Abstract: The analysis and determination of nuclear material is an important part in nuclear safeguards. Laser-induced breakdown spectroscopy (LIBS) is a very promising technology in material determination. In nuclear facility effluent air monitoring, it is necessary to measure and analyze the content of plutonium in filters sampling from vent-pipes. In order to explore the application of LIBS technology for plutonium analysis in aerosol sampling filters, the measurement of the plutonium in the off-gas of the radioactive reprocessing plant was studied by using single pulse LIBS (SP-LIBS) technology for the reason of NMA (nuclear material account) of RPP (reactor power plant). To study the feasibility of membrane quantitative analysis of plutonium content, experiments were carried out on sampling filters. In this research, sampling filters were from a glovebox in a hot cell of a certain nuclear facility, as those samples were from different position of vent pipe, and the gas was dealt with different filters before sampling, thus the concentration of plutonium on the filters was different. The radioactive activity of filters was detected and calculated before research. The main property of spectrum of plutonium in filter was investigated. By analyzing the signal intensity of plutonium in filters, the main spectral lines of plutonium on the membrane were detected, by comparing them with blank samples, the available emission spectral lines of plutonium were selected with the method of t test. Furthermore, the best delay time parameter was determined. By using the proper delay time and detecting condition, the intensity of signals of plutonium was promoted, which is helpful to the determination of plutonium content. Finally, as those samples contain different concentration of plutonium on the filter, by detecting signals of those samples, the standard working curve of uranium was obtained, so quantitative calibration curves within a relatively low concentration range were obtained through the experimental analysis of the filter membrane. The analysis results show that by using the selected spectral lines, namely PuⅡ 443.298 nm, PuⅠ 460.721 nm and PuⅡ 466.389 nm, as the emission intensity of these spectra lines are relatively high, and all of them are free of obstacle spectra lines. The above results indicate that determination bias by using quantitative calibration curves is acceptable, and RSD of the results is less than 3%. These results formed the basis of quantitative analysis of nuclear material by using LIBS technology.