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Advancement in industrialization and urbanization is a good indicator of the progress of humanity. However, it has an evil side as well. This advancement is identified as being responsible for deleterious effects on the health of human beings and aquatic biodiversity. Anthropogenic activities like mining and disposal of treated/untreated waste effluents containing toxic metals have resulted in severe deterioration of water quality, rendering serious environmental problems. The basic problem is that the wastewater generated through industries is not given the necessary pretreatment and is discharged directly into water resources. The metals beyond their permissible limits cause maximum negative impacts owing to their long biological half-lives and nondegradable nature. The condition is further worsening in economically deprived countries, where this metal-contaminated wastewater is directly used in various agricultural and day-to-day practices. As a solution to this, the extraction and removal of toxic metal ions from these polluted water resources at an industrial level is of paramount importance. This chapter provides the enthusiastic efforts of the scientific community to disseminate the fundamentals and practices of green analytical methods for metal removal. These methods are based on solid-phase extraction using functionalized silica gel for the separation and preconcentration of metal ions in polluted water resources. Ease of synthesis and extensive application of these organic-inorganic hybrid materials helps to fulfil the commitment of continual environmental improvement by remediating the wastewater.

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