Gabriel Luis Fernandez 18B

Distillation of an Unknown Liquid December 11, 2014

Data and Results

Volume (in mL) Temperature (in Celsius)
st
1 Batch 2.5 30.6
2nd Batch 2.8 60.6
3rd Batch 16.0 66.7
Volume of unknown liquid 37.0
Volume produced from 21.3
distillation
Percent Recovery 57.57%
Table 1. Volume/temperature of distillates, Starting volume of unknown liquid, Total volume
of distillates and percent recovery of unknown liquid

1mL fractions Temperature (in Celsius)

1 40.6
2 51.8
3 62.1
Table 2. 1mL fractions/temperatures of the third batch of distillate

Discussion

Simple distillation is a distillation technique that requires a boiling point difference of at

least 25 degree Celsius between the components in a solution (1). Given this definition, it is
not possible to separate n-hexane and isohexane as the boiling point of n-hexane is 68.7
degree Celsius while the boiling point of hexane is 60.3 degree Celsius. If one were to look
for the difference, the result would only be 8.4 which is less than 25 degree Celsius.

After simple distillation was conducted, the receiving flask contained the distillate of the
purified compound. On the other hand, the round bottom flask contained the boiling chips
that were used and some of the liquid that was to be distilled. Three fractions were obtained
with the first being the forerun and the third being the distillate that was supposed to be free
of impurities.

There were significant changes in temperature as the first and second batches of
distillate were being collected which implied that impurities were still present in the liquid
and/or another component of the solution was still present (2). Because of this, the first and
second batches were not used to determine the boiling point of the unknown liquid.

The atmospheric and vapour pressure determine a liquid’s boiling point. If both the
atmospheric and vapour pressure are equal, then the liquid is will boil at its normal/expected
boiling point. If the vapour pressure of the liquid is less than the atmospheric pressure, then
the liquid is expected to boil at temperatures below the expected boiling point. If the vapour
pressure of the liquid is greater than the atmospheric pressure, then the liquid will boil at
temperatures above the expected boiling point (3). When this is the case, superheating will
occur and the liquid will burst out of the distillation flask which leads to sample loss (4).

The use of boiling chips helps prevent superheating and leads to better recovery of the
experiment. Despite this, 100 percent recovery is rarely possible if simple distillation is to be
performed because an azeotrope, a mixture which has vapour and liquid phases with identical
compositions cannot be changed by simple distillation (5).

Around 3mL of distillate was left when 1-mL fractions were about to be collected. This
could be explained by the fact that the receiving flask was not covered in aluminium foil
while/after the distillate was being collected. Because of this, some of the distillate might
have evaporated. As a result, the boiling point of the liquid could not be accurately
determined because it is possible that the temperature of the liquid will continue to rise if a
fraction for 4-mL and/or 5-mL was collected. By the time the fraction for 3mL was collected,
the temperature was at 62.1 degree Celsius. The distillate appeared to be clear and it smell
was close to alcohol. Given these descriptions, it is possible that the unknown liquid is
methanol. The boiling point of methanol is at 64.5 degree Celsius and its color and smell are
similar to the unknown liquid.

Conclusion

Methanol was distilled to its pure form by converting it to a vapour phase through the
method of heating. This allowed the solution to condense and flow into the receiving flask
which contained the purified form of methanol. Verification was done by checking the
temperature range and the physical/chemical properties of methanol.

Sample Calculations

Volume produced from distillation: 2.5mL + 2.8mL + 16.0mL = 21.3mL

Percent Recovery: (21.3mL/37.0mL) * 100 = 57.567568%

References

[Author unknown]. MSDS for Methyl alcohol – ScienceLab. [Internet]. [Place unknown]:
[Publisher unkown]; 2005 [updated 2005 Oct 10, cited 2014 Dec 8]. Available from
www.sciencelab.com/msds.php?msdsId=9927227

Yanza ER. Survey of Organic Chemistry Laboratory Manual. Quezon City: Department of
Chemistry, Ateneo de Manila University, 2014.

[Author unknown]. Boiling Point. [Internet]. [Place unknown]: [Publisher unknown]; [date
unknown; cited 2014 Dec 8]. Available from
https://www.chem.purdue.edu/gchelp/liquids/boil.html

Zumdahl S, DeCoste DJ. Chemical Principles. 7th edition. Belmont, California: Cengage
Learning; 2012.

Luyben WL, Chien IL. Design and Control of Distillation Systems for Separating
Azeotropes. Hoboken, New Jersey: John Wiley & Sons, Inc., 2010.