机构地区: 南京理工大学化工学院
出 处: 《应用化学》 2011年第9期1073-1081,共9页
摘 要: 建立了用分子印迹壳聚糖/凹凸棒石(MICA)分离富集-火焰原子吸收光谱(FAAS)测定痕量铅的新方法。在动态吸附条件下,系统地研究了溶液pH值、流速、洗脱条件和干扰离子对痕量铅分离富集的影响;在pH=4.5,上样流速为0.60 mL/min的条件下,铅能被MICA定量富集;吸附的铅可用1.0 mol/L HCl-0.1 mol/L甲基异丁酮的乙醇溶液在流速为0.96 mL/min条件下完全洗脱;在优化条件下,MICA对铅的动态吸附容量为36.78 mg/g。线性范围为0~1.28 mg/L,r=0.999 7,检出限(3σ,n=11)为0.73μg/L,相对标准偏差为1.69%(n=6,ρ=0.08 mg/L),回收率在98.7%~101.4%之间。该方法操作简便、线性关系良好、灵敏度和精密度高,应用于实际水样中痕量铅的测定,结果满意。 A new method for the determination of trace Pb2+ by flame atomic absorption spectrometry(FAAS) after separation and preconcentration with molecular imprinting of chitosan/attapulgite(MICA) has been established.Under dynamic condition,the optimal pH of the solution,flow rate,elution conditions were obtained for preconcentration of trace Pb2+.And the effect of interfering ions was also investigated.It was found that Pb2+ could be quantitatively preconcentrated on MICA at pH=4.5.The flow rates of sample solutions and eluting solution with 1.0 mol/L HCl-0.1 mol/L methyl isobutyl ketone alcohol were 0.60 mL/min and 0.96 mL/min,respectively.The dynamic adsorption capacity of Pb2+ on MICA was 36.78 mg/g.The linear range for Pb2+ was 0~1.28 mg/L,correlation coefficient was 0.9997,detection limit(3σ,n=11) for Pb2+ was 0.73 μg/L,and the relative standard deviation was 1.69%(n=6,ρ=0.08 mg/L),the recovery was in the range of 98.7%~101.4%.The method is convenient,highly precise and linear in a wide range.The method has been applied to the determination of trace amount Pb2+ in water samples with satisfactory results.