Abstract: In the mass production of lithium-ion batteries, it is difficult to stabilize the concentration of N-methylpyrrolidone (NMP) in stationary pollution source exhaust due to significant fluctuations in operating conditions, making the on-site sampling and verification operations complicated. Based on the characteristics of high moisture content of exhaust gas from lithium-ion battery production and NMP recovery process, a dynamic NMP gas generation device was designed to produce NMP standard gas with stable concentration and moisture content. A solid-phase adsorption tube sampling-thermal desorption-gas chromatography method was established to determine NMP concentration. After optimization, when the sampling volume of stationary pollution source exhaust was set to 300 mL, the method detection limit of NMP reached 0.004 mg/m³, and the minimum quantitative detection limin was 0.016 mg/m³, meeting the requirements of sensitivity and detection limit.