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Diesel exhaust is a complex mixture of combustion products of diesel fuel, and the exact composition of the mixture depends on the nature of the engine, operating conditions, lubricating oil, additives, emission control system, combustion parameters and fuel composition. In a diesel engine, NOx (NO & NO2) and PM (Particulate Matter) are the most critical constituents for the emission legislation. In order to control the PM emission of diesel engine and comply with increasingly stringent exhaust legislation, more information is required on the components and genesis of PM. In general, PM from diesel engines is classified into two fractions: Insoluble Organic Fraction (ISOF) and Soluble Organic Fraction (SOF). In this experimental study, a series of 13 mode ESC cycle were run on a light duty diesel engine after optimization of combustion parameters (Injection Pressure, Injection Timing, Multiple Injections, EGR rate, etc) in successive tests and PM component was analyzed.