Urine concentrations of organic acids were determined by a gas chromatographic technique in healthy, full-term neonates at the ages of 2 and 5 days. Significant reductions in the interindividual variation were obtained by relating the levels of organic acids to urine creatinine concentration or osmolality. Citrate was the predominant organic anion found. Urine concentrations of fumarate, 3-hydroxy-3-methylglutarate, adipate, and suberate decreased during the first week of life, and their concentrations were significantly intercorrelated. It is suggested that these findings reflect the predominantly fat-utilising, hyperketonaemic state during the first days of life. The urine concentrations of the aromatic end-products, p-hydroxyphenylacetate and hippurate, increased during the first week of life, probably as an effect of dietary factors. It is concluded that analysis of intermediary organic acids in urine could be of value in the assessment of the metabolic state in neonates.