Cellulose nanocrytals and chitin nanocrystals respectively were isolated from bioresidues viz, sludge from special cellulose production and crab shell waste using acid hydrolysis. The atomic force micrscopy images showed that the diameter of CNWs ranged from 10 - 20 nm and chitin whiskers ranged from 20 - 40 nm. Thermal degrdation temperatures of nanocellulose and nanochitin whiskers were found to be 186 °C and 234 °C respectively. The crystallinity index of CNWs was 72.3 % while that of chitin nanowhiskers was as high as 87.2 %. Conductivity titration and zeta sizer studies proved the high surface charge of both CNWs and chitin nanowhiskers. Besides, chitin nanowhiskers are positively surface charged at acidic pH and negatively surface charged at alkaline pH. ICP-MS (inductively coupled plasma mass spectrometry) and XPS (X-ray photoelectron spectroscopy) will be conducted to evaluate the adsorption potential of CNWs and chitin nanowhiskers to heavy metal ions as functions of pH and surface charge.