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A method for the quantitative determination of L-alanine in triglycine sulphate crystals, in the presence of excess amounts of glycine, is described. L-alanine is determined after derivatization with 4-N,N-dimethyl-aminoazobenzene-4′-sulfonyl chloride (DABS-Cl) and in the presence of DABS-valine used as the internal standard. The results obtained indicate that the method permits the determination of alanine in triglycine sulphate crystals at concentrations of about 1%.