BACHELOR OF CHEMICAL ENGINEERING WITH HONOURS

LAB REPORT SUBMISSION FORM

<EKB 3171>: < Analytical Techniques & Instrumentation Lab 5>
NAME Nisha Fareena ID 1102171011
EXPERIMENT NO. & TITLE EXPERIMENT 2: Analysis of Aspirin through Titration

WEEK OF EXPERIMENT 2
DATE OF EXPERIMENT 2/04/2021
DATE OF SUBMISSION 17/05/2021

NAME OF GROUP MEMBERS ID

Nisha Fareena 1102171011
Ravin A/L Sinnasami 1103191004
Vimal Haasan 1103173004
Mathaneshan A/L Rajagopal 1103173003
Reventheran varathan 1103173010

MARKING SIGNATURES
DETAILS TOTAL MARKS
AWARDED
Attitude 5
CHEMICAL ENGINEEIRNG LAB VI
Participation 5 INCHARGE

Lab Report 40 MS. PREETI SHRIVASTAVA

Total 50

On-time submission Late submission

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protective equipment laboratory. Poor in time protective equipment protective equipment equipment (PPE) in the
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 LABORATORY REPORT EVALUATION FORM

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interpret their objectives, very details of important content objectives, the main result with the
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it is too long without discussion. However students can straight forward. overview and the
any important write a good summary understanding of the
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reaching by the reader.
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Missing one of the

Explain the principle of
content in the Explain the principle of
the equipment,
Copy theory from Copy theory from introduction which are the equipment,
application (at least 3),
Introduction manual without any manual with slightly principle of the application,
advantages and
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disadvantages (at least
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3). Present the content in
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less than three citation with correct format of
than three citation with
with wrong format of writing
correct format of writing
writing
 1-2 3-4 5-6 7-8 9-10
Using past tense and
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formula and formula or formula the formula formula with the
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complete important the the
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data. No discussion/explanation discussion/explanation
in details, relates in details, relates
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at all. No results and theory and fundamental. theory and
theory and theory and fundamental
explanation to the No results and fundamental.
fundamental. with citations. Objectives
objectives at all. explanation to the Objectives fulfilled
Objectives fulfilled fulfilled completely.
objectives. partially
partially.
Conclusion and 1 2 3 4 5
Recommendation Wrong summary of the Incomplete summary of Incomplete summary of Summary of the
Summary of the results
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to relate the findings or
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applicable to the
to the experimental. the experimental. Do not the experimental. to the experimental.
experimental. Suggest
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improvements in
improvements in in apparatus or in apparatus or improvements in
apparatus or
apparatus or measurement measurement apparatus or
measurement
measurement procedure, or procedure, or measurement
procedure, or
procedure, or experimental experimental procedure, or
experimental procedures
experimental procedures for future. procedures for future. experimental
for future.
procedures for future. procedures for future.
1 2 3 4 5
References More than four
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references
 1 2 3 4 5
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raw data collection. data collection. Show collection. Show collection. Show collection. Show
The sample complete sample complete sample complete sample complete sample
Appendices
calculation is not calculation. Major calculation. Minor calculation with no calculation with no
complete mistake in calculation mistake in calculation mistake. mistake. Include the final
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table
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in-text citation
 TABLE OF CONTENT

S. NO CONTENT PAGE
NO
1.0 Abstract 2

2.0 Introduction 3

3.0 Material and Method 5

4.0 Result and Discussion 7

5.0 Conclusion and Recommendation 10

6.0 Appendix 11

References 14
 TABLE OF FIGURE

S. NO LIST OF FIGURES PAGE

NO
2.1 Titration setup to analyze the purity of Aspirin. 3

2.2 Chemical reaction for the synthesis of Aspirin. 4

4.1 Aspirin neutralization reaction. 8

 TABLE OF TABLE

S. NO LIST OF TABLES PAGE NO

3.1 Apparatus and material used for the synthesis of 6

aspirin.

4.1 Actual and theoretical values of aspirin, with % 9

purity.
Titration of
Aspirin

1
1.0. ABSTRACT

The main objective of this experiment is to analyse the percentage purity of

aspirin by titration against a base to neutralize the reaction and determine the
presence of acetylsalicylic acid in the solution of various samples. The base used in
this titration is NaOH and the amount of samples used are 0.17 g of standard aspirin,
0.15 g of sample aspirin and 0.2 g of crude aspirin. These samples were dissolved in
120 cm3 of ethanol and stirred until completely soluble. The volume of NaOH used for
each of these three standard, sample and crude Aspirin were noted to be 0.9 ml, 18.2
ml and 16.6 ml respectively. The actual yield, results obtain are calculated to be 0.0972
g for standard aspirin, 1.9656 g for sample aspirin and 1.7928 g for crude aspirin. The
theoretical yield of aspirin the amount of sample used is taken to calculate the molarity
and the mass of aspirin that gives a result of 0.1728 g of standard aspirin, 0.15 g of
sample aspirin and 0.2 g of crude aspirin. After the determination of the purity of aspirin
it shows that the standard aspirin has the highest purity of 56.25%, following with a
purity of 13.0% for sample aspirin and 8.964% for crude aspirin. Some of the error
consideration can be due to the molarity of the NaOH solution to be not accurate, the
purity of aspirin can be less due to the presence of contaminates, or spilling that
resulted in discarding some useful product and titration errors can be due to the
presence of gas bubbles that results in inaccurate reading. In recommendation, the
experimental setup should be magnified to reduce the effect of contamination and dust
particles. It is also recommended to use clean equipment and ventilated laboratory
setup and rinsing the filter crucible then transferring the product from the beaker back
to the filter crucible. These recommendations can result in better yield and percentage
purity of aspirin samples.

2
2.0. INTRODUCTION
2.1. Principles

The main objective of this experiment is to analyse the percentage purity of

aspirin by titration against a base to neutralize the reaction and determine the
presence of acetylsalicylic acid in the solution of various samples. Titration is a
laboratory procedure where substances are combined under controlled condition in a
glassware, such as burettes, to determine the purity of the required chemical under
consideration. The figure 2.1 shows the titration setup below.

Figure 2.1: Titration setup to analyze the purity of Aspirin.

A burette is used to transfer liquids or solutions between containers that are

analytically recorded. A burette is marked in millilitres, the numbers are in ascending order
on the burette where at the base the stopcock controls the liquid flow. Opening and
closing of the burette occur when it is parallel to the length of the burette and
perpendicular to the length of the burette.

3
 Many reactions follows an unfavourable equilibria or are slow under direct
titration. However, aspirin is a weak acid that undergoes slow hydrolysis i.e., each
aspirin molecule reacts with two hydroxide ions. To tackle this issue excess amount
of base which in this case is ethanol is added to the sample solution and titrated
against NaOH to determine the amount of unreacted base. To determine the amount
of acetylsalicylic acid in the particular sample, precise volume as well as the
concentration of the NaOH has to be known. The equivalence point is often marked
by an indicator, a substance that changes colour at the equivalence point (Harris,
2007). The point in the titration where enough of the titrant has been added to react
exactly with the analyte is called the equivalence point, and occurs when moles of
titrant equals moles of analyte according to the balanced equation as shown in the
figure 2.2.

Figure 2.2: Chemical reaction for the synthesis of Aspirin.

NaOH serves as a secondary standard, because its concentration can change

over time. Phenolphthalein is used as an indicator to indicate the stop of a reaction by
turning into light pink – purple colour which is also known as the end point. The amount
of unreacted base is subtracted from the initial amount of base to find the amount of
base that actually reacted with the aspirin and hence the purity of aspirin is determined.

2.2. Uses of Titration

Titration is an analytical technique that is widely used in many chemical industries to:

 Determine the quantity of a reactant in a sample.

 A pH indicator is used to determine the endpoint of titrations for acid/base.
Acid/base titrations are based on the neutralisation of analytes and titrants.

4
 Titration has for many years been widely used in the pharmaceutical industry
to determine the strength of small-molecule active pharmaceutical ingredients
(APIs), intermediates, and raw materials.
 Titration is used to determine the extent of contamination in the natural
rainwater or snow.
 Titration is used to determine the magnitude of contamination and the
requirements that should be put in place in terms of filtering and cleaning the
water.
 Titration is largely used to determine the acidity of orange juice.
 Titration determines the kind of base suitable for a cosmetic, for example,
coconut oil.
 Titration is important when measuring the pH and acidity of the initial milk being
used to make the cheese.

2.3. Advantages and Disadvantages of Titration

Advantages Disadvantages
 Generally cheap, requiring  Uses large quantities of
less equipment. the substance being
 Does not require a high analysed.
level of skill.  Only requires liquid phase
 Can often be done rapidly. reaction to occur.
 Immediately available.  Limited accuracy.

5
3.0. MATERIAL & METHOD
3.1. Material and Apparatus

The material and apparatus used in order to obtain the percentage purity of aspirin in
laboratory scale are given in the table 3.1 below.

Table 3.1: Apparatus and material used for the synthesis of aspirin.

APPARATUS MATERIAL

Round bottomed flask 4g of NaOH

Burette 120cm3 of Ethanol
Beaker Distilled water
Stirrer Sample Aspirin
Filter paper Crude Aspirin
Filter funnel Standard Aspirin
Conical flask Phenolphthalein indicator
Spatula
Dropper
Retort stand
Water bath

3.2. Method of Titration

1. Obtain and prepare a burette for titration by washing and conditioning it with
titrant solution (NaOH). Fill the buret, eliminate air bubbles, and have your
instructor check for air bubble before starting your first titration.
2. Prepare 0.1M of NaOH by adding 4g of NaOH dissolved in 1000 cm 3 of
ethanol or 0.4g of NaOH in 100 cm3 of ethanol.
3. Record the initial burette reading to the correct number of decimal places,
where NaOH should not exceed more than 50ml.
4. Take a folded weigh-paper, and place it on a balance pan to note the weight
and add on ASA to the paper. Use a metal spatula to transfer a small amount
of ASA to the paper, and then return the paper to the balance.

6
5. Record the mass, and transfer the ASA to the flask, rinsing the paper with
distilled water to ensure complete transfer. Dissolve the aspirin in 120 cm3
of Ethanol.
6. The weight of all three aspirin taken were noted to be 0.17g for standard,
0.15g for sample aspirin and 0.2g for crude aspirin.
7. The solution is to be titrated slowly in the presence of NaOH, into the flask
containing the acid, while swirling the flask. Continue adding the NaOH
solution dropwise, swirling the flask constantly to ensure full mixing.
Gradually slower the addition of NaOH, while continuing to swirl the flask
and wash down the walls of the flask.
8. Stop the titration when the addition of a single drop of NaOH changes the
colour of the solution to a light pink, indicating that you have reached the
endpoint.
9. Record the final burette reading on the data table.
10. Titration should be repeated for 3 times to obtain more accurate results and
calculate and report the percent purity of your aspirin sample.

7
4.0. RESULT AND DISCUSSION

In this experiment the primary standard used will be Acetyl Salicylic Acid with
chemical formula HC9H7O4, which is abbreviated as ASA that is used to standardize
the sodium hydroxide solution. The balanced chemical equation for the reaction is
shown below in equation 4.1 and figure 4.1.

HC9H7O4 (aq) + NaOH (aq)  NaC9H7O4 (aq) + H2O (l) ---------- Eq (4.1)

Figure 4.1: Aspirin neutralization reaction.

The purpose of analysing various crude, sample and standard aspirin is to

determine the purity of aspirin. A large amount of strong base is used that neutralizes
the acid formed. The base used in this titration is NaOH and the amount of samples
used are 0.17 g of standard aspirin, 0.15 g of sample aspirin and 0.2 g of crude aspirin.
These samples were dissolved in 120 cm3 of ethanol and stirred until dissolved. The
solution was the titrated against NaOH that was placed in a burette and held inverted
on to the conical flask. The volume of NaOH used for each of these three standard,
sample and crude Aspirin were noted to be 0.9 ml, 18.2 ml and 16.6 ml respectively.
Therefore, from the result obtain the mass of aspirin can be calculated that comes out
to be 0.0972 g for standard aspirin, 1.9656 g for sample aspirin and 1.7928 g for crude
aspirin. These calculation represents the actual yield of aspirin on the other hand to
calculate the theoretical yield of aspirin the amount of sample used is taken to calculate
the molarity and the mass of aspirin that gives a result of 0.1728 g of standard aspirin,
0.15 g of sample aspirin and 0.2 g of crude aspirin.

8
 The calculation obtained from both the actual yield and the theoretical yield can
be used to determine the purity of aspirin where, the following equation 4.2 is used to
calculate the purity percentage of Aspirin.

𝐴𝑐𝑡𝑢𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
𝑃𝑒𝑟𝑐𝑒𝑛𝑡𝑎𝑔𝑒 𝑃𝑢𝑟𝑖𝑡𝑦 (%) = 𝑥 100% ---- Eq (4.2)
𝑇ℎ𝑒𝑜𝑟𝑖𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑

The table 4.1 below shows the measured and calculated values for all the three
samples and the percentage purity of each sample taken and determined through
titration against NaOH. The calculation is shown in detailed in the Appendix of the
report. Assuming the aspirin is not contaminated with other acids, the titration allows
you to quantitatively determine the purity of your aspirin.

Table 4.1: Actual and theoretical values of aspirin, with % purity.

Units: Mass of NaOH NaOH Volume Molarity Actual Theoretical Percentage

Aspirin initial final of of Mass of Mass of Purity (%)
(g) volume volume NaOH Aspirin Aspirin Aspirin (g)
reading reading taken (g) (g)
(ml) (ml) up (ml)
Standard 0.17 50 49.1 0.9 0.00054 0.0972 0.1728 56.25
Sample 0.15 50 31.8 18.2 0.01092 1.9656 0.15 13.10
Crude 0.2 50 33.4 16.6 0.00996 1.7928 0.2 8.964

After the determination of the purity of aspirin it shows that the standard aspirin
has the highest purity of 56.25%, following with a purity of 13.0% for sample aspirin
and 8.964% for crude aspirin. These results shows that the standard aspirin is
considered to be the purest containing larger amount of acetylsalicylic acid (ASA). The
sample and crude shows that there is very less amount of acetyl salicylic acid present
in the solution and the purity is low that could be due to several factors. Some of the
error consideration can be due to the molarity of the NaOH solution to be not accurate
due to weighing of pellets and error in scaling.
9
 On another hand, the purity of aspirin can be less due to the presence of
contaminates in the mixing vessel as well as exposure to the open environment. Other
possible error can be due to the result of spilling that resulted in discarding some useful
product. The experiment was carried out on a small scale therefore, a small
contamination of spillage could possibly show a tremendous effect of the percentage
purity of the product (Miller, 2014). Other common titration errors can be due to the
presence of gas bubbles that results in inaccurate reading.

There can be certain improvements in the process, one is to magnify the scale
of the experiment to give room for small contamination and dust particles. Another
improvement can be implemented by the use of clean equipment and ventilated
laboratory setup and reducing the amount of transfers from one apparatus to another.
In addition, rinsing the filter crucible then transferring the product from the beaker back
to the filter crucible. It may be possible to simply leave the product in the crucible and
rinse it directly after squeezing the excess liquid out, thus reducing the amount of lost
product due to transfers. The direction of error caused by incomplete reactions is
consistent with the result of a lower measured value of the standard acetylsalicylic
acid compared to the value listed on the chemical label.

10
5.0. CONCLUSION AND RECOMMENDATION

In conclusion, the objective if the experiment was obtained by determining the

percentage purity of the three different aspirin samples taken for titration. The purity
of aspirin it shows that the standard aspirin has the highest purity of 56.25% following
with a purity of 13.0% for sample aspirin and 8.964% for crude aspirin. From the results
obtained it can be seen that the standard aspirin has the highest percentage purity
followed by the sample obtained and the crude aspirin. The low purity count of the
standard aspirin differing from the reading on the label can be due to incomplete
reaction of acetylsalicylic acid with NaOH. Other factors that could possibly contribute
to the lower purity percentage of aspirin can be due to contamination, error in reading,
bubbles in burette and spilling of the sample. Several recommendation can be
incorporated to improve the percentage yield of the samples.

In recommendation, magnifying and expanding the scale of the experiment will

result in elimination of small contamination and dust particles in the surroundings. The
use of clean equipment and ventilated laboratory setup should be taken into account
that reduce contamination error. Proper equipment and lean stirrers should be utilized
that will reduce the amount of transfers from one apparatus to another and avoid
possible spillage.

11
6.0. APPENDIX

STANDARD ASPIRIN

Theoretical Calculation

0.17 1000 𝑚𝑜𝑙

𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑜𝑓 𝐴𝑠𝑝𝑖𝑟𝑖𝑛 = 𝑥 = 0.008
180 120 𝑑𝑚3

𝑚𝑜𝑙 0.001 𝑑𝑚3

𝑀𝑜𝑙𝑒𝑠 𝑜𝑓 𝐴𝑠𝑝𝑖𝑟𝑖𝑛 = 0.008 𝑥 𝑥 120 𝑐𝑚3 = 0.00096 𝑚𝑜𝑙
𝑑𝑚3 1 𝑐𝑚3
𝑔
𝑀𝑎𝑠𝑠 𝑜𝑓 𝐴𝑠𝑝𝑖𝑟𝑖𝑛 = 0.00096 𝑚𝑜𝑙 𝑥 180 = 0.1728 𝑔
𝑚𝑜𝑙

Actual Calculation

NaOH: Aspirin

M1V1: M2V2

0.1 x 0.`9 = M2 x 20

1000
M2 = 0.0045 = n x = 0.00054 mol
120

Mass of Aspirin = 180 x 0.00054 = 0.0972 g

Percentage Purity of Aspirin

0.0972
% purity = 𝑥 100% = 56.25%
0.1728

12
SAMPLE ASPIRIN

Theoretical Calculation

0.15 1000 𝑚𝑜𝑙

𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑜𝑓 𝐴𝑠𝑝𝑖𝑟𝑖𝑛 = 𝑥 = 0.007
180 120 𝑑𝑚3

𝑚𝑜𝑙 0.001 𝑑𝑚3

𝑀𝑜𝑙𝑒𝑠 𝑜𝑓 𝐴𝑠𝑝𝑖𝑟𝑖𝑛 = 0.007 3
𝑥 3
𝑥 120 𝑐𝑚3 = 0.00083 𝑚𝑜𝑙
𝑑𝑚 1 𝑐𝑚
𝑔
𝑀𝑎𝑠𝑠 𝑜𝑓 𝐴𝑠𝑝𝑖𝑟𝑖𝑛 = 0.00083 𝑚𝑜𝑙 𝑥 180 = 0.15𝑔
𝑚𝑜𝑙

Actual Calculation

NaOH: Aspirin

M1V1: M2V2

0.1 x 18.2 = M2 x 20

1000
M2 = 0.091 = n x = 0.01092 mol
120

Mass of Aspirin = 180 x 0.01092 = 1.9656 g

Percentage Purity of Aspirin

1.9656
% purity = 𝑥 100% = 13.10 %
0.15

13
CRUDE ASPIRIN

Theoretical Calculation

0.2 1000 𝑚𝑜𝑙

𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑜𝑓 𝐴𝑠𝑝𝑖𝑟𝑖𝑛 = 𝑥 = 0.0093
180 120 𝑑𝑚3

𝑚𝑜𝑙 0.001 𝑑𝑚3

𝑀𝑜𝑙𝑒𝑠 𝑜𝑓 𝐴𝑠𝑝𝑖𝑟𝑖𝑛 = 0.0093 3
𝑥 3
𝑥 120 𝑐𝑚3 = 0.0011 𝑚𝑜𝑙
𝑑𝑚 1 𝑐𝑚
𝑔
𝑀𝑎𝑠𝑠 𝑜𝑓 𝐴𝑠𝑝𝑖𝑟𝑖𝑛 = 0.0011 𝑚𝑜𝑙 𝑥 180 = 0.2𝑔
𝑚𝑜𝑙

Actual Calculation

NaOH: Aspirin

M1V1: M2V2

0.1 x 16.6 = M2 x 20

1000
M2 = 0.083 = n x = 0.00996 mol
120

Mass of Aspirin = 180 x 0.01092 = 1.7928 g

Percentage Purity of Aspirin

1.7928
% purity = 𝑥 100% = 8.964 %
0.2

14
 REFERENCE

D.C. Harris (2007). Quantitative Chemical Analysis. 7th ed., W. H. Freeman, NY. p.
121-122. Retrieved from:

[Link]

E.M.M Medrano, [Link], M.E. Lubrin, M. Manrique (2014). Quantitative

determination of acetylsalicylic acid in aspirin tablets by back titration. National
Institute of physics, College of Science. Retrieved from:

[Link]
etylsalicylic_Acid_inAspirin_Tablets_by_Back_titration?auto=download

Carrie Miller (2014). Spectrophotometric Analysis of Aspirin. American Chemical

Society; Washington, DC. Retrieved from:
[Link]

15