Separation of the melt

These examples involve partitioning of elements as liquids cooled and crystallized. Partial melting of a solid rock also results in partitioning of incompatible elements into the liquid phase, which contains no rigid crystalline sites. Separation of the melt then fractionates incompatible elements from the compatible elements left behind in the solid residue. 

A common difficulty in these partition experiments, with the use of either natural or synthesized samples, is in achieving perfect separation of the melt from the crystal phase for determining the noble gas content. Even a very small amount of glass (melt) contamination in crystal would increase the partition coefficient considerably, since noble gasses are much more enriched in glass. To circumvent this difficulty, Broad-hurst et al. (1990, 1992) prepared natural minerals and synthetic silicate melts that... 

The advantage of the Maillefer screw is primarily the physical separation of the melt pool and the solid bed. As a result, there is less chance of formation of a melt film between the solid bed and the screw and, therefore, there is less chance of solid bed breakup. Thus, the melting process can occur in a more stable fashion but not necessarily at a higher rate. 

Melt filtration systems can very effectively remove particulate contaminants from polymer melts, for example, continuous systems provided by Process Developments [10] and by Gneuss. Kauferle (Remaker) produced a prototype device capable of causing separation of the melt from high concentrations of aluminium from polystyrene in laminates, or copper from polyethylene in telephone wire, without the need for disposable filter screens. The solid and particle contaminant-free thermoplastic exited from one port on the separation head, while a very high concentration of contaminant embedded in... 

The commercial product, m.p. 53-55°, may be used. Alternatively the methyl -naphthyl ketone may be prepared from naphthalene as described in Section IV,136. The Friedel - Crafts reaction in nitrobenzene solution yields about 90 per cent, of the p-ketone and 10 per cent, of the a-ketone in carbon disulphide solution at — 15°, the proportions ore 65 per cent, of the a- and 35 per cent, of the p-isomer. With chlorobenzene ns the reaction medium, a high proportion of the a-ketone is also formed. Separation of the liquid a-isomer from the solid p-isomer in Such mixtures (which remain liquid at the ordinary temp>erature) is readily effected through the picrates the picrate of the liquid a-aceto compound is less soluble and the higher melting. 

The Cams Hquid-phase oxidation process is similar in principle however, it is operated continuously, its oxidation reaction vessels are of a much larger scale, and the separation of the manganate intermediate from the caustic melt is accompHshed without dilution by means of filtration (qv) (121—123). 

Reduction to Liquid Metal. Reduction to Hquid metal is the most common metal reduction process. It is preferred for metals of moderate melting point and low vapor pressure. Because most metallic compounds are fairly insoluble in molten metals, the separation of the Hquified metal from a sohd residue or from another Hquid phase of different density is usually complete and relatively simple. Because the product is in condensed form, the throughput per unit volume of reactor is high, and the number and si2e of the units is rninimi2ed. The common furnaces for production of Hquid metals are the blast furnace, the reverberatory furnace, the converter, the flash smelting furnace, and the electric-arc furnace (see Furnaces, electric). 

Separation of a chemical species from a mixture of similar compounds can also be achieved by melt crystallization, which is, for example, an important means of separatingpara- s.yXen.e (p-xylene) from the ortho and meta isomers. -Xylene is crystallized at the top of a vertical column and crystals are moved downward countercurrentiy to Hquid. The Hquid flowing upward is generated by adding heat to melt the crystals at the bottom of the column a portion of the melt is removed as product and the remainder flows up the column to contact the downward-flowing crystals. Effluent mother Hquor, consisting almost entirely of the ortho and meta isomers of xylene, is removed from the top of the column. 

Purification of a chemical species by solidification from a liquid mixture can be termed either solution crystallization or ciystallization from the melt. The distinction between these two operations is somewhat subtle. The term melt crystallization has been defined as the separation of components of a binaiy mixture without addition of solvent, but this definition is somewhat restrictive. In solution crystallization a diluent solvent is added to the mixture the solution is then directly or indirec tly cooled, and/or solvent is evaporated to effect ciystallization. The solid phase is formed and maintained somewhat below its pure-component freezing-point temperature. In melt ciystallization no diluent solvent is added to the reaction mixture, and the solid phase is formed by cooling of the melt. Product is frequently maintained near or above its pure-component freezing point in the refining sec tion of the apparatus. 

After separation of the catalyst the product was concentrated until dry, the residue was triturated with acetone, the resulting crystallizate was removed by suction and washed with acetone. The yield of N,N -bis-(2-(3, 4 -dihydroxyphenyl)-2-hydroxyethyl]-hexamethylene-diamine-dichlorohydrate was 3.3 grams, i.e., 92% of the theoretical value. A quantity of 2.8 grams having a melting point of 197,5° to 198°C was obtained by precipitation from a mixture of methanol-ether. 

The SCB distribution (SCBD) has been extensively studied by fractionation based on compositional difference as well as molecular size. The analysis by cross fractionation, which involves stepwise separation of the molecules on the basis of composition and molecular size, has provided information of inter- and intramolecular SCBD in much detail. The temperature-rising elution fractionation (TREE) method, which separates polymer molecules according to their composition, has been used for HP LDPE it has been found that SCB composition is more or less uniform [24,25]. It can be observed from the appearance of only one melt endotherm peak in the analysis by differential scanning calorimetry (DSC) (Fig. 1) [26]. Wild et al. [27] reported that HP LDPE prepared by tubular reactor exhibits broader SCBD than that prepared by an autoclave reactor. The SCBD can also be varied by changing the polymerization conditions. From the cross fractionation of commercial HP LDPE samples, it has been found that low-MW species generally have more SCBs [13,24]. 

An initial solution was prepared by the hydrofluoride method, i.e. melting of a mixture of ammonium hydrofluoride and tantalite, followed by the digestion of soluble components with water and separation of the solution by filtration. The prepared initial solution contained no free HF or any other acid, and had a pH 3. In order to obtain an optimal acidity level, sulfuric acid was added to the solution. Concentrations of Ta2Os (50-60 g/1) and Nb205 ( 30 g/1) were kept approximately constant during the preparation of the solutions. Extraction was performed using a polypropylene beaker and a magnetic stirrer. 

The separation of the excess unreacted sodium is also subject to investigation and development. Miyazaki and Kuroki [588] proposed a reactor system for the reduction of K2TaF7 or K2NbF7 with Na or K, respectively. According to this method, the reduced melt is tapped into a special chamber for solidification, while unreacted Na or K is trapped with a condenser in the gas phase for recycling. 

Many elements can be determined directly in the acid solution of the melt without the need for tedious separations. 

Eustace noticed the correlation between asymmetric /V-substitution and low melting points (at temperatures > 15 °C) of the substances [75] observed in this study. The importance of sufficiently high specific densities of the fused salts" for an efficient separation of the complex phase and the aqueous solution was emphasized. Mixtures of various quaternary ammonium... 

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