In-plane distribution of a target object contained in a sample is measured. The sample dispersedly placed on a substrate is treated to promote ionization of the target object. Then, the mass and flying amount of an ion containing the target object or a component thereof is determined by irradiating an ion beam to the sample and performing time-of-flight secondary ion mass spectrometry of the ion that flies from a portion in the sample where the ion beam is irradiated, and the in-plane distribution of the target object is determined from the mass and flying amount data obtained at plural portions by scanning the beam on the sample plane. The step of treating the sample to promote ionization of the target object includes contacting an aqueous solution of an acid that does not crystallize at ordinary temperature with the sample. A high spatial resolution two-dimensional image can be obtained.