OCR A Level Chemistry A Your notes

Physical Chemistry Practicals

Contents
Moles Determination
Acid-Base Titration
Determination of Enthalpy Changes

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Moles Determination
Your notes

PAG 1: Moles determination

There are a series of suggested practicals for PAG 1 - Moles Determination
PAG 1.1 - Determination of the composition of copper(II) carbonate basic
PAG 1.2 - Determination of the relative atomic mass of magnesium
PAG 1.3 - Determination of the formula of magnesium oxide
All three PAGs use experimental data to calculate the number of moles and the final
answer
This can be done by:
Measuring gas volumes
In these experiments, a reaction occurs which produces a gas
The number of moles of gas produced is calculated
The stoichiometric ratio of the chemical reaction is then used to determine the
final answer
For this style of experiment, the final answer could be:
The composition of copper(II) carbonate
The relative atomic mass of magnesium
Other practicals can be used in place of the suggested practicals
This means that you need to apply your knowledge to other examples
Measuring changes in mass
In these experiments, a reaction produces an increase or decrease in mass
The suggested practical for this is determining the formula of magnesium oxide
A known mass of magnesium is combusted and the mass of the magnesium
oxide product is measured
The number of moles of magnesium and oxygen are calculated to determine
the ratio of each element in the formula of the magnesium oxide
A similar practical can be performed on hydrated salts, e.g. CuSO4•xH2O
Heat the hydrated salt to a constant mass
Then, use the decrease in mass to calculate the number of moles of water of
crystallisation
This is not a PAG practical

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PAG 1.1: Determination of the composition of
copper(II) carbonate basic Your notes
Method
1. Set up the apparatus using a measuring cylinder sitting in water bath connected to a
conical flask
2. Measure a known mass of [Link](OH)2 and add it to the conical flask
3. Add an excess of sulfuric acid into the conical flask and immediately insert the stopper.
The gas produced will collect in the measuring cylinder
4. Record the final volume of carbon dioxide in the measuring cylinder

Equipment set up for gas collection by displacement

Examiner Tips and Tricks

As an alternative a gas syringe could be set up to measure the volume of gas
produced

Calculations
We can find the number of moles, n, of CO2 produced using the measured volume, v,
with the following equation:

V (dm 3 ) V ( cm 3)
n= or n =
24. 0 24000
Remember: 24.0 dm3 is the volume of 1 mole of gas
This calculation is only correct for a reaction at room temperature and pressure (101
kPa or 1 atmosphere)

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 If the calculation is completed under different conditions, then a rearranged ideal
gas equation should be used:
Your notes
PV
n=
RT
We can use the overall equation for the reaction to figure out the number of moles of
copper carbonate that reacted
CuCO3 + H2SO4 → CuSO4 + H2O + CO2
Molar ratio for CuCO3 : CO2 is 1:1
The mass, m, of CuCO3 can then be determined using:
m = n x Mr
As our original sample contained [Link](OH)2 we need to determine the percentage
by mass of CuCO3 present in the original sample

Source of errors
Some carbon dioxide may escape from the conical flask before inserting the bung
Avoid this by inserting the bung immediately after adding the acid to the conical
flask
Some of the copper carbonate may not react
Swirl the conical flask to mix the contents and ensure the reaction goes to
completion
Carbon dioxide may dissolve in the water
Use a gas syringe to measure the volume of CO2
Some copper carbonate remains on the weighing apparatus / is not transferred to the
flask
Weigh the apparatus with and without and copper carbonate
The difference between these gives the exact amount added to the conical flask

PAG 1.2: Determination of the relative atomic mass of

magnesium
This practical is completed in a similar way to PAG 1.1 - Determination of the composition
of copper(II) carbonate

Method
Set up the apparatus using a measuring cylinder sitting in water bath connected to a
conical flask
Measure a known mass of magnesium and add it to the conical flask

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 Add an excess of sulfuric acid into the conical flask and immediately insert the stopper.
The gas produced will collect in the measuring cylinder
Your notes
Record the final volume of hydrogen gas in the measuring cylinder

Calculations
We can find the number of moles, n, of H2 produced using the measured volume, v, with
the following equation:

v
n=
24
Remember: 24 dm3 is the volume of 1 mole of gas
We can use the overall equation for the reaction to figure out the number of moles of
copper carbonate that reacted
Mg + H2SO4 → MgSO4 + H2
Molar ratio for Mg : H2 is 1:1
The mass, m, of Mg can then be determined using:
m = n x Mr
Source of errors
Some hydrogen may escape from the conical flask before inserting the bung
This can be avoided by inserting the bung as soon as the acid is poured into the
conical flask
Some of the magnesium may not react
Use magnesium powder instead of ribbon
Add an excess of acid
Swirl the conical flask to mix the contents and ensure the reaction goes to
completion
Some magnesium remains on the weighing apparatus / is not transferred to the flask
Weigh the apparatus with and without and magnesium
The difference between these gives the exact amount added to the conical flask

Examiner Tips and Tricks

The relative atomic mass of magnesium cannot be determined by mass loss
experiments
This is because the mass of hydrogen lost is insignificant

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PAG 1.3: Determination of the formula of magnesium
oxide Your notes
Method
A known mass of magnesium is measured and placed in a crucible with a lid
The magnesium is then heated to react with oxygen in the air
The lid of the crucible needs to be open enough to allow sufficient air in but closed
enough to not lose the product
The mass of the product is then measured

Calculations
With the mass recordings, the original mass of magnesium is known and the mass of
oxygen can be deduced
The number of moles of magnesium and the number of moles of oxygen can then be
calculated:

mass
moles =
Mr
The molar ratio of magnesium : oxygen is then used to determine the formula of
magnesium oxide,
For example, if the molar ratio was 2 magnesium : 3 oxygen then the formula would
be Mg2O3

Sources of error
Some magnesium oxide may escape from the crucible
This cannot be avoided
It can be reduced by careful heating and careful placement of the crucible lid
Some of the magnesium may not react
Using magnesium ribbon can be better than powder because:
Once ignited, the ribbon should continue to burn
Using powder can lead to a loss of product
Using powder can result in some magnesium not reacting
If magnesium ribbon is used, it can be cleaned with sandpaper / glasspaper to
remove any oxide coating already formed
Some magnesium may remain on the weighing apparatus and not be transferred to the
crucible
Weigh the weighing apparatus with and without magnesium on it

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 The difference between these gives the exact amount added to the crucible

Practical skills reminder Your notes

These PAG 1 practicals develop core experimental techniques, including:
Accurately measuring mass using balances to determine reactant and product
quantities
Measuring gas volumes by displacement or using a gas syringe
Recording reaction time and ensuring safe procedures, such as immediate bung
insertion
Using heat sources and crucibles safely to drive reactions to completion
Applying balanced equations and molar ratios to calculate unknown quantities
Identifying and minimising sources of error in practical work
Handling equipment confidently: measuring cylinders, bunsen burners, water
baths, and conical flasks

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 Acid-Base Titration
Your notes

PAG 2: Acid-base titration

There are a series of suggested practicals for PAG 2 - Acid-base titration
PAG 2.1: Determination of the concentration of hydrochloric acid
Making a standard solution of sodium hydrogencarbonate
Titrating this against hydrochloric acid
Determining the concentration of the acid
PAG 2.2: Determination of the molar mass of an acid
Making a solution of an unknown hydrated acid (e.g. citric acid monohydrate)
Titrating this against a sodium hydroxide solution of known concentration.
Determining the molar mass of the acid and, with additional information, the
formula of the acid
PAG 2.3: Identification of an unknown carbonate
Making a solution of an unknown Group 1 carbonate
Titrating this solution against hydrochloric acid of a known concentration
Determine the molar mass of the carbonate and the identity of the metal
All three suggested practicals use volumetric analysis
This requires making standard solutions and completing titration experiments
The main difference between the practicals is how the titration results are
processed

Volumetric analysis
Volumetric analysis 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
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

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 Your notes

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
This reduces the impact of measurement uncertainties
The steps are:

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 Your notes

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

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 Concentration is usually expressed in one of three ways:
moles per unit volume (mol dm-3) Your notes
mass per unit volume (g dm-3)
parts per million (ppm)

Worked Example
Calculate the mass of sodium hydrogencarbonate, NaHCO3, required to prepare 250
cm3 of a 0.200 mol dm-3 solution
Answer:
1. Calculate the moles of NaHCO3 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
2. Calculate the molar mass of NaHCO3
Mr = 23.0 + 1.0 + 12.0 + (16.0 x 3) = 84.0 g mol-1
3. Calculate the mass of NaHCO3 required
mass = moles x molar mass
mass = 0.0500 mol x 84.0 g mol-1 = 4.2 g

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

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 Your notes

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

Titrating

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 The steps in a titration are:
Measuring a known volume (usually 20 or 25 cm3) of one of the solutions with Your notes
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 opened and the solution is slowly added 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

A typical layout and set of titration results

The volume delivered (titre) is calculated and recorded to an uncertainty of ±0.10 cm3

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 The uncertainty is doubled
This is because two burette readings are made to obtain the titre (V final – V initial) Your notes
This follows the rules for propagation of uncertainties
Concordant results are then averaged, and non-concordant results are discarded
The appropriate calculations are then done

Worked Example
PAG 2.1: Determining hydrochloric acid concentration
25.0 cm3 of hydrochloric acid was titrated with a 0.200 mol dm-3 solution of sodium
hydrogencarbonate, NaHCO3.
NaHCO3 (aq) + HCl (aq) → NaCl (aq)+ H2O (l) + CO2 (g)
Use the following results to calculate the concentration of the acid, to 3 significant
figures.

Rough Run 1 Run 2 Run 3

Initial burette reading / cm3 (±0.05 cm3) 0.00 23.15 0.20 23.00

Final burette reading / cm3 (±0.05 cm3) 23.75 45.95 23.00 46.10

Volume delivered / cm3 (±0.10 cm3) 23.75 22.80 22.80 23.10

Answer:
1. Calculate the average titre from concurrent titrations only
Concurrent titrations are within 0.10 cm3 of each other
22 . 80 + 22 . 80
Average titre = = 22.80 cm3
2

2. Calculate the number of moles of sodium hydrogencarbonate

22 . 80
Moles of NaHCO3 = x 0.200 = 4.56 x 10-3 moles
1000

3. Calculate (or deduce) the number of moles of hydrochloric acid

The stoichiometry of NaHCO3 : HCl is 1 : 1
Moles of HCl = 4.56 x 10-3 moles
4. Calculate the concentration of hydrochloric acid
moles
Concentration =
volume

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 4. 56 × 10 −3
Concentration = = 0.182 mol dm-3
(25 . 0 / 1000 )
Your notes

Worked Example
PAG 2.2: Determining the molar mass of an acid
0.133 g of an unknown monoprotic acid is added to a 1.0 dm3 volumetric flask and
made up to the mark with distilled water. This solution is titrated with 0.070 mol dm-3
sodium hydroxide solution. The average titre required for the neutralisation of the
unknown monoprotic acid is 23.40 cm3.
i) Calculate the molar mass of the unknown acid.
ii) The unknown monoprotic acid is a halogenated acid. Identify the unknown
monoprotic acid.
Answer:
Part i)
1. Calculate the number of moles of sodium hydroxide
23 . 40
Moles of NaOH = 0. 070 × = 1.638 x 10-3 moles
1000

2. State the number of moles of the unknown monoprotic acid

1. The stoichiometry of HX : NaOH is 1 : 1
Moles of HX = 1.638 x 10-3 moles
3. Calculate the molar mass of the unknown monoprotic acid
mass
Mr =
moles

0. 133
Mr = −3
= 81.20 g mol-1
1. 638 × 10

Part ii)
1. Calculate the mass of the halogen
81.20 - 1.0 = 80.2
2. Use the periodic table to identify the halogen
80.2 ≈ Bromine (79.9)
3. State the final answer
The unknown monoprotic acid is HBr / hydrobromic acid

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Examiner Tips and Tricks
You can potentially be asked to calculate the molar mass of any unknown acid Your notes
This includes monoprotic, diprotic and even triprotic acids
You must account for the stoichiometry of the neutralisation reaction
You have to be given information to deduce the identity of the unknown acid

Worked Example
PAG 2.3: IdentifYING an unknown carbonate
1.19 g of an unidentified Group 1 metal carbonate, X2CO3, was dissolved in water to
produce a 250.0 cm³ standard solution. 25.0 cm³ aliquots of this solution were
titrated with 0.150 mol dm3 hydrochloric acid. The average titre for this experiment
was found to be 14.95 cm3.
Identify the Group 1 metal in the unidentified metal carbonate X2CO3.
Answer
1. Calculate the number of moles of hydrochloric acid
14 . 95
Moles of HCl = 0. 150 × = 2.2425 x 10-3 moles
1000

2. Calculate the number of moles of X2CO3

The stoichiometric ratio is 1X2CO3 : 2HCl
2. 2425 × 10 −3
Moles of X2CO3 = = 1.12125 x 10-3 moles
2

3. Calculate the mass of X2CO3 in the 25.0 cm3 aliquot

1. 19
= 0.119 g
10

4. Calculate the molar mass of X2CO3

mass
Mr =
moles

0. 119
Mr = = 106.132 g mol-1
1. 12125 × 10 −3

5. Calculate the mass of X in X2CO3

106 . 132 − 12 . 0 − ( 3 × 16 . 0 )
= 23.066
2

6. Use the periodic table to identify the Group 1 element in X2CO3

23.066 ≈ Sodium / Na (relative mass of 23.0)

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 Examiner Tips and Tricks
Your notes
Careful: Examiners have been known to construct this question to get the mass
of X as around 86.0 - 86.5
This then gets a mixture of answers of X = rubidium or francium
This happens because students use the wrong number to identify the
element
Rubidium has a mass number of 85.5
Francium has an atomic number of 87

Practical skills reminder

These titration-based practicals help develop essential experimental techniques,
including:
Accurately measuring volumes using volumetric pipettes, burettes, and volumetric
flasks
Preparing standard solutions with appropriate equipment and minimising
measurement uncertainties
Recording burette readings to the correct precision and accounting for
instrumental uncertainty
Performing titrations safely and effectively, using indicators and controlling flow
rates near the endpoint
Calculating concentrations, molar masses, and formulae using balanced equations
and volume data
Interpreting titration data to identify unknown compounds, following correct
stoichiometric reasoning

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 Determination of Enthalpy Changes
Your notes

PAG 3: Determination of enthalpy

changes
Calorimetry is a technique used to measure changes in enthalpy of chemical reactions
A calorimeter can be 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

Specific heat capacity is the energy needed to raise the temperature of 1 g of a

substance by 1 K
The specific heat capacity of water is 4.18 J g-1 K-1
The energy transferred as heat can be calculated by:
q = m c ΔT
Where:
q = heat energy transferred, J
m = mass of water, g
c = specific heat capacity, J g-1 K-1
ΔT = temperature change, K

There are two types of calorimetry experiments for you to know:

Enthalpy changes of reactions in solution

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 Enthalpy changes of combustion
For both calorimetry experiments, you should be able to: Your notes
Outline the experiment
Process experimental data using calculations or graphical methods

PAG 3.1: Determination of the enthalpy change of

neutralisation
The principle of these calorimetry experiments is to mix stoichiometric quantities of acid
and alkali then measure the temperature change over the course of a few minutes
The apparatus needed to carry out an enthalpy of reaction in solution calorimetry
experiment is shown above
Sample method for a neutralisation reaction
1. Using a measuring cylinder, place 25.0 cm3 of 1.0 mol dm-3 hydrochloric acid into the
polystyrene cup
2. Using a measuring cylinder, place 25.0 cm of 1.0 mol dm-3 sodium hydroxide solution
into a separate polystyrene cup
3. Draw a table to record:
The initial temperature of the HCl (aq) and NaOH (aq)
The temperature of the combined reaction mixture every half minute up to 9.5
minutes
4. Put a thermometer or temperature probe in each cup, stir, and record the temperature
every half minute for 2½ minutes
5. At precisely 3 minutes, add the contents of the two cups together
DO NOT RECORD THE TEMPERATURE AT 3 MINUTES
6. Continue stirring and recording the temperature for 6 minutes
For the purposes of the calculations, the following experimental assumptions are made:
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

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 During that delay the substances may lose heat to the surroundings
This means that the true maximum temperature is never reached Your notes
To overcome this problem we can use graphical analysis to determine the maximum
enthalpy change

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
4. Extrapolate the cooling section of the graph until you intersect the time at which the
second reactant was added
For the neutralisation experiment, there can be two main possibilities:
1. The initial temperatures of the HCl (aq) and NaOH (aq) are the same
They can both be plotted as the same line
The graph can be extrapolated to determine the change in temperature at 3
minutes
The subsequent q = m c ΔT calculation can be completed
2. The initial temperatures of the HCl (aq) and NaOH (aq) are the different
The initial temperature of the HCl (aq) is plotted as one line
The initial temperature of the NaOH (aq) is plotted as a separate line on the
same graph

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 The temperature of the reaction mixture can be plotted
Two extrapolations are performed Your notes
One for the HCl (aq) and another for the NaOH (aq)
The subsequent q = m c ΔT calculations for the HCl (aq) and NaOH (aq) are
completed
Calculating the average of those two values gives the overall enthalpy change
of neutralisation

PAG 3.2 Determination of an enthalpy change of

reaction by Hess' law
This practical is an extended variation of PAG 3.1

Examiner Tips and Tricks

The exam board recommends:
The reaction of potassium carbonate with hydrochloric acid
The reaction of potassium hydrogen carbonate with hydrochloric acid
This allows the enthalpy change of reaction for the decomposition of potassium
hydrogen carbonate to potassium carbonate to be determined

Another common experiment for this Hess' law approach is hydrated copper sulfate and
anhydrous copper sulfate to form copper sulfate solution

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 Your notes

Sample method for a neutralisation reaction

1. Using a measuring cylinder, place 25.0 cm3 of 1.0 mol dm-3 hydrochloric acid into the
polystyrene cup
2. Draw a table to record:
The initial temperature of the HCl (aq)
The temperature of the combined reaction mixture every half minute up to 9.5
minutes
3. Using a top-pan balance, measure 3.25 g of potassium hydrogen carbonate , KHCO3
4. Put a thermometer or temperature probe in the cup of HCl (aq), stir, and record the
temperature every half minute for 2½ minutes
5. At precisely 3 minutes, add the potassium carbonate to the cup of HCl (aq)
DO NOT RECORD THE TEMPERATURE AT 3 MINUTES
6. Continue stirring and record the temperature for 6 minutes
7. Plot a temperature correction graph to determine the enthalpy change for the reaction
8. Repeat this experiment using 2.50 g of potassium carbonate, K2CO3
Both experiments can be repeated to find an average temperature changes
9. Use the equation q = m c ΔT to calculate:
ΔH1 (enthalpy change of reaction for KHCO3 with HCl)

ΔH2 (enthalpy change of reaction for K2CO3 with HCl)

10. Apply Hess' law to calculate ΔHr (enthalpy change for the decomposition of KHCO3 to
K2CO3)
Using ΔHr = ΔH1 - ΔH2

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PAG 3.3 Determination of Enthalpy Changes of
Combustion Your notes
The principle here is to use the heat released by a combustion reaction to increase the
heat content of water
A typical simple calorimeter is used to measure the temperature changes to the water

A simple combustion calorimeter

To complete this experiment, the following steps will need to be completed:

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 Your notes

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 Your notes

It is important that you record:

The starting temperature
The final temperature
The starting mass of the spirit burner
The final mass of the spirit burner
Using this information, the mass of the fuel burned during the reaction and the
temperature change can be deduced
This mass of fuel burned can be used to calculate the moles of fuel burned
The moles of fuel burned can be used to convert q to an enthalpy change

Key points to consider

Not all the heat produced by the combustion reaction is transferred to the water
Some heat is lost to the surroundings
Some heat is absorbed by the calorimeter
To minimise the heat losses the copper calorimeter should not be placed too far above
the flame and a lid placed over the calorimeter
Shielding can be used to reduce draughts
In this experiment the main sources of error are
Heat losses
Incomplete combustion

Worked Example
1.023 g of propan-1-ol (M = 60.11 g mol-1) was burned in a spirit burner and used to
heat 200 g of water in a copper calorimeter.
The temperature of the water rose by 30 oC.
Calculate the enthalpy of combustion of propan-1-ol using this data.
Answer:
1. Calculate q
q = m c ΔT
q = 200 g x 4.18 J g–1 K–1 x 30 K = – 25 080 J

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 2. Calculate the amount of propan-1-ol burned
mass
moles = Your notes
Mr

1. 023 g
moles = = 0.01702 mol
60 . 11 g mol −1

3. Calculate ΔH
q
ΔH =
n

− 25080 J
ΔH = = – 1 473 560 J
0. 01702 mol

ΔH = -1 474 kJ = -1.5 x 103 kJ mol-1

Practical skills reminder

These calorimetry-based experiments develop a range of essential skills, including:
Accurately measuring temperature changes using a thermometer or probe
Measuring mass using a top-pan balance (e.g. for solids or spirit burners)
Handling volumes of liquids using measuring cylinders and polystyrene cups
Recording and plotting time–temperature data to apply graphical corrections
Calculating enthalpy changes using experimental data and the formula
q = mcΔT
Applying Hess' law to derive enthalpy changes indirectly from two reactions
Identifying and explaining sources of experimental error, such as heat loss or
incomplete combustion

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