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12 Cards in this Set

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Liquid in Distilling Flask

Should onlybe 1/3 to 1/2 full, if too full will cause bumping


Do notdistill all the liquid, will cause flask to explode

Distillation Set Up

Clampflask, and fit the distilling head and thermometer (and its adapter) in complete vertical position


Attach a clampedcondenser with the inlets facing upwards, using keck clips


Attach avacuum adapter at other end and clamp and place a container underneath

Thermometer

Recordsheat of the vapor, will take a while to increase since it needs to wait for vapors to reach it (position above the sidearm)


Adjust heatso that collection rate is 1-2 drops per second

Collecting Fractions

Forerun:fractions collected below 5°C of expected boiling point that should be discarded


Record tempat which product fractions are collected

End of Distillation

Leave someresidue or else flask will overheat and break or last drops will char


Ethers,secondary alcohols and alkenes from peroxides by air oxidation and will explode if carried out to dryness

Fractional Distillation

Many vaporizations and distillations happen before the distillate is collected


Separate components of mixture based on their vapor pressure differences (less than 50 C apart)


Use a vigreux column

Fractional Distillation Process

Vapor cools to liquid as it goes up condenser then vaporizes again after it comes into contact with hotter vapor rising from below

Efficiency of Condenser

Expressed as its number of theoretical plates


One theoretical plate is equivalent to one simple distillation cycle


Reported as HETP, lower = more efficient

Surface Area

The larger,the more efficient the column will be (8 plates: 25° C apart)

Things to remember

Doublecheck set up before turning on heat; remember to add 2-3 boiling stones

Types of Distillations

Simple:remove low boiling solvent or last step in purification


Fractional:Separate mixture of 2 or more liquid compounds whose boiling points differ byless than 60°-70° C


Steam:Separate volatile compounds from complex mixtures


Vacuum:when boiling point is over 200°C (reduce atmospheric pressure)

Changing Receiving Flasks

Simple:change at 5° C beforeexpected boiling point


Fractional: change after suddenchange in temp (indicating lower temp distillation is complete)