Abstract: This paper briefly introduced the principle and operation method of tin determination in sludge disposal of cement kilns by using atomic fluorescence spectrophotometer, and focused on the optimization of experimental conditions, such as type and optimum concentration of melting sample acid and carring fluid acid, reducing agent, carrier gas and shielding gas, etc. The results showed that the method was simple, flexible, less interference and good reproducibility. The detection limit was as low as 0.30 μg/L, and the detection ability was greatly improved, which solved the problem that it was difficult to determine the content of tin in sludge by cement kiln.