NFNF2813 - PHARMACOPOEIAL METHODS FOR

DRUG ANALYSIS

PRACTICAL NO. : 1

TITLE : Titrimetry for Drug Analysis: Acid/Base Titrations

DATE : 6 November 2023

LECTURER : Assoc. Prof. Dr. Juriyati Jalil

Sem I 2023-2024

GROUP 1 - SUBGROUP 4

Name Matric No.

NUR UMAIRAH BINTI AHMAD A195151

AUBREY KHO JIN MING A194546

NURUL AIN BINTI AZMI A193061

FACULTY OF PHARMACY

UNIVERSITI KEBANGSAAN MALAYSIA

TABLE OF CONTENTS

No Item Page

Title 2

Objective 2

Introduction 2

Experiment 1 4

a. Experimental methods
b. Results
c. Calculations
d. Questions
e. Discussion

Experiment 2 11

a. Experimental methods
b. Results
c. Calculations
d. Questions
e. Discussion

Experiment 3 15

I. Experiment 3A
a. Experimental methods
b. Results
c. Calculations
d. Questions
II. Experiment 3B
a. Experimental methods
b. Results
c. Calculations
d. Questions
III. Discussion

Conclusion 26

References 27

1
 TITLE: TITRIMETRY FOR DRUG ANALYSIS: ACID/BASE TITRATIONS

OBJECTIVES:
1. To determine the concentration of NaOH used to completely neutralize potassium acid
phthalate (KHP).
2. To determine the standardisation of HCl with NaOH.
3. To understand the concept of back titration by neutralising the acid using antacids.
4. To determine the concentration of the acetic acid in the vinegar.

DATE: 31th October 2023

INTRODUCTION
Titration is a foundational and versatile technique in analytical chemistry that is
employed to determine the concentration of a substance within a given sample. Typically, the
process is carried out by gradually adding a standard solution (i.e., a known concentration) of
titrating reagent, or titrant, from a burette, essentially a long, graduated measuring tube with a
stopcock and a delivery tube at its lower end.

To analyse unknown acids and bases, we need a "standard" solution to react with the
unknowns. A standard solution is one whose concentration is precisely known. First, we'll make
a standard NaOH solution. A standard solution can be made by dissolving an accurately massed
substance and diluting it to a measured volume. The concentration can thus be calculated
precisely. However, obtaining NaOH of sufficient purity to use as a primary standard is usually
impossible. We will prepare an approximate molarity solution and standardise it against a
primary standard of known purity.

For this experiment, potassium acid phthalate (KHC8H4O4) will be the primary standard.
With a molar mass of 204.2g/mol, this is a large molecule. We will abbreviate it to KHP, where
“P” is the phthalate ion. KHP is an acidic substance, with the ionising hydrogen emphasised in

2
the formula. As a result, KHP is monoprotic and will react with NaOH in a simple 1 to 1
relationship, as shown by the equation below :

NaOH (aq) + KH3C3H4O4 (aq) → KNaC3H4O4 (aq) + H2O (l)

Following the standardisation of our base with KHP, we will use this standard base to
standardise our acid, giving us the exact concentrations of both solutions and allowing us to
easily titrate and analyse the unknowns.

In certain situations, chemicals would take too long to react and neutralisation to occur.
This makes it impossible to pin-point an exact amount of titrant used on the analyte in order to
calculate unknown concentrations. By the time the analyte has been neutralised, titrant added has
been in excess and the volume of titrant used is unknown. In the third experiment, antacids were
used to study the concept of back-titration as we determine the amount of acid neutralised per
gram of antacid. The antacid tablet was dissolved in a known excess amount of acid. This results
in an acidic solution because the tablet did not provide enough moles of base to completely
neutralise the acid. Then, the sample solution was titrated with a base of a known concentration
in order to determine the amount of acid not neutralised by the tablet. Lastly, the number of
moles of acid neutralised is subtracted from the moles of acid from the initial solution to find the
number of moles of acid neutralised by the antacid tablet. Back-titrations are too, one of the most
fundamental techniques in pharmacopoeial analysis and it is important to master it.

3
EXPERIMENT 1: STANDARDIZATION OF SODIUM HYDROXIDE

EXPERIMENTAL METHODS
a. Apparatus
● Burette (50 mL)
● Conical flask
● Measuring cylinder
● Retort stand and clamp
● Volumetric flask (500 mL)
● Beaker
● Filter funnel
● Dropper
● Analytical balance
● Laboratory spatula
● Weighing boat
b. Materials
● 1 M sodium hydroxide (NaOH)
● Potassium hydrogen phthalate (KHP)
● Distilled water
● Phenolphthalein indicator

c. Experiment procedures
1. 1 M NaOH was diluted enough to make 500 mL of 0.1 M NaOH. This is the
titrant. A buret was rinsed with water and then with a small amount of the 0.1 M
NaOH solution. The buret was filled with 0.1 M NaOH solution. The burret tip
was filled momentarily by opening the stopcock. The initial volume was read.
2. KHP was weighed 0.8xxxg accurately into a 250 mL conical flask. 100 mL of
water was added and the flask was swirled until the sample was dissolved. 3 drops

4
 of phenolphthalein indicator were added. (colorless in acidic solution; pink in
basic solution).
3. The KHP solution was titrated with the base solution to be standardised. Titration
should proceed until the faintest pink persists for 30 seconds after swirling.
4. Triplicate determinations were made, and the average molarity of the NaOH was
calculated.
RESULTS
Results of titration:
- Weight of KHP I: 0.824g
- Weight of KHP II: 0.810g
- Weight of KHP III: 0.804g
- Average weight of KHP: 0.813g

Reading of No. of Titration

I II III

Final reading 43 42 45

Initial reading 0 0 0

Volume of NaOH (mL) 43 42 45

Calculations
Dilution of NaOH
NaOH available: 1 M
NaOH needed: 0.1 M 500 mL
M1V1=M2V2
1(V1) = 0.1(0.5)
V1 = 0.05 L
NaoH needed = 50 mL diluted with 450 mL distilled water

Titration

5
- Equation of reaction: NaOH (aq) + KH3C3H4O4 (aq) → KNaC3H4O4 (aq) + H2O (l)
- The molarity of NaOH for each trial:
● I:
1 mol KHP = 1 mol NaOH
𝑚𝑎𝑠𝑠 (𝑔)
nKHP = 𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 (𝑔/𝑚𝑜𝑙)

0.824𝑔
= 204.22𝑔/𝑚𝑜𝑙)

= 4.034×10-3mol KHP
Since 1 mol KHP = 1 mol NaOH
nNaOH = 4.034×10-3mol
𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 (𝑚𝑜𝑙)
Molarity = 𝑣𝑜𝑙𝑢𝑚𝑒𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 (𝑙)
−3
4.034×10 𝑚𝑜𝑙
= 0.043

= 0.09381 M

● II:
1 mol KHP = 1 mol NaOH
𝑚𝑎𝑠𝑠 (𝑔)
nKHP = 𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 (𝑔/𝑚𝑜𝑙)

0.810𝑔
= 204.22𝑔/𝑚𝑜𝑙)

= 3.966×10-3mol KHP
Since 1 mol KHP = 1 mol NaOH
nNaOH = 3.966×10-3mol
𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 (𝑚𝑜𝑙)
Molarity = 𝑣𝑜𝑙𝑢𝑚𝑒𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 (𝑙)
−3
3.966×10 𝑚𝑜𝑙
= 0.042

= 0.09443 M
● III:
1 mol KHP = 1 mol NaOH
𝑚𝑎𝑠𝑠 (𝑔)
nKHP = 𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 (𝑔/𝑚𝑜𝑙)

0.804𝑔
= 204.22𝑔/𝑚𝑜𝑙)

6
 = 3.937×10-3mol KHP
Since 1 mol KHP = 1 mol NaOH
nNaOH = 3.937×10-3mol
𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 (𝑚𝑜𝑙)
Molarity = 𝑣𝑜𝑙𝑢𝑚𝑒𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 (𝑙)
−3
3.937×10 𝑚𝑜𝑙
= 0.045

= 0.08749 M
- The average of concentration of NaOH
∑𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑜𝑓 𝑁𝑎𝑂𝐻
= 3

0.09381+ 0.09443+0.08749
= 3

= 0.09191 M

Questions
1. Explain why the pink colour of a phenolphthalein endpoint will disappear after exposure
to atmospheric air (or the air we exhale). Include 2 balanced equations.
● The pink colour of phenolphthalein disappears after exposure to atmospheric air
(or the air we exhale) due to its reaction with carbon dioxide (CO2) in the air or
the air we exhale. The carbon dioxide will dissolve in the solution and react to
form carbonic acid. When sufficient carbonic acid is formed, the increased
hydrogen ions will decrease the pH value of the solution. Phenolphthalein is a pH
indicator that changes colour depending on the pH of the solution. In an acidic
solution, phenolphthalein remains colourless, while in a basic (alkaline) solution,
it turns pink or purplish.
● 2 balanced equations:
Formation of carbonic acid:
CO2 + H2O → H2CO3
Dissociation of carbonic acid in the solution:
H2CO3 → HCO3-+ H+
(Phenolphthalein become colourless due to formation of hydrogen ions and acidic
pH)

7
 2. Explain why the high molar mass of KHP is an advantage to its being used as a
primary standard.
● KHP's high molar mass means that a relatively small amount of KHP can be used
to prepare a solution of known concentration. This minimizes the potential for
weighing errors, which can be significant when dealing with very small quantities
of a substance.
● Higher molar mass compounds require smaller quantities to achieve the desired
concentration, leading to smaller absolute mass measurements. Smaller absolute
mass measurements can reduce measurement errors and greater precision in
preparing solutions.
● The high molar mass of KHP ensures that a relatively small amount of substance
is required to reach the endpoint of the titration, which helps maintain consistent
stoichiometry in the titration.

Discussion
Standardization is a process for precisely determining the concentration of a solution. The most
common method for standardizing a solution is titration. The standardization process requires a
reference standard solution. In this experiment, a titration was performed between a known
amount of titrant, KHP, and an unknown amount of analyte, NaOH. This reaction was used to
standardise NaOH and calculate its exact molarity. This had to be done correctly because the
molarity of sodium hydroxide determined would be used throughout the rest of the experiment.
Phenolphthalein was employed as an indicator to demonstrate the neutralisation of the solution.
The faintest pink will change the colorless solution to the faintest pink. This instant color change
indicated that the neutralization reaction had come to a complete stop. The titration procedure
was performed in triplicate to enhance the precision and accuracy of the obtained molarity.

8
 Figure 1: Outcome of titration between NaOH and KHP with phenolphthalein as indicator

NaOH (aq) + KH3C3H4O4 (aq) → KNaC3H4O4 (aq) + H2O (l)

From the experiment, we can calculate the molarity of NaOH from the mass of KHP. 1 mol of
KHP reacts with 1 mol of NaOH. As the titration was repeated three times, the average moles of
NaOH was 0.09191M. This experimental value obtained for the molarity of sodium hydroxide is
sufficiently close to the theoretical data of 0.1 M NaOH with a slight deviation of 0.00809 M.
Hence, there were some errors.

Some errors occurred during the titration. One of them is related to the amount of base that has
been added to determine the endpoint. While carrying out the titration, the change in colour
happened so quickly that it was often difficult to ensure the exact amount of base required was
added. Extra drops of the base could have been added in excess, affecting the result of the
experiment. Hence, titrant handling is crucial. When adding the titrant, do so slowly and
cautiously to avoid overshooting the endpoint. Parallax error might have also occurred due to the
incorrect positioning of the eyes with reference to the scale of the measuring instruments, such as
the burette or the measuring cylinder. This would eventually lead to inaccurate reading. Parallax

9
error can be minimised and prevented by placing the eyes of the observer perpendicularly to the
scale of the burette or measuring cylinder when taking readings.

10
EXPERIMENT 2: STANDARDIZATION OF HCL SOLUTION

EXPERIMENTAL METHODS
a. Apparatus
- Burette
- 250 mL conical flask
- Retort stand
- White tile/paper
- Pipette
- 100mL Beaker

b. Materials
- HCl
- Standardised NaOH (Experiment I)
- Water
- Phenolphthalein

c. Experiment procedures
1. About 50 mL of 0.1 M HCl solution was obtained in a beaker. The second buret was
rinsed with water and then with a small amount of 0.1 M HCl. The buret was filled with
0.1 M HCl solution.
2. The burette tip was filled by momentarily opening the stopcock. The initial volume was
recorded.
3. Approximately about 10 mL HCl was delivered into a clean 250 mL conical flask. 100
mL of water and 3 drops of phenolphthalein indicator were added to this sample flask.
4. The initial level in the standard NaOH buret was read. And the acid was titrated with the
NaOH standard to the faint pink endpoint.
5. The titration was repeated twice with another two samples and the average molarity of
the HCl was calculated.

11
RESULT :
Results of titration:
Molarity of standard NaOH: 0.09191 M

No. of Titration

I II III

Volume of HCl (mL) 10 10 10

Reading of Buret (mL)

Final Reading 10.5 11.5 11.5

Initial Reading 0 0 0

Volume of standard 10.5 11.5 11.5

NaOH (mL)

CALCULATION
Calculate:
1. the molarity of HCl for each trial.
M = mol/L

No. of Titration

HCl(aq) + NaOH (aq) → NaCl(aq) + H2O (l)

Trials I II III

Volume of standard 0.0105 0.0115 0.0115

NaOH (L)

Mole of NaOH (mol) 0.09191 x 0.0105 = 0.09191 x 0.0115 = 0.09191 x 0.0115 =

0.0010 0.0011 0.0011

HCl to NaOH mole 1:1 1:1 1:1

ratio

Mole of HCl (mol) 0.0010 0.0011 0.0011

Volume of HCl (L) 10/1000 = 0.01 10/1000 = 0.01 10/1000 = 0.01

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 Molarity of HCl (M) 0.0010 / 0.01 = 0.1 0.0011 / 0.01 = 0.11 0.0011 / 0.01 = 0.11

2. the average concentration of standardised HCl.

(0.1+0.11+0.11) / 3
= 0.11 M

DISCUSSION
This second experiment is about standardization of HCl. In this experiment, the standard 0.09191
M NaOH prepared from the first experiment was utilized in the titration opposition to 10 mL of
HCl added to a clean conical flask with 100 mL of distilled water and three drops of
phenolphthalein, that aims to produce standard HCl solution. The main role of phenolphthalein
here is to serve as an indicator. The titration is known to achieve its endpoint once it turns faint
pink. In this case, once the sample changed to fair pink the titration should now achieve its basic
pH since the HCl acid sample is titrated with the basic NaOH. The titration reaction can be
demonstrated in the following equation:

HCl(aq) + NaOH (aq) → NaCl(aq) + H2O (l)

What has happened in this reaction is that, when a hydroxyl (OH-) ion and an acid's hydrogen
(H+) ion come in contact, water is produced. Salt is created when the cation from the base, Na+,
interacts with the anion from the acid, Cl-. Since both NaOH and HCl are known to be a strong
base with strong acid titration, theoretically they both will undergo a complete dissociation
producing water and salt. Looking at the data recorded, for the first trial, the titration started with
NaOH volume 0 mL. Throughout the titration, it has taken 10.5 mL of NaOH for the titration to
reach its endpoint. With the known NaOH volume, the NaOH moles which is 0.0010 mol then
calculated to find HCl concentration. The balance reaction equation showing the ratio of NaOH
mol to HCl is 1:1 ratio. From the ratio, the HCl solution is known to have 0.0010 moles.
Substituting this information to the M = n/L formula, the concentration of HCl for the first trial is
calculated to be 0.1 M. The experiment then continued with the II and III trials. From these two
trials, both consumed the same amount of NaOH volume of 11.5 mL, which when calculated
using the formula, resulted in 0.11 M of HCl. Average molarity of all these trials, showing the

13
concentration of HCl used is 0.11 M which directly proves the value of molarity of HCl written
on the label. However, this experiment indeed was not flawless, looking at the inconsistent result
from the trials I to II and III, this might have been contributed by some accidental errors. The
NAOH dropped between those trials might not be consistent, as a result, the color didn’t come
out as accurate and the pink color is not consistent. Besides, The unparalleled eye level to the
meniscus leading to the error in reading and inaccurate data. The Burette is not vertically upright
to the table, so this made us read the number wrong. Therefore, precaution like reading of the eye
level to the meniscus and accurate dropping of solution is needed to obtain consistent and precise
results.

14
EXPERIMENT 3: TITRATION ANALYSIS OF UNKNOWN ACID AND
BASE

EXPERIMENTAL METHODS
a. Apparatus
- Burette
- 250 mL conical flask
- Mortar and pestle
- Retort stand
- White tile/paper
- pipette

b. Materials
- 0.65 g Antacid tablet
- Standardised HCl (Experiment II)
- Standardised NaOH (Experiment I)
- Methyl orange indicator
- Water
- Vinegar
- Phenolphthalein

c. Experiment procedures

A. Analysis of Antacid Tablet

1. An antacid tablet was obtained and weighed by the whole tablet. The tablet was then
ground with mortar and pestle. A portion of 0.6xxx-0.7xxx g was weighed.
2. The antacid sample was added to a 250mL conical flask. From the acid burrete of
Experiment II, approximately 60 mL of the standard HCl was added into the antacid
powder. The flask was swirled to dissolve the solid. However, some of the antacid tablets
did not dissolve because of the insoluble components.

15
 3. 4-5 drops of methyl orange indicator were added to the sample flask. The solution turned
pink-red since the HCl was added in excess. Some of the sample flasks stayed yellow, so
approximately 10 mL more acid was added.
4. After the antacid has neutralised a portion of the acid, we determined exactly how much
HCl was neutralised by titrating the acid left over with our standard base. The excess acid
in the flask was ‘back-titrated’ with the standard NaOH (from Experiment I). As it got
closer to the endpoint, the base was added drop by drop. The endpoint of the titration
occurred when the solution turned red to pale orange
5. The titration was repeated with another two antacid tablets.

RESULTS
1. Results of titration:
Concentration of standard HCl : 0.11 M
Concentration of standard NaOH : 0.09191 M

No. of titration

I II III

Weight of whole 0.65 0.65 0.65

antacid tablet (g)

Weight of antacid 0.640 0.691 0.602

sample (g)

Volume of HCl added 60 60 60

(mL)

Reading of buret (mL):

Final reading 7.0 21.9 39.2

Initial reading 0.0 7.0 21.9

Volume of standard 7.0 14.9 17.3

NaOH (mL)

16
CALCULATIONS

1. the mmol of HCl added,

Volume of HCl added: 60 mL = 0.06 L

Concentration of standard HCl = 0.11 M

n = MV
= (0.11 M) x (0.06 L)
−3
= 6.6 x 10 mol x 1000
= 6.6 mmol

2. The mmol of NaOH added,

● Concentration of NaOH = 0.09191 M

● 1 L = 1000 mL
● Mole = MV
● 1 mole = 1000 millimoles

No. of Titration

I II III

Volume of standard 7.0 14.9 17.3

NaOH (mL)

Mole of NaOH 0.09191 x 7.0 0.09191 x 14.9 0.09191 x 17.3

added (mmol) = 0.64 = 1.37 = 1.59

3. mmol of acid neutralised by the antacid.

● Mmol of HCl = 6.6 mmol

17
 ● Mole of acid neutralised by the antacid (mol) = mmol of HCl added - mmol of
NaOH added
● 1 mole = 1000 mmol

No of Titration

I II III

Mole of NaOH 0.64 1.37 1.59

added (mmol)

Mole of acid 6.6 - 0.64 6.6 - 1.37 6.6 - 1.59

neutralised by the
= 5.96 = 5.23 = 5.01
antacid (mmol)

4. mmol of acid neutralised per gram antacid.

No of Titration

I II III

Mole of acid 5.96 5.23 5.01

neutralised by the
antacid (mmol)

Weight of antacid 0.640 0.691 0.602

sample (g)

Mol of acid 5.96 / 0.640 5.23 / 0.691 5.01 / 0.602

neutralised per
= 9.3125 = 7.5687 = 8.3223
gram antacid
(mmol/g)

5. the average mmol acid neutralised/g antacid.

9.3125 + 7.5687 +8.3223
● 3
= 8.4012 mmol/g

18
QUESTIONS
1. Distinguish between a primary standard and a secondary standard.

Primary standards are used as reference materials in chemical analysis to accurately determine a
substance's concentration. They are extremely pure, stable, and have consistent concentrations.
Secondary standards, on the other hand, can alter in concentration over time and are less pure.
They are employed in routine measurements to determine the concentration of a drug in a sample
indirectly by comparing their characteristics to main standards. Secondary standards are made in
a lab and frequently contain impurities, which makes them somewhat reactive and hygroscopic,
whereas primary standards are usually pure, non-reactive, and non-hygroscopic.

2. How many times of its own weight could the antacid tablet consume excess stomach acid?
(Assume that stomach acid is 0.1 M HCl and that its density is 1.00 g/mL)

Average of mmol acid neutralised / g antacid = 8.4012 mmol/g

𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑚𝑜𝑙𝑒𝑠
Volume of stomach acid = 𝑚𝑜𝑙𝑎𝑟𝑖𝑡𝑦

0.0084012 𝑚𝑜𝑙
= 0.1 𝑚𝑜𝑙 / 𝐿

= 0.084012 L
= 84.012 mL

Mass of stomach acid neutralised by 1 g of antacid

= volume x density
= 84.012 mL x 1.00 g/mL
= 84.012 g ≈ 84 g
So, 1 g of antacid acid can neutralise 84 times of the stomach acid.

19
B. Analysis of Vinegar

Percent acidity is the basis for determining the legality of vinegar. The percent acid in a sample is
calculated as g/mL × 100. Vinegar is regulated by the Food and Drug Administration (FDA) and
must have a minimum of 5% acidity. The acid involved is acetic acid.

1. 5 mL of an unknown vinegar sample was pipetted into a 250 mL conical flask.

2. About 100 mL of water and 3 drops of phenolphthalein indicator were added. The sample
was titrated with the standardised NaOH (Experiment I)
3. Triplicate determinations were done.

RESULTS
Results of titration:

Volume of vinegar sample: 5 mL

Reading of buret No. of titration

(mL)
I II III

Final reading 36.0 36.0 38.2

Initial reading 0.0 0.0 0.0

Volume of standard 36.0 36.0 38.2

NaOH (mL)

CALCULATIONS

1. the average volume of base.

36.0 + 36.0 + 38.2
3
= 36.73 mL

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 2. The acidity of the vinegar is expressed as molarity.

● Molarity for NaOH = 0.09191 M

● 1 L = 1000 mL
● n = MV
● M = n/V
● Volume of vinegar sample = 5 mL = 0.005 L

No. of Titration

I II III

Volume of standard 36.0/1000 36.0/1000 38.2/1000

NaOH (L) = 0.036 = 0.036 = 0.0382

Mole of NaOH (mol) 0.036 x 0.09191 0.036 x 0.09191 0.0382 x 0.09191

= 0.0033 = 0.0033 = 0.0035

NaOH to acetic acid 1:1 1:1 1:1

mole ratio

Mole of acetic acid 0.0033 0.0033 0.0035

(mol)

Acidity of the vinegar 0.0033/ 0.005 0.0033/ 0.005 0.0035/0.005

(M) = 0.66 = 0.66 = 0.70

Average molarity of 0.66 + 0.06 + 0.70

= 0.67
3
the vinegar (M)

3. The acidity of the vinegar expressed as a percent.

● Mass = n x molar mass
● M = n/V
● Molar mass vinegar = 60.052 g/mol
● Volume of vinegar sample = 5 mL
● Acidity of the vinegar as a percent

21
 = (mass of acetic acid(g)/volume of vinegar sample (mL)) x 100% volume of
vinegar sample

No. of Titration

I II III

Mole of acetic acid 0.0033 0.0033 0.0035

(mol)

Molarity of acetic 0.0033/ 0.005 0.0033/ 0.005 0.0035/0.005

acid (M) = 0.66 = 0.66 = 0.70

Mass of acetic acid 0.0033 x 60.052 0.0033 x 60.052 0.0035x 60.052

(g) = 0.1982 = 0.1982 = 0.2101

Acidity of the vinegar 0.1982

x 100
0.1982
x 100
0.2101
x 100
5.0 5.0 5.0
as a percent (%)
= 3.96 % = 3.96 % = 4.20%

Average for acidity of 3.96 + 3.96 + 4.20

= 4.04%
3
the vinegar as a
percent (%)

QUESTIONS

1. Does the vinegar studied meet the commercial law specification of a minimum of 4 g of acetic
acid/100 mL of vinegar?

Yes. 4 g/ 100 mL means around 4% of acetic acid inside the vinegar. The calculated percentage
of acetic acid inside of the vinegar in this experiment is 4.04% which is almost exactly similar
compared to the minimum value stated in the commercial law specification.

22
DISCUSSION

Antacid tablets can be taken orally to relieve stomach acid, heartburn and indigestion.
The pharmacokinetics of antacid tablets use a simple concept of neutralisation that can be
demonstrated in the lab. Not only that, we can also investigate the exact amount of base
contained in an antacid tablet, and how potent it is once it is dissolved in the gut. These
properties of antacid tablets can be calculated and measured with a simple back-titration
technique. Your stomach acid contains H+ ions that make up for its pH.

HCl (aq) → H+ (aq) + Cl– (aq)

Any excess acid in the stomach can easily be neutralised by antacid. Common active
ingredients in antacids are metal hydroxide and metal carbonates. These hydroxide, OH- and
2–
carbonate ions, CO3 can react with H+ from stomach acid to form H2O.

Mg(OH)2 + 2 HCl Mg2+ + 2 Cl– + 2 H2O

CaCO3 + 2 HCl Ca2+ + 2 Cl– + CO2(g) + H2O

If we want to determine the potency of an antacid tablet, ie, the amount of base in one
tablet, we would ideally dissolve it in water and titrate it with acid. However, the main ingredient
of these antacids is CaCO3 which is a bit insoluble in water and can lead to inaccurate data. By
the time the tablet completely dissolves, we would have already added too much acid. This is
where back-titration is used to solve this problem. We can dissolve the tablet in a known amount
of excess acid, and be neutralised with a basic solution.

In experiment 3(A), the antacid tablets were first weighed entirely and then weighed
again after being grounded. It took three different samples of antacid tablets for us to find an
average value of these measurements in order to get a more accurate result. We used methyl
orange as an indicator as it turns pale pink in low pH and turns pale orange once the sample
reaches the equivalence point. With the standardised HCl and NaOH from experiment I and II,
we used 0.1 M of HCl and NaOH and 60 mL of HCl to dissolve the antacid tablets which should
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be in excess. After adding methyl orange in the sample solution, we observed a pale pinkish
colour on some samples. Some samples that stayed pale orange were added with 10 mL of more
HCl to ensure that excess acid is used to neutralise the antacids. After adding HCl into a beaker
containing grounded antacid tablets, the conical flask was swirled to ensure the bases in antacids
are completely neutralised by the acid. We then titrated the sample with the standardised NaOH
from experiment I until it turned from pinkish red to pale orange. Pale orange works as an
indicator that the sample has reached the equivalence point and that the excess acid has been
fully neutralised with the titrant, NaOH.

Figure 2: Before (right) and after (left) titration of antacid sample.

In Titration I, 0.64 g of ground antacid tablet was used and neutralised with 36 mL of
NaOH. The sample solution was titrated as usual and by the time the pink colour becomes paler,
we start to slow the frequency of the titration by tightening the stopcock. Since the number of
moles of base used to neutralise the excess acid in the antacid sample, we can safely conclude
that the amount of excess acid present equals to the number of moles of base used to neutralise
the excess acid. To calculate its moles, we can use the formula mole = [Concentration (M)] x
Volume (mL). Then, we can calculate the actual amount of base present in the antacid by
subtracting the total amount of acid added in the antacid tablet with the amount of base used to
neutralise the antacid sample. The titration process was repeated with the other 2 samples and
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each calculated separately to give us the average value. This was done to increase the accuracy
of the data. However, measurements and calculations done does not accurately reveal 100%
accuracy even after repetition due to several errors that occurred while conducting this
experiment.

Figure 3: Titration of the antacid sample right when reaching the equivalence point

Several errors can occur during this experiment that might have affected the accuracy of
the data. First of all, parallax error can occur when taking measurements, especially when taking
measurements of the burette since the burette is a very tall apparatus. This error should be
avoided by lowering the burette’s level and making sure that the level of the eye is always
perpendicular to the reading scale. Next, while conducting the titration, there could have been
leaks of the titrant from the burette while controlling the stopcock. This can greatly affect the
volume of the titrant used and thus affect the calculations. Lastly, when grinding the antacid
tablets, contaminants may also affect the purity of the sample, thus altering its pH or volume.
This error however, is a bit negligible and did not really affect our calculations.

Next, experiment 3B was conducted to verify the percentage of acetic acid inside vinegar
using the concept of acid-base titration. Using the usual neutralisation reaction, we were able to

25
determine the concentration of acetic acid inside the vinegar by titrating the acid using NaOH.
The H+ from acetic acid reacts with the OH- from NaOH to produce H2O. The chemical formula
involved in this reaction is;

H+(aq) + OH- (aq) → H2O(l)

CH3COOH(aq) + NaOH(aq) --> CH3COONa(aq) + H2O(l)

By using phenolphthalein indicator, we were able to find out the exact amount of NaOH
needed to neutralise acetic acid when the solution changed from colourless to pink indicating that
the pH of the analyte has increased. After all 3 repeated tests, we were able to obtain the
percentage of acetic acid inside 100 mL of vinegar by using 5 mL of sample commercial vinegar.
The percentage that we have obtained was 4.04% acetic acid which meets the commercial law
specification. As usual, every experiment has its flaws and the measurements we did in every
trial were not the same due to certain errors. The tools that we have used might have caused the
errors in the readings and then implemented them in the calculation. This issue, however, can be
reduced by limiting the transfer of solution from one apparatus to another. Next, parallax error
can be avoided by making sure the level of the eye is perpendicular to the measurement scale and
that the apparatus was placed on a flat surface. All in all, we have obtained the desired data that
matches with its theoretical value.

CONCLUSION

In conclusion, the two experiments aimed to determine the concentration of NaOH and
standardise HCl have provided valuable insights into the precision and accuracy of titration
methods. Both NaOH and HCl were successfully standardised in the both experiments,
producing a molarity value that was quite similar to the predicted results. Minor mistakes, like
overshooting the endpoint during the titration, were recognised, albeit they can be reduced with
caution while handling the titrant. Even though there were some differences across the trials, it's
important to remember that they were probably caused by reading mistakes and differences in
titrant drop sizes. All things considered, these studies highlight how important precise titration
techniques are for figuring out solution concentrations.

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 When direct titration does not give the optimal results for neutralisation, another
technique of analysing drug compounds is back-titration. Back-titration proves to be a useful
mechanism that solves the problem of testing the pH of insoluble compounds, especially that
many drugs use plenty of insoluble ingredients. A simple concept of neutralisation between acid
and base effectively explains how back-titration works which we have successfully mastered by
making calculations in the results section. Lastly, we can also see that acid-base titration can be
used to analyse the amount of an active ingredient present in drugs or food. For example, we can
use this method to determine the percentage of acetic acid in vinegar. This concept proves to be
useful in future career settings especially in drug safety and efficacy scope. For example, we can
see how efficacious and safe antacid tablets are by performing this experiment and making sure
that the sample complies with the law and regulations. It is very impressive to see how a simple
concept in chemistry can solve a lot of problems in drug formulations and analysis.

REFERENCES

1. Salisbury BH, Terrell JM. Antacids. [Updated 2023 Aug 8]. In: StatPearls [Internet].
Treasure Island (FL): StatPearls Publishing; 2023 Jan-. Available from:
https://www.ncbi.nlm.nih.gov/books/NBK526049/

2. University of California. (2011). Lab 4 - Determination of the Amount of Acid

Neutralized by an Antacid Tablet Using Back Titration. Www.webassign.net.

https://www.webassign.net/labsgraceperiod/ucscgencheml1/lab_4/manual.html

3. Yulian, A., Yunita, B. R., Nadia, D., Afifah, F. N., Kanza, F. P., Trianingsih, F., & Putri,

G. E. A. (2023). Analysis of antacid tablets using the alkalimetric titration method. Asian

Journal of Analytical Chemistry, 1(1), 25-31.

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 4. Mahar, S. (2022, June 3). What Is Standardization In Chemistry? We Study Here.

Retrieved November 7, 2023, from

https://westudyhere.com/what-is-standardization-in-chemistry/

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