Guest molecules in layered double hydroxides (LDHs) may
be located
both on the surface and in the interlayer gallery. In this work, a
comparative study of various IR spectroscopic methods coupled with
X-ray diffraction (XRD) is presented, which makes it possible to distinguish
between the two possibilities. During the experimental work, first,
CaAl-LDHs intercalated with nitrate/carbonate ions were transformed
to d-gluconate- and benzoate-containing solids. Depending
on the initial interlayer ion, the organic molecules may end up between
the layers and/or on the surface of the LDH. The IR spectra of the
specimens were recorded by using four different techniques, which
are different in their penetration depth (photoacoustic spectroscopy
(PAS), attenuated total reflectance (ATR), diffuse reflectance IR
spectroscopy (DRIFTS), and wide angle diffuse reflectance (WA-DRIFTS)).
By comparing the spectra obtained, the anionic species that are surface
adsorbed to LDHs were proven to be distinguishable from those intercalated
in the interlayer gallery. PAS spectra are shown to provide information
about interlamellar and bulk compounds. The screening of the surface
species could be performed using the WA-DRIFTS technique, while ATR
and DRIFTS are capable of detecting both the surface and the bulk
anions residing in the top few layers.