真空蒸馏预富集-电感耦合等离子体发射光谱法测定铂  

Vacuum Distillation Separation/Enrichment and Inductively Coupled Plasma-Atomic Emission Spectrometry for Determination of Platinum

作　　者：朱茜[1] 邓飞跃[1] 彭穗[1] 杨春玉[1] 丘克强[1] 

机构地区：[1]中南大学化学化工学院,长沙410083

出　　处：《分析化学》2010年第6期889-892,共4页Chinese Journal of Analytical Chemistry

基　　金：国家863计划(No.2006AA06Z375)资助项目

摘　　要：建立了真空蒸馏预富集-电感耦合等离子体发射光谱法测定铅试样中微量铂的方法。在真空条件下,利用Pb和Pt在较高温度下蒸汽压的差别进行分离,富集后的铂溶解制成溶液后进行电感耦合等离子体发射光谱检测,实现了真空密闭回收铅。针对试样的特点,对真空蒸馏方法理论上的可行性进行研究。结果表明:在蒸馏温度为1250K,真空度为30Pa,蒸馏时间为3h条件下,铂的富集分离效果最好,可富集至99.01%以上。线性范围为0.023～20mg/L,检出限(3σ)为0.0069mg/L,对样品测定的相对标准偏差为1.7%(n=6)。用本方法对样品中加入的铂标准溶液进行了测定,回收率为99.8%～103.0%。本方法简便快速、无污染,已应用于废电路板贵金属冶余物料中铂的测定。A method was established for the determination of platinum in lead samples by ICP-AES after separated and enriched by vacuum distillation. Under the condition of vacuum, platinum and lead can be separated at high temperature because of their different vapor pressures. The enriched platinum was determined by ICP-OES after dissovled, and also lead was recovered in vacuum. Theoretical feasibility of the vacuum distillation method and the influence factors such as temperature, time and pressure have been studied. The results indicated that content of platinum in residue is higher than 99.01% under the conditions of temperature of 1250 K, pressure of 30 Pa and time of 3 h. The detection limit （3σ） was 0.0069 mg/L with relative standard deviations of 1.7%. A wide linear range of 0.023-20 mg/L and the recovery of 99.8%-103.0% were obtained.

关 键 词：真空蒸馏预富集 电感耦合等离子体发射光谱 铂 铅 

分 类 号：O657.31[理学—分析化学] O614.826[理学—化学]