Nina Althea G.

Diaz 15B
2 – Distillation: Identification of an Unknown Liquid October 1, 2018

Data and Results

Table 1. Properties of the Unknown Liquid
Properties of the Unknown Liquid Trial 1 Trial 2
Appearance Purple, Transparent Purple, Transparent
Smell Smelled like rubbing Smelled like rubbing
alcohol alcohol
Volume 15 ml 14 ml
Temperature when forerun was collected 68ºC 69ºC

Temperature Range 68-71ºC 69-73ºC

Total Amount of Distillate <15 ml <14 ml

Table 2. Temperature for Each Fraction

Fraction Number Temperature
1st 91ºC
2nd 93 ºC
3rd 103 ºC
4th 105 ºC
5th 110 ºC
6th 115 ºC
7th 120 ºC
8th 125 ºC
9th 130 ºC

Discussion
This experiment involved the distillation of an unknown liquid in order to know its
identity through determining the boiling point. As seen in table 1, two trials were carried out
for the first part of the activity. Another trial was made because for the first trial, the forerun
was forgotten to be separated from the distillate. This means that the impurities of the sample
remained, which is why the first trial was simply discarded afterwards. However, this mistake
was then corrected for the second trial. In addition, the volume of the liquid for the second trial
was less than the needed 15 ml because there was not enough sample left. To correct these
mistakes and increase the yield, the experimenter must not neglect to change the flask after
collecting the forerun. Also, the liquid must not be distilled to dryness so that the yield may be
increased after another distillation is performed.

In the first part of the experiment, 15 ml of the unknown sample was distilled. The
forerun, or the first 20 drops released into the receiving flask, was collected separately. This is
because the forerun contains impurities and if not separated, the liquid could boil at
temperatures above and below its expected boiling point due to the presence of these impurities
[1] (AtQ 1). After separating the forerun, another batch of distillate was collected. This second
batch or fraction may not yet be used to determine the boiling point because it might still
contain impurities, which could cause the deviation in the boiling point of the sample (AtQ 2).

For the second part of the experiment, the boiling point was determined through
collecting fractions of the liquid and noting their respective temperatures. Based on table 2, the
highest temperature was 130ºC. This means that the unknown supposedly has a boiling point
of 130ºC. However, based on the physical properties of the unknown, such as its odor, its
identity is most likely to be an alcohol (ethanol or methanol). The boiling points of these
alcohols are 78.5ºC and 64.6ºC respectively [2]. An error must have occurred in the readings
of the temperature, resulting to values that were much higher. This may be caused by focusing
more on distilling the 1 ml fractions and neglecting the changes in the temperature readings. In
order to correct this mistake, one must be conscious of both the fractions being collected, as
well as their individual temperatures.

After the distillation process, it would be expected that the receiving flask contains the
distillate, while the round bottom flask contains the distilled liquid (AtQ 4). The distillate
placed in the vial had a clear and colorless appearance. With regards to percent recovery, it is
impossible to end up with a 100% recovery for this experiment because the liquid will undergo
distillation, wherein the yield will surely be lessened (AtQ 3). In addition, the identity of the
unknown may also be determined after performing distillation. The unknown liquid may be
described to be clear and transparent with a purple dye added to it. It has a low viscosity, being
able to freely flow and it also has a similar smell with rubbing alcohol. Based on these physical
properties, the identity of the unknown may either be an ethanol or methanol alcohol (At 5).

In conclusion, the activity was able to meet the objectives through performing
distillation and determining the identity of the unknown liquid. Simple distillation was used
for this experiment because the components of the unknown differed in at least 25 ºC. However,
if given two liquids with similar boiling points, another type of distillation must be used. For
example, separating a mixture of n-hexane (bp: 68.7 °C) and isohexane (2-methylpentane) (bp:
60.3 °C) must be done using fractional distillation. Fractional distillation may be performed
when the substances being separated differ in less than 25 ºC in their boiling points [3] (AtQ
6). Through using the correct type of distillation method, one may be successful in separating
the components of a liquid and be able to determine the boiling point.

Accidents and Near Misses

In performing the experiment, some near miss incidents that occurred were forgetting
to collect the forerun separately from the distillate, improperly reading the temperature
indicated on the thermometer, and not securing the setup properly. It must always be
remembered that the purpose of distillation is to purify a sample from the present impurities.
This is why collecting the forerun separately must not be forgotten in order to ensure the
success of the distillation process. In addition, the thermometer must be properly place in the
thermometer jacket so that it will give out the proper temperature of the sample. Also, in
preparing the setup, it must be ensured that the all the instruments are secured using rubber
bands so that no breakages may happen.
References
[1] Yanza E. Survey of Organic Chemistry Laboratory Manual. Ateneo de Manila University:
Department of Chemistry; 2014.

[2] Myers B.J. Common Organic Solvents: Table of Properties [Internet]. American
Chemical Society; [updated 2016 Aug 9; cited 2018 Sept 30]. Available from:
https://www.organicdivision.org/orig/organic_solvents.html

[3] Fractional Distillation [Internet]. [cited 2018 Sept 30]. Available from:
http://www.pitt.edu/~ceder/lab7/fractionaldistillation.html