This study was aimed at determining the effect of methanol-containing additive (MCA) on the emission of carbonyl compounds (CBCs) generated from the diesel engine, For this experiment, a heavy-duty diesel engine was connected with a full flow critical flow ventri (CFV) type dilution tunnel, a Schenck GS-350 DC dynamometer, and a DC-IV control system in series, The operating conditions of the heavy-duty diesel engine for both cold-start and hot-start Transient Cycle tests and for both low-load and high-load steady-stare tests were ascertained, The exhaust of CBCs collected from a 2,4-dinitrophenylhydrazine (2,4-DNPH)-coated cartridge were first converted to corresponding hydrazone derivatives, which were then solvent-eluted and analyzed by a High Performance Liquid Chromatograph (HPLC) with an ultraviolet-visible (UV) detector, When either 10% or 15% MCA was used, the emission factors of the CBCs acrolein and isovaleraldehyde increased by at least 91%. Accordingly, future studies must be done to cut down the emission of CBCs when MCA and methanol alternative fuels are used,