Crystallization purpose

The preparation of small quantities of oxygen for laboratory purposes may be conveniently effected by gently warming a mixture of fused sodium peroxide with some salt containing water of crystallisation. For this purpose crystals of sodium carbonate or sulphate arc very suitable. The oxygen is evolved in a steady stream which is readily kept under control.3... 

For diffraction purposes crystals are generally grown by a very slow precipitation from a saturated solution. The aim is to obtain a crystal about 0.1 - 0.3 mm in all dimensions. 

Major Application General purpose crystallizer. Can be used for any mode of crystallization including indirect cooling. 

Pentaerythritol PET (002) 0.874 AI-CI effects (e.g., from seconcf-order Ca K-La,3 on P K-L2.3) General-purpose crystal for this range of elements... 

Thallium hydrogenphthalate TAP 2.58 O-Mg competitive crystals General purpose crystal for this range of elements... 

Due to the pulsed radiation output of the LINAC the detectors and the detector electronics have to handle very high counting rates in very short periods. Therefore the detectors have to work in a mode, where the detector output is integrated for one or several beam pulses. For that purpose the crystals are coupled to photo- diodes. Their currents are read out and analysed by the electronic board, which has been developed for this special application. 

The visible crystals that develop during a crystallization procedure are built up as a result of growth either on nuclei of the material itself or surfaces of foreign material serving the same purpose. Neglecting for the moment the matter of impurities, nucleation theory provides an explanation for certain qualitative observations in the case of solutions. 

Cobalt is a bluish silvery metal, exhibits ferromagnetism, and can exist in more than one crystal form it is used in alloys for special purposes. Chemically it is somewhat similar to iron when heated in air it gives the oxides C03O4 and CoO, but it is less readily attacked by dilute acids. With halogens, the cobalt(II) halides are formed, except that with fluorine the (III) fluoride, C0F3, is obtained. 

Drying of crystals. Whenever possible crystals should be dried in a smdl vacuum desiccator containing a suitable desiccant. The latter depends upon the nature of the solvent used c/. p. 19). However for most purposes anhydrous calcium chloride is satisfactory. If a hydrocarbon has been used in the recrystallisation, a few thin fresh shavings of paraffin wax are efficacious. 

The oxime is freely soluble in water and in most organic liquids. Recrystallise the crude dry product from a minimum of 60-80 petrol or (less suitably) cyclohexane for this purpose first determine approximately, by means of a small-scale test-tube experiment, the minimum proportion of the hot solvent required to dissolve the oxime from about 0-5 g. of the crude material. Then place the bulk of the crude product in a small (100 ml.) round-bottomed or conical flask fitted with a reflux water-condenser, add the required amount of the solvent and boil the mixture on a water-bath. Then turn out the gas, and quickly filter the hot mixture through a fluted filter-paper into a conical flask the sodium chloride remains on the filter, whilst the filtrate on cooling in ice-water deposits the acetoxime as colourless crystals. These, when filtered anddried (either by pressing between drying-paper or by placing in an atmospheric desiccator) have m.p. 60 . Acetoxime sublimes rather readily when exposed to the air, and rapidly when warmed or when placed in a vacuum. Hence the necessity for an atmospheric desiccator for drying purposes. 

Carry out this preparation precisely as described for the a-compound, but instead of zinc chloride add 2 5 g. of anhydrous powdered sodium acetate (preparation, p. 116) to the acetic anhydride. When this mixture has been heated on the water-bath for 5 minutes, and the greater part of the acetate has dissolved, add the 5 g. of powdered glucose. After heating for I hour, pour into cold water as before. The viscous oil crystallises more readily than that obtained in the preparation of the a-compound. Filter the solid material at the pump, breaking up any lumps as before, wash thoroughly with water and drain. (Yield of crude product, io o-io 5 g.). Recrystallise from rectified spirit until the pure -pentacetylglucose is obtained as colourless crystals, m.p- 130-131° again two recrystallisations are usually sufficient for this purpose. 

Boil the mixture gently on a sand-bath for 4 hours and then decant into a conical flask and cool. Seed the cold solution if necessary with a trace of a-methylglucoside. The glucoside separates as colourless crystals. When crystallisation ceases, filter the glucoside at the pump, drain, wash quickly with a small quantity of methanol, and then recrystallise from a minimum of methanol. For this purpose methanol of good quality, but not necessarily anhydrous, should be used. The a-methylglucoside is obtained as colourless crystals, m,p. 165°. Yield, 6-7 g. 

For the latter purpose, dissolve the crystals in hot ethanol, and then add water drop by drop to the well-stirred solution until a line emulsion just appears then add more ethanol, also drop by drop, until the emulsion just redissolves. ow allow the solution to cool spontaneousK if the emulsion reappears, add a few drops of ethanol from time to time in order to keep the solution clear. Finally the o-nitrophenol separates in crystals, and the well-stirred mixture may now be cooled in ieewvater until crystallisation is complete. Filter, drain and diy either in an atmospheric desiccator, or by pressing between drying-paper. 

Picric acid is used on a large scale as a high explosive, but for this purpose requires a detonator. If a few small crystals of the pure acid are heated on a crucible lid, they first melt, and ultimately burn harmlessly with a smoky flame. Metallic salts of picric acid are much less stable than the free acid,... 

Recrystallise from methylated spirit, using animal charcoal for this purpose, use about twice the minimum quantity of methylated spirit required to obtain a clear solution, and filter through a funnel preheated by the filtration of some boiling solvent, as the tribromobenzene separates very rapidly as the solution cools. The 1,3,5-tribromobenzene is thus obtained as colourless crystals, m.p. 122° yield, 3 g. 

Place 5 ml. of benzaldehyde in a wide-necked stout-walled bottle of about 100 ml. capacity (a conical flask is too fragile for this purpose) and add 50 ml. of concentrated dy 0 880) ammonia solution. Cork the bottle securely, shake vigorously, and then allow to stand for 24 hours, by which time the layer of benzaldehyde at the bottom of the bottle will have been converted into a hard mass of hydrobenzamide. (If after 24 hours the crude hydrobenzamide is still syrupy, shake the mixture vigorously and allow to stand for another hour, when the conversion will be complete.) Break up the solid pellet with a strong spatula, filter at the pump, wash with water and drain thoroughly. Recrystallise from ethanol methylated spirit should not be used, as it contains sufficient water to cause partial hydrolysis back to benzaldehyde and ammonia. Hydrobenzamide is obtained as colourless crystals, m.p. 101° (and not 110° as frequently quoted) yield, 4 g. 

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