Purification by Steam distillation/crystallisation
Procedure
Steam Distillation:
- 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.
- Heat the mixture to avoid the condensation of steam in it.
- The water in the flask is heated & then a current of steam is passed into the mixture.
- Ortho nitro phenol is steam volatile, so it readily passes over in the steam.
- The vapour of the compound along with steam leaves the flask from the outlet & gets condensed in the water condenser.
- It is then collected in a conical flask containing ice to solidify the liquid.
- 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.