Abstract: Measuring the diffusion coefficient of the vaporized solvent in the crystal of the solid phase adsorbent is an important adsorption parameter, and the experimental teaching is difficult to meet the contemporary engineering training objectives. This paper takes the measuring experiment of gas diffusion as the object and extends it to the design and realization of experimental device for measuring the intra-crystalline diffusion coefficient of vaporized solvent in metal organic framework (MOF) (HKUST-1 type) porous materials. It combines the principle of the gas chromatograph FID detector and the principle of measuring the intra-crystalline diffusion coefficient by the zero length column(ZLC) method , puts forward the experimental design scheme, measurement method and data fitting, and makes MATLAB simulation calculation for the ZLC method. During the operation of the experiment, the experimental system is self-built by students according to the experimental principle, integrating the experimental principle, adsorption material loading, data collection and measurement, data analysis and report writing, which practices the “new engineering” talent training concept and improves the achievement of the “new engineering” talent training objectivesaaa.