Activity No.

Assay of Aspirin (ASA Tablets)

OBJECTIVES:

At the end of this activity, the student is able to:

1. discuss the assay procedure, chemical reactions taking place in the analysis
2. calculate the purity of aspirin in the sample.
3. interpret the results obtain from the analysis.

MATERIALS : Aspirin tablets, 325 mg

0.1 N Sodium hydroxide
Alcohol, neutralized
Phenolphthalein, T.S.

ASSAY PROCEDURES:

Weigh and finally powder not less than 10 tablets. Two groups may be assigned
to take samples from the same powdered 10 tablets.

1. Transfer an accurately weighed amount of the powdered tablets equivalent to

100 mg of aspirin in a 500 ml Erlenmeyer flask, add 15 ml of neutralized
alcohol and mix for about 5 minutes. Add phenolphthalein T.S. and titrate the
mixture with 0.1 N sodium hydroxide to a pink color.

2. Add to the above solution a volume of 0.1 N sodium hydroxide equal to the
volume used in the titration, then add 15 ml more. Heat the mixture in a water
bath using the air condenser fitted to the mouth of the flask through a cork for
15 minutes with frequent agitation. Remove the flask and cool to room
temperature, add 2 drops of phenolphthalein T.S. and titrate with 0.1 N sulfuric
acid to the disappearance with pink color. Perform a blank determination with
the same quantities of the same reagents (volume of 0.1 N sodium hydroxide
is the total volume used in the second titration plus 15 ml more) and in the
same manner.

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REACTIONS:

Molecules of ASA tablets is titrated with sodium hydroxide to neutralize any free
acid formed by the hydrolysis of the acetylsalicylic acid as represented by the equation:

C6H4OCOCH3COOH + HOH ------------------ C6H4OHCOOH + CH3COOH

And to neutralize the carboxyl group of the acetylsalicylic acid as:

C6H4OCOCH3COOH + NaOH ------------------ C6H4OCOCH3COONa + H2O

(sodium acetylsalicylate)

After the acetylsalicylate acid and its hydrolysis products, acetic acid and salicylic
acid have been neutralized in the first titration with 0.1 sodium hydroxide at room
temperature, the only further reaction of sample with the standard base added in excess
to the titrated mixture involves saponification of the sodium acetylsalicylate as:

C6H4OCOCH3COONa + NaOH ------------- C6H4OHCOONa + CH3COONa

DATA:

Weight of tablets = _____

Weight of aspirin powder = _____

Weight of powder = _____

Volume of blank titration = _____

Volume of sample titration = _____

Actual normality of the sulfuric acid = _____

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CALCULATIONS:

ASA/tab = (V blank – V sample) x N H2SO4 x meq wt ASA x weight/tab

Sample weight

Using titer value:

ASA/tab (mg/tab) = Vbl – Vsa x NF H2SO4 x titer x wt/tab

Sample weight

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NOTE: ASA contains not less than 99.5% and not more than 100.5% of C9H8O4 on the
dried basis. ASA tablets contain not less than 95% and not more than 105% of labeled
amount of C9H8O4.

Answer the following questions:

1. How is neutralized alcohol prepared?

 Alcohol, Neutralized —To a suitable quantity of alcohol add 2 or 3 drops of

phenolphthalein TS and just sufficient 0.02 N or 0.1 N sodium hydroxide to
produce a faint pink color. Prepare neutralized alcohol just prior to use.

2. What is the reason of adding neutralized alcohol in the assay of ASA?

 To convert the substances for reaction with the standard base and to speed
up the hydrolysis.

3. Give the purpose of heating ASA in water bath with the use of an air condenser.
 The ASA is heated in water with an air condenser so that to increase the rate of
hydrolysis of acetyl salicylic acid

4. What is the type of titration involved in the assay of ASA?

 Residual Alkalimetry Titration

5. The contents of 20 aspirin capsules were dissolved in 100 ml of alcohol. If a 10 ml

aliquot was found to contain 0.4880 g of aspirin, what is the percentage of labeled
amount (5 grains) of aspirin in the capsule?

Given:
 100 mL
 10 mL of aliquot
 0.4880 g of Aspirin
 5 gr = 0.0325 g
 1 gr = 0.065 g

Formula:

N = weight of sample
mL x mEq

% = mL x N x mEq x 100
Weight of sample

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N = weight of sample
mL x mEq

= 0.4880 g____
10 mL x 0.018016

= 0.4880 g____
18016

= 0.27087 N

% = mL x N x mEq x 100
Weight of sample

= 100 mL x 0.27087 N x 0.018016 x 100

0.325 g

= 1501.53658 %

= 1501.53658 % / 20

= 75.08%