Experimental chemistry

Content
1.1 Experimental design
1.2 Methods of purification and analysis
1.3 Identification of ions and gases
It is expected that any course in chemistry will be based on experimental work. Teachers are encouraged
to develop appropriate practical work for candidates to facilitate a greater understanding of the subject.
Candidates should be aware of the hazards and appropriate safety precautions to follow when handling
the reagents mentioned in this section.
Learning outcomes
Candidates should be able to:
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 collection of gases and measurement of rates of reaction
1.2 Methods of purification and analysis
a) describe methods of purification by the use of a suitable solvent, filtration and crystallisation,
distillation and fractional distillation, with particular references to the fractional distillation of crude
oil, liquid air and mixtures of liquids

b) suggest suitable methods of purification, given information about the substances involved

c) describe paper chromatography and interpret 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

e) deduce from given melting point and boiling point information, the identities of substances and
their purity

f) explain that the measurement of purity in substances used in everyday life, e.g. foodstuffs and drugs,
is important
1.3 Identification of ions and gases
a) describe the use of aqueous sodium hydroxide and aqueous ammonia to identify the following
aqueous cations: aluminium, ammonium, calcium, chromium(III), copper(II), iron(II), iron(III) and
zinc (formulae of complex ions are not required)

b) describe tests to identify the following anions: carbonate (by the addition of dilute acid and
subsequent use of limewater); chloride (by reaction of an aqueous solution with nitric acid and
aqueous silver nitrate); iodide (by reaction of an aqueous solution with nitric acid and aqueous silver
nitrate); nitrate (by reduction with aluminium and aqueous sodium hydroxide to ammonia and
subsequent use of litmus paper), sulfate (by reaction of an aqueous solution with nitric acid and
aqueous barium nitrate), and sulfite (by warming with dilute acid)

c) describe tests to identify the following gases: ammonia (using damp red litmus paper); carbon
dioxide (using limewater); chlorine (using damp litmus paper); hydrogen (using a burning splint);
oxygen (using a glowing splint) and sulfur dioxide (using acidified potassium manganate(VII))

d) describe a chemical test for water

Cambridge

a) name appropriate apparatus for the measurement of time, temperature, mass and volume,
including burettes, pipettes, measuring cylinders and gas syringes

Preview:
The subject of chemistry involves measurement of various physical quantities, like time, temperature,
mass, volume and density etc. Scientists all over the world use SI units and their sub-units for the
measurement of various physical quantities.
Quantities SI Units Symbols
mass kilogram kg
time second s
temperature Kelvin K
volume cubic meter m3
density kilogram/cubic meter kg m–3

Measurement of Time:

Analogue Stopwatch Digital Stopwatch

→ In laboratory, time intervals are measured using stopwatches and stopclocks.
→ SI unit for time is second (s). Other units, such as minutes (min) and hours (h) are used to measure
longer intervals of time. Remember that

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

→ A common stopwatch can measure a time interval correct upto 0.01s.

→ Example of use of stopwatch is to record data in order to determine rate of reaction i.e. how quickly
a reaction proceeds.
Measurement of Temperature:

→ In laboratory, the temperature of a liquid or gas is measured using a mercury-in-glass thermometer.

→ Alcohol-in-glass thermometer and electronic thermometer are also used.
→ Two scales, degree Celsius (°C) and Kelvin (K) are commonly used for temperature measurement.
They are related as follows

temperature in K = temperature in ℃ + 273

→ A mercury-in-glass thermometer can measure temperatures from -20 °C to 110 °C.

→ In an experiment where change in temperature is required, thermometers are used.
∆T = Tf - Ti
Measurement of Mass:

Electronic balance Beam balance

→ The mass of a substance is the amount of matter it contains.

→ SI unit for mass is kilogram (kg). However, smaller units like gram (g) and milligram (mg) are used
for smaller amounts while kilogram (kg) and tonnes are used for larger amounts. Remember that

1 tonne = 100 kg
1 kg = 1000 g
1 g = 1000 mg

→ In laboratory, the mass of a substance is measured using beam balance or electronic balance.
→ Electronic balances are more commonly used as compared with beam balance because they are
easier to use and measure accurately to 0.01 g or even 0.001 g.
→ Examples of use of balance include weighing amount of calcium carbonate to be used or in order
to determine change in mass in an experiment.
Measurement of Volume:
→ The volume of a substance is the amount of space it occupies.
→ SI unit of volume is cubic metre (m3). However, different smaller units are also used for measuring
volume such as cubic centimetres (cm3), cubic decimetres (dm3), litres (L) and millilitres (ml).
Remember that

1 m3 = 1000 dm3
1 dm3 = 1000 cm3
1 L = 1 dm3
1 L = 1000 ml

→ The various pieces of apparatus used for measuring volume of a liquid are: measuring cylinder,
plastic syringe, pipette, burette and volumetric flask.

→ Plastic syringe:

To measure small volumes of liquids with some accuracy according to the graduated marks on the
apparatus. Such syringes are used by doctors for injections.

→ Measuring cylinder:

It measures to the nearest 0.5 cm3, e.g. 41.5 cm3 or 99.0 cm3. It measures the volume of a liquid
correct to 1 cm3. Measuring cylinder is required to mix reactants as well. A measuring cylinder is
used for measuring volumes of solutions where accuracy is not so important. Many measuring
cylinders have scale divisions which are only every 2 cm3. A measuring cylinder can be used to
collect volumes of gas such as 23.6 cm3. Keep in mind that for measurement of gases, apparatuses
such as beaker, conical flask or pipette is not used.

→ Burette:

For more accurate measurement, a burette is used. Burettes are also used to dispense variable
amounts of liquid. Burette accurately measures out the volume of a liquid to the nearest 0.05 cm 3.
The scales are marked (graduated) in 0.1 cm3 divisions. It is used to deliver different volumes of
liquids, e.g. 24.00 cm3 or 38.95 cm3. It can accurately deliver up to 50 cm3 of liquid.

→ Volumetric Flask:

• Volumetric flasks are used to measure fixed volumes of liquids. Volumetric flasks of 100 cm3, 250
cm3, 500 cm3 and 1 dm3 are available in the laboratory. A volumetric flask is used to make up a
solution of a known concentration very accurately. A known mass of solute is dissolved in a small
amount of solvent in the flask. The flask is then filled to the graduation mark with solvent.
•
→ Pipette:

• A volumetric pipette can deliver a single fixed volume of liquid very accurately, for example 25.0
cm3 of sodium hydroxide solution. Pipettes of volumes 10 cm3, 20 cm3 and 25 cm3 are used in
laboratory. Apparatuses such as burette, gas syringe, measuring cylinder have graduations marked
to fill up to the desired value. In pipette, however there is a single mark indicating that the fluid is
to be filled to that level to get a fixed volume. In other words, pipettes should always be filled to
the same level. Some volumetric pipettes have scale divisions like a burette which can be read
accurately.

→ Beaker:

• A graduated beaker measures approximate volume of a liquid. Beakers are vessels in which liquid
is placed so it can be stirred, mixed or heated.
•
→ beaker → measuring cylinder → burette → pipette → volumetric flask

Increasing accuracy of measurement

→ In procedures like titration, pipette, burette and conical flask are needed.
How to Read the Volume of a liquid?
→ Whenever a liquid is placed in a container, it forms a curved surface. This curved surface is called
meniscus.
→ A meniscus may be concave or convex.
→ To read the volume of a liquid, align your eyes to the liquid level. If the meniscus is concave, read
off the scale at the bottom of the meniscus. If the meniscus is convex, read off the scale at the top
of the meniscus.

correct correct
reading reading

concave convex
meniscus meniscus

→ The liquid is measured from the bottom of the meniscus if it’s an aqueous solution and at the top
of meniscus if it is mercury. For liquids that are opaque, and the lower meniscus cannot be seen,
measurement is taken from the upper level.

→ A dropping pipette does not have great accuracy, it works like a dropper.

→ Remember that different apparatuses have different degrees of accuracy. And so even though
apparatuses such as beaker may provide an estimate of volume, they are not fit for calculation due
to low accuracy. A burette gives the reading to the nearest 0.05 cm3, a pipette is accurate to ±0.005
cm3 of the marked value and a volumetric flask is accurate to ± 0.1 cm 3 of the marked value.

A burette and pipette can measure the volume of a liquid more accurately compared to a conical
flask or a measuring cylinder. Between burette and pipette, burette can be used to measure a range
of volumes while pipette can only measure a fixed volume (e.g. 25 cm 3). The conical flask is the
least accurate measuring instrument among the four. Conical flasks hold solids or liquids that may
release gases during a reaction or that are likely to splatter if stirred or heated.

Measuring Conical Pipette

Cylinder Flask

Burette
b) suggest suitable apparatus, given relevant information, for a variety of simple experiments,
including collection of gases and measurement of rates of reaction

Collection of Gases:

→ In a chemical reaction where a gas is given off, the speed of a chemical reaction can be measured
by recording the volume of gas given off in a certain time interval. For this purpose gas syringes
are used.

→ A common gas syringe can measure the volume of a gas upto 100 cm3.
→ To collect a gas, two properties may be taken into consideration:
(i) its density with respect to air
(ii) its solubility in water
→ There are three methods to collect gases,
(i) Displacement of water
(ii) Downward Delivery (or Upward Displacement of Air)
(iii) Upward Delivery (or Downward Displacement of Air)
→ Displacement of water:
• This method is suitable for collecting gases that are insoluble or slightly soluble in water such as
carbon dioxide (CO2), hydrogen (H2) and oxygen (O2). In this method, the gas is passed through
water into an upside down jar full of water; the gas starts collecting on the top while the water gets
displaced downwards.

In an experiment to collect a gas, first few tubes of gas are rejected because it may contain nitrogen
from air already present in the flask.

→ Downward Delivery:
• This method is suitable for collecting gases that are soluble in water and denser than air such as
chlorine (Cl2) and hydrogen chloride (HCl). In this method, the gas is introduced in a gas jar. Being
heavier it starts settling at the bottom and leaving the air to escape from the mouth of the jar. This
method is also called upward displacement of air.

→ Upward Delivery:
• This method is suitable for collecting gases that are soluble in water and lighter than air such as
ammonia (NH3). In this method, the gas is introduced into an upside down gas jar. Being lighter
than air, the gas starts rising at the top and leaves the air to escape from the bottom end of the jar.
This method is also called downward displacement of air.

Note: Generally, a gas is considered to be less dense than air if its molecular mass is less than 30.
→ The table given as below shows the solubility and density of some common gases.
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 dioxide slightly soluble denser
chlorine soluble denser
hydrogen chloride very soluble denser downward delivery
sulfur dioxide very soluble denser
ammonia extremely soluble less dense upward delivery

→ All gases can be collected using a gas syringe. At the start of the experiment, the plunger is pushed
in fully to expel any gas in the syringe. As the gas from an external source (e.g. gas produced from
a chemical reaction) enters the syringe, it pushes the plunger outwards.

→ Poisonous gases should be collected in a fume cupboard.

→ If question asks collect and measure, don’t get tricked, if there are no graduation marks, the
substance cannot be measured even if it can be collected.

→ For insoluble gases, they can be collected in an inverted burette filled with water. For gases that
are soluble in water, mercury can be used.
Drying of Gases:
→ Some gases when collected over water contain water vapour as impurity. In order to collect a dry
sample of a gas, it should be passed through a drying agent.
→ Some commonly used drying agents are
(i) concentrated sulfuric acid (H2SO4)
(ii) quicklime i.e. calcium oxide (CaO)
(iii) sodalime (mixture of sodium hydroxide and calcium hydroxide)
(iv) fused calcium chloride (CaCl2) i.e. calcium chloride that has been previously heated to
remove all traces of water. It can be used to dry most gases.
→ Different sets of apparatus are used for different gases and drying agents.
→ Using concentrated sulfuric acid (H2SO4):
• To dry a gas with concentrated sulfuric acid, a double neck bottle or a conical flask with two deli-
very tubes (see the figure) are used. The tube introducing the gas should be immersed in the acid
while the exiting tube should remain out of the acid. Concentrated sulfuric acid is used to dry gases
such as chlorine (Cl2) and hydrogen chloride (HCl). An alkaline gas such as ammonia (NH3) should
not be dried using concentrated sulfuric acid as it will react with it to form a salt solution.
• Remember that base and base don’t react. Same is the case with acids; there's no reaction that will
occur when two acids are mixed.
•

dry gas
out

→ Using solid drying agents:

• Solid drying agents such as quicklime, sodalime or fused calcium chloride are used for drying gases
which may react with conc. sulfuric acid e.g. ammonia (NH3). The drying of gases through solid
drying agents require a U-shaped tube or a specially designed jar with two openings one at the
bottom and the other at the top.
•
dry gas
• out

moist gas dry gas

in out

lumps of
drying agent
lumps of
drying agent
moist gas
in

→ In some exam questions, NaOH might be given. It is useful to remember that NaOH absorbs CO 2.

→ Remember that an alkaline gas should be dried using an alkaline agent or agent that does not react
with it.

→ Exam Technique: When asked which apparatus or set of apparatus is suitable to collect X from a
XYZ, the following strategy might be useful (just think and remove until desired substance
remains). Consider this case, X is the gas that needs to be collected (insoluble in water), Y is water
and Z is soluble in water. Since X is insoluble, passing gas through water will remove Y and Z. X
can then be collected using the suitable apparatus to collect gases as explained above.
Measuring speed of chemical reactions:
The speed of a chemical reaction where a gas is given off can be measured by either collecting the gas
over a certain time interval (the gas collected in the measuring cylinder in a given amount of time gives
the rate of reaction) or recording the progressive loss in mass as the gas escapes into the air. A
convenient method of collecting a gas (especially a water soluble gas) is by using a gas syringe. In this
case, the rate of the reaction between marble chips, CaCO3, and dilute hydrochloric acid is used as an
example. Diagram 5 and 6 shows correct apparatus to measure the rate of the reaction as well. 5 is not
applicable for water – soluble gases.
1 2
loose
measuring plug
cylinder hydrochloric
acid
hydrochloric marble chips
acid
balance
water

marble chips
3 4

hydrochloric
acid burette
tap
funnel

gas syringe

CaCO3 (s) gas syringe

marble chips + HCl (aq)

5 6

burette
gas syringe

water

A stopwatch is used to record the change in mass or volume after certain time intervals.
change in mass or volume
rate =
time taken
When collecting gas over a gas syringe, the gas must not escape somewhere else i.e. it must go to the
syringe. When measuring change in mass, loose plug is used to prevent chemicals splashing out of flask.
However, the gas can escape therefore making it possible to record change of mass at fixed time
intervals. Remember rate can be measured even if it is recording the expansion of balloon due to gas
produced from a reaction.
A reaction produces carbon dioxide gas as shown in set – up 2. The mass of flask and contents is
measured at regular time intervals. The mass of flask and contents continuously decrease due to loss of
carbon dioxide.

mass

0
0 time
Remember: To measure a change in mass, the reaction must take place in a closed apparatus such as a
tube or crucible. Examples are given in the diagram below:

magnesium

magnesium
crucible
air

tripod
heat
heat

An example of incorrect set-up in this case is as follows:

metal tongs

burning
magnesium

→ Remember that reactions of metal or metal carbonate with acid produces gases so a combination of
apparatuses must be used for these experiments.

Metal + dilute acid → metal salt + hydrogen

Metal carbonate + dilute acid → metal salt + carbon dioxide

A dropping funnel is used, it carries a dilute acid which is run into a conical flask with the metal.
And so the gas evolved during the reaction is then contained in a volumetric syringe attached.

• Again, rate of reaction = rate at which volume of gas is collected or the rate at which the reaction
mixture losses mass.
Below are some examples of incorrect apparatus to measure rate of reaction:
1
funnel

measuring
cylinder
CaCO3(s)
+ HCl (aq)

water

stopper

balance

cotton wool

Experiment to collect the measured volumes of gases:

In this case, decomposition of H2O2 is used as an example:

gas syringe

hydrogen peroxide
catalyst

A set amount of hydrogen peroxide and catalyst powder is taken in a flat bottom flask fitted with a gas
syringe. As hydrogen peroxide decomposes in the presence of the catalyst, oxygen gas is produced
which enters the syringe and pushes the plunger outwards. The volume of oxygen given out every 5
seconds is measured and recorded until the gas syringe shows a constant reading.

Mark Scheme:

Way of measuring the gas collected e.g. upturned measuring cylinder / gas
syringe
Method works and is gas tight

Examiner Report:

Most candidates used a gas syringe but a small proportion of the candidates used a test tube or cylinder
that was not graduated. Many of the drawings included a means of heating the aqueous hydrogen
peroxide but this was ignored. Only a small proportion of the candidates failed to label the diagrams.

Experiment to measure speed/rate of reaction:

In this case, reaction between magnesium and dilute sulfuric acid is used as an example.

gas syringe

A small piece of magnesium is taken in a flat bottom flask fitted with dropping funnel and a gas syringe.
Sulfuric acid is added through dropping funnel and stop – clock is started. The volume of gas produced
is noted in the syringe with time. Speed of reaction is calculated with the following formula:
change in volume of gas
speed =
time
Mark Scheme:
gas syringe attached to flask/flask with cotton wool in mouth on top pan balance; [1]
measure volume of gas/mass of flask and contents over time; [1]
rate = change in volume of gas/time or change in mass/ time; [1]
Examiner Report:

Some candidates wrote good answers and drew clearly annotated diagrams. Others did not draw a
diagram. These candidates did not often describe the procedure with sufficient accuracy. Common
errors included vague descriptions e.g. ‘measure the gas in the syringe’ or ‘weigh the apparatus at the
start and at the end’, describing the effects of temperature and of catalysts on the reaction rather than
the course of the reaction or implying that the measurements were only taken once.
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