Chapter 19

Volumetric analysis involving acids

and alkalis
19.1 Standard solutions
19.2 Acid-alkali titrations
19.3 Calculations on volumetric analysis
19.4 Writing a laboratory report on volumetric
analysis
Key terms
Progress check
Summary
Concept map
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19.1 Standard solutions
A solution of accurately known molar
concentration or molarity is called a standard
solution.

Key point
A _________
standard solution is a solution of accurately
known molar concentration or molarity.

Concept check

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Apparatus for preparing standard solutions
Name Use
1. Weighing bottle It is used to hold the
(a) Glass weighing bottle sample to be
(b) Plastic weighing bottle weighed.
cap cap

(a) (b)
Table 19.1 Names and uses of the apparatus commonly used in the
preparation of standard solutions.
19.1 Standard solutions

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 Name Use
2. Electronic balance It is used to weigh
the solid quickly and
accurately (accuracy
up to (a) 0.01 g or
(b) 0.0001 g).

(a) (b)
Table 19.1 Names and uses of the apparatus commonly used in the
preparation of standard solutions.

19.1 Standard solutions

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 Name Use
3. Volumetric flask It is used to make up
a solution to a
specific volume (e.g.
250.0 cm3)
accurately.
* Before use, rinse
the volumetric flask
with distilled water.

Table 19.1 Names and uses of the apparatus commonly used in the
preparation of standard solutions.

19.1 Standard solutions

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 Name Use
4. Pipette It is used to deliver a
specific volume (e.g.
25.0 cm3) of a
solution accurately.
* Before use, rinse
bulb the pipette with
distilled water, then
with the solution it
is going to deliver.

Table 19.1 Names and uses of the apparatus commonly used in the
preparation of standard solutions.

19.1 Standard solutions

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 Name Use
5. Pipette filler It is used to suck up
(a) The simple type a solution into a
(b) The traditional type with valves pipette.
* As a safety
precaution, always
fill a pipette with a
valves pipette filler. Do NOT
use your mouth.

Table 19.1 Names and uses of the apparatus commonly used in the
preparation of standard solutions.

19.1 Standard solutions

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 Name Use
6. Beaker It is used to hold
solutions.

Table 19.1 Names and uses of the apparatus commonly used in the
preparation of standard solutions.

Class practice 19.1

19.1 Standard solutions

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Preparing standard solutions
Primary standard
A primary standard is a substance which can be
used to prepare a standard solution directly.

Learning tip
Only very few substances can be used as a
primary standard. Examples include anhydrous
sodium carbonate and oxalic acid crystals.

19.1 Standard solutions

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A good primary standard should have the following
properties:
readily available with high purity
chemically stable (should not react with
oxygen, carbon dioxide and water vapour in air)
high solubility in water
does not absorb water vapour from air.
does not lose water of crystallization to the
atmosphere on exposure to air if it is a
hydrated substance
involatile and non-toxic Example 19.1

19.1 Standard solutions

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Preparing a standard solution by dissolving a pure solid

Steps for preparing 250.0 cm3 of an approximately

0.10 M sodium carbonate solution

Stage A: Weighing the pure solid

1. Calculate the mass of anhydrous sodium carbonate
required.
Mass of Na2CO3 required
= number of moles of Na2CO3 × molar mass of Na2CO3
–3 250.0
= 0.10 mol dm × dm3 × 106.0 g mol–1
1000
= 2.65 g
19.1 Standard solutions

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2. Use an electronic balance to weigh out accurately
the required mass of anhydrous sodium carbonate.

anhydrous sodium weighing bottle

carbonate

Figure 19.1 Steps for preparing a

standard solution by dissolving a electronic
pure solid in distilled water. balance
(1) and (2)

SBA note
Do not waste time trying to weigh out exactly 2.65 g
of the solid. However, the mass weighed out should
be accurate (e.g. to be at least 0.01 g).
19.1 Standard solutions

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Stage B: Dissolving the pure solid
3. Dissolve the solid in about 100 cm3 of distilled water
in a beaker. Stir the solution with a glass rod.

100 cm3 of
distilled water
glass rod

beaker

anhydrous sodium sodium carbonate

carbonate solution

(3)

19.1 Standard solutions

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Stage C: Making up the solution to 250.0 cm3 in a
volumetric flask
4. Pour the solution to a 250.0 cm3 volumetric flask
through a filter funnel.
glass rod

sodium carbonate
solution
filter funnel

volumetric flask
(250.0 cm3 type)

(4)
19.1 Standard solutions

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5. Wash the beaker and the glass rod with distilled
water several times. Pour all the washing to the
volumetric flask.

washing distilled
plastic
water
wash bottle

distilled
water

sodium
carbonate
solution

(5)
19.1 Standard solutions

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6. Add distilled water to the volumetric flask but stop
about 2 cm below the graduation mark.
7. Use a dropper to add distilled water until the bottom
of the meniscus reaches the graduation mark.

beaker dropper
distilled distilled
water water
250.0 cm3
graduation
mark

(6) (7)
19.1 Standard solutions

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8. Stopper the flask and invert it several times to mix
the contents well.

invert it
several times

stopper

meniscus

standard sodium
carbonate solution
(8)
Example 19.2

19.1 Standard solutions

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Preparing a standard solution by diluting a
concentrated solution of known molarity
Steps for preparing 250.0 cm3 of 0.0120 M sodium
carbonate solution from
0.120 M sodium carbonate solution

1. Calculate the volume of the original solution required

for dilution.
number of moles of Na2CO3 = number of moles of Na2CO3
before dilution after dilution
M1V1 = M2V2
V1
0.120 × = 0.0120 × 250.0
1000 1000
∴ V1 = 25.0 cm3
19.1 Standard solutions

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 2. Use a pipette to transfer 25.0 cm3 of the original
solution to a 250.0 cm3 volumetric flask.
pipette meniscus
filler 0.120 M
sodium
carbonate
25.0 cm3 25.0 cm3 solution
pipette pipette

250.0 cm3
0.120 M sodium volumetric
0.120 M sodium
carbonate solution flask
carbonate solution

(1) and (2)

Figure 19.1 Steps for preparing a standard solution by diluting a
concentrated solution.
19.1 Standard solutions

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 SBA note
You should use the index finger instead of the thumb
to control the flow of solution in a pipette.

19.1 Standard solutions

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3. Add distilled water to the volumetric flask but stop
about 2 cm below the graduation mark.
4. Use a dropper to add distilled water until the bottom
of the meniscus reaches the graduation mark.
beaker
dropper
distilled distilled
water water
250.0 cm3
graduation
mark

(3) (4)
19.1 Standard solutions

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5. Stopper the flask and then invert it several times to
mix the contents well.
invert it
several times
stopper

meniscus

0.0120 M sodium
carbonate solution
(5)

Example 19.3 Class practice 19.2 Experiment 19.1

Example 19.4 Experiment 19.1

19.1 Standard solutions

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19.2 Acid-alkali titrations
Volumetric analysis and titration

Volumetric analysis
is a method to determine the amount (or
concentration) of a substance in a sample.

requires the measurement of volumes of the

solutions involved.

is also known as titrimetric analysis as it is

done by titration.

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Titration is an experimental technique used for
determining the amount (or concentration) of a
substance in a solution.
In a titration, a solution of known concentration (i.e.
a standard solution) is slowly added to another
solution of known volume, until the two solutions
have just reacted completely.

19.2 Acid-alkali titrations

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Apparatus for titration
Name Use
1. Burette It is used to deliver
variable volumes (ranging
from 0.05 to 50.00 cm3) of
a solution accurately.
* Before use, rinse the
stopcock burette with distilled
water and then with the
solution it is going to
deliver.

Table19.2 Names and uses of some apparatus used in acid-alkali titration.

19.2 Acid-alkali titrations

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 Name Use
2. Conical flask It is used to hold a
solution to be titrated. Its
conical shape allows it to
be swirled gently without
spilling out the solution.
* Before use, rinse
the conical flask with
distilled water.

Table19.2 Names and uses of some apparatus used in acid-alkali titration.

19.2 Acid-alkali titrations

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 Name Use
3. Stand and clamp They are used to support
the burette.

Table19.2 Names and uses of some apparatus used in acid-alkali titration.

19.2 Acid-alkali titrations

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 Name Use
4. White tile It is used to allow clear
observation of the colour
change of the indicator.

Table19.2 Names and uses of some apparatus used in acid-alkali titration.

19.2 Acid-alkali titrations

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Procedure for acid-alkali titration
A standard solution of an acid (or an alkali) is
slowly added to a known volume of a solution of
an alkali (or an acid), until the acid and alkali have
completely reacted with each other.
The stage at which the acid and the alkali have
just reacted completely during titration is called the
equivalence point.
Learning tip
The procedure for an acid-carbonate (e.g. HCl and
Na2CO3) titration is more or less the same as that
for the acid-alkali titration.
19.2 Acid-alkali titrations

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 Key point
The equivalence point of an acid-alkali titration is
the point at which an acid and an alkali have just
completely reacted with each other.
__________

The equivalence point of an acid-alkali titration

can be estimated by using a pH meter or a data-
logger connected with a pH sensor.

It is not possible to detect the equivalence point

using an acid-base indicator.

19.2 Acid-alkali titrations

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During the acid-alkali titration, a suitable acid-base
indicator is usually added.

The colour of the indicator changes sharply at or

very near the equivalence point, then the end
point of titration is reached.

Key point
End point is the point at which the indicator
__________
changes colour sharply.

19.2 Acid-alkali titrations

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Detection of end point by using an acid-base indicator
1. Fill the 25.0 cm3 pipette (using a pipette filler) with
the alkali until the graduation mark is reached.
Transfer 25.0 cm3 of the alkali to a conical flask.
meniscus

25.0 cm3 alkali

alkali pipette

conical flask
(1) alkali
Figure 19.3 Procedure for performing an acid-alkali titration.
19.2 Acid-alkali titrations

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2. Fill the burette with the acid. Make sure that the jet
is filled completely (no air bubbles inside the jet).
stand

acid
clamp
burette

white tile
(2)
Learning tip
The solution in the burette is often known as titrant.
19.2 Acid-alkali titrations

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3. Add a few drops of an acid-base indicator to the
alkali. Note the colour of the solution.
4. Take the initial burette reading, with your eyes on
the same level as the meniscus.

indicator
meniscus eye at
read as 0.6 cm3
proper
level
alkali
(3) (4)

19.2 Acid-alkali titrations

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5. Slowly add the acid to the alkali until the mixture
just turns to another persistent colour. This is
the end point of titration.

burette

acid

solution mixture
+ indicator
(5)
19.2 Acid-alkali titrations

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6. Take the final burette reading. Calculate the
volume of the acid added to reach the end point.

7. Repeat the titration (steps 1 to 6) at least three

times, until we get three sets of data for
calculating the average volume of the acid used.

Learning tip
The volume of titrant used to react completely with
the solution in the conical flask is called titre.

Skill corner 19.1 Example 19.5 Class practice 19.3

19.2 Acid-alkali titrations

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Choosing a suitable acid-base indicator
Methyl orange and phenolphthalein can give a
sharp colour change at the end point of titration.
Litmus is not used because it does not give a
sharp colour change.
methyl orange phenolphthalein

(a) pH = 2 pH = 12 (b) pH = 2 pH = 12
Figure 19.4 The sharp colour changes of (a) methyl orange and
(b) phenolphthalein in solutions of pH = 2 and pH = 12.
(There is often a marked change in pH at the end point of titration.
The change from pH = 2 to pH = 12 is used as an example here.)
19.2 Acid-alkali titrations

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 Suitable
Titration type Example
indicator(s)
methyl orange;
Strong acid – strong alkali HCl(aq) vs. NaOH(aq)
phenolphthalein

Strong acid – weak alkali HNO3(aq) vs. NH3(aq)

methyl orange
(Strong acid – carbonate) HCl(aq) vs. Na2CO3(aq)

Weak acid – strong alkali CH3COOH(aq) vs. KOH(aq) phenolphthalein

(no indicator
Weak acid – weak alkali CH3COOH(aq) vs. NH3(aq)
would be suitable)

Table 19.3 The correct choice of indicators for different types of acid-alkali
titrations.
Example 19.6 Class practice 19.4

19.2 Acid-alkali titrations

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Estimation of equivalence point by measuring the
change in pH of the mixture
The change in pH of the mixture during titration
can be followed by using
a pH meter or
a data-logger connected with a pH sensor

19.2 Acid-alkali titrations

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 Steps for estimating equivalence point by
measuring the change in pH of the mixture
1. Fill the 25.0 cm3 pipette with 0.1 M HCl(aq).
Transfer 25.0 cm3 of the acid to a beaker placed
on a magnetic stirrer.
2. Put the electrode of a pH meter or a pH sensor
connected with a data-logger into the beaker of acid.
3. Fill the burette with 0.1 M NaOH(aq). Make sure
that the jet is filled completely (no air bubbles inside
the jet).
4. Slowly add the alkali to the acid. The pH of the
mixture is measured immediately after each
addition of the alkali.
19.2 Acid-alkali titrations

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 0.1 M NaOH(aq)

burette

pH meter

electrode of pH meter
magnetic stirring bar 0.1 M HCl(aq)
magnetic stirrer

Figure 19.5 The experimental set-up for the estimation of equivalence

point by pH measurement.
19.2 Acid-alkali titrations

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 If the pH reading is plotted against the volume of
the sodium hydroxide solution added, a titration
curve is obtained.
There is a marked change in the pH at the
equivalence point of titration.

Learning tip
The pH of the mixture at the equivalence point may
NOT be 7 for some acid-alkali titrations.
Experiment 19.2

Experiment 19.2

19.2 Acid-alkali titrations

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 pH of the mixture
when the equivalence
point is reached
pH
equivalence point

volume of NaOH(aq) required

to reach the equivalence point

Volume of NaOH(aq) added (cm3) Think about

Figure 19.6 Titration curve for the titration of 0.1 M sodium hydroxide
solution with 25.0 cm3 of 0.1 M hydrochloric acid.
19.2 Acid-alkali titrations

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Estimation of equivalence point by measuring the
change in temperature of the mixture
Neutralization between an acid and an alkali is
an exothermic reaction.
The reaction gives out heat.

19.2 Acid-alkali titrations

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Steps for estimating equivalence point by measuring
the change in temperature of the mixture
1. Place 25 cm3 of 0.1 M HCl(aq) and a thermometer
in a polystyrene cup.
2. Record the initial temperature of the acid.
3. Add 0.1 M NaOH(aq) slowly to the acid.
4. Record the temperature of the mixture immediately
after each addition of NaOH(aq).
Learning tip
The set-up for the experiment here is very similar to
the one shown in Figure 19.5. Except that:
• a polystyrene cup is used instead of a beaker.
• a thermometer is used instead of a pH meter.
19.2 Acid-alkali titrations

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 equivalence point
E
Temperature (°C)

B
A
volume of NaOH(aq) needed
to reach the equivalence point

Volume of NaOH(aq) added (cm3)

Figure 19.7 A plot of the temperature change of the mixture against the
volume of NaOH(aq) added.
19.2 Acid-alkali titrations

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Temperature change during an acid-alkali titration
From A to E: The temperature of the mixture rises
because heat is given out when
NaOH(aq) is added to dilute HCl(aq).

At E: The temperature of the mixture reaches

the maximum because the equivalence
point is reached.

From E to B: The temperature of the mixture falls

because addition of excess NaOH(aq)
will not give out heat but cool the mixture.
Class practice 19.5

19.2 Acid-alkali titrations

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19.3 Calculations on volumetric analysis
Standardization
To standardize (i.e. to find the molarity of) a
solution of unknown molarity by titrating it with a
standard solution.

Problem-solving strategy 19.1 Experiment 19.3

Example 19.7 Experiment 19.3

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Basicity of an acid
To determine the basicity of an acid by finding out
the number of moles of sodium hydroxide required
to neutralize one mole of the acid.
Example 19.8 Class practice 19.6

Molar mass of a substance

To determine the molar mass of an acid, a metal
or a base by volumetric analysis.

Example 19.9

19.3 Calculations on volumetric analysis

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Relative atomic mass of an element
To determine the relative atomic mass of an
element by volumetric analysis.
Example 19.10 Class practice 19.7

Number of molecules of water of crystallization

To determine the number of molecules of water of
crystallization in a formula unit of a hydrated
compound by volumetric analysis.
Example 19.11 Class practice 19.8

19.3 Calculations on volumetric analysis

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Percentage by mass of a substance in a sample
Key point
Percentage by mass of a substance in a sample (%)
mass of the substance (g)
= × 100%
mass of the sample (g)

Example 19.12
Figure 19.8 The percentage by mass
Class practice 19.9
of anhydrous sodium sulphate in this
bottle is 99%.
19.3 Calculations on volumetric analysis

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Back titration
Two ways to perform a titration
direct titration
back titration

1. Direct titration

Add just the right amount of titrant (the solution

in the burette) to the solution in the conical flask.

19.3 Calculations on volumetric analysis

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2. Back titration
Direct titrations are impossible in some cases.
E.g. percentage by mass of CaCO3(s) in a sample
cannot be found by titrating standard HCl(aq) with
the sample directly.
∵ CaCO3(s) is insoluble in water and it is unable
to make an aqueous solution of it.

Learning tip
Back titration is also performed if the reaction
between the substance being analysed and
the reagent involved is too slow.
19.3 Calculations on volumetric analysis

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Steps for back titration
1. Add a known excess amount of standard HCl(aq)
to a known mass of the CaCO3(s) sample.

CaCO3(s) reacts with HCl(aq), dissolving
completely to form a solution.

2. Back titrated the unreacted acid in the solution

against a standard NaOH(aq).

Problem-solving strategy 19.2

Class practice 19.10

19.3 Calculations on volumetric analysis

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19.4 Writing a laboratory report on
volumetric analysis
Format of laboratory reports
You should use past tense to describe
Use the correct
1 specific experimental methods and
tenses
observations.
Because scientific experiments demonstrate
Write in the
facts that do not depend on the observer,
third person
2 reports should not be written in the first or
and passive
the second person. Besides, passive voice
voice
is used.
Write with Complete sentences with no grammatical
3
proper grammar mistakes should be used.
Table 19.4 Some useful guidelines in writing a laboratory report.
Class practice 19.11

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 Write the title of the experiment as given in the
laboratory manual.
1 Title
(e.g. Determining the concentration of ethanoic
acid in commercial vinegar))
Use a single sentence to state clearly the objective
of the experiment.
2 Objective
(e.g. To determine the concentration of ethanoic
acid in commercial vinegar)
List the apparatus and materials used in the
experiment as specifically as possible. This allows
Apparatus others to repeat your experiments.
3 and (e.g. electronic balance
materials beaker (100 cm3)
volumetric flask (250.0 cm3)
anhydrous sodium carbonate powder (6.30 g))
Table 19.5 Parts of a formal laboratory report.
19.4 Writing a laboratory report on volumetric analysis

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 • Describe clearly the procedure of the experiment
so that someone else can repeat what you did.
For example, describe clearly how solutions are
obtained or prepared and used in the analysis;
how measurements are done; state the amounts
4 Procedure of substances used, the volumes and
concentrations of solutions used.
• In general, write the procedure in a step-by-step
format rather than in essay form.
• In most cases, draw diagrams of the experimental
set-ups for better presentation.
• Summarize your numerical data using tables or
graphs.
Results and
• Express numerical results to the appropriate
5 number of significant figures and in the correct
observations
units.
• Record all observations clearly and fully using
appropriate terms in chemistry.
Table 19.5 Parts of a formal laboratory report.
19.4 Writing a laboratory report on volumetric analysis

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 Analysis/
• Give the equations used to work out the
answers.
6 Calculations
(if any)
• Show your calculation steps clearly.
• Provide definitions of every variable used.
• Draw valid conclusions based on the
observations and data collected.
• Describe the problems encountered in the
experiment.
Conclusions
• Discuss the sources of errors and uncertainties,
especially those due to error in laboratory
7 and
techniques and those due to imprecision of the
evaluation
apparatus.
• Give any suggestions for improvement to avoid
these errors.
• Answer the questions (if any) in the laboratory
manual at the end of the laboratory report.
Table 19.5 Parts of a formal laboratory report.
19.4 Writing a laboratory report on volumetric analysis

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Attitude of writing laboratory reports
We should not just report ‘good’ data.
Try to find out why irregularities arise, whether we
have made some mistakes while performing
experiments or we have to revise the experimental
procedures.

Experiment 19.4

Experiment 19.4

19.4 Writing a laboratory report on volumetric analysis

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Key terms
1. back titration 返滴定
2. end point 終點
3. equivalence point 當量點
4. laboratory report 實驗報告
5. primary standard 基本標準
6. standard solution 標準溶液
7. titration 滴定
8. titration curve 滴定曲線
9. volumetric analysis 容量分析

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Progress check
1. What is a standard solution?
2. Can you name the essential apparatus used in
the preparation of a standard solution?
3. What is a primary standard?
4. What are the characteristics of primary
standards?
5. Do you know how to prepare a standard solution
by dissolving a pure solid?
6. Do you know how to prepare a standard solution
by diluting a concentrated solution of known
molarity?

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7. What is volumetric analysis?
8. Can you name the essential apparatus used in
titration?
9. What is the equivalence point of an acid-alkali
titration?
10. What is the end point of an acid-alkali titration?
11. Do you know how to perform a simple acid-alkali
titration?
12. Do you know how to detect the end point in an
acid-alkali titration?
13. Can you name two common acid-base indicators
used in titration?
Progress check

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14. Do you know how to choose the correct
indicator(s) for different types of acid-alkali
titrations?
15. Do you know how to estimate the equivalence
point in an acid-alkali titration?

Progress check

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16. Can you perform the following calculations using
the concepts of concentration of solution and the
results of acid-alkali titration?
(a) Standardization
(b) Basicity of an acid
(c) Molar mass of a substance
(d) Relative atomic mass of an element
(e) Number of molecules of water of crystallization
of a hydrated compound
(f) Percentage by mass of a substance in a
sample

Progress check

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17. What are direct titration and back titration?
18. Do you know how to solve stoichiometric
problems involved in back titration?
19. Do you know how to write a laboratory report?

Progress check

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Summary
19.1 Standard solutions
1. A standard solution is a solution of accurately
known molar concentration or molarity.
2. The essential apparatus used in the
preparation of a standard solution include
volumetric flask, pipette and pipette filler.
3. A primary standard is a substance which can
be used to prepare a standard solution directly.

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4. A standard solution can be prepared by
dissolving a known mass of a pure solid or by
diluting a concentrated standard solution to a
specific volume.

19.2 Acid-alkali titrations

5. Volumetric analysis is a method to determine
the amount (or concentration) of a substance in
a sample. Titration is one of the techniques of
volumetric analysis.
6. The essential apparatus used in titration include
burette, pipette and conical flask.

Summary

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7. The equivalence point of an acid-alkali titration
is the point at which an acid and an alkali have
completely reacted with each other.
8. The equivalence point of an acid-alkali titration
can be estimated by measuring the change in
pH and the change in temperature of the
mixture.
9. End point is the point at which the indicator
changes colour sharply.

Summary

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10. The end point of titration can be detected
using the appropriate acid-base indicator(s).
The choices of indicators in acid-alkali titration
are summarized in Table 19.3 on p.15.

Summary

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19.3 Calculations on volumetric analysis
11. We can apply the concepts of concentration of
solution and acid-alkali titration results to solve
stoichiometric problems such as
(a) Standardization
(b) Molar mass of a substance
(c) Basicity of an acid
(d) Relative atomic mass of an element
(e) Number of molecules of water of
crystallization of a hydrated compound
(f) Percentage by mass of a substance in a
sample

Summary

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19.4 Writing a laboratory report on volumetric analysis
12. A laboratory report can help to communicate the
procedure and results of an experiment on
volumetric analysis.
13. A formal laboratory report should consist of the
following sections:
(a) Title
(b) Objective
(c) Apparatus and materials
(d) Procedure
(e) Results and observations
(f) Analysis and calculations (if any)
(g) Conclusions and evaluation
Summary

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Concept map

VOLUMETRIC
determines ANALYSIS apparatus

• concentration of solution
_____________________ • weighing bottle
• basicity of an acid • electronic balance
• molar mass of a substance • volumetric flask
_______________
• relative atomic mass of an • pipette
_______________
element • pipette filler
• number of molecules of • beaker
water of crystallization • _______________
burette
• percentage by mass of a • conical flask
substance in a sample

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 VOLUMETRIC
ANALYSIS

Preparation of a Titration
standard solution
________________

methods

Dissolve a known mass Dilute a solution of

pure solid
of a ____________ known molarity
________________

Concept map

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 Titration
example

Acid-alkali titration

detection of detection of
end point equivalence point

acid-base
Use an _________
indicator
_______________ Measure the Measure the
pH
change in ____ change in
of the mixture temperature
___________
of the mixture

Concept map

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