应用化学 ›› 2011, Vol. 28 ›› Issue (09): 1073-1081.DOI: 10.3724/SP.J.1095.2011.00565

• 研究论文 • 上一篇    下一篇

分子印迹壳聚糖/凹土分离富集-火焰原子吸收光谱测定痕量铅

张强华1,2,石莹莹2,熊清平2,钟秦1*   

  1. (1.南京理工大学化工学院 南京 210094;2.淮阴工学院生化学院 淮安)
  • 收稿日期:2010-09-27 修回日期:2011-02-04 出版日期:2011-09-10 发布日期:2011-09-10
  • 通讯作者: 钟秦,教授; Tel/Fax:025-84315517; E-mail:zq304@mail.njust.edu.cn; 研究方向:环境监测与治理
  • 基金资助:
    江苏省自然科学基金项目(BK2008196)

The Determination of Trace Amount of Pb by Flame Atomic Absorption Spectrometry after Separation and Preconcentration with Molecular Imprinting of Chitosan/Attapulgite

ZHANG Qianghua1,2, SHI Yingying2, XIONG Qingping2, ZHONG Qin1*   

  1. (1.Institute of Chemical Engineering,Nanjing University of Science & Technology,Nanjing 210094;
    2.Huaiyin Institute of Technology,Huaian)
  • Received:2010-09-27 Revised:2011-02-04 Published:2011-09-10 Online:2011-09-10
  • Contact: zhang

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0.73 μg/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。

关键词: 分子印迹技术, 凹凸棒石黏土, 壳聚糖, 分离富集, 火焰原子吸收光谱,

Abstract:

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 0.999 7, 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.

Key words: Molecular imprinting Technique, Attapulgite, Chitosan, Separation and preconcentration, FAAS, Pb2+

中图分类号: