- Purification of Carbon tetrachloride
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For many purposes, careful fractional distn gives adequate purification. disulfide can be removed by shaking vigorously for several hours with saturated KOH, separating, and washing with water: this treatment is repeated. The (CAS NO. ) is shaken with conc H2SO4 until there is no further coloration, then washed with water, dried with CaCl2 or MgSO4 and distd (from P2O5 if desired). It must not be dried with sodium. An initial refluxing with mercury for 2h removes sulfides. Other purification steps include passage of dry CCl4 through activated alumina, and distn from KMnO4. Carbonyl containing impurities can be removed by percolation through a Celite column impregnated with 2,4-dinitrophenylhydrazine (DNPH), H3PO4 and water. (Prepared by dissolving 0.5g DNPH in 6mL of 85% H3PO4 by grinding together, then mixing with 4mL of distd water and log Celite.)
Photochlorination of Carbon tetrachloride has also been used: CCl4 to which a small amount of chlorine has been added is illuminated in a glass bottle (e.g. for 24h with a 200W tungsten lamp near it), and, after washing out the excess chlorine with 0.02M Na2SO3, the CCl4 is washed with distd water and distd from P2O5. It can be dried by passing through 4A molecular sieves and distd. Another purification procedure is to wash CCl4 with aq NaOH, then repeatedly with water and N2 gas bubbled through the liquid for several hours. After drying over CaCl2 it is percolated through silica gel and distd under dry N2 before use.
Rapid purification: Distil, discarding the first 10% of distillate or until the distillate is clear. The distilled CCl4 is then stored over 5A molecular sieves.
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