Self-assembeld monolayers (SAMs) formed by the adsorption of 4 '-nitro-1,1-biphenyl-4-thiol (NBT) on gold substrates were studied using infrared reflection-absorption spectroscopy (IRRAS). The IRRAS results revealed that the straightforward approach for the fabrication of SAMs. namely, immersions of the gold film in organothiol solutions, leads to the formation of highly oriented SAMs. To prepare highly oriented amino-terminated SAMs, the vitro-terminated SAMs were immersed into ZnCl2/HCl solution to chemically convert the nitro group to an amino group. IR spectra recorded for this conversion revealed that the conversion is completed after a fairly short period of time (45 min.), immersion for longer lime results in the etching of the SAMs by the acidic solution.