Experiment 3 Acid and Base Titration

Аnаlyticаl Chemistry
MALAYAN COLLEGES LAGUNA

Lаborаtory
CHE130L
EXPERIMENT NO. 3
ACID- BASE TITRATION
I. OBJECTIVES
Upon completion of the experiment, the student should be able to:
 prepare standard solutions of NaOH and HCl;

 standardize the acid and base solution;
 determine the equivalent weight of an unknown acid; and
 apply the various techniques involved in the preparation of solutions, standardization of
solutions, comparison of solutions, and analysis of unknown solutions for acid-base
titrations.
II. A. LABORATORY EQUIPMENT / INSTRUMENTS
Equipment/ Accessories Quantity

50 mL beaker 2
250 mL Erlenmeyer flask 2
500 mL volumetric flask 1
Glass funnel 2
Analytical balance 1
Buret holder 2
50 mL buret 2
125 mL Erlenmeyer flask 2
25 mL volumetric pipet 1
Stirring rod 1
Iron stand 1
B. CHEMICALS AND REAGANTS
Chemical/ Reagent
NaOH pellets
1.0 M HCl
Phenolphtalein
Distilled water in wash bottle
Potassium acid phthalate (KHP, FM=204.2 g/mol)
Unknown acid
Experiment 3: Acid and Base Titration Page | 1

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EXPERIMENT NO. 3
III. DISCUSSION OF FUNDAMENTALS
Introduction
There are many types of volumetric analyses in the study of analytical chemistry. One of the
most common and easiest methods is titration/ titrimetry. This process involves an analyte of
unknown concentration, and a titrant, that usually has a known concentration. One of the best
working formulas for this is the dilution equation, which is; ,(Formula 1) wherein C1 is
the molarity of the titrant, V1 the volume of the titrant that is used to complete the reaction, V2 the
volume of the analyte which has an unknown concentration, and C2, which is what is usually the
unknown. In titrimetry there are also lots o types, and in this experiment, we are focusing on acid-
base reactions. The reaction involves mainly a base and an acid, from which either one has a known
concentration. Certain procedures must be followed in the process of acid-base titrations, such as
standardization of the acid/base solution, most laboratory techniques, etc. etc.
General Description
Titration or titrimetric analysis is a method of slowly adding a titrant, usually of known

concentration to an analyte to determine the amounts for a complete reaction (Figure 1, Hage and
Carr 2011). Titration reactions are used for a number of purposes such as standardization,
determination of amounts of analyte present in samples, and determining identities of unknown
samples. An acid-base titration involves reactants which are acids and bases.
The amounts of reactants needed to have a complete reaction are referred to as the
stoichiometric amounts. In titration, this is referred to as the equivalence point, meaning that at this
point, equivalent amount of the titrant has reacted to an equivalent amount of the base. Acid-base
reactions do not show visible physical changes when products are formed (i.e. do not form solids
nor vapors, nor show changes in temperature) and thus the equivalence point is difficult to
determine. In this regard, aside from the acid and base, another important component of an acid-
base titration is an acid-base indicator. The acid-base indicator changes its color upon adding a very
slight excess of the titrant. This amount is a visual and experimental estimate of the equivalence
point and is termed as the end point (Hage and Carr 2011). Another method that is used to
determine the end point is to use a pH meter to monitor pH of the solution as the volume of added
titrant changes and plotting these values to obtain a titration curve (Figure 1, Hage and Carr 2011).

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CHE130L
EXPERIMENT NO. 3
Figure 1. Typical Titration set-up and a sample of titration curve
Since the most usual application of acid-base reaction is determining the amount or
concentrations of analytes, one of the reacting solutions should be of known concentration. The
method of determining the exact concentration of standard solutions is referred to as
standardization. The method makes use of a solid pure substance, a primary standard to determine
the exact concentration of a secondary standard solution. Concentrations of solutions can be
expressed in units of molarity (moles solute/liter of solution) or normality (equivalents solute/liter of
solution).
Theory
Titrations, from French origins ‘titre’ means rank, and from the Latin word ‘titulus’, it means
title. It generally means that titration is the determination of the rank of concentration of the

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CHE130L
EXPERIMENT NO. 3
solution, with water as a reference with a rank of pH 7. The analyte is the one being known of its
rank, and the titrant is the one who will determine this rank.
Titrimetry is based on how certain reactions will proceed, so therefore not all reactions can be
considered to be used in a titration process. A type of reaction can be used in a titration process if it
is: has a fast rate of reaction; it proceeds in a stoichiometric way (meaning, the moles of the
unknown can be compared with that on the known substance); there is a known or a visual way of
detecting the completion of the said reaction, and; if the free energy (Gibbs energy, represented by
) is large enough to make the reaction spontaneous.
For this specific instance, we are talking about acid-base titrations. The chemical reaction that is
involved between acids and bases are called as neutralization reactions, from which the product is a
salt, and a by-product of water. The water is produced by combining the hydrogen (hydronium) ions
present in the acid, to the hydroxide ions present in the base. By knowing the concentration of an
acid using a standardized basic solution is called as alkalimetry, and the other way around we call it
acidimetry.
In an acid-base reaction, a stage which shows its completion is known as end point. Equivalence
point is a stage from which the amount of the titrant (since we are talking about titrations) added is
exactly and by stoichiometric basis, it is equivalent to the amount of the analyte in the titrated
solution. The end point is detected by some visual changes, but if there are no visual changes
present, an addition of an auxiliary reagent known as an 'indicator' will be very much needed. An
indicator is a chemical reagent that is added to the analyte before the reaction is initialized, to
recognize the completion of the titration/reaction. When the reaction is complete, it significantly
gives off a recognizable color change. For a neutralization reaction, a pH indicator is needed, i.e.
phenolphthalein. The end point and the equivalence point may not be identical. End point is usually
detected only after adding a slight excess of the titrant, but the equivalence point is the true
completion of the reaction.
Application
Some applications of acid-base titrations would be:

 Creating household items
 Chemical Industry
 An important technique, titrating and back-titrating knowledge is very useful for a chemist
 Balancing the pH of food, fertilizers, and the like.

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EXPERIMENT NO. 3
IV. METHODOLOGY
The first step was the cleaning of the

buret, which was checked of leaks
and was then rinsed with small The cooled solution was quantitavely
amount of the titrant. After, it was transferred into a 500-mL volumetric
filled with the titrant up to the zero flask.
mark.
The solution was diluted with distilled

NaOH pellets needed to prepare 500-
water up to the mark and was mixed
mL of 0.05M NaOH were fetched
by shaking.
from the prep room and the mass
was calculated.
The softdrink bottle was rinsed with

small portions of the NaOH solution.
In a 50-mL beaker, the required
The NaOH remaining was transferred
amount of NaOH pellets was weighed
to this softdrink bottle.
in a balance.
The NaOH pellets were dissolved in The bottle was labelled with the
water under the fumehood. concentration, date of preparation
and the name of the group who
prepared the solution.
The beaker was cooled by placing it Figure 2. Buret cleaning and preparation of
standard NaOH solution.
under running water, careful of not
getting any inside the beaker.

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EXPERIMENT NO. 3
The amount of 1.0M HCl needed to

prepare 500-mL of 0.05M HCL
solution was calculated.
This was diluted with distilled water
until the mark and was shake very
well.
A 500-mL volumetric flask was filled

with 250-300 mL distilled water.
The softdrink bottle was rinsed with

small portions of the HCl solution.
The HCl remaining was transferred to
Using a volumetric pipet, calculated this softdrink bottle.
volume was was transferred to the
500-mL volumetric flask. This was
done under the fumehood.
The bottle was labelled with the

concentration, date of preparation
Figure 3. Preparation of standard HCl solution
and the name of the group who
prepared the solution.

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CHE130L
EXPERIMENT NO. 3
Accurately 0.25g KHP (previously

dried at 105C for one hour) into a
labeled Erlenmeyer flask was
weighed. The final volume reading in your
buret was recorded.
It was dissolved in about 50 mL

distilled water. The normality of the standard NaOH
solution was calculated into the
proper number of significant figures
for each trial.
2 to 3 drops of phenolphthalein
indicator was added when the
solution was at room temperature.
The average normality and the

average deviation were computed
using the average normality for
The buret was filled with the titrant
succeeding calculations.
up to the zero-mark. Initial volume
reading in the buret was recorded.
The standard NaOH solution was kept

for future use.
The KHP solution was titrated with
the 0.05 M NaOH solution to the faint Figure 4. Standarization of NaOH solution
pink endpoint.

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EXPERIMENT NO. 3
One buret was filled with the

standard HCl solution and another
with the standard NaOH solution. The volume used was calculated up to
the proper number of significant
figures.
The initial volume reading in each
buret were both recorded.
The ratio of strengths of the acid and
base was calculated.
From the buret, 25 mL of HCl was

delivered into an Erlenmeyer flask. The average ratio for each of the
This was done in two trials. solutions was calculated.
About 20 mL distilled water was The volume data from this part and
added into the Erlenmeyer flask along the average normality for the NaOH
with 2 -3 drops of phenolphthalein. solution (from Part IV) was used to
calculate the concentration of
standard HCl solution for the two
The HCl solution was titrated with the trials.
NaOH solution up to the first faint
pink endpoint. Near the endpoint,
The average normality and the
titrate dropwise and at the endpoint,
average deviation were calculated
split drops.
and the average normality was used
for succeeding calculations
The final volume reading in your

buret was recorded. The standard HCL solution was kept
for future use.
Figure 4. Comparisons of standard solutions

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CHE130L
EXPERIMENT NO. 3
0.10 g of the unknown acid was

accurately weighed into a labeled
Erlenmeyer flask. This was done in
two trials.
About 50 mL distilled water was

diluted and added 2-3 drops of
phenolphthalein indicator.
The unknown acid solution was

titrated with the standard NaOH
solution up to the faint pink endpoint.
Calculate the equivalent weight of the

unknown acid for each trial and the
average EW.
Figure 5. Determination of equivalent weight of unknown acid

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EXPERIMENT NO. 3
V. DESCRIPTION OF THE APPARATUS / SET – UP
Figure 2. Burette Figure 2.1 Burette with labels
A burette (commonly spelled as buret), is a laboratory apparatus that is mainly used for
quantitative chemical analyses of liquids. It consists of a long, graduated glass tube with a stopcock
(in a liquid burette’s case, on the bottom) that is handled by a burette clamp, which is connected to
an iron stand. The volume that the burette dispenses is controlled by the stopcock, and is accurately
measured by the graduations of the glass tube.

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EXPERIMENT NO. 3
VI. DATA SHEET
A. PREPARATION OF STANDARD SOLUTIONS
Table 1. NaOH Standard solution

Condition Data
Mass of NaOH pellets 1.04 g
Total volume of solution 500 mL
Table 2. HCl Standard Solution
Condition Data
Volume of concentrated HCl solution 25 mL
Total volume of solution 500 mL
B. STANDARDIZATION OF NaOH SOLUTION
Table 3. Standardization of NaOH Solution
Conditions Trial 1 Trial 2
Primary standard
Weight of flask, g
TARED
Weight of flask + KHP, g
Weight of KHP, g 0.25 g 0.25 g
NaOH solution
Final volume reading, mL 24.5 mL 24.4 mL

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EXPERIMENT NO. 3
Initial volume reading, mL 0.00 mL 0.00 mL
Volume used, mL 24.5 mL 24.4 mL
Normality of NaOH solution 0.04997 N 0.05017 N
Average N  average d 0.05007 N
C. COMPARISON OF STANDARD SOLUTIONS
Table 4. Volume Ratios of Standard Solutions
HCl solution
NaOH solution
Ratios
1.000 mL HCl ___0.712__ mL NaOH ___0.728_ mL NaOH
Average  average d 0.720 mL
1.000 mL NaOH __1.404___ mL HCl __1.374_ mL HCl
Average  average d 1.389 mL

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EXPERIMENT NO. 3
Normality of HCl solution 0.0356 N 0.0365 N
Average N  average d 0.03605 N
D. DETERMINATION OF EQUIVALENT WEIGHT OF UNKNOWN ACID
Table 5. Determination of equivalent weight of unknown acid
Unknown Number G H
Mass of unknown 0.100 g 0.102 g
Weight of flask, g
TARED
Weight of flask + unk acid, g
Weight of unk acid , g 0.100 g 0.102 g
NaOH solution
Equivalent weight 58.74 g/mol 59.74 g/mol
Average EW  d 59.24 g/mol
Probable identity of acid Glacial acetic acid (60.05 g/mol)

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EXPERIMENT NO. 3
VII. SAMPLE COMPUTATIONS
11.1 ( )( )
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VIII. RESULTS AND DISCUSSIONS
The common unit used for expressing a solution’s concentration is molarity (M) or molar
concentration. It is defined as the number of moles of solute per liter of solution. The concentration
of a basic solution is determined, one way, by titrating it with a known volume of a standard acid
solution of known concentration required to neutralize it. The main purpose of titration is the
detection of the equivalence point of the solution with unknown concentration. The equivalence
point is the point at which chemically equivalent amounts of the reactants have been mixed. The
amount of reactants mixed at the equivalence point depends on the stoichiometry of the reaction.
A known method for determining either the concentration of a solution of unknown molarity or
the number of moles of a substance in a given sample is titration. A chemical reaction is used for this
purpose, and the reaction must be fast, complete, and have a determinable end point. Reactions of
strong acids and bases meet these criteria generally, and acid-base titrations are among the most
important examples of this method.

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EXPERIMENT NO. 3
In the neutralization reaction of HCl and NaOH, the equivalence point occurs when one mole of
HCl reacts with one mole of NaOH. Using an indicator such as phenolphthalein helps to determine
when neutralization occurs. Phenolphthalein (C20H14O4) is an example of a substance which
undergoes a distinct color change at or near the equivalence point. It changes its color to light pink
at pH range 8.2-10.0. The point at which the indicator changes color and the titration is stopped is
called the endpoint. Ideally, the endpoint should match with the equivalence point. Phenolphthalein
is colorless in acidic solution and reddish violet in basic solution.
The experiment was started off with cleaning of the glasswares and rinsing of the buret with the
titrant. This is done so that the buret will be clean of the titrant last used by students before us.
After rinsing, there came the preparation of the standard NaOH solution, which proved challenging
because filling the volumetric flask to the mark without very precise control took time. Too much
distilled water won’t do so the whole method will have to be done again. Using stoichiometry, the
amount of 1.0M HCl to prepare 500-mL HCl solution was determined. Same method as the
preparation of the NaOH solution, the HCl was diluted with distilled water and was kept of future
use.
The standardization of the NaOH solution part was where the titration was done. Acid-base
titration involves a chemical reaction known as a neutralization reaction. Titrations allow the
accurate determination of concentrations of unknown acids/bases. Analyzing unknown acids/bases,
a "standard" solution is needed to react with the unknowns. Making a standard solution requires
dissolving an accurately weighed amount of the substance and diluting it to an accurately measured
volume. Having these given, the molar concentration can be calculated exactly. But, getting NaOH of
sufficient purity to use as a primary standard is usually difficult. Obtaining a standard solution of
NaOH using an indirect method is more practical. A solution of an approximate molarity was
prepared and standardized against a primary standard of known purity. A KHP (potassium hydrogen
pthalate) solution of known molarity was titrated to its endpoint using the standard NaOH solution,
to know whether the pH of the prepared standard was accurate.
KHP, a large compound (KHC8H4O4) having a molecular mass of 204.2 g/mol, served as the
primary standard. It is a monoprotic acid and reacts with NaOH in a simple 1 to 1 relationship
according to the following equation:
NaOH(aq) + KHC8H4O4(aq) ---> KNaC8H4O4(aq) + H2O(l)

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EXPERIMENT NO. 3
After standardizing the base with potassium hydrogen pthalate, the standard base was used to
standardize the acid to know the concentrations of both solutions for the titration and analysis of
the unknowns.
IX. SUMMARY AND CONCLUSIONS
This experiment thoroughly explained us the acid-base reactions in actual, which is in the
process of titration. By theory, when an acid is combined with a base that is compatible with each
other, it will react to reach as what we call an ‘equivalence point’, from where the moles of the
analyte is equal to the moles of the titrant. This is commonly known as neutralization. But to do this,
one must need to have a standardized solution of either an acid or the base, whichever it is that is
known. Standardization is done to produce accurate results. Once the solution was standardized, we
can now begin the titration process. But in the process, the salt that forms during neutralization is
the only visual presence of reaching equivalence point, which is usually at a disadvantage since
these salts are always colorless, and is dissolved to water, its by-product. To prevent this, one must
add an indicator to the analyte, a chemical that changes in color from when the desired pH level is
reached, or when the reaction has reached it equivalence point. Regardless to say, by using the
dilution equation we can solve for the concentration of the analyte, with a known volume.
All in all, acid-base titrations can be a powerful tool for knowing certain acid-base reactions, for
knowing the concentrations of a base or an acid, as long as the titrant is standardized, to ensure
accuracy and precision of results.
X. POST LAB QUESTIONS
Post lab Q1. Will the volume used for titration be affected if the volume of water used to dissolve
the KHP is increased to 75mL distilled water? Why or why not?
Answer: No, the concentration of the acid would be the same since we will only convert the
moles of KHP, whereas it the same as converting the grams of KHP to molarity KHP, then turning
it to moles KHP by multiplying it to the volume, cancelling both figures.
Post lab Q2. What is the ideal volume used for one trial of titration? Explain your choice in terms of
precision of measurements. Using this volume, what mass of KHP must be used to standardize a
solution of approximately 0.035 M NaOH?
Answer: By computing the average of our experiments, the ideal volume for titration is
supposed to be 24.45 mL. Using this volume, we compute:

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CHE130L
EXPERIMENT NO. 3
( )( )( )
XI. REFERENCES
Christian, Gary D. 2004. Analytical chemistry (6th ed.). John Wiley and Sons Inc.
Hage, David S. and James D. Carr. 2011. Analytical chemistry and quantitative analysis. New
Jersey: Pearson Prentice Hall.
Skoog, Douglas et. al. 2004. Fundamentals of Analytical Chemistry (8th ed.). Singapore:
Thomson Learning.

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Аnаlyticаl Chemistry

MALAYAN COLLEGES LAGUNA

Upon completion of the experiment, the student should be able to:

 prepare standard solutions of NaOH and HCl;

II. A. LABORATORY EQUIPMENT / INSTRUMENTS

Equipment/ Accessories Quantity

B. CHEMICALS AND REAGANTS

Experiment 3: Acid and Base Titration Page | 1

III. DISCUSSION OF FUNDAMENTALS

Titration or titrimetric analysis is a method of slowly adding a titrant, usually of known

Experiment 3: Acid and Base Titration Page | 2

Figure 1. Typical Titration set-up and a sample of titration curve

Experiment 3: Acid and Base Titration Page | 3

Some applications of acid-base titrations would be:

Experiment 3: Acid and Base Titration Page | 4

The first step was the cleaning of the

The solution was diluted with distilled

The softdrink bottle was rinsed with

Experiment 3: Acid and Base Titration Page | 5

The amount of 1.0M HCl needed to

A 500-mL volumetric flask was filled

The softdrink bottle was rinsed with

The bottle was labelled with the

Experiment 3: Acid and Base Titration Page | 6

Accurately 0.25g KHP (previously

It was dissolved in about 50 mL

The average normality and the

The standard NaOH solution was kept

Experiment 3: Acid and Base Titration Page | 7

One buret was filled with the

From the buret, 25 mL of HCl was

The final volume reading in your

Figure 4. Comparisons of standard solutions

Experiment 3: Acid and Base Titration Page | 8

0.10 g of the unknown acid was

About 50 mL distilled water was

The unknown acid solution was

Calculate the equivalent weight of the

Figure 5. Determination of equivalent weight of unknown acid

Experiment 3: Acid and Base Titration Page | 9

V. DESCRIPTION OF THE APPARATUS / SET – UP

Figure 2. Burette Figure 2.1 Burette with labels

Experiment 3: Acid and Base Titration Page | 10

VI. DATA SHEET

A. PREPARATION OF STANDARD SOLUTIONS

Table 1. NaOH Standard solution

Total volume of solution 500 mL

Table 2. HCl Standard Solution

Volume of concentrated HCl solution 25 mL

Total volume of solution 500 mL

B. STANDARDIZATION OF NaOH SOLUTION

Table 3. Standardization of NaOH Solution

Conditions Trial 1 Trial 2

Weight of KHP, g 0.25 g 0.25 g

Final volume reading, mL 24.5 mL 24.4 mL

Experiment 3: Acid and Base Titration Page | 11

Initial volume reading, mL 0.00 mL 0.00 mL

Volume used, mL 24.5 mL 24.4 mL

Normality of NaOH solution 0.04997 N 0.05017 N

Average N  average d 0.05007 N

C. COMPARISON OF STANDARD SOLUTIONS

Table 4. Volume Ratios of Standard Solutions

Conditions Trial 1 Trial 2

1.000 mL HCl _0.712 mL NaOH ___0.728_ mL NaOH

1.000 mL NaOH 1.404_ mL HCl __1.374_ mL HCl