Pressure-Assisted Chelating Extraction as a Teaching Tool in Instrumental Analysis
Omowunmi A. Sadik, Adam K. Wanekaya, and Gelfand Yevgeny
Department of Chemistry, State University of New York at Binghamton, Binghamton, NY 13902-6016
This article describes a laboratory procedure designed for a junior-level instrumental analysis course using a pressure-assisted chelating extraction (PACE) technique to digest heavy metals from solid matrices. PACE can achieve the digestion of metals through direct contact between solids and chelates under controlled temperature and pressure. After digestion, the metals can be analyzed using flame atomic absorption spectroscopy (FAAS). The exercise requires two three-hour laboratory periods. In one lab period, students use a wet acid-digestion technique to remove heavy metals from sediment samples and analyze them using FAAS. In the second lab period, students digest the samples using PACE and similarly analyze the sediment samples by FAAS. The PACE results are then compared with the results from wet acid-digestion. In the experiments performed by the students, mean lead recoveries were 95% with an RSD of 10% with PACE, and 111% with an RSD of 37% with the acid-digestion technique. The PACE approach allows students to gain sample preparation skills using nonhazardous reagents. The combination of PACE with FAAS enabled the students to develop a greater appreciation and understanding of the highly automated, modern instrumental techniques, including sample preparation.
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Instructions for the students and notes for the instructor are available.
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JCE2004p1177W.doc (Microsoft Word)
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Sadik, Omowunmi A.; Wanekaya, Adam K.; Yevgeny, Gelfand. J. Chem. Educ.2004 81 1177.
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