This paper deals with the separation and identification of ”Sumithion”, O, O-dimethyl O-(3-metho-4-nitrophenol) thiophosphate from the stomach cantents, blood, and urine of a male vivtim who attempted suicide using organophosphorus pesticide and with cholinesterase activity in the blood. The vivtim in this case is a man of 47 years old. He seems to have ingested ”Sumithion” (unknown about amounts) after drinking sake. He had alreafy frothed at his mouth and fell into convulsion when he was discovered by one of his family. At once, he was admitted into a hospital and received a variety of emergency treatments there. Nevertheless, he died 4 hours later. In the autopsy findings, abnormal signs were not recognized. On the other hand, appreciable amounts of ”Sumithion” were detected from speciments, such as the stomach contents, blood, and urine