Homogeneous nucleation of CaSO4. 2H(2)O (gypsum) based on an optical diagnostic technique was studied within a supersaturation range of 1-4 at 25-90 degrees C. The experiments were carried out using an experimental apparatus consisting of a batch crystallizer with the related measurement devices. Signals of scattered and transmitted light coming from a He Ne laser source were analyzed to measure the induction period (t(ind)), that is, the time delay necessary for homogenous nucleation to take place. As expected from theory, it was found that t(ind) decreases when either temperature or supersaturation increase; from the dependence of t(ind) on supersaturation, it was possible to distinguish between the mechanism of homogenous and heterogenous nucleation. From the experimental data relative to homogeneous nucleation, the interfacial tension (gamma(s)) between CaSO4. 2H(2)O and the surrounding aqueous solution and the activation energy (E-att) for CaSO4. 2H(2)O crystallization were evaluated. In particular, the dependence of t(ind) on temperature made it possible to evaluate E-att at 30 kJ/mol and the dependence of t(ind) on supersaturation offered the value of gamma(s) to be about 37 mJ/m(2), which does snot vary with temperature in the interval explored

Measurements of the induction period for gypsum nucleation, when citric acid is added in solution as an additive to retard calcium sulfate nucleation, are reported in the present paper. The supersaturation ratio was varied in the interval 4-5; the concentration of citric acid was varied from 0.01 to 0.30 g/L; and, finally, different temperature levels were explored in the range 15-45 °C. The induction period values were compared to those previously obtained by using the same experimental technique in the absence of foreign ions in the mother liquor, showing that the citric acid has a strong retarding effect toward gypsum nucleation. Eventually, several values for the interfacial tension and activation energy have been estimated as a function of citric acid concentration and of temperature.

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The effect of nitrilotrimethylenephosphonic acid (NTMP) on calcium sulfate dihydrate nucleation has been studied at 25 °C in a batch crystallizer with a related optical device. This paper reports the measurement of the induction period done under different supersaturation ratios ranging from 2.60 to 4.99, while varying the NTMP concentration in the interval 0.005−0.1 g/L. The comparison of the interfacial tension values estimated in the presence of NTMP with respect to those previously obtained without any additive in the mother liquor and in the presence of citric acid, by using the nucleation-controlled mechanism, suggests that NTMP is more effective in retarding gypsum nucleation than citric acid. Besides, the examination by optical microscopy of the crystals formed indicates that NTMP also modifies the crystal habit of gypsum, resulting in less elongated platelike particles.