METHODIST GIRLS’ SCHOOL

Founded in 1887
SECONDARY 3
Chemistry
Chapter 1: Experimental Chemistry

Name ________________________________
Kayla ( ) Sec 3 ( )

Topic Description:

When carrying out experiments, chemists assemble suitable apparatus (with laboratory safety in
consideration) and decide on what to look for and measure using appropriate techniques and
apparatus. Physical quantities commonly measured include mass, volume, time and temperature. The
apparatus used depends on the quantity being measured, and on how accurate and precise the
measurement needs to be.

When matter undergoes changes, mixtures of substances can be formed. Methods of separation and
purification depend on the type of mixtures and the difference in physical properties of the substances
in the mixture. Purifying mixtures is important in manufacturing to ensure quality and to separate
useful substances from mixtures and waste products. Pure substances are important especially in
consumer products such as food and medicine. A pure substance is a single element or compound.
To assess the purity of a substance, its melting point or boiling point is measured and matched to
reference values. Chromatography is also a method to determine purity of a substance and to identify
components in mixtures.

Learning Outcomes

1.1 Experimental Design

(a) name appropriate apparatus for the measurement of time, temperature, mass and volume;
including burettes, pipettes, measuring cylinders and gas syringes
(b) suggest suitable apparatus, given relevant information, for a variety of simple experiments,
including drying and collection of gases and measurement of rates of reaction
(drying agents will be limited to calcium oxide, concentrated sulfuric acid and fused calcium
chloride)

1.2 Methods of Purification and Analysis

(a) describe methods of separation and purification for the components of mixtures, to include:
(i) use of a suitable solvent, filtration and crystallisation or evaporation
(ii) sublimation
(iii) distillation and fractional distillation (see also11.1(b))
(iv) use of a separating funnel
(v) paper chromatography

(b) suggest suitable separation and purification methods, given information about the substances
involved in the following types of mixtures:
(i) solid-solid
(ii) solid-liquid
(iii) liquid-liquid (miscible and immiscible)

(c) interpret paper chromatograms including comparison with ‘known’ samples and the use of Rf
values
(d) explain the need to use locating agents in the chromatography of colourless compounds
(knowledge of specific locating agents is not required)
(e) deduce from given melting point and boiling point data the identities of substances and their
purity
(f) explain the importance of measuring the purity in substances used in everyday life, e.g.
foodstuffs and drugs

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1.1 How are physical quantities measured?

Measuring physical quantities are important to help us study the data.

The International System of Units (SI units) is a common standard for recording
measurements.

Physical What It Measures SI Unit Symbol Other Common Units

Quantity
time how long it takes for second s minute (min), hour (h)
something to happen
temperature how hot or cold something kelvin K degree Celsius (°C)
is
length the distance between two metre m centimetre (cm),
points decimetre (dm)
mass how much matter is present kilogram kg gram (g), tonne (t)
in a substance
volume the amount of space cubic m3 cubic centimetre (cm3),
something occupies metre cubic decimetre (dm3)

1. Measurement of time

The SI unit for time is the second (s).

We can also use other units such as minute (min) and hour (h).

1 min = 60 s
1 h = 60 min
= 60 × 60
= 3600 s

Apparatus Smallest division of Value to be recorded to Example of

instrument the nearest recording
Stopwatch 0.01s 0.1 s (For Phy) 28.0 s, 28.1 s
1 s (For Chem and Bio) 20 s, 28 s

Displayed time: 10 min 51.46 s

Recorded time (nearest 0.1 s)= 10 min 51.5 s

Recorded time (nearest 1 s)= 10 min 51 s

Sources of error
Human reaction time (not human error) in starting and stopping the stopwatch leading to
inaccurate time measurement.

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2. Measurement of temperature

The SI unit for temperature is the kelvin (K)

We commonly use degree Celsius (°C) to measure temperature.

Temperature in K = Temperature in °C + 273

Apparatus Smallest division of Value to be recorded to Example of

instrument the nearest recording
Thermometer 1C 0.5 C 28.0 C, 30.5 C

Sources of error
In some experiments, heat is produced in the reaction and causes the temperature of
the reacting mixture to increase. Heat loss to the surrounding leading to temperature
recorded to be lower than expected.

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3. Measurement of length

The SI unit for length is the metre (m).

Length can also be measured in millimetres (mm) or centimetres (cm).

1 m = 100 cm = 1000 mm

Apparatus Smallest division of Value to be recorded to Example of

instrument the nearest recording
Metre rule 0.1 cm 0.1 cm 2.8 cm
Measuring 1 mm 1 mm 28 mm
tape

4. Measurement of volume of liquids

The SI unit for volume is the cubic metre (m3).

1 m3 = 1000 dm3 = 1 000 000 cm3

Apparatus Function

pipette measures accurate fixed volumes,

e.g. 10.0 cm3 or 25.0 cm3

volumetric flask measures accurate fixed volumes that are larger,

e.g. 100 cm3 or 250 cm3
measuring cylinder measures a range of volumes to the nearest 0.5 cm3,
e.g. 31.5 cm3 or 23.0 cm3
burette measures a range of volumes to the nearest 0.05 cm3,
e.g. 31.55 cm3 or 23.00 cm3

volumetric flask

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 Measuring Measuring Pipette Burette
cylinder cylinder
(10 cm3) (100 cm3)
Smallest 0.2 cm3 1 cm3 NA 0.1 cm3
division of
instrument
Value to be 0.1 cm3 0.5 cm3 NA 0.05 cm3
recorded to
the nearest
Example of 2.6 cm3, 14.0 cm3, Precise apparatus 14.00 cm3,
recording 8.7 cm3 14.5 cm3 for measuring fixed 24.55 cm3
volume of liquids
e.g. 20.0 cm3 or
25.0 cm3 liquid (use
in MGS)

Reading:
Reading: Reading:

The volume of a gas can be measured using a gas syringe.

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Experimental Technique involving Gases

In some experiments, gases are given off. The gases can be collected and identified to
help us find out more about the reactions that have occurred, The gases may also be
collected for use in another reaction.

A) Measurement of gas

gas

volume of gas
collected

B) Methods for Collecting Gases

The method of gas collection depends on 2 properties of the gas:
(i) solubility in water
(ii) density of gas compared to air

(i) Solubility of Gases in water

As the solvent temperature increases, the gas solubility decreases.
For example, air dissolved in water is driven out when water is heated.

Different gases have different solubilities in the same solvent.

For example, oxygen is more soluble than nitrogen in water (although both
solubilities are low). This dissolved oxygen in water is of importance to fish and marine
life forms which use it in respiration.

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 (ii) Density of gas compared to air
Density of gases as compared to density of air can be obtained by comparing the
Mr of gases to that of air.

As a general guide, a gas is less dense than air if its relative molecular mass, Mr, is less
than 30.

Example: find the density of carbon dioxide as compared to air.

Mr of CO2 = 12 + 2(16) = 44 (This will be covered later on)

Therefore CO2 is denser than air.

Four methods of Gas Collection:

(i) Downward Displacement of water

gas jar
- Suitable for gases that are slightly soluble or
gas (wet)
almost insoluble gases

-density does not affect gas collection

Examples are: oxygen, hydrogen, carbon

dioxide water

(ii) Downward delivery of gas

- Suitable for gases that are soluble or

insoluble in water

- gases that are denser than air

- Gas moves downward into jar; air moves

upward out of jar.

Examples are: sulfur dioxide, chlorine,

hydrogen chloride

(c) Upward delivery of gas

- Suitable for gases that are soluble in water

- gases are less dense than air

- Gas moves upward into jar; air moves

downward out of jar.

- Example: ammonia

(d) Using a gas syringe

- For collecting and measuring volume of

gases per unit time interval [speed of reaction]

NOTE:
If a gas is required DRY it must NOT be collected over water.
A soluble gas must NOT be collected over water.

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 Gas Solubility in water Density compared to air Method of collection
hydrogen not soluble less dense
oxygen very slightly soluble slightly denser
displacement of water
carbon slightly soluble denser
dioxide
chlorine soluble denser
hydrogen very soluble denser
downward delivery
chlorine
sulfur dioxide very soluble denser
ammonia extremely soluble less dense upward delivery

C) Drying of Gases
The prepared gas is then bubbled into a drying agent to be dried.

Common examples of drying agents

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 > neutral salt
-

Suitable to dry acidic & alkaline gas !!

(i) Liquid drying agent

– concentrated sulfuric acid: the gas must be bubbled into the acid in a conical flask

tube must-
must be short
n

go into the

drying agent W
Ammonia gas is alkaline.

(ii) Solid drying agents:

(a) Small lumps of basic calcium oxide [quicklime]
(b) Fused calcium chloride [calcium chloride that has been heated to remove all traces of water]

Note: Powdered drying agent NOT to be used as it would block the flow of gas. The gas is
bubbled though the solid in a U-tube.

has to be
& large lumps

Note:
Agents selected to dry a gas must NOT react with the gas.
Thus, acidic drying agent like concentrated sulfuric acid cannot be used to dry an alkaline gas
such as ammonia.

Likewise, a basic drying agent like calcium oxide cannot be used to dry acidic gases like chlorine,
sulfur dioxide, carbon dioxide and hydrogen chloride.

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Exercise 1

Thistle funnel with measuring cylinder

tap

Conical
Fl ask

The
gas is denser than Air and therefore cannot be collected

the is moist and needs to go through the concentrated sulfuric acid

gas
2

measuring cylinder

n-tube

Ammonia gas is very soluble in water so it will dissolve in the water. Hence, ammonia gas must not be
collected over water. Ammonia gas (Mr= 17) is less dense than air so it must be collected in the gas jar by
upward delivery method.
talk about
solubility

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5. Measurement of mass

The SI unit for mass is the kilogram (kg).

Mass can also be measured in grams (g) or milligrams (mg).

1 g = 1000 mg
1 kg = 1000 g
1 tonne = 1000 kg = 1 000 000 g

Apparatus Smallest division of Value to be recorded to Example of

instrument the nearest recording
Electronic 0.1 g 0.1 g 50.0 g, 151.1 g
balance
0.01 g 0.01 g 131.00 g, 131.10 g

Mass: 10.27 g Mass: 20.4 g

What is the difference between precise and accurate?

Accuracy is a measure of how close a measurement is to the known value of the

quantity being measured. The closer your measurements are to the known value, the
more accurate the measurement.

Precision is a measure of how close a series of measurements are to one another.

The closer each measurement is to the other measurements, the more precise your
measurement.

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Quick check:
The known volume of a liquid is 20.50 cm3.
State whether following sets of measurements is high or low in accuracy and precision.

a 18.60 cm3, 17.85 cm3, 19.60 cm3, 16.20 cm3

b 18.20 cm3, 18.30 cm3, 18.00 cm3, 17.95 cm3

c 20.0 cm3, 21.0 cm3, 19.5 cm3, 21.5 cm3

d 20.30 cm3, 20.50 cm3, 20.30 cm3, 20.40 cm3

1.2 How are substances in mixture separated?

What is a mixture?

A mixture consists of two or more substances that are not chemically combined.
The physical properties of the substances determine the separation techniques
to use.

Type of Mixture
Solid–Solid Mixture Solid–Liquid Mixture Liquid–Liquid Mixture
magnetic attraction filtration separating funnel
sieving evaporation to dryness chromatography

using suitable solvents crystallisation fractional distillation

sublimation simple distillation

1) Separating Solid–solid Mixtures

Using Magnetic Attraction

• Magnetic substances can be separated
from non-magnetic substances.
• Magnetic substances:
iron, cobalt, nickel and some alloys
• Waste in a landfill can be sorted
using magnetic attraction.

Sieving
• A sieve is used to separate solids with different particle sizes.

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 Sublimation
• Sublimation is used to separate solids where one substance changes from the solid to
the gaseous state directly.

The iodine sublimes and

changes directly to a gas
which cools back to a solid
on the cold filter funnel.
The sand remains in the
evaporating dish.

The mixture is placed in an evaporating

dish with an inverted filter funnel on the
top. It is then gently heated.

Using Suitable Solvents

• Solids of different solubility in the solvent can be separated.
• Solvent: liquid that dissolves solids
• Solute: solid that dissolves in the solvent
• A solute dissolves in a solvent.

To separate a mixture of two solids, we use a solvent in which one solid is soluble.
(The other solid is insoluble in that solvent.)

excess

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 2) Separating Solid–liquid Mixtures

Filtration

To separate an insoluble solid from a liquid.

An insoluble solid is one that is unable to dissolve into the liquid it is placed in.

Filtrate: liquid that passes through the filter paper

Residue: solid that remains on the filter paper

Upon filtration, the

insoluble solid that
remains on the filter paper
is called the residue.

The liquid or solution that

passes through the filter
paper is called the filtrate.

Evaporation to Dryness
• Separates a dissolved solid from its solvent
• The mixture is heated until all the solvent has vaporised.

The solid obtained by evaporation to dryness is not always pure. When all the water has been
removed, any soluble impurities will be left together with the solid.

Suitable for solid that does not decompose on heating.

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 Crystallisation

Crystallisation is used for obtaining a pure solid from its solution.

Crystallisation is used to separate a solute (that decomposed on heating) from the solvent in
a solution. Substances that decomposed on heating are copper(II) sulfate and sugar.

Preparation of Pure Copper(II) Sulfate Crystals by Crystallisation

- The crystals are obtained by filtration

Definition:
A saturated solution is one which contains the maximum mass of solute at a particular
temperature

Evaporation to dryness vs Crystallisation

Evaporation to Dryness Crystallisation

• Evaporation to dryness is used to separate • Crystallisation is used to separate
dissolved solid from a solution. The solid does not dissolved solid from a solution. Whereby
decompose on strong heating. the solid decompose s easily on strong
• Eg: sodium chloride, sodium carbonate heating.

• All the solvent is removed by evaporation. • Eg: sugar, copper(II) sulfate

• Any soluble impurities will be left on the solid

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Simple Distillation
• Separates a pure solvent (liquid) from its solution.
•

Liquid-liquid mixture
Homogeneous Mixture Heterogeneous Mixture
Miscible liquids that form a uniform solution. Immiscible liquids that do not form a uniform
solution.
The liquids separate into layers known as
phases.

Separating Funnel
• The separating funnel is used to separate two liquids which do not mix together, such
as oil and water. Such mixtures are said to be immiscible.

The less dense liquid (oil) collects

above the denser liquid (water).

When the tap is opened, the bottom layer

is allowed to drain into the beaker. The
tap is closed before the top layer of liquid
runs out.

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Fractional Distillation
Fractional distillation is used to separate a mixture of miscible liquids with different boiling points.

For example, water and ethanol are miscible and have boiling points of 100°C and 78°C respectively.

The fractionating column is usually packed with glass beads and this provides a large surface area for
condensation of vapour and evaporation of liquid.

The vapour produced moves

up the fractionating column.
Repeated evaporation and
condensation of the vapour
happen on the glass beads in
the fractionating column.
Ethanol having a lower boiling
point (boiling point 78 C),
vaporise more easily and found
at the top of the fractionating

• Applications:
o Oil refineries separate crude oil into different substances.
o Separation of liquefied air into different gases.
o Separation of ethanol from the glucose solution during fermentation.

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Chromatography

Chromatography is the method of separating two or more components that dissolve

in the same solvent.
Paper chromatography can be used to separate colours, dyes or pigments. The
chromatography paper with the separated components is called a chromatogram.

Special considerations:

The start line should be drawn in

pencil, Pencil lead is made of graphite
which is insoluble in water hence will
not interfere with the separation of the
dyes in the food colouring.
The solvent should be allowed to run
as far from the starting line as possible
to ensure better separation.
The spots marked at the start line
should be above the solvent level.
Otherwise, the spots will dissolve in the
solvent prior to the start of the
experiment.
The boiling tube or beaker used in the
experiment should be covered. This is
to prevent evaporation of the solvent
used, as many organic solvents are
volatile.

Principle Behind Paper Chromatography

• Separation of a substance into its different components depends on the relative

solubility of the component.
• The more soluble component travels faster and further up the paper than the less
soluble components.
• Identical dyes travel up the same distance and produce the same colour on the paper
when the same solvent is used.
• The chromatography paper with the separated components is called a chromatogram.

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 • The retention factor, or Rf value of a substance is a measure of its solubility in the
solvent.

• Rf value =

• Using Rf values allows us to compare chromatograms which have been run for different
durations using the same solvent, under the same temperature.

Locating agents are used for the chromatography of colourless substances.

They are chemicals that react with the colourless substances to form coloured spots.

Applications:
• Identify unauthorised substances like pesticides and poisons in food.
• Detect small quantities of banned substances in an athlete’s urine or blood.
• Separate components like DNA fragments in samples for forensic investigations.

1.4 How Can the Purity of Substances Be Determined?

A pure substance has a specific melting and/or boiling point under fixed conditions.
Mixtures melt or boil over a range of temperatures.
For example, pure water boils at 100 °C, but adding salt to water raises its boiling point.
Similarly, pure water freezes at 0 °C, but adding salt to water lowers its freezing point.
In certain countries, roads are salted throughout the winter. This prevents the formation of ice on
the roads following a significant snowfall or downpour.

Determining Purity
1. Pure solids have fixed melting points. Any presence of impurity lowers the melting point and
causes the substance to melt over a range of temperatures.
2. An example would be the addition of salt to ice. Pure ice melts exactly at 0°C. When salt is
added, it lowers the melting point to values of between –5ºC to –25ºC, depending on how
much salt is added.
3. Pure liquids have fixed boiling points. Any presence of impurity raises the boiling point.

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Downward displacement of water is used
to collect gas which is slightly soluble or
insoluble in water.
Examples:
Oxygen, hydrogen and carbon dioxide
Gas collected by downward displacement
of water is wet.
Gas
Downward delivery method is used
to collect gas which is soluble in
water and denser than air (its Mr is
greater than 30).
Examples:
Chlorine (Mr = 71)
Sulfur dioxide (Mr = 64)
Hydrogen chloride (Mr = 36.5)
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Drying of gas
Acidic drying agent like concentrated sulfuric acid
cannot be used to dry alkaline gas such as ammonia.
Basic drying agent like calcium oxide cannot be used to
dry acidic gases like chlorine, sulfur dioxide, carbon
dioxide and hydrogen chloride.
Fused calcium chloride can be used to dry acidic and
alkaline gas.
Upward delivery method is used to
collect gas which is soluble in water
and less dense than air (its Mr is
less than 30).
Examples:
Ammonia (Mr = 17)