ABSTRACT This paper discusses the ability of the fly ash (FA) and abmbient cured Alkali activated Fly ash geopolymer (FAAG) for sequestering Pb (II) ions from aqueous solution. Various physiochemical properties such as the influence of pH and contact time were investigated for achieving the conditions for maximum removal via batch mode using powdered samples. The adsorbents were characterized by employing powder X-Ray diffraction, Attenuated Total Reflection Fourier Transform Infra-Red spectroscopy, and Scanning Electron Microscopy/EDAX before and after the treatment. The adsorption capacity of Pb2+ ions by raw FA and FAAG were examined by the Inductively coupled plasma mass spectrometry (ICP-MS). The results represented that the maximum adsorption capacity of Pb2+ ions by FAAG is 75 mg/g with attained equilibrium time of 120 min whereas raw fly ash at 150 min at 21.5 mg/g capacity. The pozzolanic reactivity of fly ash in water glass hardening resulted mainly N-A-S-H gel and traces of lead silicate due to the immobilization of lead in the network. This was conformed from the binding energy lines at 139.7 eV in XPS survey lines and lead silicate at 25 and 34° 2θ as identified in XRD phase assemblages. ICP-MS test results of leachate of lead immobilized geopolymer sample are devoid of lead ions and thus sorption sites of fly ash geopolymer lead to potential safety disposal of lead. Thus, recycling of fly ash into geopolymer by less energy intensive process and subsequent use in heavy metal disposal could achieve the concept of disposal waste and recycling, which could contribute to achieve the sustainable goals.