루미놀 합성

3-나이트로프탈산에서 화학발광 화합물 만들기

Organic Synthesis Professional (Lab) 120 분 ~$30.00

목표

루미놀(3-아미노프탈히드라지드)을 합성하고 과산화수소와의 화학발광 반응을 실증한다.

배경

Luminol is a chemiluminescent compound used in forensic science to detect trace amounts of blood. It is synthesized by reacting 3-nitrophthalic acid with hydrazine, followed by reduction of the nitro group with sodium dithionite. When oxidized by hydrogen peroxide in the presence of a catalyst, luminol emits blue light.

안전 경고

  • Hydrazine is toxic and a suspected carcinogen — handle with extreme care in fume hood
  • Sodium dithionite generates SO₂ — use in fume hood
  • NaOH is corrosive
  • Wear nitrile gloves and goggles throughout

필수 개인 보호 장비

goggles gloves lab_coat

재료

  • 3-Nitrophthalic acid (1 g)
  • Hydrazine hydrate (10%) (3 mL)
    Toxic
  • Triethylene glycol (5 mL)
    High-boiling solvent
  • Sodium dithionite (Na₂S₂O₄) (3 g)
    Reducing agent
  • Sodium hydroxide (NaOH) (5 mL)
    10% solution
  • Hydrogen peroxide (H₂O₂) (10 mL)
    3% for chemiluminescence test
  • Potassium ferricyanide (0.1 g)
    Catalyst for glow test

장비

Round-bottom flask (50 mL) Reflux condenser Hot plate Buchner funnel Filter flask Darkened room Test tubes

실험 절차

1

Dissolve 1 g 3-nitrophthalic acid in 5 mL triethylene glycol in the round-bottom flask. Heat to 100°C.

5 분 Fume hood required
2

Add 3 mL of 10% hydrazine hydrate. Attach the reflux condenser and heat at 130-140°C for 30 minutes.

35 분 Hydrazine is toxic — fume hood essential
3

Cool the mixture. Add 15 mL hot water and 3 mL 10% NaOH.

5 분
4

Add 3 g sodium dithionite to reduce the nitro group. Heat at 80°C for 10 minutes.

12 분 SO₂ released — fume hood
5

Acidify the solution with glacial acetic acid until luminol precipitates.

5 분
6

Collect the luminol by vacuum filtration. Wash with cold water and dry.

10 분
7

Test chemiluminescence: dissolve a small amount of luminol in 5 mL of dilute NaOH. In a darkened room, add H₂O₂ and a trace of potassium ferricyanide.

5 분
8

Observe the blue glow. Record intensity and duration.

3 분

예상 결과

A pale yellow solid (luminol). When tested with H₂O₂ and ferricyanide catalyst in a dark room, an intense blue chemiluminescent glow should last for 15-30 seconds. The glow confirms successful synthesis.

정리

Dispose of hydrazine waste in designated hazardous waste container. Neutralize acids and bases. Rinse all glassware thoroughly. Decontaminate work area.

세부 정보

카테고리
Organic Synthesis
난이도
Professional (Lab)
소요 시간
120 분
예상 비용
$30.00
단계
8
재료
7

더 많은 실험

아세트산에틸의 피셔 에스테르화 90 min 아세트아미노펜(파라세타몰) 조제 80 min 아스피린(아세틸살리실산) 합성 90 min 식물성 기름에서 바이오디젤 생산 60 min 비누화 반응으로 비누 만들기 60 min 차에서 카페인 추출 90 min 바나나 오일(아세트산이소아밀) 합성 90 min 알돌 축합(디벤잘아세톤) 75 min 나일론 6,10 합성(나일론 로프 트릭) 30 min 슬라임 합성(가교 PVA) 20 min

Frequently Asked Questions

What is the objective of 루미놀 합성?
루미놀(3-아미노프탈히드라지드)을 합성하고 과산화수소와의 화학발광 반응을 실증한다.
How difficult is 루미놀 합성?
This experiment is rated as Professional (Lab). It takes approximately 120 minutes to complete.
What safety precautions are needed for 루미놀 합성?
Key safety precautions include: Hydrazine is toxic and a suspected carcinogen — handle with extreme care in fume hood; Sodium dithionite generates SO₂ — use in fume hood; NaOH is corrosive.
What materials are needed for 루미놀 합성?
The main materials required are: 3-Nitrophthalic acid, Hydrazine hydrate (10%), Triethylene glycol, Sodium dithionite (Na₂S₂O₄), Sodium hydroxide (NaOH).
What results should I expect from 루미놀 합성?
A pale yellow solid (luminol). When tested with H₂O₂ and ferricyanide catalyst in a dark room, an intense blue chemiluminescent glow should last for 15-30 seconds. The glow confirms successful synthesis.