Initial results are presented for a novel experimental arrangement whi
ch allows the successful study of laser-desorbed neutral species under
matrix isolation conditions. In the current work, a pulsed carbon dio
xide laser (10.6 pm) is employed for laser desorption. With the combin
ation of a previously described cryogenic trapping technique with coax
ial matrix isolation gas (xenon or argon) introduction, laser-desorbed
neutrals have been matrix isolated and their Fourier transform infrar
ed spectra recorded. Two different cinnamic acid derivatives (p-coumar
ic acid and sinapinic acid) typically employed for matrix-assisted las
er ionization (MALDI) mass spectrometry were utilized to demonstrate t
his new technique. Experimental conditions were determined for optimal
matrix isolation of the laser-desorbed species. Two different desorpt
ion geometries were examined with respect to their effectiveness for m
atrix isolation of desorbed neutrals. A covalent dimer of p-coumaric a
cid produced in an external UV photoreactor and thought to be a possib
le photoreaction product in UV MALDI was studied by this technique. Th
ermal degradation of this dimer is shown to occur above threshold irra
diance for laser desorption.