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Name: Mac Ivan Dominic C.

Fang
Section: Ch 26 A

Date Performed: 16 August 2016


Date Submitted: 23 August 2016

Experiment 1: Purification of Acetanilide


Data and Results
Table 1. Percent Recovery of Acetanilide
Mass with
Mass of
Actual
Acetanilide
Acetanilide
Percent
(g)
(g)
Recovery
(%)
TARED
TARED
1.97
53.8

Mass of
Watch
Glass (g)
Crude
Acetanilide
Purified
Acetanilide
Trial
1
2
3
Mean

27.20

28.26

Theoretical
Percent
Recovery (%)
78.5

1.06

Table 2. Melting Point Determination


Starting Temperature ()
Final Temperature ()
114.3
119.1
114.3
118.8
114.3
118.3
114.3
118.7

Discussion
Apart from purifying the crude acetanilide through crystallization, another objective
of this experiment was to determine the melting point of the purified acetanilide and to
compare it with the standard melting point of the said compound. Results show that the
standard melting point of acetanilide falls within the melting point ranges shown in Table 2.
This means that the objective of purifying the compound to obtain a melting point close to the
standard melting point was met.
But before getting to the heart of the discussion, a fine line must be drawn first
between crystallization and precipitation, which are two terms often used interchangeably
when talking about separation or purification techniques in the laboratory. In crystallization,
the crystals are a result of the change in the solubility of the solute in the solution.
Compared to precipitates, the structure of crystals is more ordered and defined. As a
consequence to the defined structure of crystals, the time it takes for the completion of
the crystallization process is longer than precipitation. In terms of selectivity,
crystallization is more selective because the impurities get excluded from the crystalline
structure. If the solution were to be slowly cooled down, crystals, excluding the
impurities from before, would be harvested (Jarvenin, 2016).
Table 1 shows the actual percentage recovery of acetanilide equal to 53.8% and
the maximum theoretical percentage recovery equal to 78.5%, which was calculated
using the proportions given in the laboratory manual. (Note: To see how the theoretical yield
was calculated, refer to the sample calculations in the appendix.) There is a significant
difference between the two and this might have been caused by too much addition of
charcoal during the decolorization process. Because of the large surface area of the
molecules of carbon, it has the ability to adsorb the colored impurities of the crude
acetanilide. However, the amount of carbon used must have been too much. If this were
the case, some of the desired compound had been adsorbed along with the impurities,
resulting in a smaller yield. This slight deviation from the standard melting point could also
be caused by the use of a hot solvent when washing crystals during suction filtration. If the

crystals were washed with the hot solvent, they would dissolve, defeating the purpose of
the experiment, which was to recrystallize acetanilide to purify it.
Table 2, on the other hand, shows the various melting point ranges of the acetanilide
obtained in this experiment. The temperature at which the crystals started melting for each
trial was all the same ( 114.3 ). The mean starting temperature is actually the standard
melting point of acetanilide but the temperature at which all the crystals melted ranged from
118.3 to 119.1 with the average equal to 118.7 . This slight deviation
could be attributed to the purity of the acetanilide obtained in the experiment (Cap,
2007). Colligative properties tell us that impurities lower the melting point of a
substance. However, the melting point of the crude acetanilide had not been recorded before
proceeding to the crystallization process so that could not be shown here.
The discrepancies in this experiment can be attributed to the various errors that (might
have) occurred in this experiment. First, if the solution containing the crude acetanilide,
water, and bits of charcoal was not boiled long enough, there could still be impurities in it,
influencing the purity of the acetanilide and its melting point. Apart from this, the filter paper
or funnel used might have been cold enough for premature crystallization to take place. This
is the reason why the funnel had to be subjected to heat first before proceeding to the
filtration process. For the determination of the melting point of acetanilide, there might have
been reading errors considering the age of the machine and its tendency to malfunction from
time to time.
Despite the melting point of the acetanilide in this experiment being close to the
standard melting point, this experiment could still have been better by minimizing the errors
committed in this experiment. Nevertheless, the aim to be familiarized with this purification
technique along with other concepts mentioned above was met.
Conclusion
Crystallization is performed to purify a given impure substance and to determine its
melting point. However, precipitation could happen instead of crystallization if the solution
were cooled quickly. Precipitation is different from crystallization because the latter is more
selective than the former. Crystallization makes sure that there are no impurities in the
crystalline structure and this is why it takes more time to crystallize than to precipitate
something out. This experiment also laid bare the effect of impurities on the melting point of
a substance, which is the lowering of the melting point of a substance with impurities in it.
References
Cap, A. (2007). Recrystallization and Melting Point Determination Lab. AdamCap. Retrieved
21 August 2016, from http://adamcap.com/schoolwork/recrystallization-and-meltingpoint-determination-lab/
Jarvenin, G. (2016). Precipitation and Crystallization Processes. Crespt.org. Retrieved 21
August 2016, from http://www.cresp.org/NuclearChemCourse/ monographs/09_
Jarvinen_FuelCycleSep%20CrystPrec12-08fin_3_2_09.pdf
Yahoo Answers. (2016). Retrieved 21 August 2016, from https://answers.yahoo.com/
question/index?qid=20081202210247AA4XEAc
Appendix
1. Mass of Acetanilide
mass of watch glass : 27.20 g
mass of a cetanilidewatch glass :28.26 g
mass of acetanilide=28.26 g27.20 g
1.06 g

2. Percent Recovery
mass of crude acetanilide :1.97 g
mass of purified acetanilide :1.06 g
mass of purified acetanilide
recovery =
100
mass of crudeacetanilide
1.06 g

100
1.97 g
53.8
3. Maximum Theoretical Yield
sol ubility of acetanilide at 0 :0.53

g
100 mL

V water :80 mL
0.53 g
x
=
100 mL 80 mL
x=0.424 g acetanilide did not crystallize
Thus , the amount of acetanilide that crystallized out is:
1.97 g0.424 g
1.55 g
max theoretical yield=

1.55 g
100
1.97 g

78.5
4. Mean Starting/ Final Temperature
final temperature , trial one :119.1
final temperature , trial two :118.8
final temperature , trial three :118.3
119.1 +118.8 +118.3
mean=
3
118.7