol/L的HNO_3作为洗脱剂.实现了氢化物发生原子荧光光谱法对铜合金中痕量锑的在线测定.方法操作简便、快速,环境污染小,线性范围为0.15～120 μg/L,相对标准偏差在3%～5%之间,检出限为0.05μg/L.方法应用于铜合金标准样品,结果与推荐值吻合.
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