Hydrazine is derived with excessive furfural. The crystal of hydrazine derivative conversion is characterized by mass spectrometry. The comparative analyses are made between the hydrazine-derived furfural crystal, solvent, as well as extraction solution of furfural derivatives of hydrazine by the method of capillary gas chromatography. Reliable qualitative and quantitative analytical information is obtained, and the conditions of derivation, extraction and chromatographic analysis are optimized. The method is evaluated by standard curve, precision and accuracy tests. Experiments show that in the case of excessive furfural, hydrazine is completely converted to 2-furaldehyde azine, whose retention time is 6.20 min. The detection limit of the method is 0.007 8 mg/L, the relative standard deviation is 2.5%, and the recovery is in the range of 98% to 100%. The method has the advantages of symmetrical peak shape, high accuracy, high sensitivity and good selectivity. It provides a rapid and accurate procedure for the analysis and determination of hydrazine under different laboratory instruments and chromatographic column conditions.