A new biosorbent, composed of Amberlite XAD-4 loaded with Anoxybacillus kestanboliensis, was developed and surface morphologies were investigated by SeM and ft-iR. it was used for solid phase column preconcentrations of co(ii) and Hg(ii) before their measurements by icp-oeS. LoDs were calculated as 0.04 and 0.06 ng mL −1 for co(ii) and Hg(ii) respectively. the maximum biosorption capacities were determined as 24.3 and 27.8 mg g −1 for co(ii) and Hg(ii) respectively. preconcentration factors were achieved for Co(II) and Hg(II) as 80. The method validation was performed by analyzing certified reference materials. The new process was successfully utilized for the preconcentration of these metals in various food samples. it should be highlighted that the sensitivity of icp-oeS was critically improved by applying developed method. Hence, ICP-OES could be an effective alternative for icp-MS and/or Gf-AAS.Some metal ions are known to be highly toxic. Therefore, a number of recent studies have focused on metal ion toxicity and carcinogenicity on human beings and other living organisms even at very low levels 1,2 . Among the various types of pollutants, toxic metal ions cannot be easily eliminated from nature 3 . Accumulation of toxic and deleterious metal ions in soft tissues of animals and humans even at low concentrations could be a major concern as they are not metabolized and can create significant damage to the body tissues 4 . Co and Hg are two typical metal ions in environmental samples which are also detected in plants and food samples. Toxicological influences such as vasodilation and cardiomyopathy are reported for Co exposure. Hg is also familiar as it is the most neurotoxic metal ion and can harm most of the human systems 3 .The usage of the biological processes is an idea for the operation of environmental metal pollution. Biological processes for the bioremediation depend on the physical nature of binding sites and chemical conditions 4 . The utilization of biomass, including alive and dead microorganisms in the possibly retention and removal of metal ions from environmental samples, has acquired significant reliability over the past few years due to its efficiency, ecofriendliness and economic choice. The major properties of biosorbents are (a) having a variety of metal binding sites, (b) having small and identical sizes, (c) being less subject to interference from alkali-earth and alkali metals than ion-exchange resins (d) being generally cheaper than functionalized polymers (e) having the possibility to be obtained via green technologies 5 .Concentrations of toxic metal ions are known as trace levels that are lower than the quantification limit of the instruments 6 . The determination, separation and analysis of low concentration of toxic metal ions in natural samples such as soil, food and water have become significant 7 . Therefore, it is necessary to develop analytical methods to preconcentrate and determine trace metal ions 6 .Alternative methods are recommended for the preconcentration and separatio...