Separation of crystals

Separation of Crystals.—This is generally effected by filtration with suction, vessels of size suitable to the quantities dealt with being selected. The crystals left on the funnel should be well pressed down and then washed a few times with small quantities of the pure solvent in order to remove the last traces of mother liquor. If the substance is easily soluble, too large quantities of solvent must not be employed for washing. When 

Often further crops of crystals can be obtained by concentrating the mother liquor generally these are less pure and require to be recrystallised. In some cases the first crop has to be recrystallised before the crystals are pure (determined by M.P.). It is often convenient, in order to separate a second crop, to dilute the mother liquor with a liquid in which the dissolved substance is sparingly soluble. Crops separated in this way generally require recrystallisation. 

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For a given structure, the values of S at which in-phase scattering occurs can be plotted these values make up the reciprocal lattice. The separation of the diffraction maxima is inversely proportional to the separation of the scatterers. In one dimension, the reciprocal lattice is a series of planes, perpendicular to the line of scatterers, spaced 2Jl/ apart. In two dimensions, the lattice is a 2D array of infinite rods perpendicular to the 2D plane. The rod spacings are equal to 2Jl/(atomic row spacings). In three dimensions, the lattice is a 3D lattice of points whose separation is inversely related to the separation of crystal planes. 

Labb recommends a slight modiflcation of the above process, by which he claims that the separation of crystals at the junction between the unabsorbed oil and the sulphite liquor is prevented, and greater accuracy in reading off the. percentage therefore attained. He employs a stoppered bulb, prolonged at the bottom into a graduated cylindrical closed tube, and into this are introduced 5 c.c. of the oil, together with... 

Kristall. m. crystal, -abscheidung, /. separation of crystals, -achse, /. crystal axis, crystallographic axis. 

If it is desired to produce well-developed crystals when recrystallising, the filtrate, in which separation of crystals often occurs even during filtration, must be reheated till a clear solution is obtained and then allowed to cool slowly without being disturbed. 

Hydrolysis of the Nitrile.—The nitrile, mixed in a porcelain basin with four times its volume of concentrated hydrochloric acid, is heated on the water bath until an abundant separation of crystals begins to take place on the surface of the liquid. The reaction mixture is then allowed to stand over night in a cool place, and the crystals which have been deposited, after being rubbed with a little water, are separated at the filter pump and washed with water (not too much). A further quantity of the acid is obtained from the filtrate by extraction with ether. The crude mandelic acid is pressed on a porous plate, dried, and purified by crystallisation from benzene. Melting point 118°. Yield about 10-15 g. 

Perforated bowls are used when relatively large particles are to be separated from a liquid, as for example in the separation of crystals from a mother liquor. The mother liquor passes through the bed of particles and then through the perforations in the bowl. When the centrifuge is used for filtration, a coarse gauze is laid over the inner surface of the bowl and the filter cloth rests on the gauze. Space is thus provided behind the cloth for the filtrate to flow to the perforations. 

Crystallisation by freezing, or freeze crystallisation, is a process in which heat is removed from a solution to form crystals of the solvent rather than of the solute. This is followed by separation of crystals from the concentrated solution, washing the crystals with near-pure solvent, and finally melting the crystals to produce virtually pure solvent. The product of freeze crystallisation can be either the melted crystals, as in water desalination, or the concentrated solution, as in the concentration of fruit juice or coffee extracts. Freeze crystallisation is applicable in principle to a variety of solvents and solutions although, because it is most commonly applied to aqueous systems, the following comments refer exclusively to the freezing of water. 

Mechanical Separation of Crystals. The first instance of resolution was by L. Pasteur who was able to resolve crystals of sodium ammonium tartrate (which recrystallizes in two distinct, nonsuperimposable forms below 2TC). Although this procedure is rarely used, one might be able to seed a racemic solution resulting in only one... 

In the above directions the concentration is as high as it is safe to make it if less water be used the yield of phenylurea decreases and there is grave danger of loss due to the sudden heating of the mixture by rapid separation of crystals. This phenomenon has been observed with a more concentrated mixture even on heating on the steam bath. 

Elemental abundances in group IIIAB iron meteorites (dots) compared to calculated fractional crystallization trends that assume complete separation of crystals and melt (solid curve) and incomplete separation of those phases (dashed curve). Modified from Haack and McCoy (2004). 

Under these conditions W. P. Bloxam obtained crystals of sulphur and of the pentasulphide, but no ruby-red crystals of the heptasulphide, and he obtained the enneasulphide by working according to J. Fritzsche s directions. P. Sabatier claims to have made the heptasulphide by digesting sulphur with the warm or cold mother liquid remaining after the separation of crystals of the pentasulphide. P. Sabatier s analysis corresponds with ammonium octomlpkide, (NH Sg. W. P. Bloxam made crystals of the hydrated salt, (NH4)2S7.fH20, by the simultaneous action of sulphur and hydrogen sulphide on aqua ammonia rather more cone, than that used in the preparation of the pentasulphide. 

The first of these, which may be used with stsel pens, and which is most readily developed on tho application of heat, is prepared in the subjoined manner — Nitrate of silver is triturated iu a mortar with an equivalent of dasiccated tartoric acid. Water is then added, which causes the. separation of crystals of tartrate of silver, nitric acid being set free. The latter is neutralized carefully by adding ammonia, which also dissolves the metallic tartrate. Gum, tinctorial matter, and water arc subsequently added in quantities which may he varied at pleasure. 

In duralumin with 4 % copper and 0.5 % magnesium, so important in modern constructions, the greater strength is produced by the separation of crystals of the compound CuA12. 

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