By means of a thermogravimetric analysis coupled with mass spectroscopy, the catalytic effect of ferrous sulfate on the pyrolysis of African Palm husk (APH) was studied. Thermogravimetric data were adjusted to the distributed activation energy model (DAEM) with four pseudo-components. Ferrous sulfate had a strong influence on the decomposition parameters of the second and fourth pseudo-components of the DAEM, which are identified as hemicellulose and lignin, respectively. The profiles of the signal intensity curves for the selected m/z ratios were successfully modeled using the kinetic parameters obtained by adjusting the thermogravimetric data. It was found that ferrous sulfate promotes the formation of fragments of m/z = 64, 95, and 96, corresponding to molecules, such as SO2, hydrocarbon ions of general formula [CnH2n‑3]+, and furfural, respectively.