The method described comprises the transformation of ammonium into ammonia, the rapid and gentle liberation of the ammonia followed by the measurement of the nitrogen in a Dohrmann nitrogen analyzer. Untreated biological samples (1-50 microliters) were pipetted onto magnesium oxide tablets at 130 degrees C and the ammonia liberated was transferred by a continuous stream of nitrogen carrier gas into the nitrogen analyzer. There the ammonia was determined by oxidative pyrolysis and subsequent chemiluminescence measurement of the excited NO2. The result could be read in nanograms ammonia nitrogen within 6.5 min. Apart from volatile amines, which are usually negligible in biological samples, the method was specific for ammonia because under the given conditions of volatilization the labile groups of glutamine and asparagine did not interfere. The assay was sensitive in the range of 1.5-150 nmol ammonia and suitable for the routine analysis of small samples.