Abstract

The main goal of this experiment was to find the concentration of a basic solution by titrating it
with a volume of a standard acid solution (of known concentration) required to neutralize it.
The purpose of the titration is the detection of the equivalence point, the point at which
chemically equivalent amounts of the reactants have been mixed. In this case aspirin from
previous experiment was used. Ethyl alcohol was added to it to dissolve the aspirin. The solution
was then titrated using NaOH.

After all the results are observed the mixture then undergoes the reverse process
of esterification or hydrolyzed by using the same titration method but using HCL.

Introduction

Pure aspirin, chemically called acetylsalicylic acid, is both an organic ester and an organic acid.
It is used extensively as a painkiller (analgesic) and as a fever-reducing drug (antipyretic). When
ingested, acetylsalicylic acid remains intact in the acidic stomach, but in the basic medium of the
upper intestinal tract, it hydrolyzes forming the salicylate and acetate ions.

The analgesic action of aspirin is undoubtedly due to the salicylate ion; however, its additional
physiological effects and biochemical reactions are still not thoroughly understood. It is known
that salicylate acid has the same therapeutic effects as aspirin; however, due in part to the fact
that it is an acid, salicylic acid causes a more severe upset stomach than does aspirin. Aspirin,
like many other organic acids, is a weak monoprotic acid. Qualitatively, the purity of an aspirin
sample can be determined from its melting point.

The melting point of a substance is essentially independent of atmospheric pressure, but it is

always lowered by the presence of impurities. The degree of lowering the melting point depends
on the nature and the concentration of the impurities. Quantitatively, the purity of an aspirin
sample can be determined by a simple acid-base titration. The acetylsalicylic acid reacts with
hydroxide ion, from a standardized sodium hydroxide solution, accordingly.

Apparatus and materials

Two 50ml burets, 600ml beaker, water bath, buret clamp, three 250ml Erlenmeyer flask, aspirin,
phenolphtalein solution, 95% ethyl alcohol.

Methodology

1. Zero point five grams of aspirin was weighed and prepared from previous experiment
onto a clean and dry 250ml Erlenmeyer flask.
2. Twenty five milliliter of ethyl alcohol was added to the flask and swirled till the aspirin
3.

dissolved completely. Later then two drops of phenolphthalein was added to the flask.
The sample then was titrated using 0.1M NaOH till faint pink was acquired. The volume
of NaOH used was recorded.

4. Fifteen milliliter of NaOH to the volume of base required from the previous titration was
added to the sample.
5. The mixture was then heated for 15 minutes in a water bath at temperature 90 to 95
and the aspirin was hydrolysed. The flask was swirled occasionally to heat the
mixture evenly.
6. The flask is then cooled by using cold tap water.
7. The initial volume of HCL was recorded. The excess base was titrated back with HCL.

Results
Molarity of NaOH= 0.1mol
Molarity of HCl= 0.1mol
Mass of aspirin= 0.5gram

Volume of NaOH required to neutralize all acid material

Final reading= 41ml

Initial reading= 0
Volume of NaOH= 41ml
Milimoles of NaOH= 4.1mmol

Volume of NaOH used in hydrolysis

Volume of NaOH= 41ml
Milimoles of NaOH= 4.1mmol
Volume of HLC in back titration
Final reading= 40.5ml
Initial reading= 0ml
Volume of HLC= 40.5ml
Milimoles of HLC= 4.05mmol
Milimoles of acetylsalicylic acid= 4.1-4.05= 0.5
Grams of acetylsalicylic acid in sample= 0.5x180/10^3= 0.09gram
Purity of aspirin= 0.09/0.5x100%= 18%

Discussion
Aspirin is slightly acidic and reacts with bases in neutralization reactions. If the reaction is
followed with an indicator, a color change will occur when the acid is completely neutralized and
one drop of excess base has been added. The number of moles of base consumed and the
number of moles of acid in the sample can be calculated form the volume of the base needed to
obtain the color change. The relationship between these two mole values is determined form the
balanced chemical equation for the reaction.
In this experiment, 0.5gram of aspirin was titrated of with a known concentration of
sodium hydroxide solution. The end point will be determined with phenolphthalein or
thymol blue indicator.

The following simplified equation describes the neutralization

reaction that will be observed in this experiment.

H-Asp (aq) + NaOH (aq) Na-Asp (aq)

+ H2O (l)

Because the mole ratio is 1:1, the number of moles of the base will equal the number of
moles of acid at the equivalence point of the titration.
The molar mass of the solid aspirin can be approximated by dividing the mass of the
aspirin by the moles of aspirin present. After this a a back-titration is done by using HCL

There are a few errors that has to be taken serious so that the experiment will achieve the
desired result;
1. The scale used in this experiment should always be tarred so that the when we
measure a mass of something it will be accurate.
2. The acids such as the NaOH should be measured accurately before adding them into
the mixtures to avoid not achieving desired results.
3. When heating or cooling certain mixtures, it should be timed correctly as per the
procedure to avoid over cooling or over heating which will mess up the experiment.
4. When using conical flask, buret and the dropper must be washed thoroughly with
water to prevent any foreign chemical to be mixed with the existing mixture.
5. Initial volume of solution in buret must me measured from 0 so that miscalculation
wont happen.
Questions
1. From your results, discuss the purity of aspirin.
From the result I achived I know realized that the aspirin has decreased
2. Explain the back titration method used in this experiment.
Many reactions are slow or present unfavorable equilibria for direct titration. Aspirin is a
weak acid that also undergoes slow hydrolysis; i.e, each aspirin molecule reacts with two
hydroxide ions. To overcome this problem, a known excess amount of base is added to
the sample solution and an HCl titration is carried out to determine the amount of

unreacted base. This is subtracted from the initial amount of base to find the amount of
base that actually reacted with the aspirin and hence the quantity of aspirin in the analyte.

CONCLUSION
Aspirin prepared from the previous laboratory experiment was relatively impure. It was found to
have a percent purity of 18%.

REFERENCE
1. http://www.chem.latech.edu/~deddy/chem104/104Aspirin.htm

accessed on 8 March

2016
2. Dr. H.B. Mohd Ismail, Prof. N. Abdullah ( 2015); Comprehensive College Chemistry
Sap Publications. accessed on 8 March 2016
3. K.P.C Vollhardt, Neil E. Schore (2007); Organic Chemistry Structure and Function
(2007) W.H. Freeman and Company accessed on 8 March 2016

Appendix

Figure 1: After the back-titration using HCL.

Figure 2: 0.5 grams of aspirin in the flask.

Figure 3: Titration Using NaOH.

Figure 4: After titration by using NaOH the solution will turned faint pink.