安息香酸の再結晶精製
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熱溶媒に溶かして冷却することで固体を精製する
目的
熱水からの再結晶により不純な安息香酸を精製し、有機固体の標準精製技術を実証する。
背景
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.
安全上の警告
- Handle hot water and hot glassware with care
- Benzoic acid dust can irritate airways
- Use heat-resistant gloves when handling hot flasks
必要なPPE
材料
-
Impure benzoic acid (3 g)Mixed with charcoal or sand
-
Distilled water (200 mL)
-
Activated charcoal (0.5 g)Optional, for decolorization
器具
手順
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.
予想される結果
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.
後片付け
Dispose of filtrate down the drain (benzoic acid is food-grade). Rinse glassware. Dispose of charcoal in solid waste.
詳細
- カテゴリ
- Crystallization
- 難易度
- Intermediate (High School)
- 所要時間
- 45 分
- 推定費用
- $10.00
- ステップ数
- 8
- 材料
- 3