摘要
使用填充三正辛胺(TOA)萃淋树脂的微型柱,采用流动注射在线分离富集与火焰原子吸收法联用技术,对微量银的测定进行了研究。在1.0mol/LHCl介质中样品流速为8.1mL/min,采样60s,以0.25mol/LHCl 0.5mol/L硫脲洗脱。在30样/h的分析速度下,富集倍率为26倍,富集效率为26/min,消耗指数为0.31mL。线性范围为0～1000μg/L,检出限为1.2μg/L。银含量为50μg/L时,连续11次测定的相对标准偏差为1.4%。对铅锌冶炼矿渣样液进行加标回收率试验,回收率为91.1%～100.6%,并应用于测定光谱纯氧化镁中的微量银。
<Abstrcat>An efficient flowinjection online Trinoclylamine(TOA) extraction resin separation and preconcentraction system was proposed for determination of trace silver by flame atomic absorption spectrometry. The microcolumn used was packed with TOA extraction resin as stationary phase. Sample in 1.0 mol/L HCl was pumped through a microcolumn at the rate of 8.1 mL/min. After 60 s of sampling and 60 s of elution, silver was absorbed and then eluted into the nebulizer of FAAS by 0.25 mol/L HCl0.5 mol/L thiourea. At the analytical frequency of 30/h, an enrichment factor of 26, a concentration efficiency of 26/min and a consumptive index of 0.31 mL were obtained. The linear calibration range for Ag is 0～1000 μg/L with detection limit (3σ) of 1.2 μg/L. The relative standard deviation at the 50μg/L level is 1.4%. The proposed method was applied to determination of trace silver in leadzinc waste slag and spectrum magnesium oxide reagent successfully.
出处
《分析试验室》
CAS
CSCD
北大核心
2002年第4期80-83,共4页
Chinese Journal of Analysis Laboratory
