Heavy metal mining and industrial waste contamination are significant environmental issues that modern civilization has been grappling with for some time. In geological ores, nickel (Ni) fire assay fusion (Ni-FA) and lead (Pb) fire assay fusion (Pb-FA) are the most crucial classical analytical chemistry methodologies used for the collection and determination of platinum group elements (PGEs) and gold (Au) from PGE ore. These classical experiments involve the pre-concentration of PGEs and Au and separation into metallic and silicate phases, which offer high accuracy and high precision with a low limit of detection. Industrial metallurgical and FA processes produce lead-contaminated cupels with high Pb concentrations, posing health risks and environmental pollution if not retrieved. In this study, we discuss waste generated during the PGE separation method, particularly from FA processes. The study explores classical methods and analytical techniques for removing and quantifying Pb, Ni, and other critical minerals from lead and nickel waste streams, considering their potential levels in different environments. The chapter provides an overview of fire assay methods for PGM preparation, current quantification trends, potential environmental impacts, energy storage options, production effort, and hazards. In comparison with the pyrometallurgy approach, studies indicate that hydrometallurgical processing is a more effective way of recovering value-added metals. Lastly, the current status and future perspective on the application of critical minerals, and repurposing for a circular economy have been outlined, indicating the economic viability of recycling.