A compact, transportable, thermoelectrically cooled cold stage for reflection geometry X-ray powder diffraction

Abstract

A cold stage for Bragg–Brentano geometry X‐ray powder diffraction is described for use in the temperature range from about 250 to 300 K. The stage is constructed in such a way that it may be removed from the diffractometer and pre‐cooled to its base temperature before the sample is loaded. After loading, thermoelectric cooling maintains the specimen at low temperature (ice free) whilst the body of the stage is allowed to return to room temperature prior to remounting on the diffractometer.

Structure, thermal expansion and incompressibility of MgSO4·9H2O, its relationship to meridianiite (MgSO4·11H2O) and possible natural occurrences

“…Stable low-temperature measurements were achieved using a thermoelectrically cooled cold stage (Wood et al, 2012). This portable cold stage was held in a plastic box filled with dry-ice pellets whilst the powder specimen was prepared and loaded.…”

Structure, hydrogen bonding and thermal expansion of ammonium carbonate monohydrate

“…The initial identification of these crystals was carried out using X-ray powder diffraction methods, for which purpose the crystals were ground to a powder in a stainlesssteel pestle and mortar under liquid nitrogen. The measurements were performed on our custom-made portable cold stage (Wood et al, 2012); this device was pre-chilled in a chest freezer at 250 K before being loaded. The stage's Peltier cooling device was connected to a power supply in the X-ray diffractometer enclosure within 30 s of leaving the cold room, ensuring that the specimen did not warm substantially above 253 K prior to the start of the measurement.…”

P–V–Tequation of state of synthetic mirabilite (Na2SO4·10D2O) determined by powder neutron diffraction

“…In order to test these hypotheses, we made X-ray powder diffraction measurements on samples of Na 2 SO 4 Á10H 2 O and Na 2 SO 4 Á10D 2 O (both prepared as described in x2) mixed with a CaF 2 standard. Each measurement was made at 248 AE 1 K on a PANalytical X'Pert Pro multipurpose powder diffractometer (using Gemonochromated Co K 1 radiation, = 1.788996 Å , and an X'Celerator multi-strip detector) equipped with a thermoelectrically cooled cold stage (Wood et al, 2012). Refinement of the unit-cell parameters revealed an extremely small difference in molar volume, ÁV/V = 0.06 (2)%, with the protonated species having the larger molar volume.…”