This research focuses on the development of Raman spectroscopy for determination of the low volatile concentration as toluene volatile and 2-Acetyl-2-thiazoline(2AT) volatile. The studies were divided into two techniques. The research was to develop surface enhanced Raman substrates (SERS) enhancedthe surface using silver metal for enhancement. In this part, there were two different types of the SERS suitable for FT-Raman. The first technique was silver colloid. This technique could build nanosilver particles, of which average size was 35.5 -140.3 nm. The detection limits were found to be at 4000 ppm in 2 AT solution. The second techniques were the silver mirror and freezing technique. The detection limits for 2AT solution 0.2 ml in vial were found to be at 4000 and 1000 ppm in the silver mirror. Results of the enhanced Raman spectra of volatile organic compounds (VOCs) contained in a sample showed that the concentration of 2AT was existed at higher level than thatof toluene. Therefore, the silver mirror type of SERS together with the FT-Raman could be used for determining 2AT in low concentration.