Precise temperature control and rapid heating/cooling of infrared spectroscopy samples with a two-stage...

The design and performance of an apparatus for heating and cooling samples during variable temperature infrared spectroscopy studies are described. The apparatus incorporates two thermoelectric device modules in a stacked configuration. The cascaded devices are powered in parallel and contained within a metal enclosure that maintains their alignment and applies clamping pressure between them to maximize thermal conductivity. By using this apparatus, sample temperatures can be increased or decreased at 2 °C s^-1 rates and isothermal temperatures can be maintained precisely (±0.1 °C). The rapid heating and cooling capabilities of the apparatus facilitate programmed temperature step heating/cooling profiles with isothermal infrared spectrum measurements at pre-selected temperatures. Using linear heating and cooling temperature ramps, subtle temperature-dependent poly(styrene) infrared spectrum changes are elucidated and correlated with sample temperature. Results obtained by using a temperature step sample heating profile are compared with those obtained by using linear temperature ramp heating and cooling to characterize silica gel dehydration and re-hydration processes. By comparing infrared spectra acquired at different temperatures while heating and cooling the sample, silica gel spectrum changes associated with water desorption/adsorption and the thermal expansion/contraction of the Si-O-Si network are differentiated.