Semi-volatile organic compounds (SVOC) are a group of compounds in engine exhaust that either form during combustion or are part of the fuel and lubricating oil. Since these compounds occur at very low concentrations in diesel engine exhaust, the methods for sampling, handling, and analyzing these compounds are critical to obtaining good results. An improved dilute exhaust sampling method was used for sampling and analyzing SVOC in engine exhaust, and this method was performed during transient engine operation. A total of 22 different SVOC were measured using a 2012 medium-duty diesel engine. This engine was equipped with a stock diesel oxidation catalyst (DOC), a diesel particulate filter (DPF), and a selective catalytic reduction (SCR) catalyst in series. Exhaust concentrations for SVOC were compared both with and without exhaust aftertreatment. Concentrations for the engine-out SVOC were significantly higher than with the aftertreatment present. Distribution of the SVOC between semi-volatile- and particulate-phase depended on the number of aromatic rings, the molecular weight, and the volatility of the compounds detected.