In this paper, a reproducible method for depositing and immobilizing biomolecules of interest on a supporting substrate for biological scanning tunneling microscopy (STM) and atomic force microscopy (AFM) studies is discussed. Adaptations of the thiol-gold chemistry introduced by Nuzzo and Allara (J. Am. Chem. Soc. 1983,105, 4481) are investigated as deposition methods for adsorbing deoxyribonucleic acid (DNA) molecules onto a Au(111) surface. The technique of Auger electron spectroscopy (AES) was utilized for these investigations to determine the amount of adsorption. These results demonstrate that thiol-gold chemistry can be employed for attachment of DNA to gold and illustrate that electron spectroscopy can be used to verify and quantify biomolecule deposition.