Batch-melting and crystallization

In order to make samples of phosphate fibers for supplying potential customers, laboratory chemists under the direction of Dr. Richard Hansen had initiated scale-ups to prepare 100-lb samples routinely. These operations were satisfactory for the purpose they served, but containment was a problem. Crucibles used to prepare melts were sacrificial because melt and crystals would grow to the walls of their containers. It was obvious that a manufacturing plant could not destroy a large part of its equipment for each batch of product produced. 

Chemical development Proof of structure and configuration are required as part of the information on chemical development. The methods used at batch release should be validated to guarantee the identity and purity of the substance. It should be established whether a drug produced as a racemate is a true racemate or a conglomerate by investigating physical parameters such as melting point, solubility and crystal properties. The physicochemical properties of the drug substance should be characterized, e.g. crystallinity, polymorphism and rate of dissolution. 

Both continuous and batch methods may be used in methanolysis. The batch mediod requires an autoclave, crystallizer, and centrifuge and a system for the melting and distillation of the DMT obtained. In the two-stage Hoechst continuous process, waste PET is melted and fed to a reactor. Preheated methanol is added to the autoclave, which is equipped with a mixer. The conversion reaches 70-90% in the first reactor, after which the reaction stream is introduced into a second autoclave at a lower temperature near the bottom, where it rises slowly and die higher density impurities settle at the bottom. The reaction stream leaves the second autoclave and its pressure is reduced to 0.3 MPa. On further reduction of the pressure and cooling, DMT precipitates and is subsequently purified.12... 

Batch partial melting will hereafter be understood as equilibrium melting, which is in contrast to fractional melting discussed in Section 9.3.3. The foundation of this model is remarkably simple and was first laid down by Schilling and Winchester (1967). A number of more or less complex modifications enabling useful information to be extracted from the data were later introduced by Gast (1968), Shaw (1970) and Albarede (1983). Bulk equilibrium crystallization of a liquid batch can be handled with equations identical to those for batch-melting. 

Eased on two main lines of evidence, Niu et al. (1997) concluded that abyssal peridotites are the end products of melt extraction followed by variable amounts of olivine crystallization. First, in their set of reconstructed compositions they found that model fractional and batch melt extraction trends could not reproduce major and minor element variations in their data set. Most importantly, they found that melt extraction models failed to account for the strong positive correlation between FeO and MgO, as well as incompatible minor-element concentrations. Specifically, at a given Na20 or Ti02 content, abyssal peridotites are enriched in MgO relative to model melt extraction residues. Niu et al. (1997) showed that these compositional anomalies can be reconciled by a model of melt extraction followed by olivine crystallization, with more MgO-enriched samples having more accumulated olivine. If correct, this model has important implications for understanding melt extraction at oceanic ridges, and it has recently been the focus of re-evaluation. 

This equation, when applied to melting, is called the equilibrium melting or batch melting equation and, when applied to crystallization, it is called the equilibrium crystallization equation. As emphasized by Langmuir et al. (1992) this equation, and others like it, is enormously powerful and can be applied to model both major elements and trace elements. This approach has received its most widespread use, however, in modeling trace element variations. 

---