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

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.