Kinetics and Thermodynamics of Lactose Mutarotation through Chromatography.

The mutarotation kinetics and thermodynamics of the reaction α-lactose ⇌ ß-lactose have been measured in dilute solutions using liquid chromatography without any derivatization step, using a C18 column and pure water as the mobile phase. The effect of temperature (0.5-45 °C) of the starting powder composition (α-lactose-rich or ß-lactose-rich powder) and of the solvent composition (water with up to 35% weight fraction of seven organic solvents) has been experimentally investigated. Increasing the temperature leads to faster kinetics, following an Arrhenius model, and to slightly decreasing concentration-based equilibrium ratio. Conversely, increasing the weight fraction of organic solvent at 25 °C resulted in slower kinetics and smaller concentration-based equilibrium ratio. The starting powder composition is shown not to influence the kinetics or thermodynamics of the process. The corresponding parameter estimation problem is thoroughly discussed, taking into account the small difference in response factors of the lactose diastereomers.

HPLC method development for the quantification of a mixture of reacting species: The case of lactose.

Preparative and analytical chromatography are impaired by analytes that undergo a chemical reaction during the chromatographic separation, leading to peak distortion and systematic errors during the subsequent quantification phase. The pitfalls are highlighted through a combination of analytical results and numerical simulations. Two different quantification strategies for partially overlapping and reacting peaks are compared. A novel method development strategy based on the valley-to-peak ratio instead of the more common resolution is proposed. The method has been used to experimentally investigate the chromatographic behavior of a mutarotating sugar, lactose. The separation of the unprotected lactose isomers, α and ß, has been optimized using a C18 column and pure water as the mobile phase. Phase dewetting phenomena during method development have also been studied and discussed.

The Role of Operating Conditions in the Precipitation of Magnesium Hydroxide Hexagonal Platelets Using NaOH Solutions.

Magnesium hydroxide, Mg(OH)2, is an inorganic compound extensively employed in several industrial sectors. Nowadays, it is mostly produced from magnesium-rich minerals. Nevertheless, magnesium-rich solutions, such as natural and industrial brines, could prove to be a great treasure. In this work, synthetic magnesium chloride and sodium hydroxide (NaOH) solutions were used to recover Mg(OH)2 by reactive crystallization. A detailed experimental campaign was conducted aiming at producing grown Mg(OH)2 hexagonal platelets. Experiments were carried out in a stirred tank crystallizer operated in single- and double-feed configurations. In the single-feed configuration, globular and nanoflakes primary particles were obtained, as always reported in the literature when NaOH is used as a precipitant. However, these products are not complying with flame-retardant applications that require large hexagonal Mg(OH)2 platelets. This work suggests an effective precipitation strategy to favor crystal growth while, at the same time, limiting the nucleation mechanism. The double-feed configuration allowed the synthesis of grown Mg(OH)2 hexagonal platelets. The influence of reactant flow rates, reactant concentrations, and reaction temperature was analyzed. Scanning electron microscopy (SEM) pictures were also taken to investigate the morphology of Mg(OH)2 crystals. The proposed precipitation strategy paves the road to satisfy flame-retardant market requirements.