| Summary: | This work was on the comparative evaluation of the property effects obtainable when acetylation is applied to parts of selected agro fibers that are obtainable within common localities. The fibers were subjected to different concentrations of acetylation treatment at ambient temperature for 3 h. The physico-chemical, morphological, and tensile properties of the fibers were examined after the treatment. It was discovered from the results that the procedures variedly influenced the constituents of the fibers, their resulting tensile properties as well as their post-acetylation treatment surface morphology. The proportion of crystalline cellulose in the starting fibers greatly influenced their post treatment composition, behaviour and properties. The results show that plantain fibers had the highest aspect ratios, followed by banana fibers with values of about 1000 and 417, respectively. These fibers exhibited the least density and are thus potential plant fibers for composite development. Banana fiber had the least density of about 1.38 g/cm<sup>3</sup> while that of <i>Dombeya</i><i>Buettneri</i> fiber possessed the highest value of 1.5 g/cm<sup>3</sup>. There was significant enhancement in the hemicellulose content of <i>Combretum Racemosum</i>, while the lignin content of the plantain fibers was highly reduced. The treatment favoured the enhancement of the tensile properties in <i>Combretum Racemosum</i> fibers, which had enhanced tensile strength and strain at all compositions of the treatment. Optimum tensile strength and strain values of 155 MPa and 0.046, respectively, are achieved at 4% composition. <i>Dombeya Buettneri</i> fibers showed the highest ultimate tensile strength among the plant fibers in the untreated condition, which was gradually decreased as the concentration of the reagents was increased. Overall, 4% acetylation treatment is optimum for tensile properties’ enhancement for most of the natural fibers evaluated.
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