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作 者:屈东方[1] 周方钦[1] 刘琳[1] 李文山[1]
机构地区:[1]湘潭大学化学学院环境友好化学与应用省部共建教育部重点实验室,湖南湘潭411105
出 处:《分析测试学报》2011年第11期1262-1266,共5页Journal of Instrumental Analysis
基 金:国家自然科学基金面上项目资助(21005068)
摘 要:制备了新型纳米B2O3/TiO2吸附材料,并采用扫描电镜(SEM)及红外光谱(IR)对其进行表征,优化了纳米B2O3/TiO2复合材料对试液中痕量银的吸附和解吸条件,建立了纳米B2O3/TiO2分离富集-原子吸收光谱测定痕量银的新方法。当pH 4.3时,在22℃下振荡20 min,Ag+能被该材料快速吸附,其静态饱和吸附容量为11.72 mg/g,吸附在纳米B2O3/TiO2上的Ag+可用0.1 mol/L HNO3-0.05 mol/L硫脲(1∶4)完全洗脱。该方法的检出限为2.01μg/L,线性范围为0.01~4.00 mg/L,相对标准偏差(RSD)为1.8%,加标回收率为95%~105%。方法应用于实际矿渣样品中痕量银的测定,结果满意。Nano B2O3/TiO2 composite as a new sorbent was synthesized, and the characteristic of the synthesized material was studied by scanning electron microscope (SEM) and infrared spectrometry (IR). By investigating the optimal conditions of adsorption and desorption of nano B2O3/TiO2 composite for Ag + , a new method for the determination of trace silver was proposed. After oscillated for 20 minutes at 22 ℃ and pH 4. 3, silver could be quantitatively adsorbed by nano Be B2O3/TiO2 eomposi.te, and the adsorption capacity was obtained to be 11.72 mg/g. The adsorbed silver could be eluted from the surface of the absorbent with 0. 1 mol/L HNO3 - 0.05 mol/L thiourea( 1 : 4). Under the optimum experimental conditions, the calibration curve was linear over Ag + concentration in the range of 0.01 -4.00 mg/L, with a detection limit(3σ) of 2.01 μg/L. The RSD(n = 11 ) for determination of 0. 4 mg/L Ag+ was 1.8% . The spiked recoveries ranged from 95% to 105% . The method was applied in the determination of trace silver in slag samples with satisfactory results.
关 键 词:纳米B2O3/TiO2复合材料 分离富集 火焰原子吸收法(FAAS) 银
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