At present, the development of China′s photovoltaic industry has accelerated, but a large amount of fluorine-containing wastewater has been produced.In order to accurately determine the soluble silicon content in fluorine-containing wastewater of photovoltaic industry, this paper mainly uses silicon molybdenum yellow spectrophotometry to conduct exptl. research.The method of detection and anal. of soluble silicon content in fluorine-containing wastewater before and after defluorination treatment was established by establishing silico-molybdenum yellow method, and interference tests were carried out on interfering ions such as Al3+, F- and P in water samples.The test results show that the presence of low concentration of Al3+ and F- plasma in the water sample has no interference on the determination of soluble silicon content, and the interference of P element is more serious, while oxalic acid can mask the interference of phosphorus, and 1 mg of phosphoric acid corresponds to 0.6 mL 10 g/L oxalic acid solution has the best interference effect; c (Si) has good linearity at 0∼2.0 mg·L-1, R2>0.999; the precision test results show that the spiked recovery of the sample is 100%±3.00%, When c (Si) was 34.475 mg·L-1 and 3.332 mg·L-1, the relative standard deviations were <3%.Therefore, the determination of soluble silicon in the fluorine-containing wastewater of the photovoltaic industry can be carried out by using the molybdenum-lime yellow spectrophotometry.