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Article

Linkage Isomerization by Two-Dimensional 31P Nuclear Magnetic Resonance Spectroscopy. An Undergraduate Inorganic Laboratory Experiment

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Ahmad M. Al-Ajlouni

Department of Chemistry, Jordan University of Science & Technology, Irbid, Jordan

Rathindra N. Bose and Erika Volckova

Department of Chemistry, Kent State University, Kent, OH 44240

J. Chem. Educ., 2001, 78 (1), p 83

DOI: 10.1021/ed078p83

Publication Date (Web): January 1, 2001

Abstract

An application of two-dimensional ³¹P NMR spectroscopy is demonstrated through the characterization of linkage isomers of tetraammine(triphosphato)cobalt(III) chelates and metal-promoted hydrolysis of inorganic triphosphate ion. Unambiguous assignments of ³¹P resonances for two isomers, α,γ and β,γ chelates, were achieved by the direct through-bond connectivities among the three phosphate groups. The lack of such connectivity also helped to identify cobalt(III)-catalyzed hydrolysis products, orthophosphate and pyrophosphate ions. The experiment provides background information on 2-D NMR spectroscopy including the significance of pulse calibration, relaxation, evolution and mixing times, data processing, and finally, hands-on training for performing 2-D NMR experiments. The experiment is ideally suited for a senior laboratory course and may be included in the core inorganic curriculum required for a certified ACS B.S. degree.