Abstract— Techniques and instruments for measuring the luminescence, fluorescence. and phosphorescence of proteins and nucleic acids are described. Emphasis is placed on the principles of the instruments and the procedures which are necessary to measure quantitatively the luminescence from biological macromolecules at 77°K. Examples are given of the effect of denaturation on luminescence of both proteins and nucleic acids. on ways in which the luminescence can be associated with particular constituents, and finally on the influence that electronic energy transfer has on the excitation spectra of protein luminescences. These examples typify the relationship of luminescence spectra to the conformation and constitution of macromolecules.