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Name: Arlene Jane Chang

Section: A

Locker number: 7A
Date Submitted: July 12, 2010

Experiment #2: Simple Distillation of an Unknown


Abstract: This experiment used simple
distillation process to obtain the unknown
through its boiling point. Distillation is the
separation
of
components
through
difference in volatility.
Based on the
results
yielded,
the
unknown
was
determined to be water since the
temperature shown on the thermometer
was around 98 C-100C and the unknown
had no odour- both of which are consistent
with the properties of water.

Introduction:
Distillation is one of the oldest known separation techniques known to man. In
distillation, it separates liquids through the use of vaporization and condensation. There
are many types of distillation but for this experiment, the focus was simple distillation.
Simple distillation is used to separate components with large differences in volatility
(Silberberg, 2007, p. 74).

Generally, simple distillation is used if there is a large

difference of the boiling point in the mixture and usually the liquids have a boiling point
below 150 C (Zubrick, 1993, p. 195).

Methodology:
The first step in the experiment was setting up the distillation apparatus. (See
appendix for picture) then 15 mL of the unknown was obtained from the lab technician.
Next, the unknown was obtained and placed in the round bottom flask together with
some boiling chips and then was clamped to start distilling. During the distillation

process, the receiving flask was then replaced after the appearance of forerun. After a
small amount of liquid unknown remained in the round bottom flask and the receiving
flask had now collected the desired batch of distillate, the temperature when it was
obtained was measured and the % recovery was computed for.

For the boiling point determination, the round bottom flask was first triple
washed by acetone, and then the distillate obtained in the first part was distilled again.
Throughout the distillation process, 1 mL fractions were collected using 10 mL
graduated cylinder while at the same time the temperature was being recorded. After
obtaining the boiling point, it was then compared to the common solvents in the lab.

Results and Discussion:


Distillation is commonly used in purifying substances. During distillation, this
is what occurs: First, the unknown in the round bottom flask will be brought to a boil,
(note: in order for a liquid to boil, the vapour pressure it exerts must be greater than the
atmospheric pressure which is 1 bar) next after the unknown is already boiling, the
gas or the vapour escapes and goes to the condenser, then from the condenser,
water will be used to rapidly cool the gas back to liquid form, and that liquid would be
the one that would go to the receiving flask (Bettleheim and Landesberg,1998,p.49).

The main objective of this experiment was to determine the given unknown
using distillation. When 15 mL sample was first given, the solution had a tinge of yellow
and there was no scent. Through the first distillation run, the receiving flasks solution
was clear while in the distilling flask; the little liquid left had a much stronger yellow

color. One interesting thing here to note was that both liquids had no scent. Since this
experiment was simple distillation, the temperature was monitored throughout the
experiment.

I.

Table of temperature recorded:

First Distillation:
Temperature (during forerun)

99 C

Temperature (after forerun)


Second Distillation (B.P
determination)
Average Temperature

98 C - 100 C

98 C

As stated in the table above, it can be observed that the temperature given
at the second distillation was 98 C to 100 C. Water is the closest compound to this
temperature range. (Water boils at 100 C) One major indicator also that gave the idea
that water was the unknown was the lack of scent. If it was propanol or ethanol, it would
have a strong distinguishing smell.

The percent recovery meanwhile was only 57.0%. This low figure can be
attributed to the experimenters attempt to minimize the chance of explosion in case
organic solids are present. Since if too little was left at the distilling flask, it might
contain substances, such as organic solids, which are explosive at high temperatures
(Guidote, 2005, p.66),
The difficulty encountered was only during the set up and the anticipation of
the forerun. The set-up was particularly hard because the glassware had to be secured

using rubber bands to avoid it separating from each other; also the tubings were also
problematic because it kept folding. (If it was left to fold, the tubing might erupt from
pressure) The forerun meanwhile was taking too long to form, then suddenly after it had
appeared, it was hard to switch flask to collect the distillate wanted. But overall, the
experiment ran smoothly.

In the experiment, there were few key things that were noted. First was filling
up the round bottom flask with only or 2/3 of the solution. Putting too little of the
unknown in the flask might cause significant product loss while putting too much could
cause the unknown to propel to the condenser and contaminate the distillate. Second
was the result. The boiling point obtained was lower than the given or natural. This
could attribute to the impurities present because impurities usually lower the boiling
point of the substance. Third was the use of water condenser instead of air condenser.
Water condenser was used since the one being distilled doesnt have a really high
temperature; air condenser is only used in boiling high temperature to avoid cracking
the glassware. Lastly were the intermolecular forces that broke during boiling. Since
boiling doesnt really change the chemical properties of a substance (only its physical
characteristics) the covalent bonds werent really broken, it was only the hydrogen
bonds which are the weaker associations with water molecules.

Conclusion:
The simple distillation process was one of the easiest methods the
experimenter had encountered. It was easy to handle and was very straightforward.

During the first distillation, the yellow coloured substance had completely separated with
the unknown giving a clear solution, while during the second distillation; the unknown
then again gave a clear solution. Throughout this distillation process, the temperature
never dropped from 98 C and it never went above 100 C. This together with the
absence of color and smell had led to the conclusion that the unknown was really water.

Reference:
Silberberg, M.S. . (2007). Chemistry: the molecular nature of
matter and change. Philippines: McGraw-Hill.
Zubrick, J.W. . (1993). The Organic chem lab survival manual: a
student's guide to techniques [third edition]. Retrieved from
http://www.ebookee.net/The-Organic-Chem-Lab-SurvivalManual-A-Student-s-Guide-to-Techniques_217816.html
Guidote, A., Del Rosario, D.R., & Abuzo, A.L. (2005). Experiencing organic chemistry: A
laboratory manual. Loyola Heights, QC: Ateneo de Manila University
Bettleheim, , & Landesberg, . (1998). Laboratory experiments for general, organic &
biochemistry. Saunder College Pub..
Intermolecular
forces.
(n.d.).
Retrieved
http://www.answers.com/topic/intermolecular-force

Appendix i:

from