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This research paper aim to investigate the enhancement potential of mesophilic Anaerobic Digestion (AD) of Algerian date palm (Phoenix dactyliferaL.) leaflets from H'miracultivars using an alkaline pretreatment approach. The experiment was conducted for the first time in semi-continuous digesters. NaOH was applied at various percentages (6 %, 12 % and 18 %) to chemically pretreat the substrate for 5 days at 37 °C. The chemical pretreatment results were interpreted for the first time with in-depth FTIR spectroscopic analyses. The Hydraulic Retention Time (HRT) was fixed at 15 days, and the Organic Loading Rate (OLR) at 2 g MO/L/day. The results showed that the methane (CH4) production values were stabilized with a clear distinction at averages of 211.85, 177.26, 143.36 and 123.07 ml of CH4/day, i.e. a CH4yield of 105.92, 88.63, 71.68 and 61.53 ml of CH4/gVS/day for the reactors containing substrates pre-treated with 12 %, 6 %, 18 % NaOH and the substrate without pre-treatment respectively. Compared to the substrate without pre-treatment, the CH4production rates were improved 1.72, 1.44 and 1.16 times for the reactors containing 12 %, 6 % and 18 % NaOH respectively. These findings were perfectly in accordance with FTIR spectroscopy results. These findings demonstrate that the semi-continuous AD process can be an attractive energy recovery solution from such waste compared to batch digesters, (on one day, it produce 77–105 % of the CH4produced during 21–55 days in batch digesters), as well as the importance of adequate pre-treatment prior to the AD. FTIR Spectroscopic analysis technology can also be widely used to analyze pre-treatment data for lignocellulosic biomass, as it gives very encouraging results.