Purification by Steam distillation/crystallisation

Procedure

Steam Distillation:

  1. The organic mixture together with some water is placed in an R.B flask which is then connected to a steam generator on one side & a water condenser on the other.
  2. Heat the mixture to avoid the condensation of steam in it.
  3. The water in the flask is heated & then a current of steam is passed into the mixture.
  4. Ortho nitro phenol is steam volatile, so it readily passes over in the steam.
  5. The vapour of the compound along with steam leaves the flask from the outlet & gets condensed in the water condenser.
  6. It is then collected in a conical flask containing ice to solidify the liquid.
  7. Pure o-nitro phenol is filtered at the Buchner funnel and the residue in the distillation flask contains p-nitro phenol.

Points to Remember while Performing the Experiment in a Real Laboratory:

  • Always wear a lab coat and gloves when you are in the lab. Switch on the exhaust fan upon entering.
  • Ensure all required chemicals and reagents are available; if not, prepare them accordingly.
  • Adjust the Bunsen burner flame properly — a small blue cone is ideal.
  • Clean all apparatus with chromic acid and distilled water. Ensure they are free from water droplets.
  • Calibrate the electronic weighing balance before measurements.
  • Ensure the desiccator contains sufficient desiccant (e.g., silica gel).
  • Clean the crucible with chromic acid, heat it, and cool it before placing in the desiccator. Use tongs or tissue — never touch with bare hands.
  • Set the hot air oven to 130°C and handle with cotton gloves.
  • Clean Kipp’s apparatus tubes and ensure they are loaded with solid material (iron sulfide) and H2SO4 for producing H2S gas.
  • Clean all glassware with soap and distilled water. Recap reagent bottles after use.
  • Before leaving the lab, turn off the lights, exhaust fan, oven, and gas cylinder.
  • Dispose of used gloves in the appropriate waste bin.