안식향산 재결정 정제
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뜨거운 용매에 녹인 후 냉각하여 고체 정제하기
목표
뜨거운 물에서 재결정으로 불순한 안식향산을 정제하고, 유기 고체의 표준 정제 기술을 실증한다.
배경
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.
안전 경고
- Handle hot water and hot glassware with care
- Benzoic acid dust can irritate airways
- Use heat-resistant gloves when handling hot flasks
필수 개인 보호 장비
재료
-
Impure benzoic acid (3 g)Mixed with charcoal or sand
-
Distilled water (200 mL)
-
Activated charcoal (0.5 g)Optional, for decolorization
장비
실험 절차
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.
예상 결과
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.
정리
Dispose of filtrate down the drain (benzoic acid is food-grade). Rinse glassware. Dispose of charcoal in solid waste.
세부 정보
- 카테고리
- Crystallization
- 난이도
- Intermediate (High School)
- 소요 시간
- 45 분
- 예상 비용
- $10.00
- 단계
- 8
- 재료
- 3