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Reduction of particulate emissions from diesel engine is an important theme from the view point of air pollution. Experiments were carried out using a four-stroke single cylinder direct-injection diesel engine. A new method to measure diesel particulates has been developed. Particulates were sampled with a freezing method just behind an exhaust valve and examined through a scanning electron microscope. Shape and structure of particulates and the size distributions are measured under wide operating conditions obtained with above method. The total mass of particulate emissions was measured using a dilution tunnel sampling system. The heat release processes were analyzed using indicator diagrams and the relation between burning condition and particulate emissions were discussed, after systematic experiments under constant revolution speed of 2000 r/min for several load and injection timing conditions.