solute in a solvent at or near its It is necessary to filter the solution boiling point. At this high while still hot because according on temperature, the solute has a greatly the principles of solubility, increased solubility in the solvent, so a much smaller quantity of hot compounds tend to be more soluble solvent is needed than when the in hot liquids, if you allowed it to solvent is at room temperature. cool, the solute is no longer soluble When the solution is later cooled, in the solvent and forms crystals of after filtering out insoluble impurities, pure compound. the amount of solute that remains dissolved drops precipitously. At the Because some of the compounds cooler temperature, the solution is will solidify and precipitate when the saturated at a much lower solution is not hot. As a result the concentration of solute. The solute compound will be collected as the that can no longer be held in solution solid residue instead of the liquid forms purified crystals of solute, filtrate. which can later be collected.
Recrystallization works only when
A hot filtration is generally used in the proper solvent is used. The some crystallization, when a solid solute must be relatively insoluble in contains impurities that are insoluble the solvent at room temperature but in the crystallization solvent. It is much more soluble in the solvent at also necessary in crystallization higher temperature. At the same when charcoal is used to remove time, impurities that are present highly colored impurities from a must either be soluble in the solvent solid, as charcoal is so fine that it at room temperature or insoluble in cannot be removed by decanting. the solvent at a high temperature. A filtration procedure called "hot I assume you are talking gravity filtration" is used to separate about recrystallisation, a insoluble impurities from a hot solution. Hot filtrations require fluted technique of purifcation of filter paper and careful attention to solids. the procedure to keep the apparatus A solvent is chosen which warm but covered so that solvent will dissolve the compound of does not evaporate. Hot gravity interest when hot but not filtrations are no longer included in cold, but not dissolve the the routine procedures for the impurity when hot or cold. experiments in the organic chemistry teaching labs. If you need to do such The mixture is taken up in a filtration, read the procedure in the the minimum amount of hot Handbook and consult your TA. solvent to dissolve all the desired compound, filtered to The principle behind recrystallization is that the amount of solute that can remove the insoluble impurity be dissolved by a solvent increases and then allowed to cool. On with temperature. In recrystallization, cooling the purified desired compound will crystallise out compound must be a solid at room of solution. temperature. Recrystallization is often used as a final clean-up step, after other methods (such as If you did not filter while hot, extraction or column then the solid which came chromatography) that are effective at out of the cold solution would removing larger amounts of still contain the insoluble impurities, but that do not raise the impurities. purity of the final compound to a You filter the solution to sufficiently high level. remove the insoluble In hot filtration, the impurity less impurities. If not filtered hot, soluble than the sample will remain the solution might crystallize on the filter paper. quickly thus trapping the insoluble impurities. The funnel has to be kept hot , to Although the terms "crystallization" avoid crystallization on its stem . and "recrystallization" are sometimes used interchangeably, they technically refer to different processes. Crystallization refers to the formation of a new, insoluble product by a chemical reaction; this product then precipitates out of the reaction solution as an amorphous solid containing many trapped impurities. Recrystallization does not involve a chemical reaction; the crude product is simply dissolved into solution, and then the conditions are changed to allow crystals to re- form. Recrystallization produces a more pure final product. For this reason, experimental procedures that produce a solid product by crystallization normally include a final recrystallization step to give the pure compound. Recrystallization is a method of purifying a compound by removing any impurities that might be mixed with it. It works best when the compound is very soluble in a hot solvent, but very insoluble in the cold version of the same solvent. The 2. What are the methods of inducing crystal formation from solution? liquid to evaporate (very slowly) a) increasing The first thing is by concentrations of the "scratching" or rubbing constituents until the solubility constant the flask with a glass conditions are reached. This rod or metal spatula. A can be done by removing second tactic is the use solvent, by adding one or of seed crystals. Taking several constituents in just a few crystals from concentrated form, or by the previous crop and changing the state of putting them in your constituents into the form solution will promote the that will cause crystallization. growth of more crystals. Often, it is enough to b) providing nuclei for just stir the solution with crystallization to avoid a spatula that has formation of supersaturated touched some of the solutions. desired crystals. reduce the volume of the Supersaturated solutions hold more solvent (boiling, solute than should be possible. evaporation, low pressure) Hence they are very unstable. There are a few ways to make the solute crystallize: add solvent which the Put in a crystal of the solute. solute is not soluble in, e.g. Sometimes any small particle, or adding ethanol to water even dust, will do the trick. precipitates some things Scratch the glass container (on the inside) A ferm knock or shake cooling (and heating, when the solubility of the compound relies on the presence of a dissolved gas e.g. CaCO3 - limescale)