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Hydrolysis Studies and Quantitative Determination of Aluminum Ions Using 27Al NMR. An Undergraduate Analytical Chemistry Experiment

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Maria A. Curtin , Laura R. Ingalls , Andrew Campbell and Magdalena James-Pederson

Department of Chemistry, Stonehill College, Easton, MA 02357

J. Chem. Educ., 2008, 85 (2), p 291

DOI: 10.1021/ed085p291

Publication Date (Web): February 1, 2008

Section:

History, Education, and Documentation

Abstract

This article describes a novel experiment focused on metal ion hydrolysis and the equilibria related to metal ions in aqueous systems. Using ²⁷Al NMR, the students become familiar with NMR spectroscopy as a quantitative analytical tool for the determination of aluminum by preparing a standard calibration curve using standard aluminum solutions in dilute nitric acid keeping the aluminum in the hexaaquoaluminum ion form, Al(H₂O)₆³⁺. The technique has a large linear dynamic range, and in this experiment it ranges from 10 to 1000 ppm. Once the quantitative technique is validated, the goal of the experiment is to investigate the hydrolysis of Al³⁺ ions in aqueous solution by determining the concentration of the Al(H₂O)₆³⁺ ion by ²⁷Al NMR for a series of solutions with the same total concentration of aluminum but at various pHs ranging between 1.0 to 4.5. This experiment is also suitable for an instrumental analysis or inorganic chemistry course.

Keywords (Audience):

Upper-Division Undergraduate

Keywords (Domain):

Analytical Chemistry

Keywords (Pedagogy):

Hands-On Learning / Manipulatives

Keywords (Subject):

Aluminum

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This article has been cited by 1 ACS Journal articles (1 most recent appear below).

Probing Halide Distribution in [AlX₄]⁻ Anions via ²⁷Al NMR: Application of the Pairwise-Additivity Model
Craig M. Davis and Bridget M. Dixon
Journal of Chemical Education2011 88 (3), 309-310
- Probing Halide Distribution in [AlX₄]⁻ Anions via ²⁷Al NMR: Application of the Pairwise-Additivity Model
  Craig M. Davis and Bridget M. Dixon
  Journal of Chemical Education2011 88 (3), 309-310
  A laboratory exercise using 27Al NMR spectrometry to study the tetrahedral tetrahaloaluminate anions has been developed. Spectra of the homoleptic complexes [AlX4]− and the dihalide anions [AlX4Y4−n]− (X, Y = Cl, Br, or I) are acquired, then the pairwise-...
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Received: August 03, 2009

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Hydrolysis Studies and Quantitative Determination of Aluminum Ions Using 27Al NMR. An Undergraduate Analytical Chemistry Experiment