Experiment no.

2
Alkalimetry
Assay of Aspirin (Acetylsalicylic acid)Tablets

I. Principle Involved
The assay of aspirin tablets involves the use or residual titration methods for alkalimetric
analysis. In this particular experiment, phenolphthalein TS serves as the indicator. The end point
is indicated by a change in color from colorless to red at a pH range of 8.3-10.0.

II. Procedure
Weigh and finely powder not less than 10 acetylsalicylic acid tablets. Weigh accurately a
portion of the powder , equivalent to about 500mg of acetylsalicylic acid, transfer it
completelty to an Erlenmeyer flask with the aid of 20mL of neutralized alcohol, prev
cooled to 15 to 10 degreew\s, add phenolphthalein TS, and titrate the solution
immediately with 0/1N NaOH. Add to the titrated solution a volume of 0.1N NaOH equal
to the one used in the titration plus 15 mL more and heat the mixture in abath of
boiling water for 15 mins w/ frequent agitation. Remove the flask from the water bath.
Cool it quikly to room temp and titrate w/ 0.1N sulfuric acid. [erform a blank
determination. Each mL of 0.1 N sodium hydroxide consumed in the second titration is
rquiv. To 18.2 mg of aspirin. ]
(USP 16, p. 21))

III. Official Requirement

Acetylsalicylic acid tablets contain not less than 95% and not more than 105% of the labelled
amount of C9H8O. (USP 16, p. 20 )
IV. Clean-Up procedures
Acetic Acid is neutralized with 5% NaOH Or soiduium carbonate and pured into the drain. P.
V. Reasons for Important Steps

1. Alcohol is added as it is the recommended solvent for the indicator,

phenolphthalein. It is important that the added alcohol is neutralized so it will not
impart acidity to the solution which might consume an additional amount of base.
This would result in a greater amount of base that must be delivered, resulting to
a computed normality lower than normal. (Jenkins, p.69)
2. The temperature must be kept to 15-10 as this the temperature which
phenolphthalein gives a stable value. Many indicators give different values at
different temperatures. (Jenkins, p.103) Keeping the temperature at 15 20o
also suppresses the further hydrolysis of aspirin. (Jenkins, p111)
CHEMICAL EQUATION

3. The sample is titrated with NaOH to neutralize any free acid formed by hydrolysis
of the acetylsalicylic acid as represented by the first equation and to neutralize
the carboxyl group of the acetylsalicylic acid.(Jenkins)
4. After the acetylsalicylic acid and its hydrolysis products, acetic acid and salicylic
acid, have been neutralized in the first titration with 0.1N NaOH, carried at room
temperature or slightly below, the only further reaction of the sample with the
 78\\standard base added in excess to the titrated mixture involves saponification
of the sodium salicylate.(Jenkins)
5. Heating the mixture in a bath of boiling water with frequent agitation promotes the
hydrolysis of the sodium salicylate
6. Cooling to room temperature before titrating with H2SO4 ensures that the color
change of the phenolphthalein will be correct because its pKa is temperature
dependent.
7. A blank determination is done to account for the moisture and CO2 that might be
present in the system and can affect the assay.
8. The liquid to be titrated should be brought to room temperature before titration as
many indicators give different values at different temperatures, (Knevel,103)
VI. Chemical Equations