The paper studied the determination of micro molybdenum in rocks (soil) by flame atomic absorption spectrometry, including the acidity of extraction in determination, volume ratio of organic facies and water facies, the effects of tartaric acid, ascorbic acid, potassium and nitric - sulphuric acid volume, meanwhile, made an interference determination of coexisting elements after extraction and fractionation. Through the comparative analysis with the national first class standard samples, it is verified that result accords with the national standard.