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In order to investigate the combustion phenomena in a combustion chamber of the diesel engine at transient operations, the simultaneous measurements of temperatures of flame and wall surface in a combustion chamber were conducted. The new technique for simultaneous measurements of flame temperature and wall surface was developed. Laser-Induced phosphorescence was used for the measurement of wall surface temperature which was coupled with the flame temperature measurement by a two-color pyrometry. The NOx and soot emissions were also measured simultaneously in transient operations. The relation between the temporal changes of emissions and temperatures of flame and surface wall are discussed. The results show that the temporal change of NOx emission during transient operation is similar to that of the average gas temperature in a chamber. On the other hand, the temporal change of soot emission is similar to neither that of flame temperature nor that of average gas temperature.