The increase in nitrogen oxides has been pointed out in the first cycle of the spark ignition engines. The new test equipment is developed in order to clarify this fact. The combustion gas in the first cycle is introduced in the chamber where argon gas filled with, by means of the fast sampling valve installed in exhaust pipe. Nitrogen oxides in the combustion gas chemically frozen in argon gas are measured by the NOx analyzer. It is shown that the data of nitrogen oxides are rational and that this new measuring technique is effective.