Umkristallisation von Benzoesäure
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Reinigung eines Feststoffs durch Lösen in heißem Lösungsmittel und Abkühlen
Ziel
Unreine Benzoesäure durch Umkristallisation aus heißem Wasser reinigen und dabei die Standardreinigungsmethode für organische Feststoffe demonstrieren.
Hintergrund
Recrystallization exploits the difference in solubility of a substance at different temperatures. Benzoic acid is very soluble in hot water but nearly insoluble in cold water. By dissolving impure benzoic acid in hot water and cooling slowly, pure crystals form while impurities remain in solution.
Sicherheitswarnungen
- Handle hot water and hot glassware with care
- Benzoic acid dust can irritate airways
- Use heat-resistant gloves when handling hot flasks
Erforderliche PSA
Materialien
-
Impure benzoic acid (3 g)Mixed with charcoal or sand
-
Distilled water (200 mL)
-
Activated charcoal (0.5 g)Optional, for decolorization
Ausrüstung
Durchführung
Weigh 3 g of impure benzoic acid and record the mass. Note the appearance (color, particle size).
Add the impure sample to 100 mL of distilled water in the Erlenmeyer flask. Heat to boiling while stirring.
If the solution is colored, add 0.5 g activated charcoal, swirl, and filter hot through fluted filter paper.
Allow the clear filtrate to cool slowly to room temperature. Do not disturb.
Cool further in an ice bath to maximize crystal yield.
Collect the crystals by vacuum filtration. Wash with a small amount of ice-cold water.
Dry the crystals on a watch glass. Weigh and calculate percent recovery.
Determine the melting point (pure benzoic acid: 122°C) and compare with the impure sample.
Erwartete Ergebnisse
White, needle-like crystals with a sharp melting point at 121-123°C. Typical recovery is 60-80%. The purified crystals should be whiter and have a sharper melting point than the crude material.
Aufräumen
Dispose of filtrate down the drain (benzoic acid is food-grade). Rinse glassware. Dispose of charcoal in solid waste.
Details
- Kategorie
- Crystallization
- Schwierigkeit
- Intermediate (High School)
- Dauer
- 45 Min.
- Geschätzte Kosten
- $10,00
- Schritte
- 8
- Materialien
- 3