流动注射在线分离富集-火焰原子吸收光谱法测定钯  

FAAS Determination of Palladium with FI-On-line Pre-enrichment

作　　者：白祖海[1] 周方钦[2] 

机构地区：[1]长沙市疾病预防控制中心,长沙410001 [2]湘潭大学化学学院,411105

出　　处：《理化检验（化学分册）》2009年第6期629-631,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：将聚氯乙烯-丁二酮肟复膜树脂作为固定相填充到自制的微型柱中,将流动注射在线分离富集与火焰原子吸收光度法联用,组成同时富集、顺序反向洗脱的环内双柱复线流路及检测系统,对废催化剂中微量钯进行测定。废催化剂样品经盐酸(5+95)溶液溶解后,过滤所得残渣溶于王水中。分析时将pH 2的试液以7.5 mL.min-1速率采样90 s,用乙二-胺20 g.L-1氢氧化钠(1+9)混合溶液作为洗脱液,从柱上将钯(Ⅱ)洗脱并引入原子吸收光谱仪的雾化器中进行测定,线性范围为1.25 mg.L-1以内,检出限(3S/N)为15μg.L-1,应用此方法分析了地质标样及铂矿样等已知样品,测得结果与标准值或已知值相符,其相对标准偏差(n=7)均小于2.5%。Preparation of a micro-column filled with model 717 ion-exchange resin, which was covered with a thin membrane of dimethylglyoxime dispersed in PVC, was described and used for the separation and pre-enrichment of Pd（ Ⅱ）. Based on a LZ-2000 FI-analyzer, manifold for enrichment of Pd（ Ⅱ ） on the microcolumn, elution of Pd（ Ⅱ ） from the column with a mixture of ethylenediamine and 20 g·L^-1 NaOH solution （mixed in the ratio of 1＋ 9 by volume）, and introduction of the eluate into the atomizer of AAS instrument was designed, fabricated and its operation given in detail. Waste catalyst sample was treated with HC1 （5＋95） solution, and the insoluble residue was collected by filtration and dissolved in aqua regia. The solution, after adjusting its acidity to pH 2, was introduced into the FI-manifold for analysis. Rate and time of sample solution introduction were 7. 5 mL · min^-1 and 90 s. Linear relationship between values of absorbance and concentration of Pd（ II ） was kept in the range within 1.25 mg·L^-1. Detection limit （3S/N） of the method was found to be 15μg·L^-1. Precision and accuracy of the method were checked by analysis of 3 samples of geological standards and platinum ores, the results obtained were in consistency with the standard or known values, with values of RSD＇s （n=7） less than 2. 5%.

关 键 词：火焰原子吸收光谱法 流动注射在线预富集 钯 

分 类 号：O657.31[理学—分析化学]