This work assesses the potential of the adsorptive material nano zirconium oxide/boron oxide (ZrO2/B2O3) for removal of trace Mn(II) and Ni(II) from environmental samples. This method is based on the sorption of Mn(II) and Ni(II) ions directly onto nanosorbent, followed by the elution and determination by flame atomic absorption spectrometry (FAAS). Experimental parameters, including pH of sample solution, volume and concentration of eluent, sample volume, and flow rate of sample solution, that affect the recovery of the Mn(II) and Ni(II) ions from model solutions have been optimized. Under the optimum conditions, adsorption isotherms and adsorption capacities have been examined. The recoveries of Mn(II) and Ni(II) were 96% +/- 2% and 95% +/- 3% at 95% confidence level, respectively. The analytical detection limits for Mn(II) and Ni(II) were 1.9 and 4.9 mu g L-1, respectively. Adsorption capacities of the nano ZrO2/B2O3 were found as 92.8 mg g-1 for Mn and 168.4 mg g-1 for Ni. The accuracy of the method was checked by analyzing certified reference material (SPS-WW1 wastewater) and spiked real samples. The method was applied for the determination of analytes in water samples.