EXPERIMENT 4

DETERMINATION OF ASPIRIN BY INDIRECT TITRATION

Pagkanlungan, Aldrey Q., Reyes, Ruthlaine Joyce A., Romin, Maelyn Nicole T.

College of Science

University of the Philippines Baguio

Abstract

This experiment aims to familiarize various titration methods and gain a mastery of the concepts
involving volumetric analysis and calculations, as well as integrate the proper techniques
necessary in laboratory equipment utilization. In the preparation and standardization of HCl
solution, the previous NaOh was used. The calculations yielded a mean of 0.111 mole/L HCl
and normality was computed to be similar to molarity since there is only one acidic hydrogen
that reacted to the NaOH. In addition, the calculated relative standard deviation was only 2.9%,
which suggests that there is low variation in the results. In the analysis of aspirin tablet, it was
found out that the mean amount of acetylsalicylic acid or ASA was 0.0248 grams with an
absolute uncertainty of 土0.0001. Moreover, the ASA mean percentage was calculated to be
23.59% with a low relative standard deviation of 0.53%. This reveals that the results were close
to each other and with little to no error. Furthermore, the titration resulting to a light shade of
yellow indicates that all of the trials reached endpoint and was not over titrated.

Introduction reagent in excess (Sandell and West,

1969).
Titration is the process in which a
Aspirin or acetylsalicylic acid, a
quantity of a sample is determined by
salicylate which is commonly used as a pain
adding a measured sample an exactly
reliever, to reduce fever,anti-inflammatory
known substance that reacts in exact and
drug and can be used as a blood
definite proportion. This process is usually
thinner(Awtry and Loscalzo, 200).
carried out by gradually adding a standard
In this experiment, indirect titration
solution until an equivalent point is reach.
method was employed to determine the
Indirect titration or back titration, in
purity of aspirin from the grounded
comparison, is a titration method where the
analgesic tablet. Since a single aspirin
concentration of the analyte is reacted to an
reacts with two hydrogen ions, it undergoes
excess amount of known reagent. The
a relative slow hydrolysis. A known excess
solution is then subjected to direct titration
base such as NaOH is added to the solution
to determine the amount of the excess
to hasten the hydrolysis and the solution is
titrated with HCl.
This experiment aims to determine
the purity of the grounded analgesic tablet
and recognize the techniques for the proper
usage of laboratory equipment involving
indirect titration and dilution of a solution to
a definite volume and the use of a
volumetric pipet and be familiarize with the
calculation involving back titration.

Methods

In the preparation of 0.1 N HCl, The

volume of the HCl solution was determined
using the equation:

Where N N aOH (0.1 N) is the

normality of NaOH solution, V N aOH (250
ml) is the volume of NaOH solution that is
used in titration and N HCl has a given
normality is 12 N yielding a calculated HCl Figure 1. Volumetric titration set-up using
volume of 2.08 ml. the standard NaOH solution.

Before putting the HCl in the erlenmeyer

flask, a small amount of distilled water was
placed first to avoid unwanted reactions,
since HCl is a strong acid. In the
preparation of the solution, the volumetric
flask was also inverted to mix the solution
thoroughly. Then, it was titrated until color
changed to pale pink.
 A. Analysis of Aspirin Table 2. ​Shows various statistical analysis of
the standardized HCl solution
Mean normality of 0.110 N (土0.9)
HCl

Relative Standard 2.92%

Deviation

Sodium hydroxide solution, which

was used in the previous experiment, was
utilized to titrate and standardize the
prepared hydrochloric acid solution. Sodium
hydroxide is considered as a secondary
standard because it was systematized
against a primary standard (Harvey, 2019).
In the standardization of HCl, the
concentration of the HCl was computed to
have a mean of 0.111 mole/L with an
absolute uncertainty of (0.003). In addition
to that the normality of HCl is identical to its
molarity for there is only one acidic
hydrogen in one particle of HCl.
Furthermore, the relative standard
Results and Discussions deviation was calculated to be 2.9% of the
0.111 M mean, this implies that the data
Table 1. ​Calculated table values for acquired are closely related. The smaller
standardization of HCl solution by titrating the relative standard deviation value the
against standardized NaOH solution. more clustered the data is around the mean
Trial Volume of Volume Normality and the lesser it is spread out.
HCl of NaOH of HCl
titrated (土 used
0.02) (土0.05)

1 20.0 ml 21.1 ml 0.113 N

(土0.9)

2 20 mll 21.0 ml 0.112 N

(土0.9)

3 20 ml 19.9 ml 0.106 N
(土 1)
 solution was then titrated with hydrochloric
acid and the excess NaOH that reacted was
used to calculate the amount of ASA in the
solution.
The result of the calculations revealed
that the mean amount of ASA in the sample
was 0.0248 grams with an absolute
uncertainty of 土0.0001.
In addition, the computed relative
standard deviation was 0.53% and the
Figure 1. ​Shows three trials of HCl solution
calculated mean ASA percentage was
titration using the standardized NaOH
23.59%. These suggest that there is a low
solution.
variation and low to little error in the result of
the experiment.
In the titration of HCl solution using
standardized NaOH solution, trials 1 and 3
exhibited a color change from clear to pale
pink and trial 2 from clear to light pink. The
change in color indicates the end point of
titration. The end point is just a rough
estimate of the equivalence point, in which
the presence of hydronium and hydroxide
ions are chemically equal (Skoog et al,
2013).

Table 2. ​Calculated table values for the

analysis of ASA sample
Trial Volume Mass %ASA
of HCl ASA in
used (​土 sample
0.05) (​土
0.0001)

1 3.7 mL 0.0247 g 23.76%

2 3.5 mL 0.0248 g 23.86%
3 3.5 mL 0.0248 g 23.86%
The purity of ASA was determined by
hydrolyzing 0.1 gram grounded tablet with
0.1 N sodium hydroxide and since the
hydrolyzation process is slow due to 2
hydrogen ion reacting to a single ASA
molecule, the solution was heated. The
Figure 2. ​Trials of HCl titration using
hydrolyzed ASA solution
During the titration of HCl, there is
expected color change in the solution. Trials
1 to 3 exhibited color change from a clear
solution to yellow. This is the effect of the
reaction between the excess NaOH in the
solution and HCl, and indicates that the
endpoint of the titration was met (Skoog et
al, 2013).
 Post Lab Questions
1. pH would be lower for the dilute solution compared to the normal pH value of the
standard solution, and, the nature of the solution will be change as more neutral ions of
water is poured in. Furthermore, it changes the value of titrant needed to complete the
equivalence point and end point in titration.
2.
mg ASA
eq weight ASA
+= (V N aOH)(N N aOH) − (N HCl)(V HCl)

250 (90%) ASA

180 mg ASA + (5N HCl)(10mL HCl)
2
1 N N aOH
V N aOH = 2.0 mL N aOH

Appendix

A. Standardization of HCl solution

(C N aOH ) (V N aOH)
C HCl = V HCl
● Trial 1

(0.108 ±0.001 M ) (0.0211 ± 0.05 L)

C HCl = 0.020 ± 0.02 L = 0.113 M

(0.108 ±0.9% M ) (0.0211 ± 0.2 % L)

Relative uncertainty = 0.020 ± 0.1% L = 0.113 ± 1.2% M

√(0.9)
2
Absolute uncertainty = + (0.2)2 + (0.1)2
=0.113 ± 0.9%
= 0.113 ± 0.001M

● Trial 2

(0.108 ±0.001 M ) (0.0210 ± 0.05 L)

C HCl = 0.020 ± 0.02 L = 0.112 M

(0.108 ±0.9% M ) (0.0210 ± 0.2 % L)

Relative uncertainty = 0.020 ± 0.1% L = 0.112 ± 1.2% M

√(0.9)
2
Absolute uncertainty = + (0.2)2 + (0.1)2
=0.112 ± 0.9%
 = 0.112 ± 0.001M

● Trial 3
(0.108 ±0.001 M ) (0.0199 ± 0.05 L)
C HCl = 0.020 ± 0.02 L = 0.106 M

(0.108 ±0.9% M ) (0.211 ± 0.3 % L)

Relative uncertainty = 0.020 ± 0.1% L = 0.106 ± 1.3% M

√(0.9)
2
Absolute uncertainty = + (0.3)2 + (0.1)2
=0.113 ± 0.95%
= 0.107 ± 0.001%

0.113 + 0.113 +0.107

mean = 3 = 0.111 ± 0.003
Normality of HCl

N = molar mass x f

● Trial 1

0.113 M x 1 = 0.113 N
● Trial 2
0.112 M x 1 = 0.112 N
● Trial 3
0.106 M x 1 = 0.106 N

B. Analysis of Sample
 0.0247g + 0.0248 g + 0.0246 g
M ean mass ASA = 3 = 0.0248 ± 0.0001

References:
.​Skoog, D.A., West, D.M., Holler, F.J., and Crouch, S.R. (2013). Fundamentals of Analytical
Chemistry – 9th ed. United States: Cengage Learning. Pages. 326

Harvey, D. (2019). Analytical Standards. Retrieved from

https://chem.libretexts.org/Bookshelves/Analytical_Chemistry/Book%3A_Analytical_Chemistry_
2.0_(Harvey)/05_Standardizing_Analytical_Methods/5.1%3A_Analytical_Standards

E. B. Sandell, T. S. West. (1969). Recommended Nomenclature for Titrimetric Analysis​, Pure

Appl. Chem. ​18, 427 .