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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》2016年第4期495-499,共5页Journal of Analytical Science
基 金:国家自然科学基金(No.21005068)
摘 要:本文采用化学修饰技术制备了新型固相萃取材料罗丹宁-壳聚糖,用傅立叶红外(IR)光谱对其进行了表征。以该材料作为固相萃取剂,采用火焰原子吸收(FAAS)法为检测手段,在动态条件下系统研究了该吸附材料对痕量Ag+的吸附性能。研究结果表明:在pH=5.0,室温下以1.8mL/min速度流过分离柱,试液中的Ag+能被该材料定量吸附,其动态饱和吸附容量为72.62mg/g。吸附的Ag+可用8mL 0.1mol/L硫脲-0.05 mol/L HNO3混合液以0.7 mL/min流速完全洗脱,洗脱液中的Ag+用FAAS法测定。该方法对Ag+的检出限(3σ,n=11)为8.50μg/L,线性范围为0.01~5.0mg/L,相对标准偏差(RSD)为0.72%;加标回收率在97.8%~102.7%之间。方法用于实际环境水样中痕量Ag+的测定,结果满意。In this study, a novel solid phase extraction material-rhodanine chitosan was successfully prepared by the chemical modification, and was characterized by Fourier transform infrared (FT-IR) spectrometer. The rhodanine chitosan was used as solid phase extraction adsorbent, and it's adsorption properties for Ag+ were investigated by dynamic method,and the flame atomic absorption spectrometry (FAAS) was used as the detection method. The results showed that when the solution was adjusted to pH=5.0 at room temperature and flowed at the speed of 1.8 mL/min,Ag+ can be fully adsorbed by the adsorption materials. The dynamic saturated adsorption capacity for Ag+ was 72.62 mg/g. The adsorbed Ag+ could be eluted with 8 mL mixture of 0.1 mol/L thiourea and 0.05 mol/L HNOa at the speed of 0.7 mL/min. Under the optimum conditions,linear response of Ag+ in the range from 0.01 to 5.0 mg/L was obtained with the detection limit (3a,n= 11) of 8.50 μg/L. The relative standard deviation (RSD) was 0. 72% and the recoveries were 97. 8%-102. 7%. The proposed method was applied to the determination of trace Ag+ in real environmental water samples with satistfactory results.
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