Sintesis Luminol

Membuat senyawa kemiluminesensi dari asam 3-nitroftalat

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

Tujuan

Sintesis luminol (3-aminoftalilhidrazida) dan demonstrasikan reaksi kemiluminesensnya dengan hidrogen peroksida.

Latar Belakang

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.

Peringatan Keselamatan

  • 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

APD yang Diperlukan

goggles gloves lab_coat

Bahan

  • 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

Peralatan

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

Prosedur

1

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

5 menit 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 menit Hydrazine is toxic — fume hood essential
3

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

5 menit
4

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

12 menit SO₂ released — fume hood
5

Acidify the solution with glacial acetic acid until luminol precipitates.

5 menit
6

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

10 menit
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 menit
8

Observe the blue glow. Record intensity and duration.

3 menit

Hasil yang Diharapkan

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.

Pembersihan

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

Detail

Kategori
Organic Synthesis
Tingkat Kesulitan
Professional (Lab)
Durasi
120 menit
Perkiraan Biaya
$30,00
Langkah
8
Bahan
7

Eksperimen Lainnya

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Frequently Asked Questions

What is the objective of Sintesis Luminol?
Sintesis luminol (3-aminoftalilhidrazida) dan demonstrasikan reaksi kemiluminesensnya dengan hidrogen peroksida.
How difficult is Sintesis Luminol?
This experiment is rated as Professional (Lab). It takes approximately 120 minutes to complete.
What safety precautions are needed for Sintesis Luminol?
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 Sintesis Luminol?
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 Sintesis Luminol?
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.