Abstract: A method was presented for the determination of total sulfur in milligram diesel fuel and kerosene samples by HNO 3-HCL-H 2O 2 sealed digestion system using high-resolution Inductively Coupled Plasma-Mass Spectrometry.In the special designed sealed digestion vessel,sulfur from diesel and kerosene samples could completely be transformed to sulfate in aqueous solution.Furthermore,the sulfate in aqueous solution was able to be measured by HR-ICP-MS at medium resolution 3000 to separate the interferences from 16 O 16 O + and 14 N 18 O +ions.As a result,the method has a recovery of 97%～103%,range of 0.00006%～1% for 30 to 100 mg sample,uncertainty of 7% less.