In-situ TOPO decomposition was accomplished by applying a vacuum at elevated temperatures to a precursor solution in the presence of oxygen, leading TOPO to oxidize to di-n-octylphosphinic acid (DOPA) and octylphosphonic acid (OPA). The mixed ligand system of tetradecylphosphonic acid (TDPA), DOPA and OPA produced CdSe QRs on the order of 4 nm in diameter and 20 nm in length. Solvent and ligand identification was performed by mass spectrometry and (31)P nuclear magnetic resonance spectroscopy. Transmission electron microscopy (TEM) was utilized to determine the morphology, size and crystal growth of the CdSe QRs. This method of CdSe QR synthesis is unique in that the phosphonic acids responsible for anisotropic growth are formed in situ, prior to the nucleation and growth of the nanorods. Without the oxidation of TOPO, CdSe quantum dots (QDs) were synthesized instead, as reported previously. This discovery reinforces the efficacy of DOPA and OPA molecules as critical ligands in the formation of 1-dimensional (1D) nanostructures.