ABSTRACT

This experiment focuses in the purification of the given compounds, carbon tetrachloride and p-
dichlorobenzene, with the use of simple and steam distillation. Simple distillation is considered to be effective
if the samples under investigation have at least 50 degrees of boiling point difference. steam distillation, on
the other hand, is used in temperature sensitive compounds. This experiment aims to properly install
distillation set ups and to identify and recognize the significance of each parts of it. 86.76 and 84.28 percent
recovery was obtained from the simple distillation and steam distillation, respectively.
Introduction
Several distillation variations are used in organic laboratories and it varies with the properties of the mixture under
investigation. Distillation is a process used to separate liquids in a mixture based on their relative boiling points
(Trubiano, 2018). The process involves heating a mixture and collecting vapor that rise from it. Moreover, distillation is
a physical process rather than a chemical one since it does not involve the creation or modification of the compounds
within the mixture. It primarily concerns the vapor point and volatility of the compound which are all physical properties.
Simple distillation involves mixtures that have wide-ranging boiling point differences. According to Yoder (2019), it can
be effectively used to separate liquids which have at least 50 degrees difference in their boiling point. In this process,
as the liquid sample is being heated vapor will be collected as one component of the mixture reaches its boiling point.
There are times that organic compounds exert low vapor pressure even at high temperatures. Thus, it results in the
decomposition of the organic compound. Therefore, steam distillation is used. Steam distillation is a special type of
distillation that primary deals with temperature sensitive aromatic compounds. The use of water to provides additional
vapor pressure to help a nonvolatile compound to boil off and be distilled even at temperature lower than its boiling
point.
This experiment focuses in the purification of the given compounds, carbon tetrachloride and p-dichlorobenzene, with
the use of simple and steam distillation. Furthermore, it aims to give mastery of assembling a simple and steam
distillation set up and to identify the significance of each part of the set up.
MATERIALS AND METHODS
This activity was accomplished with the use of the following materials and reagents: quick fit, pipette, hot plate,
Erlenmeyer flask, ice, impure carbon tetrachloride, impure p-dichlorobenzene and distilled water.
In the first part of the experiment, a set up of simple distillation with the use of quick fit was assembled. A 15 mL impure
carbon tetrachloride sample was transferred into the pear-shaped flask using a pipette. The obtained sample was
heated on a heat regulated hot plate. The distillate was collected at different temperatures at the rate of 1 drop per
second. The distillation of the mixture was continued until a volume of 1-2mL was left in the pear-shaped flask.
In the steam distillation part of the experiment, a set-up was also assembled using a quick fit. A 2g-sample of impure
dichlorobenzene was dissolved in a pear-shaped flask with 5mL of water while heating. As the sample was fully
dissolved, the flask containing the sample and the Erlenmeyer flask that contains boiling water that serves as the steam
generator was connected to the set up. The steam distillation proceeded, and the distillate was collected. However,
there are times that the condenser became clogged and to clog it out the water supply is immediately turned off before
heating the condenser with a Bunsen burner. The collected distillate was cooled, filtered and then dried. The dried
sample was weighed to determine the percent recovery of the compound.

RESULTS AND ANAYSIS

Figure 1. Plot of Temperature vs Volume

45 41 41 41 41 41 41.5 42 42 42 42 42 42
39
40
35
30
Temperature Degree Celcius

30
25
20
15
10
5
0
0 2 4 6 8 10 12 14
Volume of Distillate (mL)

Figure 1 shows the relationship between the temperature of the sample and the volume of distillate being collected as
the sample reaches its boiling point. It is observed from the results that there is an increase in the volume of sample
as it approaches higher temperature. As the temperature raises, the vapor amount also increases and that results to
increase in the volume of sample being collected as the vapor evaporate and condense.
Table 1. Data obtained from Simple Distillation

Boiling Point of the Sample 42 oC

Total Volume Collected (mL) 13
Percent Recovery 86.67%

From the 15mL impure carbon tetrachloride sample, a 13mL pure compound was collected. This shows an 86.67%
recovery of the sample which is a significantly high recovery. However, yielding a high amount of recovery there are
still errors in this experiment that possibly came form the unseen leaks in the installation of the set up. To avoid leaks,
make sure that the quick fit parts are attached tightly to each other.
Table 2. Data obtained from Steam Distillation

Melting point of crude sample oC T1 = 75.7 T2 = 89.3

Melting point of purified sample oC T1 = 71.2 T2 = 76.6
Weight of crude sample 2.99g
Weight of purified sample 2.52g
Percentage Recovery 84.28%

Presented in Table 2 are the data gathered upon doing steam distillation. It is determined in the experiment that the
2.99g of impure sample yielded a 2.52g of pure p-dichlorobenzene. The product of distillation is considered pure since
the observed melting point has a low difference. Yet, this does not mean that there are no errors encountered in this
part of the experiment. Steam distillation requires more careful handling of the set up to avoid errors. To avoid such
errors, make sure that the quick fit set up was installed properly and free from leaks. Also make sure that the sample
was fully dissolved, and no adhering solution was left in the container since it adds to the loss of the product. Lastly,
the product from the receiving container in the distillation set up was all transferred into the filter paper before
undergoing vacuum filtration.

CONCLUSION
The purification of impure carbon tetrachloride and p-dichlorobenzene sample was successfully done through the
proper installment of the simple distillation and steam distillation set up. The proper installation of the distillation set
ups was achieved through correctly identifying the parts of the set up and recognizing its significance.
The success of this experiment depends on the proper installation of the distillation set ups. In conducting future
experiments, it is recommended to properly inspect the set up to ensure that it is free from leaks so that no loss is
added to the product.

REFERENCES
Trubiano, C. (2018, April 30). Steam Distillation vs. Simple Distillation. Retrieved from
https://sciencing.com/steam-distillation-vs-simple-distillation-8407975.html
Yoder, C. (2019). Distillation. Retrieved from
http://www.wiredchemist.com/chemistry/instructional/laboratory-tutorials/distillation