In order to realize the rapid, nondestructive detection of organic compounds, a two-dimensional analysis method based on technology of laser Raman spectroscopy was proposed. The results show that using 532 nm laser as excitation light source, the observation of 236.2, 348.9, 449.4 and 513.6 cm-1, the four vibrational Raman spectra, and the intensity ratio of 6.4∶1.7∶9.4∶1.0 can determine the existence of tetrachloroethylene. The observation of 707.5, 1 087.9, 1 175.8 and 3 078.6 cm-1, the four vibrational Raman spectra, and the intensity ratio of 9.6∶6.4∶1.0∶3.9 can determine the existence of chlorobenzene. In other words, that through the comprehensive study of spectral lines and intensity ratio of some spectral lines, the presence of organic compounds in the mixed solution can be determined quickly. In the aspect of quantitative analysis, using multi-spectral analysis combined with least square fitting method can improve the reliability of the measurement, The accuracy of sample concentration was 98.4%. This spectral measurement method is a potential tool for organic component identification and concentration analysis which has a prosperous application prospects.