Abstract: Aqua regia bath solution samples were used to treat the same bottom solution differently so that the determination of iron and sulfur by inductively coupled plasma emission spectrometer, bismuth and lead by inductively coupled plasma mass spectrometer, and elements such as antimony, arsenic and mercury by atomic fluorescence spectrometer was realized. Its determination accuracy was from 0.001to 0.035 with precision from 0.076% to 8.90%. Three kinds of instruments were used for the test respectively with the same base solution, which achieved the goal of combinatorial and efficient determination of multiple elements. Such method was characterized by simple operation, wide measurement range, low environmental requirements, strong anti-jamming capability, meeting the current requirements of Multipurpose Regional Geochemical Survey Specification (1:250 000) (DZ/T 0258-2014).