The preparation of ayurvedic bhasma is particularly challenging, as mass production in modern facilities often lacks the standardized equipment needed to ensure consistent quality, leading to concerns about toxic elements like mercury and arsenic in the final products. Addressing these concerns necessitates the standardization of the synthesis process through the implementation of stringent quality control measures at every stage of preparation. This study is dedicated to the synthesis and comprehensive characterization of lauha (iron) bhasma, employing both traditional methodologies and advanced analytical techniques. The synthesis process began with samanya shodhana (general purification), followed by vishesh shodhana (special purification) and marana (incineration) The resultant product then underwent amrutikaran, involving heating with aloe vera extract at an elevated temperature of 750°C.The synthesized lauha bhasma was meticulously characterized using a combination of classical Ayurvedic techniques and modern analytical methods, including Fourier Transform Infrared Spectroscopy (FTIR), Atomic Absorption Spectroscopy (AAS), X-ray Diffraction (XRD), Brunauer-Emmett-Teller (BET) surface analysis, Scanning Electron Microscopy (SEM), Particle Size Distribution (PSD), and Energy Dispersive X-ray (EDX) analysis. The final product, post-Amrutikaran, successfully passed all traditional Ayurvedic evaluations, affirming the proper formation of bhasma. XRD analysis revealed the formation of rhombohedral α-Fe₂O₃ with only trace amounts of free iron, indicating high purity. SEM and PSD analyses demonstrated the creation of nanosized particles ranging from 50 to 200 nm, complemented by a specific surface area of 12.55 m²/g as determined by BET studies. Crucially, EDX analysis confirmed that the amrutikaran process effectively eliminated mercury from the bhasma, ensuring its safety and compliance with stringent quality standards.