Phase system preparation

Emulsions are two-phase systems formed from oil and water by the dispersion of one liquid (the internal phase) into the other (the external phase) and stabilized by at least one surfactant. Microemulsion, contrary to submicron emulsion (SME) or nanoemulsion, is a term used for a thermodynamically stable system characterized by a droplet size in the low nanorange (generally less than 30 nm). Microemulsions are also two-phase systems prepared from water, oil, and surfactant, but a cosurfactant is usually needed. These systems are prepared by a spontaneous process of self-emulsification with no input of external energy. Microemulsions are better described by the bicontinuous model consisting of a system in which water and oil are separated by an interfacial layer with significantly increased interface area. Consequently, more surfactant is needed for the preparation of microemulsion (around 10% compared with 0.1% for emulsions). Therefore, the nonionic-surfactants are preferred over the more toxic ionic surfactants. Cosurfactants in microemulsions are required to achieve very low interfacial tensions that allow self-emulsification and thermodynamic stability. Moreover, cosurfactants are essential for lowering the rigidity and the viscosity of the interfacial film and are responsible for the optical transparency of microemulsions [136]. 

Kang S Y and Kim K 1998 Comparative study of dodeoanethiol derivatized nanopartioles prepared in one and two phase systems Langmuir 14 226... 

Recovery. The principal purpose of recovery is to remove nonproteinaceous material from the enzyme preparation. Enzyme yields vary, sometimes exceeding 75%. Most industrial enzymes are secreted by a microorganism, and the first recovery step is often the removal of whole cells and other particulate matter (19) by centrifugation (20) or filtration (21). In the case of ceU-bound enzymes, the harvested cells can be used as is or dismpted by physical (eg, bead mills, high pressure homogenizer) and/or chemical (eg, solvent, detergent, lysozyme [9001 -63-2] or other lytic enzyme) techniques (22). Enzymes can be extracted from dismpted microbial cells, and ground animal (trypsin) or plant (papain) material by dilute salt solutions or aqueous two-phase systems (23). 

The laboratory preparation of the Udel-type polymer has been described. Bis-phenol A is mixed with chlorobenzene (solvent) and dimethyl sulphoxide (active solvent) and heated to 60°C to obtain a clear solution. Air is displaced from the system by nitrogen or argon and an aqueous solution of caustic soda added. This results in a two-phase system, one predominantly chlorobenzene the... 

Alkanesulfinyl chlorides have been prepared by the action of thionyl chloride on alkanesulfinic acids and by the solvolysis of alkylsulfur trichlorides with water, alcohols, and organic acids. The present procedure, which appears to be general for the preparation of sulfinyl chlorides in either the aliphatic or the aromatic series, is based on an improvement in the solvolysis method whereby the use of inert solvent is eliminated and the reaction is carried out in a one-phase system. ... 

An expression for the maximum charge that can be placed on a column without impairing resolution has already been derived, but the approach, when dealing with an overloaded column for preparative purpose, will be quite different. For preparative purposes the phase system is chosen to provide the maximum separation of the solute of interest from its nearest neighbor. It should be pointed out that the separation may, but probably will not, involve the closest eluting pair in the mixture. Consequently, the maximum resolving power of the column will not be required for the purpose of separation and the excess resolution of the solute of interest from its nearest neighbor can be used to increase the column load. 

Reactions between A -(l-chloroalkyl)pyridinium chlorides 33 and amino acids in organic solvents have a low synthetic value because of the low solubility of the amine partner. A special protocol has been designed and tested in order to circumvent this drawback. Soon after the preparation of the salt, an aqueous solution of the amino acid was introduced in the reaction medium and the two-phase system obtained was heated under reflux for several hours. However, this was not too successful because sulfur dioxide, evolved during the preparation of the salt, was converted into sulfite that acted as an 5-nucleophile. As a result, A -(l-sulfonatoalkyl)pyridinium betaines such as 53 were obtained (Section IV,B,3) (97BSB383). To avoid the formation of such betaines, the salts 33 were isolated and reacted with an aqueous solution of L-cysteine (80) to afford thiazolidine-4-carboxylic acids hydrochlorides 81 (60-80% yields). 

Preparation of 2-Bromo-3-Hexyne A solution of 13B g of 3-hexyne-2-ol and 9 g of pyridine in 13B ml of anhydrous ether was treated with 175 g of phosphorus tribromide, added dropwise over a period of about 20 minutes at a temperature of about -10°C. The reaction mixture was permitted to come to room temperature while stirring for about 3 hours, and was then heated to refluxing for about 1 hour. After cooling, the reaction mixture was poured over about 50 g of crushed ice. A two-phase system formed, and the ether layer was separated, washed with dilute sodium bicarbonate solution, dried over anhydrous potassium carbonate and fractionally distilled. The 2-bromo-3-hexyne formed in the reaction was collected at 75°C at the pressure of 50 mm of mercury. 

Proteins (BSA or ovomucoid, OVM) have also been successful in the preparative resolution of enantiomers by liquid-liquid extraction, either between aqueous and lipophilic phases [181] or in aqueous two-phase systems (ATPS) [123, 180]. The resolution of d,l-kynurenine [180] and ofloxacin and carvediol [123] were performed using a countercurrent extraction process with eight separatory funnels. The significant number of stages needed for these complete resolutions in the mentioned references and others [123, 180, 189], can be overcome with more efficient techniques. Thus, the resolution of d,l-kynurenine performed by Sellergren et al. in 1988 by extraction experiments was improved with CCC technologies 10 years later [128]. 

The micrographs in Fig. 7.88 show clearly how from a knowledge of the AG -concentration diagrams it is possible to select the exact reaction conditions for the production of tailor-made outermost surface phase layers of the most desired composition and thus of the optimum physical and chemical properties for a given system. In addition it shows that according to thermodynamics, there can be predictable differences in the composition of the same outermost phase layer prepared at the same conditions of temperature but under slightly different vapour pressures. 

A novel oxidation of sulphilimines using ruthenium tetroxide (generated in situ from ruthenium dioxide in a two-phase system) for the preparation of sulphoximines has been reported and proceeds in yields greater than 85%185. 

In sample preparation, it is assumed that the type of phase system that will be used for the separation has been established using pure samples... 

The use of other important phase systems such as exclusion media, ion exchange media and polar stationary phases such as silica gel have not been discussed as this chapter is primarily concerned with sample preparation. The last chapter will give examples of the use of these other phase systems and explain the separations obtained on a basis of molecular interactions and, at that time, the subject of solvent choice will again be discussed. 

Silicone rubber-hydrogel composite is a two-phase system that is capable of swelling in water. The hydrogels prepared have different chemical compositions, size and shape of particles, and correspondingly different specific surfaces. It was found that the mechanical properties of silicone rubber-hydrogel composites depend mostly on the magnitude of the contact surface of both phases. ... 

Since a-tocopherol destroys nitrite in the system in absence of the oil phase, we may postulate that the ineffectiveness of these two oil soluble inhibitors resulted from their absence from the aqueous phase. Diethanolamine is miscible with water and presumably its nitrosation occurs in the aqueous phase. There is a significant difference in the solubility characteristics of ascorbyl palmitate. The reducing portion of the molecule is water soluble. Thus the ascorbate moiety may be in the aqueous phase while the fatty acid tails may lie within the oil globules. The a-tocopherol and the BHA may well be effective if they are dispersed in the aqueous phase after preparation of the emulsion. This will be investigated in future experiments. 

Sample Preparation. Liquid crystalline phases, i.e. cubic and lamellar phases, were prepared by weighing the components in stoppered test tubes or into glass ampoules (which were flame-sealed). Water soluble substances were added to the system as water solutions. The hydrophobic substances were dissolved in ethanol together with MO, and the ethanol was then removed under reduced pressure. The mixing of water and MO solutions were made at about 40 C, by adding the MO solution dropwise. The samples for the in vivo study were made under aseptic conditions. The tubes and ampoules were allowed to equilibrate for typically five days in the dark at room temperature. The phases formed were examined by visual inspection using crossed polarizers. The compositions for all the samples used in this work are given in Tables II and III. 

An aqueous colloidal polymeric dispersion by definition is a two-phase system comprised of a disperse phase and a dispersion medium. The disperse phase consists of spherical polymer particles, usually with an average diameter of 200-300 nm. According to their method of preparation, aqueous colloidal polymer dispersions can be divided into two categories (true) latices and pseudolatices. True latices are prepared by controlled polymerization of emulsified monomer droplets in aqueous solutions, whereas pseudolatices are prepared starting from already polymerized macromolecules using different emulsification techniques. 

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