Cation exchange capacity is a crucial metric for managing soil fertility and promoting agricultural sustainability. An alternative technique for the non-destructive assessment of important soil parameters is reflectance spectroscopy. The main focus of this paper is on how to analyze and predict the content of various soil cation exchange capacities (CEC) in arid conditions (Sohag governorate, Egypt) at a low cost using laboratory analysis of CEC, visible near-infrared and shortwave infrared (Vis-NIR) spectroscopy, partial least-squares regression (PLSR), and Ordinary Kriging (OK). Utilizing reflectance spectroscopy with a spectral resolution of 10 nm and laboratory studies with a spectral range of 350 to 2500 nm, 104 surface soil samples were collected to a depth of 30 cm in the Sohag governorate, Egypt (which is part of the dry region of North Africa), in order to accomplish this goal. The association between the spectroradiometer and CEC averaged values was modeled using PLSR in order to map the predicted value using Ordinary Kriging (OK). Thirty-one soil samples were selected for validation. The predictive validity of the cross-validated models was evaluated using the coefficient of determination (R2), root mean square error (RMSE), residual prediction deviation (RPD), and ratio of performance to interquartile distance (RPIQ). The results indicate that ten transformation methods yielded calibration models that met the study’s requirements, with R2 > 0.6, RPQ > 2.5, and RIQP > 4.05. For evaluating CEC in Vis-NIR spectra, the most efficient transformation and calibration model was the reciprocal of Log R transformation (R2 = 0.98, RMSE = 0.40, RPD = 6.99, and RIQP = 9.22). This implies that combining the reciprocal of Log R with PLSR yields the optimal model for predicting CEC values. The CEC values were best fitted by four models: spherical, exponential, Gaussian, and circular. The methodology used here does offer a “quick”, inexpensive tool that can be broadly and quickly used, and it can be readily implemented again in comparable conditions in arid regions.