Background: Manahsila (Realgar; Arsenic Disulfide) is an important mineral drug in Ayurvedic Rasa Shastra. Due to its inherent toxicity, classical Ayurvedic texts recommend Shodhana (purification) before its therapeutic use. Although Shodhana is believed to reduce harmful impurities and improve the safety and quality of the drug, scientific evidence validating these transformations remains limited. Objective: The present study aimed to scientifically evaluate the physicochemical changes occurring in Manahsila before and after Shodhana using X-ray Fluorescence (XRF) and X-ray Diffraction (XRD), thereby providing analytical evidence for the Ayurvedic purification process. Methods: Raw Manahsila was subjected to Shodhana according to the classical Ayurvedic procedure. Both untreated and purified samples were analysed using XRF to determine elemental composition and XRD to investigate crystalline phase characteristics. The analytical findings obtained before and after Shodhana were comparatively evaluated. Results: XRF analysis demonstrated variations in the elemental composition following Shodhana, indicating the possible removal or reduction of extraneous impurities while preserving the principal constituents of Manahsila. XRD analysis revealed that the characteristic crystalline structure of realgar was largely retained after purification, with minor variations in peak intensity and crystallinity that may reflect structural modifications induced during the purification process. These observations suggest that Shodhana primarily improves the physicochemical quality of the material without causing significant alteration of its fundamental mineral phase. Conclusion: The findings provide scientific support for the classical Ayurvedic concept of Shodhana by demonstrating measurable physicochemical changes in Manahsila. XRF and XRD proved to be valuable analytical tools for the standardization and quality assessment of purified mineral drugs. The study contributes to the scientific validation of traditional Ayurvedic purification procedures and may facilitate the development of standardized and safer Rasaushadhi formulations.