In this research, the appropriateness of alkali pre-treatment on coconut by-products was managed by exposing coconut husk and shell to 2M NaOH. The powdered samples were analysed for morphology observation, Fourier Transform Infrared (FTIR), Particle Size Analyzer (PSA), and water quality tests. Weakening the hemicellulose structure resulted from subjecting the coconut shell to alkali pre-treatment shown in the morphology observation. Furthermore, the FTIR analysis exhibited the presence of O-H stretch in all pre-treated samples representing an indication for occurring the lignin breakdown, while an absence of the C=O functional group was shown in both additive samples after their subjection to alkali pre-treatment. In PSA analysis, the particles of all samples were found finer than the particle size distribution standards, in which the smallest D50 was obtained for the treated coconut shell (TCS), followed by untreated coconut shell (UCS), untreated coconut husk (UCH), and treated coconut husk (TCH). Among all the powdered samples (TCS, UCS, UCH, and TCH) analysed in this study, only TCH values met the ranges provided and recommended by the Urban Stormwater Management Manual for Malaysia (MSMA) and the Australian Department of Sustainability, Environment, Water, Population, and Communities (DSEWPC). Meanwhile, a poor removal rate for total suspended solids (TSS) was attained due to the contribution of TSS by the filter media which caused the TSS rates to surpass the inlet values. Additionally, the presence of a high concentration of total phosphorous (TP) in all the tested samples indicated their capabilities to provide PO43 in the bioretention cell, which is a vital nutrient for the plant’s growth. In contrast, Ammoniacal Nitrogen (AN) with a concentration rate as low as 4 mg/L was observed throughout the test periods which showed a significant reduction compared to the rate of AN at the inlet samples ranged between 5.2 and 11.4 mg/L. The findings indicated that coconut by-products, when subjected to an alkali pre-treatment process, are appropriate for incorporation as additives in bioretention filter media.