INTRODUCTION: 50 0C difference in their respective boiling points.

As the
liquid is subjected to heating, the first compound having
The boiling point of a liquid is the indicated temperature the lowest boiling point will evaporate first. Purified
at which the vapor pressure and the atmospheric compounds will boil, and thus turn into vapors, over a
pressure are in equilibrium to each other. Under this relatively small temperature range (2 or 3°C); by carefully
condition, addition of heat results into phase transition of watching the temperature in the distillation flask, it is
liquid into vapor. According to Encyclopedia Britannica possible to affect a reasonably good separation. As
(2018), at any temperature a liquid partly vaporizes into distillation progresses, the concentration of the lowest
the space above it until the pressure exerted by the vapor boiling component will steadily decrease. Eventually the
reaches a characteristic value called the vapour pressure temperature within the apparatus will begin to change; a
of the liquid at that temperature. As the temperature is pure compound is no longer being distilled. The
increased, the vapor pressure increases; at the boiling temperature will continue to increase until the boiling
point, bubbles of vapor form within the liquid and rise to point of the next-lowest-boiling compound is approached.
the surface. The boiling point of a liquid varies according When the temperature again stabilizes, another pure
to the applied pressure. fraction of the distillate can be collected. This fraction of
Idealized models of distillation are essentially governed distillate will be primarily the compound that boils at the
by Raoult's law and Dalton's law and assume that vapor– second lowest temperature. This process can be
liquid equilibria are attained. Raoult's law states that the repeated until all the fractions of the original mixture have
vapor pressure of a solution is dependent on 1) the vapor been separated.
pressure of each chemical component in the solution and For an effective distillation method, one must consider the
2) the fraction of solution each component makes up. This following (De Castro,Baluyut, 2016):
law applies to ideal solutions, or solutions that have
different components but whose molecular interactions  The substances to be separated must have a
are the same as or very similar to pure solutions. large volatility difference. Often, this translates
(Wikipedia, 2019) to a boiling point difference of around 80°C to
100°C. Otherwise, both compounds may be
distilled off and will not be separated from each
other.
 Heat must be supplied to the distilling flask
gently.
 The thermometer bulb used to measure the
boiling of the distilling liquid must be at the level
of the sidearm.
 The distilling flask must always be in an upright
Figure 1. Two liquid-vapor equilibrium diagram position.
The two liquid-vapor equilibrium lines (one curved, the  Glass beads or ceramic material must always
other straight) now enclose an area in which liquid and be present inside the distilling flask prior to
vapor can coexist; outside of this region, the mixture will heating of the mixture.
consist entirely of liquid or of vapor. At this particular  Fresh cooled water must always fill the
pressure (part where number 1 is located), the intercept condenser, therefore, running water should be
(part where number 2 is located) with the upper boundary applied to the condenser.
of the two-phase region gives the mole fractions of A and
On the other hand, steam distillation is a separation
B in the liquid phase, while the intercept (part where
process used to purify or isolate temperature-sensitive
number 3 is located) with the lower boundary gives the
materials, such as natural aromatic compounds. Steam
mole fractions of the two components in the vapor.
or water is added to the distillation apparatus, lowering
(LibreTexts, 2019)
the boiling points of the compounds. The goal is to heat
In relation to distillation, a simple distillation method can and separate the components at temperatures below
be used effectively to mixed compounds of having at least their decomposition point. Because water and organics
tend to be immiscible, the resulting liquid generally The experiment is divided into two parts: the simple
consists of two phases: water and the organic distillate. distillation method; and the steam distillation method.
Decantation or partitioning may be used to separate the
two layers to obtain the purified organic material. For simple distillation method (refer to Figure 2 for set-
up), transfer 15 mL of impure carbon tetrachloride in the
When organics are distilled, the vapor is condensed. pear-shaped flask (the flask should only contain 1/3 of its
When a mixture of two immiscible liquids (e.g., water and volume). To begin the distillation, turn on the hot plate as
organics) is heated and agitated, the surface of each the source of heat. Observe the receiving flask for any
liquid exerts its own vapor pressure as though the other presence of distillate. Afterwards, record the volume per
component of the mixture was absent. Thus, the vapor drop per time of the distillate in the receiving flask and per
pressure of the system increases as a function of change in temperature.
temperature beyond what it would be if only one of the
components was present. When the sum of the vapor For steam distillation, weigh two grams sample of p-
pressures exceeds atmospheric pressure, boiling begins. dichlorobenzene. Prior to distillation boil 100 mL of water
Because the temperature of boiling is reduced, damage in the Erlenmeyer flask and connect it to the set-up (this
to heat-sensitive components is minimized. will serve as the steam generator). After which, connect
(Helmenstine, 2019) the sample (p-dichlorobenzene) in the set-up. Continue
the process until the distillate is collected. Filter the
distillate with Buchner funnel , weigh and test for its
melting point to determine its purity.

REFERENCES:

Wikipedia. (2019). Distillation. Retrieved October

Figure 2. Set-up for distillation
7, 2019, from
The distillation method set-up composed of three main https://en.wikipedia.org/wiki/Distillation.
parts: steam generator which supplies sufficient steam
to the organic compound; distilling flask which contains Lower, S. (2019, June 17). 4.5: Separating Volatile
the sample and is connected to the source of heat; and Solutions - Distillation. Retrieved from
receiving flask which will contain the distillate. https://chem.libretexts.org/Courses/University_of
_California_Davis/UCD_Chem_002BH/Text/Unit
Given the knowledge about this method, one should be
precautious of the following (De Castro,Baluyut, 2016): _II:_Physical_Equilibria/IV:_Solutions/4.5:_Separ
ating_Volatile_Solutions_-_Distillation.
 Both the steam generator and the sample flask
must contain boiling chips before heating is Helmenstine, A. M. (2019, July 25). When and
started. How Is Steam Distillation Used in Chemistry?
 Heat is supplied to both the steam generator Retrieved October 7, 2019, from
and the sample flask gently. https://www.thoughtco.com/definition-of-steam-
 The condenser must always be filled with fresh distillation-605690.
water during the entire process.
 The compound being steam distilled must not
have any reaction with water.

METHODOLOGY: