The resonance fluorescence of iron, cobalt, and nickel atoms in air-hydrogen, air-acetylene, and hydrogen-oxygen-argon flames has been measured with a modified Techtron AA-4 atomic absorption spectrophotometer. High intensity, hollow cathode lamps are used as primary excitation sources. Fluorescence spectra are studied in detail and the strongest fluorescence emission is observed at 2483, 2407, and 2320 A, for iron, cobalt, and nickel, respectively. The effects of source parameters, optical arrangement, uptake of the sample solution, organic solvents, inorganic acids, and of 13 other elements are investigated. A comparison was made between the total consumption atomizer-burner and the Techtron premix system. The premixed hydrogen flame was used for atomic fluorescence measurements of methyl isobutyl ketone extracts of iron, cobalt, and nickel chelates with ammonium pyrrolidine dithiocarbamate. Practically the same detection limits of 0.02, 0.01, and 0.003 ppm of iron, cobalt, and nickel, respectively, were found for aqueous solutions both in premixed hydrogen-oxygen-argon and turbulent air-hydrogen and hydrogen-oxygen-argon flames. Using extraction method, detection limits of 0.0002, 0.0004, and 0.0001 ppm of iron, cobalt, and nickel, respectively, were obtained. © 1969, American Chemical Society. All rights reserved.