Taking advantage of θ-θ scanning (vertical goniometer) sealed and ceramic X-ray tube full-automatic diffractometer, which can be heated and detected at the same time when the temperature is between normal temperature and 1 200 ℃, and X-ray fluorescence, and combining surface feature with character, high tin bronze mirror which had been daubed “tin amalgam” was detected and analyzed. It can prove that phase with Hg will disappear gradually when the sample is heated to the temperature higher than the boiling point of Hg; It indicates that bronze surface cannot be as a proof of “tin amalgam” used whether it contains Hg, moreover, it is not necessary that bronze mirror is covered with “tin amalgam” in terms of application.