ppt课件-chem333lablecture.pptVIP

Recrystallization Lab New Techniques Recrystallization: method of purifying an organic solid Gravity Filtration: method of removing insoluble impurities from recrystallization solution Suction Filtration: method of isolating pure solid from liquid (filtrate) using vacuum In Lab Recrystallization Determine best solvent for recrystallization Weigh crude solid Recrystallize Weigh purified product After Lab Let recrystallized solid air dry on shelf. Weigh dry crystals and take a melting point (next week). Calculations: % recovery: [mass crude/mass recrystallized] x 100 Conclusions: Discuss effectiveness of recrystallization process in terms of purity and percent recovery. Discuss role/attributes of solvent, sources of error, etc. Theory of Recrystallization Steps in Recrystallization 1. Dissolve crude solid in hot solvent (saturated solution) 2. Let solution cool to room temperature, so that crystal lattice reforms. 3. Cool solution in an ice bath. 4. Suction filter the pure solid, leaving impurities in solution. 5. Let solid air dry to remove traces of solvent. Recrystallization Recrystallization Recrystallization An Ideal Recrystallization Solvent Should should dissolve all of the compound when the solvent is hot (boiling). should dissolve none of the compound when the solvent is at room temperature. should have different solubilities for the compound and the impurities. should have a lower boiling point than the melting point of the compound. should have a fairly low boiling point should be cheap, non-toxic, non-reactive, and non-smelly * Pure solid: Tight crystal lattice Impurities disrupt the crystal lattice 1. Add hot solvent until solid dissolves: (use minimum amount of hot solvent) 2. Let solvent cool slowly to room temperature, so crystal lattice can reform. 3. Cool in ice bath to make sure that the maximum amount of solid has crystallized. (Suction filtration gets cold!) 4. Suction filter solid away from impurities. 5. Let crys