薄样技术-能量色散X射线荧光光谱法测定钯铂金  

Determination of palladium,platinum and gold by energy dispersive X-ray fluorescence spectrometry with thin sample technology

作　　者：邬旭然[1,2] 韩晓锋[1,2] 王丽[1,2] 吕建刚[1,2] 薛光 田宇纮[1] 

机构地区：[1]烟台大学化学化工学院,山东烟台264005 [2]山东黄金工程技术研究中心(工业应用),山东烟台264005

出　　处：《冶金分析》2013年第10期34-39,共6页Metallurgical Analysis

基　　金：国家自然科学基金资助项目(21045005)

摘　　要：采用树脂分离富集金矿和铜阳极泥中的Pd、Pt、Au,结合薄样技术,利用自制X射线荧光（XRF）能谱仪同时测定这3种元素.对3种型号树脂进行了选择,确定了Amberlyst A26树脂为分离树脂,并采用单因素法对Amberlyst A26树脂柱高、流速和盐酸浓度进行了优化,确定了最佳实验条件分别为柱高10 cm、流速3 mL/min和盐酸浓度0.2 mol/L.同时对XRF分析方法进行了方法学验证.XRF能谱仪采用Mo靶激发,新型SDD探测器,结合优化的薄样技术,基本消除基体效应,可用内标法定量;仪器检出限（LLD） Pd、Pt、Au分别为0.021、0.019、0.015 μg/mL,方法检出限（LDM）分别为0.066、0.062、0.050 μg/mL;采用11种元素的混合标准测得RSD在1.6％～7.5％之间.所测金矿样品的结果与国标法结果一致,铜阳极泥的测定结果与ICP-MS法结果基本一致.Palladium,platinum and gold in gold ore and copper anode slime were separated and enriched by resin.Combining with thin sample technique,these three elements were simultaneously determined using self-made X-ray fluorescence energy spectrometer.Three types of resin were tested and Amberlyst A26 resin was finally selected for the separation.The column height of Amberlyst A26 resin,flow rate and concentration of hydrochloric acid were optimized by single factor method.The optimal experimental conditions were as follows：column height of 10 cm,flow rate of 3 mL/min and hydrochloric acid concentration of 0.2 mol/L.Meanwhile,the methodology validation of X-ray fluorescence spectrometry was performed.The energy dispersive X-ray fluorescence spectrometer used Mo excitation target and novel SDD detector.The matrix effect could be basically eliminated combining with optimized thin sample technique.The quantitative analysis could be realized by internal standard method.The lower limit of detection （LLD） of instrument was 0.021,0.019 and 0.015 μg/mL for Pd,Pt and Au,respectively.The limit of detection of method （LDM） was 0.066,0.062 and 0.050 μg/mL,respectively.The relative standard deviations （RSD） of mixed standard of 11 elements were between 1.6％ and 7.5 ％.The determination results of gold ore samples were consistent with those obtained by national method,and the determination results of copper anode slime were consistent with those obtained by ICP-MS.

关 键 词：AMBERLYST A26树脂 金 铂 钯 能量色散X射线荧光光谱法 金矿 铜阳极泥 薄样技术 

分 类 号：TG115.33[金属学及工艺—物理冶金] O657.31[金属学及工艺—金属学]