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Partially premixed low temperature combustion (LTC) in diesel engines is a strategy for reducing soot and NOX formation, though it is accompanied by higher unburned hydrocarbon (UHC) emissions compared to conventional mixing-controlled diesel combustion. In this work, two independent methods of quantifying light UHC species from a diesel engine operating in early LTC (ELTC) modes were compared: Fourier transform infrared (FT-IR) spectroscopy and gas chromatography-mass spectroscopy (GC-MS). A sampling system was designed to capture and transfer exhaust samples for off-line GC-MS analysis, while the FT-IR sampled and quantified engine exhaust in real time. Three different ELTC modes with varying levels of exhaust gas recirculation (EGR) were implemented on a modern light-duty diesel engine. GC-MS and FT-IR concentrations were within 10 % for C2H2, C2H4, C2H6, and C2H4O. While C3H8 was identified and quantified by the FT-IR, it was not detected by the GCMS.