J. Garcla-guinea et al., Examining hydrated minerals using optically stimulated X-ray diffraction, an inexpensive modification of traditional diffractometers, J SED RES, 70(4), 2000, pp. 964-967
Optically stimulated X-ray diffraction (OSXRD) modifies a traditional powde
r XRD by attaching a thermocouple, a precision temperature controller (PID
control), and a thyristor power regulator firing a halogen lamp (75 w, 220
V, red-infrared) that provides up to 210 degrees C to the sample. The inclu
ded OSXRD software allows the diffractometer to be controlled and sequentia
l profiles (ASCII files) to be obtained. These profiles are subsequently pr
ocessed, obtaining new files: (1) Three-dimensional (cps versus 2 theta ver
sus time-temperature), (2) peak areas and (3) maximum 2 theta positions. Th
e automatic temperature control loop, using the proportional-integraI-deriv
ative control (PID) method, and the modifications of the XRD chamber are de
scribed. Some examples of hydrated minerals were examined in the OSXRD prot
otype: (1) the epsomite-hexahedrite phase transition in different isotherma
l analyses (28 degrees C, 30 degrees C, 32 degrees C) and (2) the dehydrati
on of the interfaces of a fibrous aragonite. Three-dimensional plots show t
he epsomite-hexahedrite phase transition in detail. However, in the case of
aragonite (no phase transition) the 3D plot does not show visible changes,
but the graph of peak-areas distribution versus temperature increases in s
inusoidal shape, suggesting steps during the dehydration processes.