FORMAL LABORATORY REPORT ON

ANALYTICAL CHEMISTRY LABORATORY

(CHY56A)

TTH 7:00 - 10:00 am

Experiment 8

DETERMINATION OF ASPIRIN USING BACK TITRATION

Submitted by:

JYLLA A. ANGWAY

Group 1 Laboratory

Alcano, Jason

Esparrago, Moreen Roce

Ganza, Ram Hannah

Redondo, Jay Marianne

Date Performed:
 October 8, 2019

Date Completed:

October 8, 2019

Submitted to:

Mrs. Aileen Ang, R.Ch, MS

I. INTRODUCTION

Titration is a procedure used in determining the concentration of a solution (analyte) by

allowing it to react completely with another solution of known concentration (titrant). In any titration
method, the point of chemical equivalence called the end point is indicated by a color change or
change in instrumental responses (Skoog et, al. 2014). In other experiments, it is sometimes
necessary to add an excess of a known titrant to the analyte where the excess is then titrated with a
second standard reagent. This process is called a back titration or indirect titration (Harris, 2010).

In this experiment, the process of back titration is used to determine the percent composition
of aspirin (acetylsalicylic acid) in aspirin tablets. Aspirin is made by combining two acids therefore it
has two acid portions needed to be neutralized and makes it consume two moles of base (San, 2016).
The base in this experiment will be a previously standardized Sodium hydroxide (NaOH). In order to
neutralize the two acidic portions of aspirin, an excess of Sodium hydroxide (NaOH) is added to the
sample solution and the excess base is then titrated with Hydrochloric acid (HCl) in order to
determine the amount of the unreacted base. In determining the composition of the aspirin in the
analyte, the unreacted base is subtracted from the initial amount of base which reacted with the
aspirin.

The objectives of this experiment are to explain the concept of back titration, determine the
percent composition of as aspirin in the analyte, and explain why back titration is used for this
analysis.
II. METHODOLOGY

Chemicals and Apparatus

The experiment required the following apparatuses: mortar and pestle, 50 mL buret, buret
clamp, graduated cylinder, iron stand, buret brush, boiling chips, 1 unit of hotplate (Corning
420D), six 250 mL Erlenmeyer flasks and 1 unit of analytical balance (Shimadzu AX200). For
this experiment, the chemicals used were about 1 gram of crushed aspirin tablets (Scheeprin),
phenolphthalein indicator, ethanol, 0.0970 N of Sodium hydroxide (NaOH) and 0.0978 N of
Hydrogen chloride (HCl).

Procedure

A. Sample Preparation

Using the mortar and pestle, the aspirin tablets were crushed to produce about 1 gram of
powder. On the analytical balance, about 0.3 grams of powder was then weighed into three
250-mL Erlenmeyer flasks. With the use of the graduated cylinder, 20 mL of ethanol was added
to each flask along with three drops of phenolphthalein indicator. The contents of the flasks was
then swirled gently for homogeneity.

B. Blank Determination

For the blank determination, 20 mL of ethanol and 3 drops of phenophthalein was placed
into each of three 250 mL Erlenmeyer flasks. Each of the flask was then titrated to endpoint. The
volume of the base added was then recorded to be used as a correction factor.

C. Aspirin Titration with Base

The buret was rinsed and filled with the previously standardized 0.0970 N NaOH solution.
The first aspirin sample was then titrated to the first permanent cloudy pink color. For the
completion of the reaction, the amount of needed excess NaOH was calculated and and added to
the sample using the buret. The total volume added was recorded and the same procedure was
repeated for the other aspirin sample solution.
 D. Heating the Reaction to Completion

Boiling chips were added to each flask as each was heated for 15 minutes in a water bath in
order for the hydrolysis reaction to speed up. During the heating process, the flasks were swirled
occasionally and after 15 minutes was removed from the water bath. It was then allowed to cool
for 5 minutes.

E. Back Titration with Acid

Using the previously standardized 0.0978 N HCl as the titrant, the excess base in each flask
was titrated until the pink color disappeared. The volume of acid added was recorded.

Calculations used in the experiment

A. Calculation for Moles of Aspirin, mol

Moles of aspirin = T otal moles of base added (based oncorrected volume) - Total moles of acid added

B. Calculation for Percent Aspirin, %

Weight of Aspirin
Percent Composition of Aspirin   100%
Weight of Sample

III. RESULTS

Shown in this chapter are the data gathered during the conduct of experiment.

In table 1 below are the data obtained during the blank determination.

Table 1. Results of Blank Determination

 Trials

Trial 1 Trial 2 Trial 3

Volume of base added, mL 0.10 0.10 0.10

Mean volume of base added,

mL 0.10

Shown in the following table are the results obtained from the analysis of the titration of
aspirin.

Table 2. Results of the Back Titration of Aspirin

Trials

Trial 1 Trial 2 Trial 3

Weight of sample, g 0.3003 0.3000 0.3014

Volume of base added to reach 6.90 6.80 7.25

endpoint, mL
Volume of additional base 16.90 16.80 17.25
added (excess only), mL
Total volume of base added, 23.80 23.60 24.50
mL
Corrected volume of base 23.70 23.50 24.40
added, mL
Total moles of base added
(based on corrected volume), 0.00230 0.00228 0.00237
mol
Volume of acid used for back 8.50 9.00 9.30
titration, mL
Total moles of acid added, mol 0.000831 0.000880 0.000910

Moles of base reacted with 0.00147 0.00140 0.00146

aspirin, mol
Moles of aspirin, mol 0.000734 0.000670 0.000729

Weight of aspirin, g 0.1322 0.1261 0.1313

 Percent aspirin, % 44.03 42.02 43.56

Mean percent aspirin, % 43.20

IV. DISCUSSION

In this chapter is the obtained data will be given an interpretation.

Back titration is an indirect procedure and is commonly used for slow reactions such as the
hydrolysis of aspirin as using forward titration would be difficult to identify the endpoint because
aspirin is a weak acid and reactions may proceed slowly. However, using back titration, the endpoint
is more easily recognised, as it is a reaction between a strong base and a strong acid, NaOH and HCl
respectively. This type of reaction occurs at a fast rate and thus produces an endpoint which is abrupt
and easily seen (Medrano et, al. 2014)

In this experiment, before the titration of the sample solution, a blank determination was
performed. As shown in table 1, the blank determination yielded a mean volume of 0.10 mL base
added to the blank which was ethyl alcohol (CH3CH2OH) and phenolphthalein indicator. As ethanol
is known to be slightly acidic, it is expected that it would consume a small amount of the base
Sodium hydroxide (NaOH) (Gutbezahl and Grunwald, 2010).The results of the blank determination
was used to correct the volume of the base added to the sample solution as seen on the corrected
volume of base added in table 2.

As the titration of the sample solution starts, the first stage of this reaction is that of alkaline
hydrolysis. This involves reacting the aspirin solution with a measured amount of sodium hydroxide;
an amount that will exceed the amount of aspirin present. Because the hydrolysis reaction occurs at a
very low rate at room temperature it was heated to increase the reaction rate as shown in the reaction
below (Spurlock, 2013.)

CH 3COOC 6 H 4 COOH + 2 NaOH 


Δ
CH 3 COONa + HOC 6 H 4 COONa + H 2O

Going back to the obtained results in table 2, the total volume of the base added was
calculated following the principle of the hydrolysis of aspirin consuming two moles of base as it is
made of two acids, acetic acid (CH3COOH) and salicylic acid (C7H6O3). The base first neutralizes the
acetic acid then releases a new acid, salicylic acid. Salicylic acid cannot be neutralized until the acetic
acid is released. This new acid also has to be neutralized so a second portion of base must be added.
It is therefore possible to titrate aspirin in two portions, the first neutralizing the acetic acid and the
second neutralizing the salicylic acid (Pall, 2010). An additional excess of 10 mL of base is also
added to ensure complete reaction.

The second stage then involves back titration of the hydrolysed sodium hydroxide solution
with hydrochloric acid. This process reacts the excess sodium hydroxide with hydrochloric acid like
in the chemical equation below (Spurlock, 2013)

NaOH + HCl 
 NaCl + H 2O

And as the excess base is then back titrated using Hydrochloric acid (HCl), it would then be
easy to calculate for the moles of the aspirin following the formula:

Moles of aspirin = T otal moles of base added (based oncorrected volume) - Total moles of acid added

As the mole of aspirin is determined, its weight in grams can also be obtained through the

use of the gravimetric factors and from there the percent composition of the aspirin was calculated

with the aid of the formula:

Weight of Aspirin
Percent Composition of Aspirin   100%
Weight of Sample

With this formula, the percent composition of aspirin in each of the sample solution was
determined. The three trials yielded 44.03 % aspirin, 42.02 % aspirin and 43.56% aspirin with
which had a mean percent composition of 43.20 % aspirin.

V. CONCLUSION
 Through the process of back titration, the percent composition of aspirin was known to have
a mean value of 43.20% aspirin. Determining the mean percentage composition of aspirin was made
efficient by using the concept of back titration. By this experiment, it can be assumed that back
titration was used for the analysis of aspirin because the method is suitable in order to ensure the
completion of the reaction by adding excess reagent and determining the percent composition by
back titrating the unreacted base.

For this experiment, it would be recommended to obtained a theoretical value of the

percentage composition of aspirin in order to compare the results of the experiment and to see
whether the actual value coincides with the theoretical value.

VI. REFERENCES

Gutbezahl, Boris, Grunwald Ernest. (2010).The Acidity and Basicity Scale in the System
Ethanol—Water. The Evaluation of Degenerate Activity Coefficients for Single
Ions1a. Journal of the American Chemical Society 1953 75 (3), 565-574

doi: 10.1021/ja01099a015

Harris, Daniel C. (2010). Quantitative Chemical Analysis. (8th ed.). W.H. Freeman and Company.
New York City. NY 10010

Medrano, E.M.M., Pasco, J.M., Lubrin M.E.,ManriqueM.. (2014).Quantitative Determination of

Acetylsalicylic Acid in Aspirin Tablets by Back-titration. Retrieved from
/12405205/_Chem_28_Quantitative_Determination_of_Acetylsalicylic_Acid_in_
Aspirin_Tablets_by_Back-titration(Accessed on Nov. 4, 2019)

Pall, Sativa. (2010). Analysis of Aspirin. Retrieved from http://www.savitapall.com/medicines_

drugs/labs/Analysis%20of%20Aspirin.pdf(Accessed Nov 1, 2019)

San, Kee Tze. (2016). Analysis of Aspirin. Chemical Engineering Laboratory I. SEGi University.
Retrieved from www.scribd.com/document/360173569/Analysis-of-Aspirin-

Lab-Report(Accessed Nov. 3, 2019)

Skoog, D. A., West, D. M., Holler, F. J., & Crouch, S. R. (2014). Skoog and Wests Fundamentals of
Analytical Chemistry (9th ed.). Hempshire: Cengage learning. doi:
10.1007/s00216-013-7242-1

Spurlock, D. (2013). Standardization of a Base, NaOH Class Notes. Indiana University Southeast.
Retrieved from http://homepages.ius.edu/ DSPURLOC/c121/week11.html
(Accessed Nov. 1, 2019)