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QUANTITATIVE ANALYSIS OF ACETYLSALICYLIC ACID IN ASPIRIN

TABLETS BY BACK TITRATION


J.L. CORPUZ
DEPARTMENT OF CHEMICAL ENGINEERING, COLLEGE OF ENGINEERING
UNIVERSITY OF THE PHILIPPINES, DILIMAN, QUEZON CITY, PHILIPPINES
DATE PERFORMED: FEBRUARY 28, 2018
INSTRUCTOR’S NAME: E.C. GALLEPOSO

1. Discuss the use of a more dilture fast reaction and a slow reaction which
NaOH solution for the is its rate determining step. This slow
standardization of NaOH reaction is impractical for titration
cases. It is therefore strategic to use
 1M of NaOH is a high concentration to excessive NaOH to the aspirin solution
use in titration. Per drop or volume of to optimally hasten reaction time, then
titrant from burette, the graduations heated to further hasten the hydrolysis
of moles reacting are sudden and high reaction. The remaining unreacted
which causes a very quick end point NaOH excess is then titrated with HCl
but this experimental end point would back-titration. Because the NaOH
be farther away from the true value equivalence with ASA is 1:1, the
compared to 0.05M NaOH in which reacted NaOH was therefore
over-titration would bear less impact computed and was used to determine
on values upon over titration1 the amount of ASA in the aspirin
sample.
2. Explain the rationale behind the
dilution and aliquoting of the 4. What is the importance of
aspirin sample simmering the tablet in NaOH for 20
minutes.
 Since the titrant was diluted, the
titration would be much slower.  The ASA dissociated to its acetic acid
Therefore, it is necessary to dilute the and salicylic acid components. It was
analyte to achieve the end point faster reacted to the excess NaOH with
in proportion to the diluted titrant simmering done to hasten hydrolysis.
with less volume of excess NaOH This also hastened the neutralization
needed for neutralization and less of acids to completion.
volume of HCl for back-titration. The
aliquots serve as back-up analytes in 5. Discuss the possible sources of
case of over-titration, and as reference errors and their effect on the
samples2 calculated parameters

3. Discuss the principles behind the a. Weighing and


use of back titration in the analysis Standardization Error
of aspirin tablets High molarity of NaOH in
standardization will cause
 Acetylsalicylic acid is a weak acid higher number of excess NaOH
which hydrolyzes in two-step which in turn will also increase
elementary reactions which involves a the computed %ASA. This is
also the case for weighing
where a lower mass will cause References:
a smaller denominator in [1] Abrash, S. A. Chem 141 Titration Lab
percent calculation which Lecture Notes. Dr. Samuel A. Abrash.
increases %ASA, while a
https://facultystaff.richmond.edu/~sabrash/
higher mass will lower the
%ASA. 141Lab/Chem_141_Titration_Lab_Lecture_No
tes_F10.pdf (accessed March 07, 2018).
b. Incomplete hydrolysis of
aspirin sample [2] Harris, D. C. Sample Preparation. In
Incomplete hydrolysis would Quantitative Chemical Analysis, 7th ed.; W.
produce less acid which means H. Freeman and Company: New York,
more unreacted or excess
2007; pp 8, 645.
NaOH. These unreacted NaOH
will falsely signify greater
%ASA calculated. [3] Christian, G. D.; Dasgupta, P. K.; Schug, K. A.
Experiment 9 Determination of Aspirin Using
c. Non-homogenous aliquot Back Titration. In Analytical Chemistry, 7th ed.;
sample John Wiley : New Jersey, 2014; pp E16-E18.
If the main solution was not
mixed before taking an aliquot,
the resulting %ASA might
either become higher or lower.
It may go higher if the aliquot
taken has a more ASA mass
compared to the ideal. While
an aliquot that contained less
mass of ASA compared to the
ideal will show less %ASA in
the computations.

d. Over-titration
The volume of HCl titrant will
exceed the true amount from
over-titrating. Therefore, in
the computations, it will falsely
signify higher moles of NaOH
excess which will increase the
acquired %ASA.