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DETERMINATION OF ASPIRIN BY INDIRECT TITRATION

Legaspi, Maria Susana V., Marquez, Ma. Rica Paulene B., Marzan, Shemaiah Mae T., Nomil, Jan Wyne T.
Department of Biology, College of Science, University of the Philippines Baguio

Nov. 26, 2013


ABSTRACT

Back titration is determining the concentration of an analyte by reacting it with a known number of
moles of excess reagent. The excess reagent is then titrated with a second reagent. The concentration
of the analyte in the original solution is then related to the amount of reagent consumed. This
experiment aims to evaluate the purity of an aspirin, develop techniques for the proper dilution of a
solution to definite volume and how to carry out calculations involving back-titration. Preparation and
standardization of 0.1 N HCl solution will be prepared and to be diluted with the standard NaOH
solution used from Experiment 3 until a permanent faint pink color is achieved after performing three
trials. And an analysis of aspirin will be exercised, solution of hydrolyzed aspirin will be titrated using
standardized HCl solution using 2-3 drops of phenolphthalein indicator.

INTRODUCTION
Direct Titration is a treatment of a
soluble substance contained in a vessel with
an appropriate standard solution and the
endpoint is being determined visually by an
indicator. Indirect Titration, doesnt involve
measuring the substance itself but knowing
the quantity of a reagent to be added with a
specific reaction and a titration is done to
determine the unknown excess. Aspirin, an
acetyl derivative of salicylic acid, is a white,
crystalline, weakly acidic substance, with a
melting point of 136 C (277 F), and a boiling
point of 140 C (284 F), also known as
acetylsalicylic acid salicylate drug, often used
as an analgesic to relieve minor aches and
pains, as an antipyretic to reduce fever, and
as an anti-inflammatory medication. It is
derived from two acids, Acetic acid and
salicylic acid. It can be hydrolyzed and
neutralized with the two components
simultaneously.
[1]


RESULTS
Concentration of NaOH: 0.0927 N = 0.0927 M
Table 1 Volume of HCl
Trial 1 Trial 2 Trial 3
25 mL 25 mL 25 mL
*Table 1 shows the volume HCl that was
titrated for the standardization of HCl
Table 2 Volume of NaOH used in HCl
Volume
of NaOH
Trial 1
(in mL)
Trial 2
(in mL)
Trial 3
(in mL)
Initial 1.4 22.9 13.1
Final 22.9 46.2 33.9
Used 21.5 23.3 20.8
*Table 2 shows the volume of NaOH used to
titrate 25 mL HCl
Mass of Aspirin: 0.1074 g
Table 3 Aliquot of Aspirin
Trial 1 Trial 2 Trial 3
50 mL 50 mL 50 mL
*Table 3 shows the aliquot volume of the
ground aspirin to be titrated with the
standardized HCl
Table 4 Volume of HCl used in Aspirin
Volume
of HCl
Trial 1
(in mL)
Trial 2
(in mL)
Trial 3
(in mL)
Initial 13.1 15.5 17.2
Final 15.5 17.2 20.4
Used 2.4 1.7 3.2
*Table 4 shows the volume of HCl that was
used in the titration of the ground aspirin

DISCUSSION
The worlds most commonly used pain-
relieving drug, the Acetylsalicylic acid is
generically known as ASA or Aspirin. It is an
acetyl derivative of salicylic acid that is a
white, crystalline, weakly acidic substance,
with melting point 137C. It is useful in the
relief of headache and muscle and joint aches.
Aspirin is also effective in reducing fever,
inflammation, and swelling and thus has been
used for treatment of rheumatoid arthritis,
rheumatic fever, and mild infection.
HC9H7O4(s) (ASA) is an organic acid (carbon
chain) similar to that of acetic acid, HC2H3O2
(l) reacts with strong bases such as sodium
hydroxide in the same way. There are several
complicating factor that arise from the nature
of ASA tablets.
[2]

The experiment consists mainly of two parts:
(1) the preparation and standardization of 0.1
N HCl solution (2) and the determination of
ASA in aspirin.
In the preparation of the 0.1N HCl, 8.3mL 12
M HCl was mixed with water to generate a
100mL 0.1N HCl. The prepared chemical was
then standardized using the NaOH. (The
NaOH used was already standardized in the
previous experiment) Table 1 and 2 shows the
volume of HCl and NaOH used. The
standardized HCl was then used in the
analysis of the aspirin.
In the analysis of the aspirin, 0.1
grams of the aspirin sample was pounded and
a 20.00 ml of the standardized NaOH was
added to it. The mixture was boiled then for
10-15 minutes. Simmering was done to
hydrolyze the aspirin sample. Three trials
were made for the analysis of the aspirin. The
mixture was cooled, and was transferred into
a 250 ml volumetric flask. The flask was
washed several times with 10 ml portions of
distilled water and was filled to the mark.
Then, the hydrolysed aspirin was titrated with
the standardized HCl using phenolphthalein as
the indicator. Table 3 and 4 shows the volume
of aspirin aliquot and HCl used.
To calculate the number of moles of
NaOH the formula used was: molarity of
NaOH times average volume of NaOH used.
The molarity of NaOH is 0.0927 M and its
volume for every trial as shown in Table 2.
The computed moles per trial were 1.99 x 10
-3

mol, 2.16 x 10
-3
mol, and 1.93 x 10
-3
mol of
NaOH respectively.
The mole of excess NaOH was
computed by multiplying the molarity of HCl
by the volume of HCl used. The molarity of
HCl was given as 0.1 M and the volume for
every trial was given in Table 4. The calculated
results were 2.4 x 10
-4
mol, 1.7 x 10
-4
mol , and
3.2 x 10
-4
mol for first, second and third trial
respectively.
One of the main objectives of this
experiment was to determine the
concentration of the acetylsalicylic acid in the
aspirin tablet. The computed number of
moles of the acetyl salicylic acid in the aspirin
was 8.92 x 10
-4
mol.

CONCLUSION
The objectives of this experiment
were successfully met and back titration was
properly performed and introduced. It is
observed that the volume of NaOH used to
titrate HCl do not greatly vary, same as with
the volume of HCl used to titrate aspirin. The
number of moles of Aspirin computed was
8.92 x 10
-4
mol.
LITERATURE CITED
[1]http://www.pharmacopeia.cn/v29
240/usp29nf24s0_c541.html. Schrr, Karsten
(2009). Acetylsalicylic acid. Wiley. ISBN 978-3-
527-32109-4. Date Removed December 16,
2013
[2] RET Lab Lesson Plan.
http://www.njit.edu/precollege/docs/. Date
Retrieved December 16, 2013
Then then ASA in Analysis. http://survival-
training.info/Library/. Date Retrieved
December 16, 2013
Titration of Synthesized Aspirin: A
continuation of the aspirin synthesis lab.
http://www.whatcom.ctc.edu/. Date
Retrieved December 16, 2013
Skoog, D. A., West, D. M., Holler, F. J., &
Crouch, S. R. (2004). Titration Curves
for Weak Acids. In Fundamentals of
Analytical Chemistry 8th Edition (pp.
378-382). Canada: Thomson Learning
Inc.

ANSWERS TO QUESTIONS
1. What would be the effect of a more dilute
solution of NaOH on the titration?

pH values would be lower for the
dilute solution than the normal pH value of
the standard solution, and, therefore, changes
the amount of titrant needed to complete the
equivalence point in titration.

2. What volume of 1.0N NaOH is used in the
hydrolysis of four 250mg tablets of aspirin
(90%pure acetylsalicylic acid) if 10.00ml of
0.05N HCl is consumed in the back titration.

*Given:
N HCL = 0.05
V HCL = 10.00 ml
N NaOH = 1.0
V NaOH = ?
weigth of aspirin = 250mg(4) = 1g
*Formula:
% ASA =
( )(

)
()

[()( ) ()()](

)


[()( )
()()] (

)
[()( )
()()]()
()( ) ()
()( )

*10.49ml of NaOH was used to hyrolyzed 1g
aspirin; 90% pure ASA.

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