Синтез люминола

Получение хемилюминесцентного соединения из 3-нитрофталевой кислоты

Organic Synthesis Professional (Lab) 120 мин ~$30,00

Цель

Синтезировать люминол (3-аминофталгидразид) и показать его хемилюминесцентную реакцию с пероксидом водорода.

Предпосылки

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.

Предупреждения по безопасности

  • 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

Требуемые СИЗ

goggles gloves lab_coat

Материалы

  • 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

Оборудование

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

Процедура

1

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

5 мин 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 мин Hydrazine is toxic — fume hood essential
3

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

5 мин
4

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

12 мин SO₂ released — fume hood
5

Acidify the solution with glacial acetic acid until luminol precipitates.

5 мин
6

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

10 мин
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 мин
8

Observe the blue glow. Record intensity and duration.

3 мин

Ожидаемые результаты

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.

Уборка

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

Детали

Категория
Organic Synthesis
Сложность
Professional (Lab)
Продолжительность
120 мин
Прим. стоимость
$30,00
Шаги
8
Материалы
7

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Frequently Asked Questions

What is the objective of Синтез люминола?
Синтезировать люминол (3-аминофталгидразид) и показать его хемилюминесцентную реакцию с пероксидом водорода.
How difficult is Синтез люминола?
This experiment is rated as Professional (Lab). It takes approximately 120 minutes to complete.
What safety precautions are needed for Синтез люминола?
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 Синтез люминола?
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 Синтез люминола?
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.