YOUR NOTES

International A Level Chemistry Edexcel 

3. Practical Skills in Chemistry I

CONTENTS
3.1 Physical Chemistry Core Practicals
3.1.1 Molar Volume of a Gas
3.1.2 Determining Enthalpy Change of Reaction
3.1.3 Determining Concentrations
3.1.4 Standard Solutions
3.2 Inorganic & Organic Chemistry Core Practicals
3.2.1 Hydrolysis of Halogenoalkanes
3.2.2 Chlorination of 2-Methylpropan-2-ol
3.2.3 Propan-1-ol Oxidation
3.2.4 AS Qualitative Analysis
 3.1 Physical Chemistry Core Practicals YOUR NOTES
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3.1.1 Molar Volume of a Gas

Core Practical 1: Measuring the Molar Volume of a Gas

Measuring gas volumes
The volume of gas produced in a reaction can be measured by collecting the gas with a gas
syringe or by the displacement of water

Gas syringe equipment for collecting the gas produced in a reaction

Displacement of water equipment for collecting the gas produced in a reaction

Sample method
For the reaction of hydrochloric acid and sodium carbonate
Na2CO3 (s) + 2HCl (aq) → 2NaCl (aq) + H2O (l) + CO2 (g)
1. Measure out a fixed volume of hydrochloric acid, e.g. 25.0 cm3, into a conical flask
2. Add a known mass of sodium carbonate, e.g. 0.05 g, to the conical flask
3. Immediately connect the gas syringe delivery tube
4. Allow the reaction to go to completion
5. Record the volume of carbon dioxide produced
6. Repeat the experiment with different masses of sodium carbonate, e.g. 0.10 g, 0.15 g, 0.20
g, 0.25 g... 0.50 g
7. Some assumptions are made about the experiment:
The amount of gas lost between adding the sodium carbonate and connecting the
delivery tube is negligible
The delivery tube set up is airtight so no gas is lost
The reaction does go to completion
Sample results
Mass Volume Results Table
 YOUR NOTES
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The results are then plotted on to a graph

Mass of sodium carbonate on the x-axis and volume or carbon dioxide produced on
the y-axis
Anomalous results are ignored and one straight line (or one smooth curve) of best fit is
added

Analysis
Read off the volume of gas produced for a sensible mass of sodium carbonate, e.g. 0.35 g
produces 79.0 cm3
The mass of sodium carbonate may be specified in an exam question
Na2CO3 (s) + 2HCl (aq) → 2NaCl (aq) + H2O (l) + CO2 (g)
From the reaction equation, one mole of sodium carbonate produces one mole of carbon
dioxide
Calculate the molar mass of sodium carbonate
(2 x 23.0) + 12.0 + (3 x 16.0) = 106.0
Calculate the number of moles of sodium carbonate, using the mass from your graph
reading
mass 0. 35
Moles = = = 0.0033 moles
molar mass 106 . 0
Convert the volume of carbon dioxide from your graph reading from cm3 to dm3
 79 . 0 cm 3
= 0.079 dm3 YOUR NOTES
1000

Calculate the molar volume of gas produced:
volume 0. 079
Molar gas volume = = = 23.93 dm3
moles 0. 0033

Application
This experiment can be used to determine the identity of an unknown metal, M, in a metal
carbonate, MCO3
This process can be applied to thermal decomposition of metal carbonates as well as their
reaction with acid

 Worked Example
At room temperature and pressure, 0.950 g of a Group 2 metal carbonate, MCO3,
reacted with hydrochloric acid to produce 226.0 cm3 of carbon dioxide.
Deduce the identity of the metal M.

Answer:
Step 1: Find the number of moles of carbon dioxide released using the volume produced at
room temperature and pressure:
volume of gas (dm 3 )
number of moles of CO2 =
molar gas volume (dm 3 )
0. 226
n(CO2) = = 0.009417 mol
24

Step 2: Find the number of moles of metal carbonate, MCO3

One mole of metal carbonate will release one mole of carbon dioxide
Number of moles of CO2 = number of moles of MCO3
n(MCO3) = 0.009417 mol
Step 3: Calculate the molar mass of MCO3
 Mr = mass
YOUR NOTES
moles
0. 950 
Mr = = 100.9 g mol-1
0. 009417

Step 4: Calculate the atomic mass of M in MCO3 and deduction of the Group 2 metal
Mr = Σ(atomic masses)
100.9 = M + 12.0 + (3 x 16.0)
M = 100.9 - 60.0 = 40.9 g mol-1
The closest Group 2 atomic mass is calcium at 40.1 g mol-1, therefore the metal M is
calcium

 Exam Tip
Careful: Examiners can write these questions to include the following distractions:
The molar mass of the metal carbonate / MCO3 is close to the mass of a Group
2 metal
The mass of the carbonate ion needs to be subtracted from the molar
mass in order to deduce the identity of the metal
The atomic mass of the metal is close the atomic mass of another metal, not
necessarily a Group 2 metal
Read the question as it will provide information about the metal
The above points can be applied to any metal carbonate, not just Group 2 metal
carbonates although they are the most common

Hazards, risks and precautions

The hazards associated with acids depend on the type and concentration of the acid
Most dilute acids either require no hazard symbol or they are an irritant, so require the
symbol to show they are harmful to health
Eye protection should be worn when handling
Moderately concentrated acids are often corrosive
In addition to eye protection, gloves should also be worn
Some concentrated acids, e.g. nitric acid, are oxidising which can cause or intensify a fire in
contact with combustible materials
Eye protection and gloves are necessary when handling concentrated acids and the
use of a fume cupboard is often required
 3.1.2 Determining Enthalpy Change of Reaction YOUR NOTES
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Core Practical 2: Determining Enthalpy Change of Reaction
Measuring enthalpy changes
Calorimetry is a technique used to measure changes in enthalpy of chemical reactions
A calorimeter can be made up of a polystyrene drinking cup, a vacuum flask or metal can

A polystyrene cup can act as a calorimeter to find enthalpy changes in a chemical reaction
The energy needed to raise the temperature of 1 g of a substance by 1 K is called
the specific heat capacity (c) of the liquid
The specific heat capacity of water is 4.18 J g-1 K-1
The energy transferred as heat can be calculated by:

Equation for calculating energy transferred in a calorimeter

Enthalpy changes for reactions in solution
The principle of these calorimetry experiments is to carry out the reaction with an excess of
one reagent and measure the temperature change over the course of a few minutes
 The apparatus needed to carry out an enthalpy of reaction in solution calorimetry YOUR NOTES
experiment is shown above 
Sample method for a displacement reaction
1. Using a measuring cylinder place 25 cm3 of the 1.0 mol dm-3 copper(II) sulphate solution
into the polystyrene cup
2. Weigh about 6 g of zinc powder - as this is an excess there is no need to be very accurate
3. Draw a table to record the initial temperature and then the temperature and time every half
minute up to 9.5 minutes
4. Put a thermometer or temperature probe in the cup, stir, and record the temperature every
half minute for 2.5 minutes
5. At precisely 3 minutes, add the zinc powder to the cup (DO NOT RECORD THE
TEMPERATURE AT 3 MINUTES)
6. Continue stirring and record the temperature for an additional 6 minutes
For the purposes of the calculations, some assumptions are made about the experiment:
That the specific heat capacity of the solution is the same as pure water, i.e. 4.18 J g-
1 K-1
That the density of the solution is the same as pure water, i.e. 1 g cm-3
The specific heat capacity of the container is ignored
The reaction is complete
There are negligible heat losses
Temperature correction graphs
For reactions which are not instantaneous there may be a delay before the maximum
temperature is reached
During that delay the substances themselves may be losing heat to the surroundings, so
that the true maximum temperature is never actually reached
To overcome this problem we can use graphical analysis to determine the maximum
enthalpy change
 YOUR NOTES
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A temperature correction graph for a metal displacement reaction between zinc and
copper sulfate solution. The zinc is added after 4 minutes
The steps to make a temperature correction graph are:
1. Take a temperature reading before adding the reactants for a few minutes to get a steady
value
2. Add the second reactant and continue recording the temperature and time
3. Plot the graph and extrapolate the cooling part of the graph until you intersect the time at
which the second reactant was added
Analysis
Use both extrapolated lines to calculate ΔT as shown on the graph
Use the equation q = mcΔT to calculate the energy transferred
q = energy transferred
m = mass - this will be the mass of the 25 cm3 solution which will be 25 g (assuming a
density of 1 g cm-3)
c = specific heat capacity - this will be assumed to be 4.18 J g-1 K-1, which is the specific
heat capacity of water
ΔT = the temperature change from the graph
Convert your value for energy transferred from J into kJ
q
Then use the equation ΔH = to calculate the enthalpy change for the reaction
n
q = energy transferred
n = number of moles - this would be the number of moles of the limiting reagent, which
means that you will have an extra calculation to do to determine whether this is the zinc
or the copper sulfate
Remember that in the example above, the temperature of the reaction mixture increased
which means that the reaction is exothermic and should, therefore, have a negative value
 3.1.3 Determining Concentrations YOUR NOTES
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Core Practical 3: Hydrochloric Acid Concentration
Performing the Titration
The key piece of equipment used in the titration is the burette
Burettes are usually marked to a precision of 0.10 cm3
Since they are analogue instruments, the uncertainty is recorded to half the smallest
marking, in other words to ±0.05 cm3
The end point or equivalence point occurs when the two solutions have reacted
completely and is shown with the use of an indicator

The steps in a titration

A white tile is placed under the conical flask while the titration is performed, to make it easier
to see the colour change
 YOUR NOTES
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Titrating
The steps in a titration are:
Measuring a known volume (usually 20 or 25 cm3) of one of the solutions with
a volumetric pipette and placing it into a conical flask
The other solution is placed in the burette
To start with, the burette will usually be filled to 0.00 cm3
A few drops of the indicator are added to the solution in the conical flask
The tap on the burette is carefully opened and the solution added, portion by portion,
to the conical flask until the indicator starts to change colour
As you start getting near to the end point, the flow of the burette should be slowed
right down so that the solution is added dropwise
You should be able to close the tap on the burette after one drop has caused the
colour change
Multiple runs are carried out until concordant results are obtained
Concordant results are within 0.1 cm3 of each other
Recording and processing titration results
Both the initial and final burette readings should be recorded and shown to a precision of
±0.05 cm3, the same as the uncertainty
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A typical layout and set of titration results

The volume delivered (titre) is calculated and recorded to an uncertainty of ±0.10 cm3
The uncertainty is doubled, because two burette readings are made to obtain
the titre (V final – V initial), following the rules for propagation of uncertainties
Concordant results are then averaged, and non-concordant results are discarded
The appropriate calculations are then done
 YOUR NOTES
 Worked Example

25.0 cm3 of hydrochloric acid was titrated with a 0.200 mol dm-3 solution of
sodium hydrogencarbonate, NaHCO3.
NaHCO3 + HCl → NaCl + H2O + CO2
Use the following results to calculate the concentration of the acid, to 3 significant
figures.

Answer
Step 1: Calculate the average titre
22. 80 + 22. 80
Average titre = = 22.80 cm3
2
Step 2: Calculate the number of moles of sodium hydrogencarbonate
22. 80
Moles = x 0.200 = 4.56 x 10-3 moles
1000
Step 3: Calculate (or deduce) the number of moles of hydrochloric acid
The stoichiometry of NaHCO3 : HCl is 1 : 1
Therefore, the number of moles of sodium hydrogencarbonate is also 4.56 x 10-3
moles
Step 4: Calculate the concentration of hydrochloric acid
moles 4 . 56 × 10−3
Concentration = = = = 0.182 mol dm-3
volume (25. 0 / 1000)
 3.1.4 Standard Solutions YOUR NOTES
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Core Practical 4: Preparing a Standard Solution
Volumetric Analysis
Volumetric analysis is a process that uses the volume and concentration of one chemical
reactant (a volumetric solution) to determine the concentration of another unknown
solution
The technique most commonly used is a titration
The volumes are measured using two precise pieces of equipment,
a volumetric or graduated pipette and a burette
Before the titration can be done, the standard solution must be prepared
Specific apparatus must be used both when preparing the standard solution and when
completing the titration, to ensure that volumes are measured precisely

Some key pieces of apparatus used to prepare a volumetric solution and perform a simple
titration
1. Beaker
2. Burette
3. Volumetric Pipette
4. Conical Flask
5. Volumetric Flask
Making a Volumetric Solution
Chemists routinely prepare solutions needed for analysis, whose concentrations are
known precisely
These solutions are termed volumetric solutions or standard solutions
They are made as accurately and precisely as possible using three decimal place balances
and volumetric flasks to reduce the impact of measurement uncertainties
The steps are:
 YOUR NOTES
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Volumes & concentrations of solutions

The concentration of a solution is the amount of solute dissolved in a solvent to make 1
dm3 of solution
The solute is the substance that dissolves in a solvent to form a solution
The solvent is often water
A concentrated solution is a solution that has a high concentration of solute
A dilute solution is a solution with a low concentration of solute
Concentration is usually expressed in one of three ways:
 moles per unit volume YOUR NOTES
mass per unit volume 
parts per million

 Worked Example
Calculate the mass of sodium hydroxide, NaOH, required to prepare 250 cm3 of a
0.200 mol dm-3 solution

Answer:
Step 1: Find the number of moles of NaOH needed from the concentration and volume:
number of moles = concentration (mol dm-3) x volume (dm3)
n = 0.200 mol dm-3 x 0.250 dm3
n = 0.0500 mol
Step 2: Find the molar mass of NaOH
M = 22.99 + 16.00 + 1.01 = 40.00 g mol-1
Step 3: Calculate the mass required
mass = moles x molar mass
mass = 0.0500 mol x 40.00 g mol-1 = 2.00 g
 3.2 Inorganic & Organic Chemistry Core Practicals YOUR NOTES

3.2.1 Hydrolysis of Halogenoalkanes

Core Practical 5: Investigating Halogenoalkane Hydrolysis

Halogenoalkanes can be hydrolysed with an aqueous solution of sodium hydroxide
(NaOH) or potassium hydroxide (KOH)
This reaction is very slow at room temperature, so the reaction mixture is warmed
The rate of this reaction depends on the type of halogen in the halogenoalkane
The stronger the C-X bond, the slower the rate of the reaction
In terms of bond enthalpy, C-F > C-Cl > C-Br > C-I
Fluoroalkanes do not react at all, but iodoalkanes have a very fast rate of reaction

The halogen is replaced by the nucleophile, OH-

This reaction could also be done with water as the nucleophile, but it is very slow
The hydroxide ion is a better nucleophile than water as it carries a full negative charge
In water, the oxygen atom only carries a partial charge

A hydroxide ion is a better nucleophile as it has a full formal negative charge whereas the
oxygen atom in water only carries a partial negative charge; this causes the nucleophilic
substitution reaction with water to be much slower than the aqueous alkali
Measuring the rate of hydrolysis
Acidified silver nitrate can be used to measure the rate of hydrolysis of halogenoalkanes
Set up three test tubes in a 50 oC water bath, with a mixture of ethanol and acidified silver
nitrate
Add a few drops of a chloroalkane, bromoalkane and an iodoalkane to each test tube and
start a stop watch
Time how long it takes for the precipitates to form
The precipitate will form as the reaction progresses and the halide ions are formed
A white precipitate will form from the chloroalkane, a cream precipitate will form from the
bromoalkane and a yellow precipitate will form from the iodoalkane
The yellow precipitate will form the fastest
This is because the C-I bond has the lowest bond enthalpy, so it is the easiest to break YOUR NOTES
and will cause the I- ions to form the fastest 
The white precipitate will form the slowest
This is because the C-Cl bond has the highest bond enthalpy, so it is the hardest to
break and will cause the Cl- ions to form the slowest
 3.2.2 Chlorination of 2-Methylpropan-2-ol YOUR NOTES

Core Practical 6: Chlorination of 2-Methylpropan-2-ol
Synthesis of a haloalkane from an alcohol
Measure 8 cm3 of 2-methylpropan-2-ol in a measuring cylinder
Pour the 2-methylpropan-2-ol into a separating funnel
Using a fume hood, add 20 cm3 of concentrated hydrochloric acid to the separating funnel
in small portions of 2 - 3 cm3 making sure to release the pressure by opening the stopper
after each addition
Leave the separating funnel to stand in the fume hood for 20 minutes and gently shake the
separating funnel at 2 minute intervals
Allow the layers to separate and dispose of the lower aqueous layer by opening the tap
Add add sodium hydrogen carbonate solution in small portions to the funnel and gently
shake the funnel, again, release the pressure at regular intervals
This removes acidic impurities
Once these layers have separated, open the tap once more and dispose of the queues
layer
Pour the organic layer into a clean dry conical flask and add two spatulas of magnesium
sulfate
This will remove water
Once clear, decant the liquid into distillation apparatus
Distill the liquid and collect the distillate in the range of 47 - 53oC

A separating funnel allows the product to be cleaned and isolated

 Exam Tip YOUR NOTES
 This practical requires a fume hood as concentrated hydrochloric acid is very volatile

at room temperature and hydrogen chloride gas is released from the solution
quickly when the cover to a container or bottle is removed.
When using a fume hood you must make sure the window is not open above the
safety line, otherwise, the exhaust system will not be strong enough to draw in the
fumes. Therefore toxic, poisonous, harmful or irritant fumes will escape into the
laboratory
If heating is involved in the experiment taking place in the fume hood, having the
window open above the safety line will mean that carbon monoxide or soot could
also escape.
 3.2.3 Propan-1-ol Oxidation YOUR NOTES

Core Practical 7: Oxidation of Propan-1-ol
Oxidation of propan-1-ol
Primary alcohols can be oxidised to form aldehydes which can undergo further oxidation to
form carboxylic acids
When propan-1-ol is oxidised, ethanal is produced and when oxidised further
propanoic acid will be formed
Synthesis and purification of propanal and propanoic acid
Carefully add 20 cm3 of acidified potassium dichromate(VI) solution, K2Cr2O7 (aq), to a 50
cm3 pear-shaped flask and cool the flask in an iced water bath
Set up the reflux apparatus keeping pear shaped flask cool
Place anti-bumping granules into the pear shaped flask
Measure out 1 cm3 of propan-1-ol
Using a pipette, slowly add the propan-1-ol drop wise into the reflux condenser
When the propan-1-ol has been added remove the ice bath and allow to warm up to room
temperature
Position the flask over an electric heater or in a water bath and heat for 20 minutes
Propan-1-ol is flammable, therefore. naked flames should not be used when heating
which is why the use of an electric heater or water bath is an important safety
precaution
Purify the product using distillation apparatus

Reflux apparatus for the oxidation of propan-1-ol to propanoic acid

 YOUR NOTES


Oxidation of propan-1-ol by acidified K2Cr2O7 to form propanal by distillation

Hazards, risks and precautions
 YOUR NOTES


The alcohols used are flammable and often harmful to health, e.g, propan‐1‐ol, butan‐1‐ol,
pentan‐1‐ol
The alcohols should be kept away from naked flames, e.g. a Bunsen burner
Avoid contact with the skin and breathing in the vapour
A fume cupboard can be used for harmful alcohols
Potassium dichromate is a strong oxidising agent and should be handled with care
Spillages should be mopped up right away with plenty of water
 3.2.4 AS Qualitative Analysis YOUR NOTES

Core Practical 8: Analysis of Inorganic and Organic Unknowns
Test Tube Reactions
Simple test tube reactions can be done to identify the following ions:
Ammonium ions (NH4+)
Halide ions (X-) - covered in 2.3.4 Halide Ion Reactions
Carbonate ions (CO32-) and hydrogencarbonate ions (HCO3-)
Sulfate ions (SO42-)
If the sample to be tested is a solid, then it must be dissolved in deionised water and made
into an aqueous solution
Testing for Ammonium Ions
About 10 drops of a solution containing ammonium ions, such as ammonium chloride,
should be added to a clean test tube
About 10 drops of sodium hydroxide should be added using a pipette
Overall equation: NH4Cl (aq) + NaOH (aq) → NH3 (g) + H2O (l) + NaCl (aq)
Ionic equation: NH4+ (aq) + OH- (aq) → NH3 (g) + H2O (l)
The test tube should be swirled carefully to ensure that it is mixed well
The test tube of the solution should then be placed in a beaker of water, and the beaker of
water should be placed above a Bunsen burner, so that it can become a water bath
As the solution is heated gently, fumes will be produced
A pair of tongs should be used to hold a damp piece of red litmus paper near the mouth of
the test tube, to test the fumes
The red litmus paper will change colour and become blue in the presence of ammonia gas
 Damp red litmus paper turning blue in the presence of ammonia gas YOUR NOTES
Testing for Carbonate Ions 
A small amount (around 1 cm3) of dilute hydrochloric acid should be added to a test tube
using a pipette
An equal amount of sodium carbonate solution should then be added to the test tube using
a clean pipette
Overall equation: 2HCl (aq) + Na2CO3 (aq) → 2NaCl (aq) + CO2 (g) + H2O (l)
Ionic equation: 2H+ (aq) + CO32- (aq) → CO2 (g) + H2O (l)
As soon as the sodium carbonate solution is added, a bung with a delivery tube should be
attached to the test tube
The delivery tube should transfer the gas which is formed into a different test tube
which contains a small amount of limewater (calcium hydroxide solution)
Carbonate ions will react with hydrogen ions from the acid to produce carbon dioxide gas
Carbon dioxide gas will turn the limewater milky

When carbon dioxide gas is bubbled into limewater it will turn cloudy as calcium carbonate
is produced
A similar reaction is seen with sodium hydrogen carbonate, but the equations are:
Overall equation: HCl (aq) + NaHCO3 (aq) → NaCl (aq) + CO2 (g) + H2O (l)
Ionic equation: H+ (aq) + HCO3- (aq) → CO2 (g) + H2O (l)
Testing for Sulfate Ions
 Acidify the sample with dilute hydrochloric acid and then add a few drops of aqueous YOUR NOTES
barium chloride 
If a sulfate is present then a white precipitate of barium sulfate is formed:
Ba2+ (aq) + SO42- (aq) → BaSO4 (s)

A white precipitate of barium sulfate is a positive result for the presence of sulfate ions

 Exam Tip
HCl is added first to remove any carbonates which may be present and would also
produce a precipitate and interfere with the results.

Flame tests
Metal ions produce a colour if heated strongly in a flame
Ions from different metals produce different colours YOUR NOTES
The flame test is thus used to identify metal ions by the colour of the flame they produce 
Dip the loop of an unreactive metal wire such as nichrome or platinum in concentrated
acid, and then hold it in the blue flame of a Bunsen burner until there is no colour change
This cleans the wire loop and avoids contamination
This is an important step as the test will only work if there is just one type of ion present
Two or more ions means the colours will mix, making identification erroneous
Dip the loop into the solid sample and place it in the edge of the blue Bunsen flame
Avoid letting the wire get so hot that it glows red otherwise this can be confused with a
flame colour

Diagram showing the technique for carrying out a flame test

Colours Observed in Flame Tests
YOUR NOTES
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