Crystallisation prevention

B) A hot solution has to be filtered to remove traces of insoluble impurities, and kept hot meanwhile to prevent crystallisation of the main solute, which would otherwise choke up the filter. 

Hydrolysis of />-Tolunitrile. As in the case of benzonitrile, alkaline h> drolysis is preferable to hydrolysis by 70% sulphuric acid. Boil a mixture of 5 g. of p-tolunitrile, 75 ml. of 10% aqueous sodium hydroxide solution and 15 ml. of ethanol under a reflux water-condenser. The ethanol is added partly to increase the speed of the hydrolysis, but in particular to prevent the nitrile (which volatilises in the steam) from actually crystallising in the condenser. The solution becomes clear after about i hour s heating, but the boiling should be continued for a total period of 1-5 hours to ensure complete hydrolysis. Then precipitate and isolate the p-toluic acid, CH3CgH4COOH, in precisely the same way as the benzoic acid in the above hydrolysis of benzonitrile. Yield 5 5 g. (almost theoretical). The p-toluic acid has m.p. 178°, and may be recrystallised from a mixture of equal volumes of water and rectified spirit. 

Finally, add an excess of concentrated hydrochloric acid slowly with stirring to the alkaline filtrate remaining from the original reaction product. As the solution becomes acid, the sulphonyl-aniline separates as a thick sticky syrup which, when stirred, rapidly crystallises. Cool the mixture in ice-water if necessary, and then filter off the solid product at the pump, wash well with water, and drain. Recrystallise from a mixture of 2 volumes of ethanol and i volume of water to prevent the sulphonyl-aniline from separating as an emulsion, allow the hot solution to cool spontaneously (with occasional stirring) until crystallisation starts, and... 

Solid organic compounds when isolated from organic reactions are seldom pure they are usually contaminated with small amounts of other compounds ( impurities ) which are produced along with the desired product. Tlie purification of impure crystalline compounds is usually effected by crystallisation from a suitable solvent or mixture of solvents. Attention must, however, be drawn to the fact that direct crystallisation of a crude reaction product is not always advisable as certain impurities may retard the rate of crystallisation and, in some cases, may even prevent the formation of crystals entirely furthermore, considerable loss of... 

To carry out a steam distillation, the solution (or mixture or the solid with a little water) is placed in the flask B, and the apparatus is completely assembled. Steam is passed into the flask B, which is itself heated by means of a small flame to prevent too rapid an accumulation of water, at such a rate that it is completely condensed by the condenser C. The passage of steam is continued until there is no appreciable amount of water-insoluble material in the distillate. If the substance crystallises... 

In a 1 5 or 2-Utre rovmd-bottomed flask, prepare cuprous chloride from 105 g. of crystallised copper sulphate as detailed in Section 11,50,1. Either wash the precipitate once by decantation or filter it at the pump and wash it with water containing a httle sulphurous acid dissolve it in 170 ml. of concentrated hydrochloric acid. Stopper the flask loosely (to prevent oxidation) and cool it in an ice - salt mixture whilst the diazo-tisation is being carried out. 

High test molasses (invert molasses) is produced from cane sugar when sucrose manufacture is restricted because of overproduction. The cane sugar at ca 55 wt % solids is en2ymatically converted to invert symp to prevent crystallisation and evaporated to a symp. The product is used in the same applications as blackstrap molasses. 

Sterile aqueous D-sorbitol solutions are fermented with y cetobacter subo >gichns in the presence of large amounts of air to complete the microbiological oxidation. The L-sorbose is isolated by crystallisation, filtration, and drying. Various methods for the fermentation of D-sorbitol have been reviewed (60). A.cetobacter suboyydans is the organism of choice as it gives L-sorbose in >90% yield (61). Large-scale fermentations can be carried out in either batch or continuous modes. In either case, stefihty is important to prevent contamination, with subsequent loss of product. 

Properties. Cyanamide [420-04-2] also called carbamodiimide or carbamic acid nitrile, crystallises from a variety of solvents as somewhat unstable, colorless, orthorhombic, dehquescent crystals (2). Dimerization is prevented by traces of acidic stabilizers such as monosodium phosphate and by storage at low temperature. 

The less simple polymers (like the epoxies, the polyesters and the formaldehyde-based resins) are networks each chain is cross-linked in many places to other chains, so that, if stretched out, the array would look like a piece of Belgian lace, somehow woven in three dimensions. These are the thermosets if heated, the structure softens but it does not melt the cross-links prevent viscous flow. Thermosets are usually a bit stiffer than amorphous thermoplastics because of the cross-links, but they cannot easily be crystallised or oriented, so there is less scope for changing their properties by processing. 

As the temperature is decreased, free-volume is lost. If the molecular shape or cross-linking prevent crystallisation, then the liquid structure is retained, and free-volume is not all lost immediately (Fig. 22.8c). As with the melt, flow can still occur, though naturally it is more difficult, so the viscosity increases. As the polymer is cooled further, more free volume is lost. There comes a point at which the volume, though sufficient to contain the molecules, is too small to allow them to move and rearrange. All the free volume is gone, and the curve of specific volume flattens out (Fig. 22.8c). This is the glass transition temperature, T . Below this temperature the polymer is a glass. 

The fi-compound is dissolved in 50 c c. pure dry ether, and dry hydiogen chloride is passed in with constant shaking to prevent the delivery tube from becoming blocked. Colourless crystals of the hydrochloride of the /3-o ime separate and aie filtered and washed with dry ether and then placed in a separating funnel and covered with a layer of ether. A. concentrated solution of sodium carbonate is gradually added with constant shaking until no further effervescence is observed. Sodium chloride is precipitated and the /3-oxime dissolves in the ether. The ether extract is sepaiated, dehydrated over sodium sulphate, and the ether remoi ed as rapidly as possible at the ordinary temperature by evaporation in vacuo. The residue crystallises, and when pressed on a porous plate leaves a mass of small silky needles, m. p. 126—130A It may be re-... 

It may be prepared synthetically by reducing cinnamic aldehyde diacetate, and saponifying the resulting cinnamyl esters. Cinnamic alcohol is a crystalline body, although commercial specimens frequently contain traces of impurities which prevent crystallisation. It has the following characters —... 

Amorphous thermoplastics These are made from polymers which have a sufficiently irregular molecular structure to prevent them from crystallising in any way. Examples of such materials are polystyrene, poly methyl methacrylate and polyvinyl chloride. 

Note in making up the chromic acid solution it is advisable to dissolve the silver nitrate separately and add it to the boiling chromic acid to prevent excessive crystallisation of the silver chromate. The chromic acid must be free from sulphate to avoid attack on the zinc. Immerse each specimen for 15 s in a 6% solution of hydriodic acid at room temperature to remove the remaining corrosion products. Immediately after immersion in the acid bath, wash the samples first in tap water and then in absolute methanol, and dry in air. This procedure removes a little of the zinc and a correction may be necessary. 

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