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Supersaturation, in crystallization

Larson, M.A. and Klekar, S. A., 1973. In-situ measurement of supersaturation in crystallization from solution. Presented at American Institute of Chemical Engineers 66th Annual Meeting, Philadelphia, November. [Pg.313]

Mullin, J.W. and Sohnel, O. (1977) Expressions of supersaturation in crystallization studies. Chemical Engineering Science, 32, 683-686 and 33, 1535-1538. [Pg.560]

Control of supersaturation is an important factor in obtaining crystal size distributions of desired characteristics, and it would be useful to have a model relating rate of cooling or evaporation or addition of diluent required to maintain a specified supersaturation in the crystallizer. Contrast this to the uncontrolled situation of natural cooling in which the heat transfer rate is given by... [Pg.355]

Schierholtz and Stevens (1975), Noor and Mersmann (1993) and Chen etal. (1996) determined nucleation rates by integrating the total crystal number formed over a period and related it to an estimate of supersaturation in the precipitation of calcium carbonate, barium carbonate and barium sulphate respectively. [Pg.135]

In all such laboratory studies, plant conditions and compositions should be employed as far as possible. Agglomeration rates tend to increase with the level of supersaturation, suspension density and particle size (each of which will, of course, be related but the effects may exhibit maxima). Thus, agglomeration may often be reduced by operation at low levels of supersaturation e.g. by controlled operation of a batch crystallization or precipitation, and the prudent use of seeding. Agglomeration is generally more predominant in precipitation in which supersaturation levels are often very high rather than in crystallization in which the supersaturation levels are comparatively low. [Pg.188]

In this case, the co-solvent dosage rate is programmed in order to control the transient level of supersaturation in an effort to improve on the product crystal size distribution from simply dumping in all the solvent at the start of the batch. An experimental crystallizer within which a programmed microcomputer determines the set point of a variable speed-dosing pump is shown in Figure 7.7. Controlled co-solvent dosing improves the product crystal size, with a consequent increase in the filterability of the product. These process concepts are developed further in Chapter 9. [Pg.202]

It has been shown that an increase in crystallizer residence time, or decrease in feed concentration, reduces the working level of supersaturation. This decrease in supersaturation results in a decrease in both nucleation and crystal growth. This in turn leads to a decrease in crystal surface area. By mass balance, this then causes an increase in the working solute concentration and hence an increase in the working level of supersaturation and so on. There is thus a complex feedback loop within a continuous crystallizer, illustrated in Figure 7.11. [Pg.212]

Although cooling crystallization is the most common method of inducing supersaturation in batch crystallization processes, other methods can be used, as discussed in Chapter 10. For example, evaporation can be used, in which case the profile of the rate of evaporation through the batch can also be optimized7. Indeed, the profiles of both temperature and rate of evaporation can be controlled simultaneously to obtain greater control over the level of supersaturation as the batch proceeds7. However, it should be noted that there is often reluctance to use evaporation in the production of fine, specialty and pharmaceutical products, as evaporation can concentrate any impurities and increase the level of contamination of the final product. [Pg.302]

Some of the reports are as follows. Mizukoshi et al. [31] reported ultrasound assisted reduction processes of Pt(IV) ions in the presence of anionic, cationic and non-ionic surfactant. They found that radicals formed from the reaction of the surfactants with primary radicals sonolysis of water and direct thermal decomposition of surfactants during collapsing of cavities contribute to reduction of metal ions. Fujimoto et al. [32] reported metal and alloy nanoparticles of Au, Pd and ft, and Mn02 prepared by reduction method in presence of surfactant and sonication environment. They found that surfactant shows stabilization of metal particles and has impact on narrow particle size distribution during sonication process. Abbas et al. [33] carried out the effects of different operational parameters in sodium chloride sonocrystallisation, namely temperature, ultrasonic power and concentration sodium. They found that the sonocrystallization is effective method for preparation of small NaCl crystals for pharmaceutical aerosol preparation. The crystal growth then occurs in supersaturated solution. Mersmann et al. (2001) [21] and Guo et al. [34] reported that the relative supersaturation in reactive crystallization is decisive for the crystal size and depends on the following factors. [Pg.176]

Condensation is generally a transient operation in which, as discussed by Ueda and Takashima(106), simultaneous heat and mass transfer are further complicated by the effects of spontaneous condensation in the bulk gaseous phase. After the creation of supersaturation in the vapour phase, nucleation normally occurs which may be homogeneous in special circumstances, but more usually heterogeneous. This process is followed by both crystal growth and agglomeration which lead to the formation of the final crystal product. As a rate process, the condensation of solids from vapours is less well understood than vaporisation(98). Strickland-Constable(107) has described a simple laboratory technique... [Pg.880]

Early on in the drug development program, only small amoimts of material are available for crystallization studies. Parallel crystallization technique in test tubes allows for the identification of many solvent systems using small amoimts of material. On a small scale, it is not easy to control the rate of cooling or the rate of evaporation to achieve supersaturation. However, the antisolvent addition strategy to achieve supersaturation in combination with seeding, allows rapid identification of several crystallization systems using a minimum amount of compound. [Pg.249]

NUCLEATION. Nucleation creates a new phase that is organizationally more related to the crystal lattice than to the monomeric species that undergoes crystallization. This process permits solutions that are of high relative supersaturation to crystallize and thereby reach equilibrium between liquid and sohd phases . Nucleation occurs when the local concentration of components that will comprise the solid phase exceeds a threshold level as a result of short-range concentration fluctuations in the bulk solution. In this respect, the kinetics of nucle-... [Pg.91]

An experiment was performed to examine the supposition that increases in supersaturation lead to greater impurity content in crystals. In a batch unseeded cooling crystallizer supersaturation is expected to be high at the point of nucleation, diminish rapidly after nucleation and then approach zero as the batch is... [Pg.93]

DL-threonine and L-threonine crystals were supplied from Ajinomoto Co. Inc. and were used without further purification. Excess amounts of DL-threonine crystalline particles were dissolved in water kept at 55, 57, 58 or 60 C. After decantation and filtration each saturated solution was placed in the crystallizer maintained at 50 C. The difference between the saturation temperature and the crystallization temperature was defined as the initial supersaturation in terms of supercooling of the solution and was the driving force for the crystallization. [Pg.252]

In Figure 4 the corresponding changes in the crystal purity are shown. For the solutions with the initial supersaturation At=5 C, the purity was always 100% for three hours, while purity decrease started very soon for the solution having higher initial supersaturation such as At=10 C. Since with different initial supersaturations, the crystallization rate are very different, the purity decrease should be compared on the basis of either the supersaturation change or the crystal mass grown in the solution rather than the crystallization time. [Pg.254]


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See also in sourсe #XX -- [ Pg.55 ]




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