QUANTITATIVE ANALYSIS OF ACETYLSALICYLIC ACID

TABLETS BY BACK-TITRATION

IN

ASPIRIN

S.A.P. SAAVEDRA1, J. C. VILLASIS2, J.T. LIM2 AND M.C.Z. PORTEZA3

1NATIONAL INSTITUTE OF PHYSICS, COLLEGE OF SCIENCE
2DEPARTMENT OF FOOD SCIENCE AND NUTRITION, COLLEGE OF HOME ECONOMICS
3
DEPARTMENT OF MINING, METALLURGICAL AND MATERIALS ENGINEERING, COLLEGE OF ENGINEERING
UNIVERSITY OF THE PHILIPPINES, DILIMAN, QUEZON CITY, PHILIPPINES
DATE PERFORMED: JUNE 22, 2016
INSTRUCTORS NAME: GARRERO, M.J.

1. Discuss the use of a more dilute NaOH

solution for the standardization of
NaOH.
NaOH solution is very much concentrated
compared to the KHP standard. If the 1.0 M
NaOH solution is used for standardization,
very little volume of the solution will be used
in the titration, making the data imprecise.
Diluting NaOH will increase the volume of
NaOH used for titration, and thus increases
precision 1.
2. Explain the rationale behind the
dilution and aliquoting of the aspirin
sample.

Dilution and aliquoting of the aspirin

sample is done so that lesser volume of excess
NaOH is needed for neutralization and
consequently, lesser volume of HCl for backtitration. The aliquot samples are used for
replicates and will serve as representative for
the aspirin sample 2.
3. Discuss the principles behind the use
of back titration in the analysis of
aspirin tablets.

Aspirin is a weak acid that undergoes

hydrolysis in a two-step reaction: a fast
reaction then a slow one 3 . The slow reaction
makes it unfavorable for direct titration, thus,
back-titration method is used.

Known amount of excess NaOH is added

to the aspirin sample to overcome the slow
reaction and then heated to speed up
hydrolysis. Unreacted, excess NaOH is then
determined through back-titration using HCl
standard. Quantity of NaOH that actually
reacted with aspirin is now determined as
well as amount of aspirin sample, through
stoichiometric and volumetric calculations.
4. What is the importance of simmering
the tablet in the NaOH solution for 20
minutes.
The aspirin, degraded into its component
acids (acetic acid and salicylic acid), is reacted
to the excess NaOH solution. Simmering is
done to speed up hydrolysis of the acids
formed. It also makes sure that all acids have
been neutralized to completion.

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5. Discuss the possible sources of errors

and their effect on calculated
parameters
The possible sources of error throughout
the experiment and their effect on calculated
parameters are discussed in Table 1 below.

TABLE 1. Possible Sources of Errors and

its Effect on Calculated Parameters
Source of
Parameter and Error
Error
Errors
in Having lower molarity
weighing,
during standardization will
standardization lead to higher %ASA.
Errors in weighing aspirin
sample resulting in lower
mass will also result in
higher %ASA.
Incomplete
Fewer acids will react with
hydrolysis of NaOH, having more excess
aspirin sample NaOH during back-titration.
%ASA calculated will be
less than the actual value of
ASA present in aspirin
sample.
NonAliquot of the diluted
homogeneity of aspirin sample must be
aliquot sample homogenous in order to
obtain accurate data 2 . Nonhomogeneity
due
to
impurities will cause higher
%ASA obtained than actual
value.
Over-titration
Volume of HCl titrant
added will be greater than
actual volume needed. This
will consequently lead to
calculations of higher molar
concentration for excess
NaOH, leading to lower
%ASA than actual value.

REFERENCES
[1] Abrash, S. A. Chem 141 Titration Lab
Lecture Notes. Dr. Samuel A. Abrash.
https://facultystaff.richmond.edu/~sabra
sh/141Lab/Chem_141_Titration_Lab_Lect
ure_Notes_F10.pdf (accessed June 26,
2016).

[2] Harris, D. C. Sample Preparation. In

Quantitative Chemical Analysis, 7th ed.; W.
H. Freeman and Company: New York,
2007; pp 8, 645.

[3] Christian, G. D.; Dasgupta, P. K.; Schug, K. A.

Experiment 9 Determination of Aspirin
Using Back Titration. In Analytical
Chemistry, 7th ed.; John Wiley : New
Jersey, 2014; pp E16-E18.

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