The paper describes the use of attenuated total reflection fourier transfor
m-infrared (ATR FT-IR) microspectroscopic techniques for the verification o
f the structure of chemical compounds synthesised on polystyrene beads in c
ombinatorial chemistry. A six step reaction sequence is characterised compl
etely by infrared (IR) spectroscopic investigations of single beads. Incomp
lete reactions or the occurrence of side products are clearly indicated. Qu
antitative information can be extracted with high precision using absorptio
n bands of the polymer matrix as internal standard. Compared to other IR te
chniques, the ATR micro IR technique shows clear advantages with respect to
sensitivity and resolution. The technique has the potential to be used for
the characterisation of single beads in split and combined synthesis techn
iques. (C) 1999 Elsevier Science B.V. All rights reserved.