中孔分子筛Ti-MCM-48的合成及其对痕量银(Ⅰ)的吸附性能研究与应用  

Synthesis of Mesoporous Ti-MCM-48 and Its Adsorption Performance for Trace Silver(Ⅰ)

作　　者：毛燕芬 周方钦[1] 唐壮娜 贺锦灿 李春艳[1] 

机构地区：[1]环境友好化学与应用省部共建教育部重点实验室,湘潭大学化学学院,湖南湘潭411105

出　　处：《分析科学学报》2013年第1期39-43,共5页Journal of Analytical Science

基　　金：国家自然科学基金(No.21005068)

摘　　要：以正硅酸乙酯、钛酸丁酯为原料,十六烷基三甲基溴化铵为表面活性剂合成中孔分子筛Ti-MCM-48。研究了中孔分子筛Ti-MCM-48分离富集材料对银(Ⅰ)的吸附性能,优化了影响其吸附和解吸的主要条件。结果表明,在pH=3.0的柠檬酸-柠檬酸钠缓冲溶液中,恒温35℃振荡25min时,银(Ⅰ)能被该材料吸附完全,其静态饱和吸附容量为2.96mg/g。吸附在中孔分子筛Ti-MCM-48上的银(Ⅰ)可用5mL 0.5mol/L HNO3-0.1mol/L硫脲洗脱液完全洗脱。采用火焰原子吸收光谱法(FAAS)测定洗脱液中银(Ⅰ)的方法检出限(3σ)为21.39ng/mL,线性范围为0.02～5.0μg/mL(r=0.9995),相对标准偏差(RSD)为1.25%,加标回收率在96%～102%之间。方法可用于实际样品中痕量银的测定。The mesoporous Ti-MCM 48 was synthesized with ethyl silicate and tetrabutyl titanate as raw materials and cetyltrimethylammonium bromide as surfactant. A method was proposed for the determination of trace silver using mesoporous Ti-MCM-48 as separation and preconcentration material and flame atomic absorption spectrometry（FAAS） for detection. The optimal conditions of adsorbing and desorbing silver（ I ） on mesoporous Ti-MCM-48 material were investigated. Silver（ I ） could be quantitatively adsorbed by mesoporous Ti-MCM-48, and the capacity of static saturated adsorption was 2.96 mg/g. The adsorbed silver（ I ） could be eluted with 0.5 mol/L HNO3-0.1 mol/L thiourea. Under the optimum experimental conditions, the obtained linear calibration curve was over silver（ I ） concentration of 0.02-5.00 μg/mL, with a detection limit（3o） of 21.39 ng/mL. The relative standard deviation for determination of 1.00 μg/mL silver（ I ） was 1. 25% （n= 7） . The recoveries for spiked samples ranged from 96%-102%. The method was applied for the determination of trace silver（ I ） in slag samples with satisfactory results.

关 键 词：中孔分子筛Ti-MCM-48 合成 吸附性能 分离富集 银 

分 类 号：O658.11[理学—分析化学]