Precipitation processes definition

The direct synthetic process is described in U.S. Patent 2,772,280. A solution of 73.3 g (0.332 mol) of (3-aminoxyalanine ethyl ester dihydrochloride in 100 ml of water was stirred in a 500 ml 3-necked round-bottomed flask cooled in an ice-bath. To the above solution was added over a 30-minute period 65.6 g (1.17 mols) of potassium hydroxide dissolved in 100 ml of water. While the pH of the reaction mixture was 7 to 10.5, a red color appeared which disappeared when the pH reached 11 to 11.5. The light yellow solution was allowed to stand at room temperature for 14 hour and then added to 1,800 ml of 1 1 ethanol-isopropanol. The reaction flask was washed twice with 10 ml portions of water and the washings added to the alcohol solution. The precipitated salts were filtered out of the alcohol solution and the filtrate cooled to 5°C in a 5 liter 3-necked round-bottomed flask. To the cold, well-stirred solution was added dropwise over a 35-minute period sufficient glacial acetic acid to bring the pH of the alcohol solution to 6.0. When the pH of the solution had reached 7 to 7.5, the solution was seeded and no further acetic acid added until Crystallization of the oil already precipitated had definitely begun. The crystalline precipitate was collected on a filter, washed twice with 1 1 ethanol-isopropanol and twice with ether. The yield of 4-amino-3-isoxazolidone was 22.7 g. 

Despite the lack of definitive theoretical proof, some form of the rule of stages does seem to operate often enough for it to be regarded as important to bear in mind when, for example, operating large-scale precipitation processes (section 7.2.6). The most probable explanation of the phenomenon lies in the kinetics of the transformation, the deciding factor being the relative rates of... 

A common method for producing a precipitate is to mix two reactant solutions together as quickly as possible, but the analysis of this apparently simple operation can be exceedingly complex. Precipitation processes, almost by definition, involve the creation of highly supersaturated systems and the main practical difficulty is to maintain reasonably uniform conditions throughout the reaction vessel. The choice of the method of mixing the reactants is therefore very important and the aim should be to avoid any accidental development of zones of excessive supersaturation. The sequence of reactant mixing can... 

A subcritical aggregate having fewer subunit components than a nucleus. When this term is applied in the kinetics of precipitation, n refers to the number of subunits in a particle and n defines the number of subunits in a particle of critical size. This definition avoids confusion by distinguishing between subcritical (n < n subunits), critical (n = n subunits), and supercritical (n > n subunits) particle sizes. If a nucleus is defined as containing n n subunits, then an embryo contains n n subunits. Note that in this treatment, we are not using a phase-transition description to describe nucleation, and we are focusing on the smallest step in the process that leads to further aggregation. 

Oxygen in the air is now a sufficiently strong (and cheap ) oxidizing agent to effect the solution of the gold. It may then be reduced and precipitated by an active metal such as zinc powder (E° - -0.763 V). Such hydrometalluigica] processes offer definite advantages ... 

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