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3AL-Lecture5 - Purifying Solids Sublimation/Deposition...

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Purifying Solids ! Sublimation/Deposition ! Chromatography ! Recrystallization
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Recrystallization Step 1: Choosing the right equipment The Glassware " Test tube " Erlenmeyer flask Richard Erlenmeyer Large surface area Constricted opening
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Step 1: Choosing the right equipment The heating source " Water bath " Oil bath " Sand bath NEVER USE A BUNSEN BURNER FOR HEATING LIQUIDS IN THE ORGANIC CHEMISTRY LABORATORY!
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Step 2: Choosing a Solvent The Goal To find a solvent in which the solid is soluble at a higher temperature and less soluble or insoluble at a lower temperature. Heat Up Cool Down " G mixture = " H mixture - T " S mixture
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Step 2: Choosing a Solvent The Most Common Solvents water and ethanol H O H O H Other Common Solvents acetone, hexane , isopropanol , ethyl acetate O O O OH Boiling Range > 50 # 100 °C Low boiling solvents evaporate too easily and don’t allow for much energy input. High boiling solvents make it difficult to “dry” the crystals after they have been recovered from the solution. Try to keep the boiling point of the solvent below the melting point of the solid to avoid melting the solid before it dissolves.
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