ASPIRIN LAB PART II- PURIFICATION AND

CHARACTERIZATION
DIGITAL LAB REPORT PREPARED BY MANASA TARIGOPPULA

DATE: 18TH OCTOBER 2018

LAB ROOM: MILLIS 210

PROCEDURE:

I. Weighing and washing crude aspirin-

~0.5 g of crude aspirin was transferred into a new vial, which was placed in the

desicooler. The mass of the remaining crude aspirin sample was taken using a piece

of weigh paper. The remaining crude product was transferred to a 150 ml beaker. 50

ml DI water was added to the crude aspirin and mixed well with a glass stir rod.

Vacuum filtration was performed to remove the aqueous layer and collect the solid.

The crystals were allowed to dry for 5 minutes using the vacuum aspirator. A 50 ml

Erlenmeyer flask was obtained, in which the solid was transferred.

II. Recrystallization-

A hot plate was obtained and ~20 ml of 95% ethanol was heated in a 100 ml beaker.

The beaker was clamped to the ring stand, and covered with a watch glass. 2 pipettes

of warm 95% ethanol was added to the Erlenmeyer flask containing the solid, and

swirled. The flask was placed on to the heater. Ethanol was added until the solid

dissolved. The flask was then covered with a watch glass and allowed to cool slowly

to room temperature. By scratching the inside of the flask with a glass rod, crystals
 were formed. It was then placed in an ice bath for 10 minutes. Then, a vacuum

filtration was performed on the mixture. The crystals were left to dry for 5 minutes

using the vacuum aspirator.

III. Drying the aspirin-

The solid was then transferred to a watch glass and placed in an oven for 15 minutes.

Meanwhile, the mass of a clean vial was taken. The purified aspirin was transferred to

the vial, and the mass was taken to calculate the mass of aspirin by difference.

IV. Melting point range-

A melting point tube was obtained and loaded with 1-2 mm of the crude aspirin

sample. The Mel-Temp apparatus was used ay ~40 V to determine the melting point

of the crude sample. The temperature ranges where the crystals just started to melt

and the crystals completely melted were recorded. The same process was done for the

pure aspirin sample.

V. Titration-

About 0.1400 g of crude aspirin was weighed out onto a piece of weigh paper and

recorded. It was transferred into a 150 ml beaker. The aspirin sample was dissolved

with 10 ml ethanol and 40 ml DI water. About 100 ml of 0.1127 M NaOH was

obtained. The burette was primed and filled. 4 drops of phenolphthalein were added

to the crude aspirin sample mixture. The solution was titrated to the endpoint (faint

pink). The final burette reading was recorded. The same process was repeated for the

sample of pure aspirin.

OBSERVATIONS:
The crude aspirin solution took some time to dissolve in the 95% ethanol.

When scratched with a glass rod, crystallization began to take place as a white

precipitate began to form.

The melting point ranges of the crude aspirin sample are much higher than those of

the pure aspirin sample.

In the titration, the sample turned from colorless to faint pink (the endpoint).

DATA TABLES:

The data obtained during Recrystallization is as follows:

Mass of crude aspirin (before 0.5062

recrystallization) (g)
Mass of empty vial (g) 21.0944
Mass of vial + pure aspirin (g) 21.4462
Mass of pure aspirin (g) 0.3518

The data obtained during the melting point range reading are as follows:

Crude Pure
Start of melting (°C) 98.6 77.1
End of melting (°C) 122.1 92.2

The data obtained during the titration of the aspirin samples with NaOH are as

follows:

Crude Pure
Mass of aspirin (g) 0.1514 0.1495
Volume of ethanol (ml) 10.00 10.00
Volume of water (ml) 40.00 40.00
Initial burette volume 0.00 0.00
(ml)
Final burette volume (ml) 7.40 5.50
 Total volume of NaOH 7.40 5.50
used (ml)

CALCULATIONS:

% recovery:

% Recovery = (mass of aspirin recovered after purification (g) / mass of aspirin

before purification (g)) x 100

% recovery = (0.3518 g / 0.5062 g) x 100

= 69.4982 %

Molar mass:

Molar mass = mass sample / (M NaOH x V NaOH)

Molar mass of crude aspirin is calculated as follows:

Molar mass = 0.1514 g / (0.1127 M NaOH x 7.40 ml)

= 181.5391 g/mol

RESULTS:

By conducting the experiment for recrystallization of aspirin and determining the

melting points of crude and pure aspirin, the following results can be deduced:

For % recovery,

% recovery from recrystallization 69.4982

 For molar masses,

Crude aspirin Pure aspirin

Calculated molar mass 181.5391 241.1874
(g/mol)

CONCLUSIONS:

1. a. In both the characterization methods (melting point and titration), the crude aspirin

sample was more pure. From the data obtained, the melting point range of the pure

sample was 77.1-92.2 °C, while that of the crude sample was 98.6-122.1 °C. The higher

the melting point range, the lesser the impurities. It can thus be said that the crude aspirin

sample was more pure. In the titration, the pure aspirin sample used 5.50 ml NaOH, while

the crude sample used 7.40 ml NaOH. Since the pure aspirin sample used less NaOH to

reach the endpoint, it can be said that it is more pure than the pure aspirin sample.

b. Human errors from performing the two methods could result in inconsistencies. For

example, in the melting point, the reading could be taken wrong, while in the titration, the

endpoint could be altered, resulting in incorrect final volumes. If a student had consistent

results, then he/she must have made one or more of these kind of errors, leading to the

wrong results.

2. Melting point is used to test the purity and identity of a solid compound. The higher the

melting point, the purer the sample is. However, it cannot be accountable for whether the

substances contained aspirin or not, although it can provide insight into how pure a sample is. By

conducting titration, the molar mass of a compound can be calculated. A crude sample would

have a lower molar mass, while a pure sample would have higher molar mass.
3. In Experiment 3, sublimation and filtration were used to separate the mixture into its

individual components. The physical properties of the individual components were unique to

themselves, making it easier to separate, and hence easier processes to separate them.

Recrystallization, however, is a much more complex process. It is primarily used to separate

impurities from an impure sample, where the impurities are very much similar in their physical

properties to the actual pure component. Recrystallization makes this difficult separation much

more efficient. Hence, it is chosen over other techniques used earlier.