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The data presented in this article is related to the research article entitled, “Structural Characterization and Evaluation of Municipal Wastewater Sludge (Biosolids) from two Rural Wastewater Treatment Plants in East Texas, USA” (Onchoke et al., [1]). The XRD profiles and composition of biosolids from two wastewater treatment plant is presented. This study describes the composition of XRD crystalline phase patterns of the wastewater sludge. After the removal of the Kα2 peaks the d-spacing and hkl values were determined. In addition, the ion chromatographic profile of the seven anions (normalNO3−, normalNO2−, Br−, Cl−, F−, normalSO42−, and normalPO43−) in biosolids is presented.