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利用叠氮化介孔二氧化硅与炔丙胺反应,制备了炔丙胺介孔二氧化硅吸附材料,采用傅立叶红外光谱仪对其进行表征,并用于水样中痕量镉的富集。吸附材料在溶液pH 7.5时,恒温振荡30 min能高效吸附痕量Cd~(2+),吸附的Cd~(2+)用1 m L 1 mol/L HNO_3振荡30 min完全洗脱,火焰原子吸收法测定。在最佳实验条件下,方法的线性范围为0.5~50 ng/m L,方法检出限为0.06 ng/m L(3σ,n=20),富集倍数可达50倍,对20 ng/m L Cd~(2+)测定相对标准偏差为1.9%(n=20),加标回收率为95.5%~97.5%。吸附材料可循环使用25次以上并用于水样中Cd~(2+)的测定。
The propargyl mesoporous silica adsorbent was prepared by the reaction between azidated mesoporous silica and propargyl amine. The mesoporous silica adsorbent was characterized by Fourier transform infrared (FTIR) spectroscopy and was used for the enrichment of trace cadmium in water sample. At pH7.5, adsorption of Cd2 + on the surface of the adsorbent at constant temperature for 30 min could completely adsorb Cd2 +, and the adsorbed Cd2 + could elute completely with 1 mL of 1 mol / L HNO3 for 30 min. Flame atom Absorption method. Under the optimal experimental conditions, the linear range of the method was 0.5-50 ng / m L, and the detection limit was 0.06 ng / m L (3σ, n = 20) The relative standard deviation of m L Cd 2+ determination was 1.9% (n = 20), and the recoveries were 95.5% -97.5%. Adsorbent material can be recycled more than 25 times and used for determination of Cd2 + in water sample.