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- Set up a distillation assembly / carry out an assembly with
the backward flow.
- In a 250 mL dicol, pour 20 ml of pure glacial ethanol
acid, 15 mL of isoamyl
alcohol (or 3 - methylbutan - 1- ol), then 1 mL of
concentrated sulfuric
acid.
- Add a few grains of pumice, then heat the whole with the backward
flow for 30 minutes.
- Cool the dicol, then pour its content into a 250 mL separatory
funnel.
- Add 25 mL of sodium
bicarbonate solution.(CAUTION
: A strong bubbling occurs. As soon as the gas evolution
has almost ceased, seal the funnel, then shake / stir it with
its valve open to eliminate the gas which is produced, and let
it decant.)
- Throw away the aqueous phase into the sink, and pour the organic
phase into a dry Erlenmeyer flak.
- Dry the organic phase with some anhydrous magnesium
sulfate. Filtrate it on a paper folded filter, then
collect the fitrate into a 100 mL ground-in monocol fat flask
/ a ground-in boiling flask.
- Distil the dry organic phase, and collect the portion over 137°
temperature into a ground-in 50 mL Erlenmeyer flask (isoamyl
acetate or ethanoate
of 3 - methylbutyl).
CAUTION : It is important to work
under a hood and to wear gloves and safety goggles
while manipulating glacial ethanol
acid and concentrated sulfuric
acid.
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Boiling point ( p = 1 bar)
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Density
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Solubility in water
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Isoamyl alcohol
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131
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0,81
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slightly soluble
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Ethanol
acid
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117
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1,05
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highly soluble
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Isoamyl acetate
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142
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0,87
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slightly soluble
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Ilustrations |
© minc.f.
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