Extraction and depolymerisation of chitin and chitosan from prawn shells was carried out using various chemical procedures. Sodium hydroxide and hydrochloric acid solutions were used for deproteination and demineralisation, respectively, while acetone was used for decolourisation. The amount of chitin and subsequently chitosan obtained was ∼35% and 25% respectively of the dry weight of the shells. The chitin was deacetylated using sodium hydroxide at 100 °C and the influence of the concentration of the reagent and duration of the reaction was investigated. The degree of deacetylation (DD) of the chitosan was evaluated by FTIR and NMR spectroscopy and the molecular mass distribution was determined by Gel Permeation Chromatography. It was found that the final DD was significantly higher using 50% sodium hydroxide solution (73% ± 9%) compared to 25% sodium hydroxide solution (40% ± 5%). It was noted also that the deacetylation reaction was more than 80% completed after 2 h but the chitosan produced had higher molecular mass while chitosan produced after 10 h had lower molecular mass and higher degree of deacetylation. The molecular mass distribution was bimodal for all the samples and consisted of a broad high molecular mass peak (peak 1) and a sharp low molecular mass peak (peak 2). The Mw of peak 1 decreased from ∼1.3 × 106 after 2 h reaction with sodium hydroxide to 3.1 × 105 after 10 h reaction indicating that depolymerisation and deacetylation occurred simultaneously. Peak 2 had a Mw of ∼2.4–9.9 × 103.