Chapter 4

CONCLUSION AND RECOMMENDATION

Fractional distillation is an effective way of separating two or more miscible liquids. The separation is based
on the boiling point differences of the mixture that is usually less than 25 degrees Celsius. Binary liquid is a type of
two liquids that are completely miscible with one another. The boiling point of the binary solution depends upon the
solution composition. Binary distillation is done by boiling the mixture creating two phases which are liquid and vapor.
As the assumption by McCabe-Thiele method stated, every mole of liquid vaporized a mole of vapor is condensed.

In the experiment, a mixture of glacial acetic acid and water was prepared. Fractional distillation is used to
separate the mixture and the distillate and residue was both titrated using the standardized NaOH. As fractional
distillation was made step by step, we observed that the first distillate had the highest volume of titration and the last
distillate has the lowest. This made a positive result that the concentration of acetic acid is decreasing and also to its
mole percent as the fractionating column is used to allow for repeated simple distillation of the two liquids in a step by
step process. The boiling point also decreases as columns were made. With this result, we also concluded that the
water has a lower boiling point than the acetic acid thus it vaporizes first and a more concentrated acid was left in the
flask. The higher the concentration of acetic acid, the higher the boiling point of the mixture. Based on this result, the
concentration of acetic acid is greater in the residue than in the distillate. As moles of acetic acid decreases in the
mixture, the moles of water increases. Lower total pressure than room pressure asserts the idea that attraction
between unlike molecules are greater than between like molecules thus, acetic acid and water tend to adhere to each
other.

In the boiling point – composition diagram made, the line of vapor lies higher than the liquid form which
followed the phase diagram. This is deemed as a positive result since the higher curve is called the dew point at
which saturated vapor starts to condense and the lower curve is called the bubble point at which liquid starts to boil.
Above the dew point is the superheated vapor and below the bubble point is the subcooled liquid. The region
between the two curves represents a two phase mixture. Another important variable is the relative volatility of acetic
acid and water. It is an indication whether it would be easy or hard to separate the liquids. If relative volatility is very
close with one another, it would be hard since they have very similar boiling points and vapor pressure.

For further improvement of this experiment, the students should also know the effect of azeotrope or a
constant boiling point mixture of liquids whose proportions cannot be changed by distillation and whose vapor has the
same composition as the liquid. The students should also know how to break an azeotrope such as adding a third
substance, use of molecular sieve, and a pressure-swing distillation. To have an ideal and uniform equilibrium curve,
accurate volume of distillate must be taken and the titration of the solution must be accurate. The students should
also know and consider the effect of relative volatility in distilling mixtures because it can also be an error in executing
this experiment.
DOCUMENTATION

Figure 1. Distillation Set-Up

Figure 2. Collecting the Residue

Figure 3. Collecting the Distillate

Figure 4. Titrating the Distillate and Residue