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Analytical techniques such as X–ray Fluorescence Spectroscopy (XRF) and Atomic Absorption Spectroscopy (AAS) coupled with statistical package for multivariate analyses were used to characterize silica sand deposit obtained along Cross River in Cross River State, South Eastern Nigeria. Samples were collected from five locations along the river which include: Ikom-Okuni, Obubra-Ofumbogha, Abi-Ediba, Biase-Agwagune and Etung-Effraya. The results of analyses revealed that silicon dioxide (SiO2) forms the predominant metal oxide in the entire samples followed by iron oxides (Fe203), sodium oxide (Na20). Other Oxides such as aluminum oxide (AI2O3), potassium oxide (k2O) etc were also present. Further beneficiation of the silica sand samples gave increased silica dioxide content across all the samples and increase and decrease of other metal oxides. The acid demand value (ADV) and pH value of the silica sand determination revealed a moderately low ADV and neutral pH value of all the samples. A correlation between the mean values of SiO2 and Fe2O3 in all the samples across all the sampling locations showed an inverse relationship between SiO2 and Fe2O3. Furthermore, comparison using population t – test of observed mean of SiO2 and Fe2O3, with their observed minimum standard (90.52%, 0.005%) shows that the silica sand samples from Ediba and Agwagune can be used as a source of SiO2 for glass making due to their high SiO2 and low levels of Fe2O3 content.

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