This research focused on optimizing a protocol to acquire 2D NMR data correlating carbons and hydrogens within a molecule. Additionally, this NMR experiment would be used in tandem with 1H, 13C, DEPT, COSY and other 2D NMR techniques to contribute to the identification of unknown organic compounds. This would then be incorporated into an undergraduate organic chemistry laboratory course. Pulse programs HSQCEDETGP and HSQCETSPISP were tested using an SEI probe. HSQCEDETGP was chosen for its ability to represent various degrees of hydrogen substitution. Ideal parameters, including sw, o1p, o2p, TD, RG, NS, and DS were tested and determined based on spectral quality and acquisition time. HSQC has proven beneficial in the assignment and/or confirmation of carbon and hydrogen peaks for 2,4-dichlorotoluene, 3,3-dimethyl-2-butanol, 1-penten-3-ol, allyl phenyl ether, and γ-valeractone. Allyl phenyl ether, 2,4-dichlorotoluene, and γ-valeractone, require additional spectral data for complete identification.