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Purification by Steam distillation/crystallisation
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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 in to 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:

 

  1. Always wear lab coat and gloves when you are in the lab. When you enter the lab, switch on the exhaust fan and make sure that all the chemicals and reagents required for the experiment are available. If it is not available, prepare the reagents using the components for reagent preparation.
  2. Properly adjust the flame of the Bunsen burner. The proper flame is a small blue cone; it is not a large plume, nor is it orange.
  3. Make sure to clean all your working apparatus with chromic acid and distilled water and ensure that all the apparatus are free from water droplets while performing the experiment.
  4. Make sure to calibrate the electronic weigh balance before taking the measurements.
  5. Ensure that the desiccator  has sufficient amount of desiccant; Silica gel
  6. Use chromic acid to clean the crucible, then heat it and make sure to cool it and before placing in the desiccators. Ensure that you are handling the crucible, with cleaned tongs or with tissue paper .Never touch it with your hand.
  7. Switch on the oven and adjust the temperature to 1300 C. Make sure to use a cotton glove while working with a hot air oven.
  8. Make sure to clean the Kipp's apparatus tube with water and ensure that it has sufficient solid material; iron sulfinide and acid, H2SO4 for producing H2S gas.
  9. Clean all glass wares with soap and distilled water. Once the experiment completed recap the reagent bottles. Switch off the light, exhaust fan, hot air oven and Gas cylinder before leaving the lab.
  10. Discard the used gloves in a waste bin.

 

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