In order to reduce the pollution of the environment, China has implemented a new ultra-low emission control regulations for polluting gas, requiring new coal-fired power plant emissions SO2 less than 30ppm, NO less than 75ppm, NO2 less than 50ppm, Monitoring low concentration of NO and SO2 mixed gases , DOAS technology facing new challenges, SO2 absorb significantly weaken at the original absorption peak, what more the SNR is very low, it is difficult to extract the characteristic signal, and thus cannot obtain its concentration. So it cannot separate the signal of NO from the mixed gas at the wavelength of 200~230nm through the law of spectral superposition, it cannot calculate the concentration of NO. The classical DOAS technology cannot meet the needs of monitoring. In this paper, we found another absorption spectrum segment of SO2, the SNR is 10 times higher than before, Will not be affected by NO, can calculate the concentration of SO2 accurately, A new method of segmentation and demagnetization separation technology of spectral signals is proposed, which achieves the monitoring the low concentration mixed gas accurately. This function cannot be achieved by the classical DOAS. Detection limit of this method is 0.1ppm per meter which is higher than before, The relative error below 5% when the concentration between 0∼5ppm, the concentration of NO between 6∼75ppm and SO2 between 6∼30ppm the relative error below 1.5%, it has made a great breakthrough In the low concentration of NO and SO2 monitoring. It has great scientific significance and reference value for the development of coal-fired power plant emission control, atmospheric environmental monitoring and high-precision on-line instrumentation.