A rapid micro procedure for the determination of sulfonate and sulfate type surfactants was developed by modification of the methylene blue titration method. The method is based on the oxidation of methylene blue chloride to dimethylthionoline, a red dye, in the presence of chloroform and sodium hydroxide.In a typical procedure 5 ml of sample solution (0.5-4 mmolg) is pipetted into titration bottle. To the sample solution are added 1 ml of methylene blue solution as the indicator and 10 ml of chloroform after adjustment of pH at 11-12 with 0.5 N sodium hydroxide. The solution is titrated with cationic standard solution. The end point is reached when the chloroform layer turns clear red.The results show that the anionic active component of various amphoterics (taurine type, sunfonate betain type, sulfate imidazoline type) and various anionics can be determined rapidly and with accuracy (deviation 71%) by this method. But carboxylic acid type amphoterics and soap can not be determined accurately.