Recrystallization 2100L and 2211L Recrystallization is an important method for the purification of solids In this experiment you will be given an impure sample of an unknown organic solid which you will purify by recrystallization and identify by determining its melting point You should read sections T2 and T3 of your lab text before writing your prelab for thorough explanations of recrystallization and melting points Safety Be certain to add a boiling chip to any liquid before heating it Procedure Add about 150 mL of water and a boiling chip to a 250 mL Erlenmeyer flask and heat the water to a boil In a 125 mL Erlenmeyer flask add one gram of a solid unknown and a boiling chip Add about 10 mL of boiling water to the unknown and keep the mixture hot on a hot plate Stir the hot mixture for about one minute Continue to add boiling water to the flask 2 3 mL at a time and stirring for one minute after each addition until the unknown dissolves Some insoluble impurities may remain and can be distinguished from the unknown by their appearance Filter the hot solution by gravity through a powder funnel containing fluted or folded filter paper into a 125 mL Erlenmeyer flask The solution must remain hot during this operation It is always a good idea to moisten the filter paper with some hot solvent water in this experiment prior to filtration to prevent cooling Rinse the filter paper with 2 3 mL of boiling water to dissolve any crystals that may have formed from cooling Allow the filtrate to cool slowly to room temperature If no crystals have formed after cooling scratch the inner wall of the flask with a glass rod to induce crystallization Once crystal formation has ceased cool the flask in an ice bath for 10 minutes to precipitate more crystals Collect the recrystallized solid by vacuum filtration using a B chner funnel Wash the crystals with a few mL of cold water and press them down with a spatula Allow the vacuum to pull for at least 10 minutes to help dry the crystals Scrape the crystals onto a tared watch glass and determine the mass of the recrystallized unknown Determine the melting point of the unknown and try to identify it from the table below Conduct a mixed melting point experiment by melting a mixture of your unknown and the authentic sample you believe your solid unknown to be If you observe a melting point depression of 5 oC or greater repeat the mixed melting point experiment with the unknown with the next closest melting point Solid Unknowns Compound vanilin ethyl 3 5 dinitrobenzoate o toluic acid acetanilide benzoic acid benzamide m nitrobenzoic acid o nitrobenzoic acid salicylic acid o nitrobenzamide p anisic acid mp oC 83 95 105 115 122 130 142 148 161 178 185 Discussion Your report should state the identity of your unknown and a discussion on how you determined it Calculate the percent recovery of your unknown Questions 1 solvent to your unknown when attempting to recrystallize it 2 recrystallization How could you explain a percent recovery that was greater than 100 after your What could be done without starting over if you added significantly too much
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