Crystal Growth by Slow Cooling of the Solvent Substances that are much more soluble in a solvent at high temperature

than at low temperature are good candidates for crystal growth by slow cooling. Suggestions: - Make a saturated, or nearly saturated, solution just below the boiling point of the solvent. Filter while hot if any solid remains. Allow the solution to cool slowly. Sometimes just turning off the heat and letting the solution slowly cool on the hot plate (without stirring, of course) works well. - If the solution cools too quickly, owing to the coolness of the room, you may surround the beaker with insulation. Commercial ovens are available, but a Styrofoam cup or packing base from acid bottles covered with metal foil may work as well to slow the rate of cooling. With more volatile solvents, remove from the hot plate when dissolution is complete, and place on an insulated surface, such as a large cork, to cool. Most bench tops are relatively cold and the heat lost from the solution may be too rapid if the solution is placed on the bench top. - If the compound is rather soluble at room temperature, try putting the solution in the refrigerator to cool.

Crystal Growth by Slow Evaporation of the Solvent Substances that are moderately soluble at room temperature, and which are either not much more soluble or are unstable at higher temperatures are good candidates for crystal growth by slow evaporation. Suggestions: - Prepare a saturated solution, filter it, and place it in a beaker. Cover the beaker with foil or wax into which a few small holes have been punched. 2-3 pin-holes in parafilm over a 10 mL beaker works well, as long as the solvent does not dissolve the parafilm. Aluminum foil may be used if parafilm is a problem. - Check the solution each day. It is important to harvest the crystals before all of the solvent has evaporated.

Crystal Growth by Evaporation from a Two Solvent System Substances that are very soluble in one solvent and insoluble in a second solvent may be good candidates for crystal growth by vapor diffusion, two solvent evaporation or liquid diffusion. The two solvents must be miscible

(soluble in each other in all proportions). For evaporation, the good solvent must be much more volatile than the poor solvent. Suggestions: - Add a small volume (1 mL or more) of the poor solvent to a saturated solution. Add more of the good solvent if any precipitation occurs. Stir to ensure a homogeneous mixture. Cover the solution with foil or wax with a few pin-holes to allow the solution to slowly evaporate. - Some possible "good solvent/poor solvent" pairs are: chloroform/decane, acetone/m-xylene.

Crystal Growth by Liquid Diffusion Substances that are very soluble in one solvent and insoluble in a second solvent may be good candidates for crystal growth by vapor diffusion, two solvent evaporation or liquid diffusion. The two solvents must be miscible (soluble in each other in all proportions). For liquid diffusion, the two solvents should have different densities. Suggestions: - Make and filter a saturated solution of the substance. Carefully layer the solution and the poor solvent in a long, thin tube. (NMR tubes or glass tubing with one end closed, for example.) This layering may also work in a beaker or round-bottom flask, but it is easier to observe the crystal growth in the thin tubes. The liquid with the greater density should be on the bottom and the less dense liquid added so as not to cause mixing at the interface. - Some possible "good solvent/poor solvent" pairs are: aromatics/alkanes (Toluene/hexane, for example.), aromatics/ alcohols, and THF/hexane. (Caution: tetrahydrofuran tends to disorder in crystals.) Thanks to Dan Smith, Goshen College, for useful discussions. Crystal Growth by Vapor Diffusion Substances that are very soluble in one solvent and insoluble in a second solvent may be good candidates for crystal growth by vapor diffusion, two solvent evaporation or liquid diffusion. The two solvents must be miscible (soluble in each other in all proportions). For vapor diffusion, the poor solvent should be more volatile than the good solvent. Suggestions: - Put about 5 mL of a saturated solution in a 10 mL beaker. Place the beaker in a jar that contains about 15 mL of the more volatile, but poorer solvent. Put the lid on the jar and allow the solvents to reach equilibrium. - The liner of the lid to the jar should not react with the solvents. Lids with Teflon liners work well. Some possible "good solvent/poor solvent" pairs are: water/ethanol, chloroform/ether, acetone/pentane.