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Experiment # 4

Distillation

Impure compound

Isolation

Extraction

Purification

Recrystallization Solids only Distillation Liquids only Chromatography Solids or Liquids

Establishing purity

Melting point Boiling point Spectroscopy

Distillation
Purification of liquids by vaporization and condensation

liquid

vaporization

vapor

condensation

liquid

Purification methods for liquids

Distillation Simple distillation Fractional distillation Vacuum distillation Steam distillation

Simple Distillation
Separating liquids from a. Non volatile impurities b. Another liquid boiling at least 400 C higher than the first.

Theory of simple distillation


Diagram of dependence of vapor pressure on temperature. Blue curve is for pure water, and green curve is for a solution of water and sugar

Vapor pressure(torr)

Simple Distillation
Purpose
Purification of Cyclohexane (b.p. 810C at 760 torr), volatile organic liquid, containing a nonvolatile impurity, Dye

Setting Up

Simple Distillation

Simple Distillation
Dos and Don'ts
Place 10 mL of cyclohexane, 2 drops of dye, stir bar in R.B flask Place the heating mantle after adding the liquid to the round bottom flask (fig. 3) The top of the mercury bulb of the thermometer should be adjacent to the side arm of the still head. (fig. 5) Use Keck clips to hold the condenser, vacuum adapter, and receiver in place ( fig.8)

Simple Distillation
Begin heating the R.B. flask. As soon as the liquid begins to boil and the condensing vapors have reached the thermometer bulb, regulate the heat supply so that distillation continues steadily at a rate of 2-4 drops per second If a drop of liquid cannot be seen suspended from the end of the thermometer, the rate of distillation is too fast. As soon as the distillation rate is adjusted and the head temperature is constant, note and record the temperature Stop heating when only 2-3 ml of impure cyclohexane remains in the distillation flask . Record the volume of distilled cyclohexane that you obtained

Simple Distillation
Cyclohexane + Dye

Simple distillation

Residue

Distillate ( 78-840C or actual)

Dye

Cyclohexane

Fractional Distillation
The technique can be used to separate pure liquid components from a mixture containing two or more volatile substances if their boiling points are close to each other

It involves multiple simple distillations

Theory of Fractional Distillation

Fractional Distillation
Purpose
To separate the two volatile components, Cyclohexane ( b.p. 810C), and Toluene ( b.p. 1100C)

Fractional Distillation
Setting Up

Fractional Distillation
Dos and Donts
Place 10 mL of cyclohexane, 20 mL of toluene, stir bar in R.B. flask

When packing the column, be careful not to break off the glass indentations at the base of the column

Do not pack the column too tightly The top of the mercury bulb of the thermometer should be adjacent to the side arm of the still head.

Use Keck clips to hold the column, condenser, vacuum adapter, and receiver in place

Fractional Distillation
As the mixture is heated, the head temperature will rise to 810C(760 torr), and distillation will begin

Regulate the heat so that distillation continues steadily at a rate no faster than one drop of distillate every 1-2 sec

If a drop of liquid cannot be seen suspended from the end of the thermometer, the rate of distillation is too fast

Fractional Distillation
Collecting fractions Collect the first fraction at 810C 30C , label it A Change to the second receiver and increase the heat, label it B Collect the last fraction when temperature reaches 1100C, label it C

Results The temperature range while the distillation is steady ( 1 & 3 fractions ) The volume of distillate collected in each receiver

Fractional Distillation

Save samples, Waste disposal


Three fractions obtained from fractional distillation should be saved for the future lab gas chromatography

Dispose of glass beads in used glass beads container

The cyclohexane obtained from simple distillation should be disposed of in non halogenated waste container

Lab report
This experiment has two separate lab reports for simple distillation and fractional distillation which must include the following: 1.Date and title of the experiment 2. Introduction ( principle ) 3. Flow chart 4. Observations 5. Results 6. Conclusions and discussions