NMR can provide a wealth of information on the dynamic processes of proteins in their natural aqueous environment and is the only technique that can determine polypeptide or protein structure in solution. The procedures and strategies that are common today for studying structure and dynamics of biological systems have been developed in the course of the last twenty years (2). Despite the establishment of NMR in biochemical research, this technique has not been incorporated into many biochemistry laboratory courses. The paucity of advanced biochemistry laboratory experiments motivated us to create this experiment, which illustrates basic 1- and 2-D NMR techniques used to study specific proton dissociation in peptides.