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Syntheses in organic solvents provide access to a wide range of copper-based materials and nanoparticles [1].However,the correlation between organic reactions in solution and nucleation and growth of nanoparticles is not well understood.Here,we utilize the Multivariate Curve Resolution–Alternative Least Square(MCR-ALS)methodology [2,3] to examine spectroscopic data recorded in situ during synthesis of copper-based nanoparticles [4].