The methyl isobutyl ketone-dimethyl benzene solution of sample was emulsified into emulsion by emulsifier Triton X-100. The standard addition method was used to determine with polyisobutylene emulsion as the reference. An analytical method for rapid determination of iron and nickel in crude oils by FAAS had been developed. A principle and method of preparing blank solution had been advanced. Choices of solvent and emulsifier, preparing blank solution were studied. The determination results were consistent with those obtained by ashing method-FAAS.