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Fuel-borne catalysts (FBC) have demonstrated efficacy as an important strategy for integrated diesel emission control. The research summarized herein provides new methodologies for the characterization of engine-out speciated emissions. These analytical tools provide new insights on the mode of action and chemical forms of metal emissions arising from use of a platinum and cerium based commercial FBC, both with and without a catalyzed diesel particulate filter. Characterization efforts addressed metal solubility (water, methanol and dichloromethane) and particle size and charge of the target species in the water and solvent extracts. Platinum and cerium species were quantified using state-of-the-art high resolution plasma mass spectrometry. Liquid-chromatography-triple quad mass spectrometry techniques were developed to quantify potential parent Pt-FBC in the PM extracts. Speciation was examined for emissions from cold and warm engine cycles collected from an engine dynamometer.