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Thiocarbamide is used in photography, pharmaceutical and pesticide manufacture and in textile chemicals. It is recorded on HPV list of OECD presently. But thiocarbamide is a carcinogen and mutagen and this chemical is on the Special Health Hazard Substance List(U. S. EPA). It has been shown to cause thyroid, liver and other cancers in animals. Exposure can damage the bone marrow causing reduced red blood cell, white cells and reduced platelets. Repeated exposure can cause goiter and causes reduced thyroid hormone. HPLC/UVD method of thiocarbamide on OSHA has a complex process and bad repetition. so superior method is needed. The aim of this study is making the method. Thiocarbamide and 1,1,3,3-tetraethoxypropane make 2-mercaptopyrimidine in mixed solvent(c. HCI : Et-OH :H20 = 1 : 1 : 8 (v/v)). Then, 2-mercaptopyrimidine is detected on HPLC/UVD. 2-mercaptopyrimidine's LDL(Low Detection Limit) is about 0.051 ppm(mg/l). Molar extinction coefficient of 2-mercaptopyrimidine was 29900 at 286nm in contrast of which thiocarbamide was 25800 at 208nm 2-Mercaptopyrimidine of more lower concentration will be detected , if use more sensitive detector as electrochemical detector(ECD)