Name: Sanglad, Chariezza Lei J.

Date Performed: June 23, 2017

Group No:5 Date Submitted: June 30, 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 Percent

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

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

Discussion:
As for the melting point data, the range of the crude sample was 120-124˚C and the range
of the purified sample was 122-124˚C. Comparing the results to the literature value of 135˚C, both
the purified and crude had a precise value BUT since the purified sample has a narrower range, it
is logically more comparable to the literature value .
In our experiment, pure aspirin was obtained after filtering out the impurities and excess
reagent through filter paper. 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. In our
experiment, the melting point range of the product was observed to be 129.5°C to 137.5°C. The
percentage yield of the final product was calculated to be 68.23%.

It can be concluded that by recrystallizing the crude aspirin, though it decreased the percentage
yield from 75.65% to 68.23%,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
crude product had a melting range of 117.5°C-123°C, and the final product one of 129.5°C-
137.5°C. The percentage error of the crude product was 10.93%, while that of the final product
was significantly lower at 1.11%.

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%