BAB I PROSEDUR KERJA

Prosedur dari Furniss : Ethanol of a high degree of purity is frequently required in preparative organic chemistry. For some purposes ethanol of c.99,5 per cent purity is satisfactory; this grade may be purchased ( the absolute alcohol of commerce ), or it may be conveniently prepared by the dehydration of rectified spirit with calcium oxide. Rectified spirit is the constant boiling point mixture which ethanol forms with water, and usually contains 95,6 per cent of ethanol by weight. Whenever the term rectified spirit is used in this book, approximately 95 per cent ethanol is to be understood. Ethanol which has been denaturated by the incorporation of certain toxic additives, notably methanol, to render it unfit for consumption, constitutes the industrial spirit ( industrial methylated spirit, IMS ) of commerce; it is frequently a suitable solvent for recrystallisations. Dehydration of rectified spirit by calcium oxide. Pour the contents of a Winchester bottle of rectified spirit ( 2 2,5 litres ) into a 3-litre roundbottomed flask and add 500 g of calcium oxide which has been freshly ignited in a muffle furnace and allowed to cool in a desiccator. Fit the flask with a double surface condenser carrying a calcium chloride guard-tube, reflux the mixture gently for 6 hours (preferably using a heating mantle) and allow to stand overnight. Reassemble the condenser for downward distillation via a splash head adapter to prevent carry-over of the calcium oxide in the vapour stream. Attach a receiver flask with a side-arm receiver adapter which is protected by means of a calcium chloride guard-tube. Distil the ethanol gently discarding the first 20 ml of distillate. Preserve the absolute ethanol (99,5%) in a bottle with a well fitting stopper.