An ultramicro technique for the digestion of organic nitrogen and phosphorus compounds in wastewater samples is described. The digests are analyzed simultaneously for phosphate and ammonia in the range of 0.02-2.00 mg PA. and of 0.06-10.00 mg NA. using automated spectrophotometry at the rate of 30 samples/h. The accuracy, precision, and tolerance to common interferences of the ultramicro method are discussed. Comparability testing of the ultramicro and standard methods shows a small but statistically significant difference for the phosphorus but not for the nitrogen results.