熔沸点的测定重点分析.ppt

Melting Point and Boiling Point 1. Purpose 1.1 Learn the knowledge of melting point and boiling point. 1.2 Grasp the methods to test melting point and boiling point with Capillary Tubes. 1.3 Grasp the usage of Digital melting-point apparatus. 2. Principle 2.1 Melting Point Definition: The melting point of a substance is defined as the temperature at which the liquid and solid phases exist in equilibrium with one another . Figure1. Phase change with time and temperature Sharp increase after melting, so heat slowly If heat is added to a mixture of the solid and liquid phases of a pure substance at the melting point, ideally no rise in temperature will occur until all the solid has melted and been converted to liquid. The melting point and freezing point of a pure substance are identical. A pure organic compound have a settled melting point, usually lower than 350℃, with a temperature range of 0.5～1 ℃. Figure2. The effects of impurities on melting point According to Raoults law, at a certain pressure and temperature conditions, if we put solute into a solvent, the partial pressure of solvent vapor will obviously decreased. The solid and liquid phases intersect at points M1, which represents the boiling point of compounds containing impurities are lower than that of pure compounds. 当含杂质时（假定两者不形成固熔体），根据拉乌耳定律可知，在一定的压力和温度条件下，在溶剂中增加溶质，导致溶剂蒸气分压降低，固液两相交点M′即代表含有杂质化合物达到熔点时的固液相平衡共存点，T1为含杂质时的熔点，显然，此时的熔点较纯粹者低，熔点距扩大。 因此，熔点是判断晶体化合物纯度的重要指标之一。 2.2 Melting point methods and apparatus (1) Capillary tubes and sample preparation Commercially available capillary tubes have one end already sealed and the other opened end to permit introduction of the sample（2-3mm）。 熔点管制备：将毛细管一端用酒精灯烧熔封口，呈45°角，不停旋转。 注意事项： 样品需研细，可填装结实，有空隙则不易传热，影响结果。 样品装实后2～3mm。 样品装填需迅速，防治吸潮。 Samples Preparations 表面皿 桌面 玻璃管 样品(2~3 mm) 样品 样品管 样品只可用一次 （2） Thiele tube apparatus b形管 石蜡油浴 橡皮圈 熔点管 样品 温度计 1 2 4 3 5 Proper use of the Thiele tube is critical to obtain reliable melting points。 Heating rate. Firstly, the heat