结晶时油状物处理.docVIP

结晶时油状物的处理(in english) treat about the oil just few ways ,followed : The separation of a second liquid phase, commonly known as an oil, instead of the expected crystalline solid, sometimes occurs during recrystallisation. The oil often solidifies on standing, although at times a considerable period may elapse before crystallisation occurs. The resulting crystals will probably occlude some of the mother liquor, and the purity will therefore not be high. If the substance has a low melting point, it must not be assumed that this apparently abnormal behaviour is due to the presence of impurities ; it is probably an example of a system in which the solid phases consist of the pure components and the components are only partially miscible in the liquid state (see Section 1,18). The separation of the oil may be avoided by diluting the solution considerably, but this will lead to large losses. It is probably best to re-heat the mixture until a clear solution is obtained, and allow it to cool spontaneously; immediately the oil commences to separate, the mixture is vigorously stirred so that the oil is well dispersed in the solution. Eventually, crystals will separate and these will grow in the bulk of the solution and not in a pool of oil, so that occlusion of the mother liquor is considerably reduced. When all the oil has disappeared, stirring may be stopped and the crystals allowed to accumulate. Sometimes the addition of a minute quantity of the crude compound in order to seed the solution may facilitate the initial crystallisation. Occasionally substances form supersaturated solutions from which the first crystals separate with difficulty ; this is sometimes caused by the presence of a little tar or viscous substance acting as a protective colloid. The following methods should be tried in order to induce crystallisation:— 1. By scratching the inside of the vessel with a glass rod. The effect is attributed to the breaking off of small particles of glass which may act