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 Purification of Diethyl ether (Ethyl ether)
  • Purification of Diethyl ether (Ethyl ether)
  • Usual impurities of Diethyl ether (CAS NO. ) are water, EtOH, diethyl peroxide (which is explosive when concentrated), and aldehydes. Peroxides [detected by liberation of iodine from weakly acid (HCl) solutions of KI, or by the blue colour in the ether layer when 1mg of Na2Cr2O7 and 1 drop of dil H2SO4 in 1mL of water is shaken with 10mL of ether] can be removed in several different ways. The simplest method is to pass dry ether through a column of activated alumina (80g Al2O3/700mL of ether). More commonly, 1L of ether is shaken repeatedly with 5-10mL of a soln comprising 6.0g of ferrous sulfate and 6mL of conc H2SO4 in 110mL of water. Aqueous 10% Na2SO3 or stannous chloride can also be used. The ether is then washed with water, dried for 24h with CaCl2, filtered and dried further by adding sodium wire until it remains bright. The ether is stored in a dark cool place, until distd from sodium before use. Peroxides can also be removed by wetting the ether with a little water, then adding excess LiAlH4 or CaH2 and leaving to stand for several hours. (This also dried the ether.)

    Werner removed peroxides and aldehydes by adding 8g AgNO3 in 60mL of water to 1L of ether, then 100mL of 4% NaOH and shaking for 6min. Fierz-David shook 1L of ether with 10g of a zinc-copper couple. (This reagent was prepared by suspending zinc dust in 50mL of hot water, adding 5mL of 2M HCl and decanting after 20sec, washing twice with water, covering with 50mL of water and 5mL of 5% cuprous sulfate with swirling. The liquid was decanted and discarded, and the residue was washed three times with 20mL of ethanol and twice with 20mL of diethyl ether).

    Aldehydes can be removed from Diethyl ether by distn from hydrazine hydrogen sulfate, phenyl hydrazine or thiosemicarbazide. Peroxides and oxidisable impurities have also been removed by shaking with strongly alkaline satd KMnO4 (with which the ether was left to stand in contact for 24h), followed by washing with water, conc H2SO4, water again, then drying (CaCl2) and distn from sodium, or sodium containing benzophenone to form the ketyl. Other purification procedures include distn from sodium triphenylmethide or butyl magnesium bromide, and drying with solid NaOH or P2O5.


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