Results of thermal analysis in CsH2PO4 (CDP) and RbH2PO4 (RDP), using
combined differential scanning calorimetry (DSC) and high-resolution a
c calorimetry, are presented. For single crystal samples, a sequence o
f phase transitions in both salts above room temperature is found that
is very dependent of their thermal treatments. For CDP, the ac data s
how a broad heat capacity anomaly near T1 = 420 K for freshly prepared
samples at room temperature or non-annealed samples above T2 = 500 K,
and an endothermic peak at T2 on heating runs and at 470 K on cooling
runs. For RDP, much more variations were observed in the region where
two transitions were previously reported for different prepared sampl
es that occurred near 352 K and 380 K, respectively.