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PREPARATION FOR THE ENTRY COMPETITION TO MAJOR
SCHOOLS AND FACULTIES

GCE CHEMISTRY PRACTICAL GUIDE

***********************

CHEMISTRY

How much better to acquire wisdom than gold! How much better to acquire the
intelligence is better than money
Table of Contents
4.1 PHYSICAL CHEMISTRY PRACTICALS .................................................................................................. 3
4.1.1 Making a Volumetric Solution ......................................................................................................... 5
Making a Volumetric Solution ............................................................................................................ 5
4.1.2 Performing a Titration & Volumetric Analysis ............................................................................... 8
Volumetric Analysis ............................................................................................................................ 8
4.1.3 Measurement of an Enthalpy Change .......................................................................................... 11
Measurement of an Enthalpy Change .............................................................................................. 11
4.1.4 Factors Affecting the Rate of a Reaction ...................................................................................... 17
Rate of Reaction ................................................................................................................................. 17
ORGANIC AND INORGANIC CHEMISTRY PRACTICALS ....................................................................... 20
4.2.1 Reactions of Group 2 Elements ..................................................................................................... 20
Reactions of Group 2 Elements ........................................................................................................ 20
4.2.2 Identifying Anions & Cations ......................................................................................................... 22
Identifying Anions & Cations ............................................................................................................ 22
4.2.4 Testing for Organic Functional Groups ........................................................................................ 28
Testing for Organic Functional Groups............................................................................................ 29
PHYSICAL CHEMISTRY PRACTICALS II ................................................................................................... 33
8.1.1 Required Practical 7 ........................................................................................................................ 33
Required Practical 7 .......................................................................................................................... 33
8.1.3 Required Practical 9 ........................................................................................................................ 40
Required Practical 9 .......................................................................................................................... 40
8.1.9 Titration Curves................................................................................................................................ 42
Titration Curves................................................................................................................................. 42
8.2.1 Required Practical 11 ...................................................................................................................... 44
Required Practical 11 ........................................................................................................................ 44
8.2.4 Redox Titrations ............................................................................................................................... 47
Redox Titrations ................................................................................................................................ 47
4.1 PHYSICAL CHEMISTRY PRACTICALS

4.1.1 Making a Volumetric Solution

Making a Volumetric Solution
REQUIRED PRACTICAL 1
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:
Volumes & concentrations of solutions

• The concentration of a solution is the amount of solute dissolved in a solvent to make 1

dm3 of solution
o The solute is the substance that dissolves in a solvent to form a solution
o 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:
o moles per unit volume
o mass per unit volume
o 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

4.1.2 Performing a Titration & Volumetric

Analysis
Volumetric Analysis
REQUIRED PRACTICAL 1
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
o 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

• The steps in a titration are:

o 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
o The other solution is placed in the burette
▪ To start with, the burette will usually be filled to 0.00 cm3
o A few drops of the indicator are added to the solution in the conical flask
o 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
o 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
o 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
o 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

Percentage Uncertainties

• Percentage uncertainties are a way to compare the significance of an absolute uncertainty on a

measurement
• This is not to be confused with percentage error, which is a comparison of a result to a literature
value
• The formula for calculating percentage uncertainty is as follows:

Adding or subtracting measurements

 • When you are adding or subtracting two measurements then you add together
the absolute measurement uncertainties
• For example,
o Using a balance to measure the initial and final mass of a container
o Using a thermometer for the measurement of the temperature at the start and the end
o Using a burette to find the initial reading and final reading
• In all these example you have to read the instrument twice to obtain the quantity
• If each you time you read the instrument the measurement is ‘out’ by the stated uncertainty,
then your final quantity is potentially ‘out’ by twice the uncertainty

4.1.3 Measurement of an Enthalpy Change

Measurement of an Enthalpy Change
REQUIRED PRACTICAL 2
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

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

o Enthalpy changes of reactions in solution
o Enthalpy changes of combustion
• In both cases you should be able to give an outline of the experiment and be able to process
experimental data using calculations or graphical methods

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 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 2½minutes
5. At precisely 3 minutes, add the zinc powder to the cup (DO NOT RECORD THE TEMPERATURE AT
3MIN)
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:
o That the specific heat capacity of the solution is the same as pure water, i.e. 4.18 J g-1 K-1
o That the density of the solution is the same as pure water, i.e. 1 g cm-3
o The specific heat capacity of the container is ignored
o The reaction is complete
o 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

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

Enthalpy of Combustion Experiments

• 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:

 • It is important that you record the starting temperature, and the final temperature in order to
complete the calculations
• You must also record the starting mass of the spirit burner and the final mass of the spirit
burner, so that you can work out the mass of the fuel burned during the reaction
o This will then be used to calculate the moles, which will be used to convert Q to an
enthalpy change in your calculations

Key points to consider

• Not all the heat produced by the combustion reaction is transferred to the water
o Some heat is lost to the surroundings
o 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
o Heat losses
o 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:

Step 1: Calculate q

q = m x c x ΔT

q = 200 g x 4.18 J g-1 K-1 x 30 K = – 25 080 J

Step 2: Calculate the amount of propan-1-ol burned

moles = mass ÷ molar mass = 1.023 g ÷ 60.11 g mol-1 = 0.01702 mol

Step 3: Calculate ΔH

ΔH = q ÷ n = -25 080 J ÷ 0.01702 mol = – 1 473 560 J = -1 474 kJ = -1.5 x 103 Kj

4.1.4 Factors Affecting the Rate of a Reaction
Rate of Reaction
REQUIRED PRACTICAL 3
Factors which affect the rate of a chemical reaction

• During a reaction, the reactants are used up and changed into the products
• The rate of a chemical reaction can be calculated using the following equation:

• As a reaction proceeds, the concentration of the reactants is decreasing and the concentration
of the products is increasing
• Because of this, the rate of the reaction is not the same throughout the reaction but changes
• The rate of reaction during the reaction can be calculated from a concentration-time graph
• A tangent will have to be drawn at a certain point on the graph, to calculate the rate at that
specific time
• The following graph is an example of cyclopropane being converted to propene
o The concentration of cyclopropene, the reactant, is decreasing over time as the reaction
progresses
 The rate of reaction at 3 different concentrations of cyclopropane is calculated by drawing
tangents at those points in the graph

The Disappearing Cross Experiment

• A simple experiment which can be done to determine how rate of reaction is affected by
concentration is the disappearing cross experiment
• It is set up as follows:
 The Disappearing Cross Experiment

• This experiment can be done for a number of different reactions, but taking the following
reaction as an example:

Na2S2O3 (aq) + 2HCl (aq) → 2NaCl (aq) + H2O (l) + SO2 (g) + S (s)

• In this reaction, sodium thiosulphate reacts with hydrochloric acid

• The key product which allows this experiment to work, is the sulfur which is a solid, and causes
the solution to become opaque
• There are actually two factors which can be investigated using the disappearing cross reaction:
o Changing the temperature
o Changing the concentration of the HCl
• You can plot graphs of concentration against time if the concentration of HCl was changed, or
plot 1/t against temperature if the temperature was changed
o You plot 1/t because the rate is proportional to 1/time and the graph you want is rate
versus temperature

Exam Tip
The disappearing cross experiment can be used for any reaction where a solid is produced as one
of the products, as this will cause the solution to become cloudy. It does not have to be done in a
conical flask, it could be done in a test tube with the cross placed underneath the test tube rack.
Watch out: this is a very simple experiment, but exam questions could try and make this seem
more complicated than it is!
ORGANIC AND INORGANIC CHEMISTRY

PRACTICALS
4.2.1 Reactions of Group 2 Elements
Reactions of Group 2 Elements
• Although there is no required practical specifically based around the reactions of Group 2
elements, these reactions are important and students tend to not do very well on these
questions in the exam
• Practical style questions can be asked on this topic - you should learn this in detail

Reactions of Group 2 Elements

• The reaction of all Group 2 metals with oxygen follows the following general equation:

2M (s) + O2 (g) → 2MO (s)

Where M is any metal in Group 2

• Sr and Ba also form MO2

• The reaction of all metals with water follows the following general equation:

M (s) + 2H2O (l) → M(OH)2 (s) + H2 (g)

Except for, Be which does not react with water

• The reaction of all metals with dilute HCl follows the following general equation:

M (s) + 2HCl (aq) → MCl2 (aq) + H2 (g)

• The reaction of all metals with dilute H2SO4 follows the following general equation:

M (s) + H2SO4 (aq) → MSO4 (aq) + H2 (g)

• SrSO4 and BaSO4 are insoluble

Group 2 Reactions with Oxygen & Water Chemical Equations

Group 2 Reactions with Dilute Hydrochloric Acid & Dilute Sulfuric Acid Chemical
Equations
4.2.2 Identifying Anions & Cations
Identifying Anions & Cations
REQUIRED PRACTICAL 4
Test Tube Reactions

• Simple test tube reactions can be done to identify the following ions:
o Group 2 ions (M2+)
o Ammonium ions (NH4+)
o Halide ions (X-)
o Hydroxide ions (OH-)
o Carbonate ions (CO32-)
o 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 Group 2 Metals

• Four test tubes should be placed in a test tube rack

• Around 10 drops of 0.1 mol dm-3 barium chloride solution should be added to the first test tube
• Around 10 drops of dilute sodium hydroxide solution (NaOH) should be added to the same test
tube
• Swirl the test tube carefully to mix well
• Continue to add sodium hydroxide dropwise to the test tube, until it is in excess
• This should then be repeated in the other test tubes, for calcium bromide solution, magnesium
chloride solution and strontium chloride solution
• Any observations should be noted down in a suitable results table
• The same test as above can also be done using ammonia solution and sulfuric acid solution

The positive results testing for the presence of Group 2 ions

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
• 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
Testing for Halide Ions

• The sample being tested should be added using a pipette to a test tube
• The test tube should be placed into a test tube rack
• A small amount of nitric acid should be added to the sample using a pipette, followed by a small
amount of silver nitrate solution
• A precipitate will form, either white, cream or yellow, if a halide ion is present in the sample

The white, cream and yellow precipitates formed when halide ions react with silver nitrate
solution

• The white precipitate will form if chloride ions are present in the sample
o The white precipitate is AgCl
• The cream precipitate will form if bromide ions are present in the sample
o The cream precipitate is AgBr
• The yellow precipitate will form if iodide ions are present in the sample
o The yellow precipitate is AgI
Further Test using Ammonia
 Results of the test with ammonia to further distinguish between silver halide precipitates

Testing for Hydroxide Ions

• A small amount (around 1 cm3) of the solution should be added to a test tube using a pipette
• Test the pH of the solution using red litmus paper or universal indicator paper
o The presence of hydroxide ions will turn the red litmus paper blue and the pH will be
clearly alkaline on the universal indicator paper if hydroxide ions are present

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
• As soon as the sodium carbonate solution is added, a bung with a delivery tube should be
attached to the test tube
o 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

Testing for Sulfate Ions

• Acidify the sample with dilute hydrochloric acid and then add a few drops of aqueous 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.

4.2.4 Testing for Organic Functional Groups

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Testing for Organic Functional Groups
REQUIRED PRACTICAL 6

• For this practical, you need to be able to give the tests and positive results for the following
functional groups:
o Alkenes
o Alcohols
o Aldehydes
o Carboxylic Acids

Testing for an Alkene

• Halogens can be used to test if a molecule is unsaturated (i.e. contains a double bond)
• Br2(aq) is an orange-yellow solution, called bromine water
• The unknown compound is shaken with the bromine water
• If the compound is unsaturated, an addition reaction will take place and the coloured solution
will decolourise

The bromine water test is the standard test for unsaturation in alkenes

Testing an Alcohol

• Alcohols can be classified as either primary, secondary or tertiary, depending on the placement
of the -OH group
• Primary and secondary alcohols can both be oxidised, but tertiary alcohols cannot
• To test for the alcohol functional group, add a small amount (1 cm3) of the substance to a test
tube using a pipette
 • Then, add a small amount (1 cm3) of a suitable oxidising agent to the sample using a different
pipette
o The most commonly used oxidising agent for this test is acidified potassium dichromate
solution (K2Cr2O7, acidified with H2SO4)
• Add a stopper to the test tube and shake well
• Place in a hot water bath (heated to around 60 oC) for a few minutes
• If a primary or secondary alcohol are present, then the colour will change from orange to green
o If a tertiary alcohol is present, then nothing will happen - the solution will remain orange

Positive test results of the oxidation of a primary, secondary and tertiary alcohol

Testing for an Aldehyde

Fehling’s solution

• Fehling’s solution is an alkaline solution containing copper(II) ions which act as the oxidising
agent
• When warmed with an aldehyde, the aldehyde is oxidised to a carboxylic acid and the Cu2+ ions
are reduced to Cu+ ions
o In the alkaline conditions, the carboxylic acid formed will be neutralised to a carboxylate
ion (the -COOH will lose a proton to become -COO– )
o The carboxylate ion (-COO–) will form a salt with a positively charged metal ion such as
sodium (-COO–Na+)
• The clear blue solution turns opaque due to the formation of a red precipitate, copper(I) oxide
• Ketones cannot be oxidised and therefore give a negative test when warmed with Fehling’s
solution
 The copper(II) ions in Fehling’s solution are oxidising agents, oxidising the aldehyde to a
carboxylic acid and getting reduced themselves to copper(I) ions in the Cu2O precipitate

Tollens’ reagent

• Tollens' reagent is an aqueous alkaline solution of silver nitrate in excess ammonia solution
o Tollens' reagent is also called ammoniacal silver nitrate solution
• When warmed with an aldehyde, the aldehyde is oxidised to a carboxylic acid and the Ag+ ions
are reduced to Ag atoms
o In the alkaline conditions, the carboxylic acid will become a carboxylate ion and form a
salt
• The Ag atoms form a silver ‘mirror’ on the inside of the tube
• Ketones cannot be oxidised and therefore give a negative test when warmed with Tollens’
reagent
 The Ag+ ions in Tollens’ reagent are oxidising agents, oxidising the aldehyde to a carboxylic
acid and getting reduced themselves to silver atoms

Testing for a Carboxylic Acid

• Carboxylic acids in solution have a pH of around 3, so measuring the pH is a way of testing for
the presence of the carboxylic acid functional group in an organic sample
• The end of a glass rod could be dipped into the solution and then carefully dripped onto
indicator paper
• Or, a pH probe could be used, which would give you an exact pH
• Since carboxylic acids are acids, they will react with a carbonate solution to produce carbon
dioxide gas
• 1-2 cm3 of sodium carbonate (Na2CO3) or sodium hydrogen carbonate solution (NaHCO3) could
be added using a pipette
• If bubbles of gas are seen, this is a good indicator that the solution is a carboxylic acid
o If an exam question asks you to simply distinguish between different types of organic
compound, and the carboxylic acid is the only organic compound present which would
react in this way with a carbonate solution, then this is enough
• The gas produced could then be bubbled into limewater
• If the limewater turns milky or cloudy, then this proves that the gas produced was carbon
dioxide
PHYSICAL CHEMISTRY PRACTICALS II

8.1.1 Required Practical 7

Required Practical 7
Required Practical 7: Measuring the rate of a reaction

• There are two ways to measure the rate of reaction

o By an initial rate method
o By a continuous monitoring method

An initial rate method: The reaction between magnesium and hydrochloric acid

• This reaction can be used to investigate the effect of varying the concentration of the acid while
keeping the temperature constant
• When a gas is released in a reaction you can either try to measure the volume of gas given off or
the mass change in the reaction flask
o However, in this case the gas hydrogen is too low in density so the mass change will be
far too small to register on a laboratory balance
• Volume can be measured either by displacement of water into an inverted measuring cylinder
or by using a gas syringe

The rate of reaction between magnesium and dilute hydrochloric acid can be measured using
a gas syringe and stopwatch

Steps in the procedure

• Before you begin you need to check your apparatus is gas tight
 o This can be done by assembling everything without the acid or magnesium and trying to
move the plunger
o If you feel resistance the apparatus is gas tight
• The acid will go in first because it is quicker to drop a piece of magnesium ribbon in than to pour
in the acid
• To vary the concentration of the acid you need to dilute it by measuring portions of acid in a
measuring cylinder and then portions of distilled water in another measuring cylinder and
adding them to the conical flask
• Choose a suitable volume of acid to match the size of the flask, e.g. 40 cm3
• You don't want to use acid that is stronger than 2 mol dm-3 because the reaction will be too fast,
so its best to start with 2 mol dm-3 and perform a serial dilution, e.g. 40 cm3(acid) + 0
cm3 (water), 35 cm3 (acid) + 5 cm3 (water), etc

Practical tips

• Make sure the plunger is fully inserted before you start the experiment otherwise you will have
a volume error
• If the magnesium does not look new and shiny, you may need to clean the surface with a bit of
sandpaper
• Make sure the plunger is secure and does not fall out of the barrel if the volume exceeds 100
cm3

Specimen Results

• Here is a set of typical results for this experiment

Rate of reaction between magnesium and acid results table

Graphing the results

Graph showing typical results for the rate of reaction between hydrochloric acid and
magnesium at different concentrations

Analysis

• The lines of best fit are drawn for each concentration on the same graph
• A tangent is then drawn starting from (0,0) since this method is to find the initial rate of
reaction
• The gradient of the tangent is determined which gives the rate of reaction
• In the example above, the rate of reaction for 2.0 mol dm-3 acid is

o Gradient 1.05 mol dm-3 s-1

A continuous monitoring method: The iodination of propanone

• The iodination of propanone provides a suitable experiment in which the rate of reaction can be
measured throughout the reaction by using a colorimeter
• The reaction is carried out using a catalyst of dilute sulfuric acid
 • The iodine decolourises during the reaction as it turns into iodopropanone and hydrogen iodide:

CH3COCH3 + I2 → CH3COCH2I + HI

• The colorimeter measures colour absorbance which is proportional to the concentration of the
coloured species
• Before the investigation beings it is necessary to measure the absorbance of a set of standard
solutions of iodine and obtain a calibration curve
• For example here is a calibration curve for a transition metal ion that allows you to convert
colorimeter readings into concentrations:

A calibration curve showing the relationship between colour absorbance and concentration

Steps in the procedure

• The colorimeter uses very small volumes of solutions, so four burettes can be filled with
solutions of 0.02 mol dm-3 iodine, 1.0 mol dm-3 propanone and 1.0 mol dm-3 sulfuric acid and
distilled water
• By varying the volumes of solutions while maintaining a constant total volume with the use of
distilled water, you can obtain a number of different concentrations
• The solutions are measured into a small beaker, leaving the iodine in a separate beaker - this
starts the reaction, so it can be added when you start a timer or stop watch
• The iodine is added to the other liquids, the contents mixed and then quickly transferred into
the cuvette (small receptacle) and the colorimeter/data logger started
 The set up for using a colorimeter and data logger to continuously measure the rate of
reaction

• A typical set of volume compositions could be as follows:

Volume Compositions Table

Practical tip

• Choose a filter that gives the strongest absorbance for the solution you are using - this will be
the complementary colour to the colour of the solution under investigation

Specimen Results

• Here is a set of typical results for this experiment

Graphing the results

Graph showing the change in concentration of iodine during the course of the reaction

Analysis

• To find the rate of reaction at any point, a tangent is drawn and the gradient is determined
• The gradient gives the rate of reaction
• For example, in the graph above, the rate of reaction at 300 seconds can be found
o A vertical line is drawn from the 300 s mark until it meets the curve, then a tangent is
drawn

o Gradient 1.19 x 10-5 mol dm-3 s-1

o The gradient is the rate of reaction at that point

Exam Tip
Whichever rates experiments you carry out, make sure you can

• describe the steps in the procedure

• name all the apparatus used
• draw data tables which include headings and units
• draw graphs showing labels, units and best fit lines
• determine an initial gradient or at any point in the curve
8.1.3 Required Practical 9
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Required Practical 9
Required Practical 9: Investigating pH changes

The experimental set up for measuring pH changes in titrations

Steps in the procedure

• Measure out 50 cm3 of 1.0 mol dm-3 ethanoic acid using a measuring cylinder and transfer it to a
200 cm3 beaker
• Place the beaker onto a magnetic stirrer and add a magnetic stirrer bar
• Position the pH probe so that it does not interfere with the movement of the stirrer bar
• Take an initial pH reading
• Fill the burette with 1.0 mol dm-3 sodium hydroxide
 • Add 2 cm3 of sodium hydroxide from the burette into the beaker and take the pH reading
• Continue adding 2 cm3 portions until you get to 20 cm3 then switch to 1 cm3 portions
• The pH begins to rise rapidly- when it begins to slow down then you can switch back to 2
cm3 portions
• Plot a graph of pH versus volume of base added
• The procedure can then be repeated with 1.0 mol dm-3 hydrochloric acid and 1.0 mol dm-
3 ammonia solution

Practical tips

• You may need to wait a few seconds until the pH stabilises before you take a reading
• Make sure the stirrer is not moving too fast as a rapid spin generates bubbles in the solution
which gives an unsteady pH reading

Specimen Results

• The pH curves for a weak acid with a strong base, and a strong acid with a weak base are shown
below:

pH curves from weak acid + strong base, and strong acid + weak base

Analysis

• The pH curves show a characteristic s-shape curve and the midpoint of the inflection is called
the equivalence or stochiometric point
• From the curves you can
o Determine the pH of the acid by looking where the curve starts on the y-axis
o Find the pH at the equivalence point
o Find the volume of base at the equivalence point
o Obtain the range of pH at the vertical section of the curve
8.1.9 Titration Curves
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Titration Curves
• Titration or pH curves are obtained by reacting known concentrations of acid with alkalis and
measuring the pH during the neutralisation
• A suitable selection to use would be 1.0 mol dm-3 solutions of
o hydrochloric acid
o ethanoic acid
o sodium hydroxide
o ammonia solution
• A pH probe is calibrated by placing the tip of the probe in pH 4 buffer solution and adjusting
until the reading is 4.0
o The probe is washed in distilled water and then checked against pH 9 buffer
o If is it working correctly it should read 9.0
o This is known as a two-point calibration
• 25cm3 of ethanoic or hydrochloric acid is measured using a volumetric pipette and filler and
then transferred into a beaker
• Its pH is measured and recorded
• The alkali (either sodium hydroxide or ammonia solution) is placed in the burette
• 5cm3 at time is added to the beaker and the pH measured after each addition, until a total of 50
cm3 has been added
• The procedure is repeated for all four combinations of acids and alkalis

Specimen Titration Curve Results Table

Analysis

• The four characteristic titration curves are shown below

• The more data points that are available; the easier it is to draw the shape of the curves.
o So, it is often better to add smaller portions nearer the equivalence point
 The four characteristic acid-base titration curves

Exam Tip
You need to:

• Be familiar with the shapes of the four titration curves

• Be able to identify the type of acid and base (weak/strong)
• Know where to locate the equivalence point

8.2.1 Required Practical 11

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Required Practical 11
Required Practical 11: Carry out simple test-tube reactions to identify transition metal ions
in aqueous solution
 • This practical covers a number of key laboratory skills
o use water bath or electric heater or sand bath for heating
o use laboratory apparatus for a variety of experimental techniques
o safely and carefully handle solids and liquids, including corrosive, irritant, flammable
and toxic substances
• The key to success in Required Practical 11 is following instructions carefully and recording
coherent detailed observations of what you see
• The aim of the practical is to record the reactions of three unknown solutions, L, M and N

Key steps in the procedurePart 1

• 10 drops of solution L are added to a clean test tube

• Drops of dilute sodium hydroxide are added until in excess (i.e. you have exceeded 10 drops)
• Observations are recorded
• This procedure is then repeated with solution M and N

Part 2

• The test tubes from part 1 are place in a beaker of hot water for around 10 minutes

Part 3

• 10 drops of sodium carbonate solution are added to a clean test tube

• 10 drops of solution L are then added to the test tube and observations made
• The procedure is repeated with solution M and N

Part 4

• 10 drops of solution L are added to a clean test tube

• 10 drops of silver nitrate solution are then added to the test tube and observations made
• The procedure is repeated with solutions M and N and the tubes left to rest for around 10
minutes

Required Practical 11: Specimen Results Table Parts 1 & 2

 Required Practical 11: Specimen Results Table Part 3

Required Practical 11: Specimen Results Table Part 4

Required Practical 11: Identities of solutions L, M and N

Practical Tip

• Always use clean test tubes and pipettes as the tests are very sensitive and you don't want to
cross-contaminate the solutions
• It's a good idea to label your test tubes to avoid confusing ones that have the same appearance,
especially when they are in a water bath and not arranged in a test tube rack
 • To observe colour changes more clearly, using a white background such as a piece of paper can
help

8.2.4 Redox Titrations

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Redox Titrations
Redox Titrations

• Iron has variable oxidation states and this characteristic can be exploited in redox titrations of
Fe2+ with MnO4- or Cr2O72-
• Both the manganate(VII) ion and dichromate(VI) ions can be used as strong oxidising agents to
find the amount of iron(II) ions in solution
• You need to be able to perform these separate redox titrations with Fe2+ and understand the
colour changes in each example

Potassium manganate(VII) titrations

• In these redox titrations the manganate(VII) is the oxidising agent and is reduced to Mn2+(aq)
• The iron is the reducing agent and is oxidised to Fe2+(aq) and the reaction mixture must be
acidified, to excess acid is added to the iron(II) ions before the reaction begins
• The choice of acid is important, as it must not react with the manganate(VII) ions, so the acid
normally used is dilute sulfuric acid
o As it does not oxidise under these conditions and does not react with the
manganate(VII) ions
• You could be asked why other acids are not suitable for this redox titration in the exam so make
sure you understand the suitability of dilute sulfuric acid

Table explaining why other acids are not suitable for the redox titration
Indicator and end point

• Potassium permanganate acts as its own indicator, as the purple potassium permanganate
solution is added to the titration flask from the burette and reacts rapidly with the Fe2+(aq)
o The burette used in this practical should be one with white numbering not black, as you
would struggle to read the values for your titres against the purple colour of the
potassium permanganate if black numbering was used
• The manganese(II) ions, Mn2+(aq), have a very pale pink colour but they are present in such a
low concentration that the solution looks colourless
• As soon as all of the iron(II), Fe2+(aq), ions have reacted with the added manganate(VII) ions,
Mn7+(aq), a pale pink tinge appears in the flask due to an excess of manganate(VII) ions, Mn7+(aq)

Redox titration colour change for potassium permanganate and iron(II) ions

Worked Example
Equations

Find the stoichiometry for the reaction and complete the two half equations:

MnO4- (aq) + 5e- + 8H+ (aq) → Mn2+ (aq) + 4H2O (l)

Fe2+ (aq) → Fe3+ (aq) + e-

Answers:
Balance the electrons:

MnO4- (aq) + 5e- + 8H+ (aq) → Mn2+ (aq) + 4H2O (l)

5Fe2+ (aq) → 5Fe3+ (aq) + 5e-

Add the two half equations:

MnO4- (aq) + 8H+ (aq) 5Fe2+ (aq) → Mn2+ (aq) + 4H2O (l) + 5Fe3+ (aq)

Potassium dichromate(VI) titrations

• Dichromate(VI) is a powerful oxidising agent when it changes from +6 oxidation state in the
dichromate(VI) ion, Cr2O72-, to the +3 oxidation state in Cr3+
• The two half equations are:
o Cr2O72- (aq) + 14H+ (aq) + 6e- → 2Cr3+ (aq) + 7H2O (l)
o 6Fe2+ (aq) → 6Fe3+ (aq) + 6e-
• Overall equation is:
o Cr2O72- (aq) + 14H+ (aq) + 6Fe2+ → 2Cr3+ (aq) + 6Fe3+ (aq) + 7H2O (l)

Indicator and end point

• The colour change for this titration is from orange to bluish green
o to give a more definitive and visible endpoint, the indicator sodium
diphenylaminesulfonate is used
o This turns from colourless to purple at the endpoint

Exam Tip
General sequence for redox titration calculations

1. Write down the half equations for the oxidant and reductant
2. Deduce the overall equation
3. Calculate the number of moles of manganate(VII) or dichromate(VI) used
4. Calculate the ratio of moles of oxidant to moles of reductant from the overall redox equation
5. Calculate the number of moles in the sample solution of the reductant
6. Calculate the number of moles in the original solution of reductant
7. Determine either the concentration of the original solution or the percentage of reductant in a
known quantity of sample

Worked Example
An iron tablet, weighing 0.960 g was dissolved in dilute sulfuric acid. A titre of 28.50 cm3 of
0.0180 mol dm-3 potassium dichromate(VI) solution was needed to reach the endpoint.

What is the percentage by mass of iron in the tablet?

Answer:

•
o Cr2O72- (aq) + 14H+ (aq) + 6Fe2+ → 2Cr3+ (aq) + 6Fe3+ (aq) + 7H2O (l)

•
o 1 : 6 ratio of Cr2O72- : Fe2+

o Number of moles of Cr2O72- = = 5.13 x 10-4 moles

•
o Moles of iron(II) = 6 x 5.13 x 10-4 = 3.078 x 10-3 moles

•
o Mass of iron(II) = 56.0 x 3.078 x 10-3 = 0.1724 g

o Percentage by mass = = 18%