SOP: Synthesis and Characterization of Azo Dyes from Schiff Base
Title
Synthesis and Characterization of Azo Dyes from Schiff Base with Studies on Their Degradation Efficiency
1. Objective
To synthesize azo dyes using Schiff bases as intermediates, characterize the dyes using spectroscopic
techniques, and evaluate their degradation efficiency under photocatalytic conditions.
2. Materials Required
Chemicals:
- Aromatic amines (e.g., aniline, p-toluidine)
- Aromatic aldehydes (e.g., salicylaldehyde, benzaldehyde)
- Sodium nitrite (NaNO2)
- Hydrochloric acid (HCl)
- Phenol or other coupling components
- Sodium hydroxide (NaOH)
- Titanium dioxide (TiO2) or Zinc oxide (ZnO)
- Ethanol or methanol
- Distilled water
Equipment:
- Magnetic stirrer
- Ice bath
- UV-Vis spectrophotometer
- FTIR spectrometer
- NMR spectrometer (if available)
- pH meter
- Hot plate
- Filtration apparatus
- UV lamp or sunlight exposure setup
SOP: Synthesis and Characterization of Azo Dyes from Schiff Base
3. Procedure
Step 1: Synthesis of Schiff Base
- Dissolve equimolar amounts of aromatic amine and aldehyde in ethanol and stir for 23 hours.
- Heat gently if needed and monitor by TLC.
- Filter, wash, and dry the product.
Step 2: Diazotization
- Dissolve Schiff base in dilute HCl and cool to 05C.
- Add sodium nitrite solution dropwise under stirring, keeping temperature below 5C.
Step 3: Coupling Reaction
- Prepare cold alkaline phenol solution.
- Add diazonium salt solution dropwise while maintaining pH 810.
- Stir for 12 hours, filter, wash, and dry the dye.
4. Characterization
a) UV-Visible Spectroscopy: Measure max and absorbance.
b) FTIR Spectroscopy: Identify N=N, OH, C=N groups.
c) 1H NMR (if available): Confirm structure via proton shifts.
d) Melting Point: Check purity.
5. Photocatalytic Degradation Study
a) Prepare 1050 ppm dye solution.
b) Add photocatalyst and stir in dark for 30 min.
c) Expose to UV or sunlight, sample every 1020 min.
d) Use UV-Vis to measure absorbance and calculate degradation %:
Degradation (%) = ((A0 - At) / A0) 100
SOP: Synthesis and Characterization of Azo Dyes from Schiff Base
6. Safety Precautions
- Wear lab coat, gloves, goggles.
- Handle acids and nitrites with care.
- Keep temperature low during diazotization.
- Dispose of waste properly.
7. Conclusion
This SOP outlines the synthesis, characterization, and degradation study of azo dyes using Schiff
bases. It supports eco-friendly dye development and wastewater remediation research.