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Synchrotron-based small- and wide-angle X-ray scattering (SAXS/WAXS) was used to examine in situ the precipitation of gypsum (CaSO4·2H2O) from solution. We determined the role of (I) supersaturation, (II) temperature and (III) additives (Mg2+ and citric acid) on the precipitation mechanism and rate of gypsum. Detailed analysis of the SAXS data showed that for all tested supersaturations and temperatures the same nucleation pathway was maintained, i.e., formation of primary particles that aggregate and transform/re-organize into gypsum. In the presence of Mg2+ more primary particle are formed compared to the pure experiment, but the onset of their transformation/reorganization was slowed down. Citrate reduces the formation of primary particles resulting in a longer induction time of gypsum formation. Based on the WAXS data we determined that the precipitation rate of gypsum increased 5-fold from 4 to 40 °C, which results in an effective activation energy of ~30 kJ·mol−1. Mg2+ reduces the precipitation rate of gypsum by more than half, most likely by blocking the attachment sites of the growth units, while citric acid only weakly hampers the growth of gypsum by lowering the effective supersaturation. In short, our results show that the nucleation mechanism is independent of the solution conditions and that Mg2+ and citric acid influence differently the nucleation pathway and growth kinetics of gypsum. These insights are key for further improving our ability to control the crystallization process of calcium sulphate.We acknowledge support by the CSIC Open Access Publication Initiative through its Unit of Information Resources for Research (URICI).This work has been carried out within the framework of the project CGL2010-16882 of the\udSpanish MINECO. Mercedes Ossorio acknowledges the JAE-Predoc fellowship. This work was partially supported\udby a Marie Curie grant from the European Commission in the framework of the MINSC ITN (Initial Training\udResearch network), Project No. 290040. We thank Diamond Light Source for access to beamline I22 through a\udgrant to Liane G. Benning, Alexander E.S. Van Driessche, Mercedes Ossorio and Juan Diego Rodríguez-Blanco\udThis research was partially made possible by Marie Curie grant from the European Commission in the framework\udof NanoSiAl Individual Fellowship, Project No. 703015 to Tomasz Stawski. Tomasz Stawski and Liane G. Benning\udalso acknowledge the financial support of the Helmhol

Physicochemical and Additive Controls on the Multistep Precipitation Pathway of Gypsum