In this study, glycerol as an abundant green feedstock was used as a hydrogen source to investigate the reaction of water-glycerol solution decomposition by microwave-assisted catalytic to produce hydrogen over NiO/zeolite catalyst. The catalyst was prepared by inception wetness and then characterized through X-ray diffraction (XRD), scanning electron microscopy (SEM), Energy diffraction X-ray (EDX), and transmission electron microscope (TEM) measurements. The conversion process of glycerol into hydrogen was performed in a fixed-bed microwave-assisted reactor. Effect of microwave power, NiO content, and feed flow rate (FFR) on glycerol conversion and hydrogen selectivity were studied. The results of XRD and EDX measurement showed that NiO crystalline exists on the catalyst sample. The particle size of NiO/zeolite was determined in the range of 30–300 nm, and the particle was found well dispersed on the zeolite surface as confirmed by TEM. Furthermore, the maximum conversion rate can achieve about 96.67 %, while the highest hydrogen production was found up to 73.5 % with the condition of 20% of NiO as an active site on natural zeolite. It was found that the NiO content of 20% gave the best glycerol conversion at the microwave power of 600 W and FFR 0.5 ml/min. Microwave-assisted catalytic irradiation of glycerol appears to be a promising candidate for the production of H
2
from an aqueous glycerol solution.