Name: Sanglad, Chariezza Lei J.

Date Performed: June 23, 2017

Group No:5 Date Submitted: July 4, 2017

Experiment no:2

PURITY OF ASPIRIN: MELTING POINT DETERMINATION

Objectives:
1. To be able to estimate the purity of aspirin through determining its melting point.
2. To be able to determine the melting point of aspirin.

Procedure:
Assemble apparatus shown in Figure 1
use oil-filled beaker as heating bath
crush some aspirin crystals on watch glass
form mound from powder
push open end of melting capillary into mound
allow powder to drop into bottom of tube
repeat process until plug reached ¾ to 1 cm long
attach filled capillary to thermometer with string
immerse to oil bath
bath rapidly with alcohol lamp to about 100°C
(melting point approached, crystals will begin to soften)
report melting point at which last crystals disappear
(transparent tube)
Melting Point Set-up:

Figure 1
Data and Results
Table1. Observation for the Melting Point of Aspirin.

Trial Sample Treat- Observation Theoretical Percent

(inside ment Temperature reading Average value Error
capillar every 20s interval Melting (melting
y tube) Point point)

1
Aspirin Oil bath 138.67°C 135°C 0.03%
137ᵒC 139ᵒC 140ᵒC
2
Aspirin Oil bath 139°C 135°C 0.03%
138ᵒC 139ᵒC 140ᵒC

Discussion:
Melting point analysis can also provide information about the purity of a sample. A
substance (solid) containing soluble impurities usually melts at a lower temperature than the pure
compound. It can also melt over a wide range of temperatures. This is called the “melting point
depression”. In general, the smaller the range of melting temperatures, the higher the purity of
the sample.

In our experiment, as for the melting point data, the range of the trial 1 sample was 137-
140˚C and the range of the trial 2 sample was 138-140˚C. Comparing the results to the literature
value of 135˚C, both the two trials had a precise value. The percentage yield of the final product
was calculated to be 85.01%. It can be concluded that by recrystallizing the aspirin, though it
decreased the percentage yield, a significantly purer aspirin was produced, as shown by the more
feasible and realistic melting range. Aspirin has a theoretical melting range of 134-136°C. The
percentage error for the first trial was 0.03% and for the second trial was also 0.03%.

Pure aspirin was obtained after filtering out the impurities and excess reagent through
filter paper since the melting point of first and second trials were closed to the theoretical melting
point of aspirin. A method to check a solid compound's purity after re-crystallization is to check
its melting point. Impurities will always lower the melting point of a sample.
Calculations:

Melting Range Percentage Error

As the melting point is a range, the average value of the range will be found before
calculating percentage error.

Average of actual melting range in trial 1 = 138.67°C

Expected melting point = 135°C
Theoretical Value−Actual value
Percentage error = x 100%
Theoretical Value

135−138.67
=/ /x 100%
135
=0.03%

Average of actual melting range in trial 2 = 139°C

Expected melting point = 135°C
Theoretical Value−Actual value
Percentage error = x 100%
Theoretical Value

135−139
=/ /x 100%
135
=0.03%