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Preconcentration of Trace Heavy Elements Pb, Cd, Cu with Mesoporous Molecule-sieve MCM-41 Prior to Determination by Atomic Absorption Spectrometry

Author: ZuoJie
Tutor: ZhouFangQin
School: Xiangtan University
Course: Analytical Chemistry
Keywords: Mesoporous molecular sieve Separation and enrichment Flame atomic absorption spectrometry Adsorption of lead , cadmium , copper
CLC: O657.31
Type: Master's thesis
Year: 2011
Downloads: 46
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Abstract


This thesis is based on access to a large number of Chinese and foreign literature, based on the structure and pore characteristics of mesoporous molecular sieves, self-prepared mesoporous molecular sieve MCM-41 as a novel adsorption material, flame atomic absorption spectrometry as a detection means The systematic study of the separation and enrichment of the MCM-41 mesoporous molecular sieve heavy metal ions lead, cadmium, copper behavior, and thus establish a sensitive and efficient new method for rapid analysis of trace heavy metal elements. This paper as follows: in the detection of trace heavy metals in the research and application of a determination of heavy metals in recent years, and the methods of separation and enrichment and separation and enrichment materials. The details of the structural characteristics of mesoporous molecular sieves, synthetic methods and applications in the adsorption of heavy metal ions. Separation and enrichment materials adsorption and mesoporous molecular sieve as a new method for determination of heavy metal ions. Second, to synthesize a new adsorbent materials - mesoporous molecular sieve Ti-MCM-41. By transmission electron microscopy (TEM), scanning electron microscopy (SEM) and pore size analysis to characterize them (BJH). Investigate the adsorption properties of mesoporous molecular sieve Ti-MCM-41 to trace lead, as well as the best experimental conditions. Mesoporous molecular sieve Ti-MCM-41 to lead the static adsorption capacity of 5.0 mg / g. The linear range of 0.5 ~ 20μg/mL, the method detection limit (3σ) of 3.3 ng / mL, and the relative standard deviation was 4.05%. This method has been successfully applied to the Determination of Trace Lead in drugs, the recovery rate from 97.1% to 99.5%. Third, on their own synthesis of mesoporous molecular sieve Al-MCM-41 scanning electron microscopy (SEM) and infrared (IR) characterization. Separation and enrichment of the molecular sieve - atomic absorption spectrometry determination of trace amounts of lead in water samples. Experiments to optimize the mesoporous molecular sieve Al-MCM-41 test solution in trace amounts of lead in the best adsorption and desorption conditions. The dynamic adsorption capacity of 6.0 mg / g. The method of determination of Pb2 linear range of 0.5 ~ 30μg/mL, the detection limit (3σ) of 0.05 ng / mL, and the relative standard deviation was 1.20%. The method used for the determination of the actual water samples of lead recoveries between 98.9% to 103.9%. Al-MCM-41 mesoporous molecular sieve as the separation and enrichment materials, atomic absorption spectrometry as a means of detection, determination of trace amounts of copper in the Chinese herbal medicine. The experiment of acidity, temperature, time and interfering ions on copper adsorption rate. The method of determination of copper static saturated adsorption capacity of 5.0 mg / g detection limit (3σ) was 0.55 ng / mL, the linear range of 0.5 ~ 20μg/mL linear regression equation is A = 0.1347 · c (μg / mL) 0.0454, relative standard deviation of 1.16%. Determination of the recoveries of the Chinese herbal medicine in the copper content of 98.5% to 100.3%, with satisfactory results. Mesoporous molecular sieves Ti-MCM-41 as the stationary phase micro-column line preconcentration and separation - atomic absorption method for the determination of trace amounts of cadmium. Systematic study of the adsorption properties of cadmium, to determine the best adsorption and elution conditions. The linear range of 0.5 ~ 5μg/mL, the detection limit (3σ) was 0.06 ng / mL, the relative standard deviation of 1.80%, the recovery rate of 97.3% to 101.6% for actual water samples marks the amount of cadmium in the detection, the results are satisfactory.

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CLC: > Mathematical sciences and chemical > Chemistry > Analytical Chemistry > Instrument analysis ( physics and physical chemistry ) > Photochemical analysis ( spectral analysis method) > Atomic emission spectrometry
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