UNIT 6 - Practical Skills in Chemistry II

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YOUR NOTES
International A Level Chemistry Edexcel 
6. Practical Skills in Chemistry II
CONTENTS
6.1 Advanced Physical Chemistry Core Practicals
6.1.1 Rates of Reaction - Titrimetric Method
6.1.2 Rates of Reaction - Clock Reaction
6.1.3 Activation Energy
6.1.4 Finding Ka Values
6.1.5 Electrochemical Cells
6.2 Advanced Inorganic & Organic Chemistry Core Practicals
6.2.1 Redox Titration - Iron(II) & Manganate(VII)
6.2.2 Redox Titration -Thiosulfate & Iodine
6.2.3 Transition Metal Complexes
6.2.4 A-Level Qualitative Analysis
6.2.5 Aspirin Preparation
Page 1 of 37
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6.1 Advanced Physical Chemistry Core Practicals YOUR NOTES


6.1.1 Rates of Reaction - Titrimetric Method
Core Practical 9a: Titrimetric Methods

The reaction between iodine in an acidic solution and propanone is
CH3COCH3 (aq) + I2 (aq) → CH3COCH2I (aq) + H+ (aq) + I- (aq)
We can follow the rate of this reaction by using a continuous monitoring method and
therefore we will be able to deduce the order of reaction with respect to a substance using
a concentration line graph
We can calculate the order of reaction with respect to iodine as the propanone and acid are
in a large excess so their concentration do not change during the reaction
Once a portion of the reaction mixture has been removed, we stop the reaction by adding
sodium hydrogencarbonate
Performing a titration again sodium thiosulfate(VI) solution and using starch as an indicator
is used to determine the concentration of iodine
2S2O32- (aq) + I2 (aq) → 2I- (aq) + S4O62- (aq)
Steps in the procedure
Mix 25 cm3 of 1.0 mol dm-3 aqueous propanone with 25 cm3 of 1.0 mol dm-3 sulfuric acid in
a beaker
Add 50 cm3 of 0.02 mol dm-3 iodine solution
Start the stop clock as soon this is added to the beaker
Using a pipette, withdraw 10 cm3 portion of the reaction mixture and transfer this to a
conical flask
Stop this portion of the reaction by adding a spatula of sodium hydrogen carbonate
Titrate this sample against 0.01 mol dm-3 sodium thiosulfate(VI) solution using starch as an
indicator
Record your result
Withdraw 10 cm3 of the reaction mixture every 3 minutes and repeat the process of
stopping the reaction and titrating against the sodium thiosulfate(VI) solution
Practical tips
Note the time at which the sodium hydrogencarbonate is added to the withdrawn portions
of reaction mixture as this is when the reaction will be stopped and the concentration of
iodine can be calculated accurately
Keep the clock running and note the time throughout the practical rather than stopping the
clock
Have everything ready and set up before beginning the procedure
Results
Sample Data from the Reaction
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YOUR NOTES

This graph is a straight line graph

As the gradient is constant, the rate of reaction is constant, and therefore independent
of the concentration of the iodine solution
This means the reaction is zero order with respect to the iodine
The rate equation for the reaction is
Rate = k[CH3COCH3 (aq)] [H+ (aq)]
Concentration-time graphs of a zero-order reaction
Page 3 of 37
6.1.2 Rates of Reaction - Clock Reaction YOUR NOTES


Core Practical 9b: Investigating a Clock Reaction
Clock reactions are so called because they show a sharp dramatic colour change after a
period of time has elapsed
They make ideal reactions for studying kinetics
Iodine clock reactions come in a number of variations, but they generally all use starch to
show a sudden purple-black colour at the end of the reaction
A common iodine clock reaction uses the reaction between hydrogen peroxide and iodine
H2O2 (aq) + 2I- (aq) + 2H+(aq) → I2 (aq) + 2H2O (l)
Adding sodium thiosulfate to the reaction mixture uses up the iodine and acts as the
reaction timer
2S2O32- (aq) + I2 (aq) → 2I- (aq) + S4O62- (aq)
The amounts chosen are such that the iodine produced is in excess compared to the other
reagents
Therefore, as soon as the iodine is in excess the blue-black colour of iodine in starch is
seen
The iodine clock reaction provides a good way to study reaction kinetics
The solutions are measured in burettes and placed in a small beaker
The sulfuric acid is in excess so can be measured in a measuring cylinder rather than burette
The reaction is started by adding 1cm3 of 0.25 mol dm-3 hydrogen peroxide and starting a
timer
The timer is stopped when the blue black colour appears
Suitable volume compositions to use could be as follows:
Page 4 of 37
Iodine Clock Volume Compositions Table YOUR NOTES


Practical tips
Hydrogen peroxide is typically found in 'volume' concentrations, based on the volume of
oxygen given of when it decomposes:
2H2O2 (aq) → O2 (g) + 2H2O (l)
For example in school laboratories, a suitable concentration of hydrogen peroxide may be
listed as 3% or '10 vol'
'10 vol' means that when 1cm3 of hydrogen peroxide decomposes it generates 10
cm3 of oxygen
'10 vol' or 3% hydrogen peroxide has a concentration of 0.979 mol dm3
Specimen Results
Here is a set of typical results for the iodine clock reaction
Specimen Results for the Iodine Clock Reaction Table
Analysis
Page 5 of 37
The time of reaction is converted to rate of reaction by calculating the reciprocal value YOUR NOTES
A graph is plotted of rate versus concentration 
A rate- concentration graph for the iodine clock reaction

From this graph we can see that the rate of reaction is directly proportional to the
concentration of potassium iodide:
As concentration doubles; the rate of reaction also doubles
This tells us that the reaction is first order with respect to potassium iodide
Page 6 of 37
6.1.3 Activation Energy YOUR NOTES


Core Practical 10: Finding the Activation Energy of a Reaction
In this practical the activation energy for the reaction between bromide ions and
bromate(V) ions will be determined
BrO3- + 5Br- + 6H+ → 3Br2 + 3H2O
C6H5OH + 3Br2 → C6H2Br3OH + 3HBr
The bromine produced in the first reaction reacts with the phenol
When the phenol is ‘used up’, the bromine is no longer removed
The bromine then bleaches the indicator at the ‘end of the reaction’
Common indicators for this reaction are methyl red and methyl orange
Steps in procedure
Pipette 10.0 cm3 of phenol solution and 10.0 cm3 of a bromide / bromate solution into one
boiling tube
Add four drops of methyl red indicator to the mixture
Pipette 5.0 cm3 of sulfuric acid solution into a separate boiling tube
Use a kettle and a beaker to prepare a water bath with a temperature of 37 °C (±1 °C) and
stand the two boiling tubes in the water bath
When the contents of the boiling tubes have reached the water temperature, mix the
contents of the two tubes by pouring rapidly from one tube into the other and then pouring
the mixture back into the empty test tube
Start the stop clock at the same time
Leave the boiling tube containing the reaction mixture in the water and time until the methyl
red indicator disappears
Record the results
Repeat the whole experiment at different temperatures
Use ice to achieve the lowest temperature if required
Sample Data
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YOUR NOTES

Graph plotted from data
Page 8 of 37
YOUR NOTES

Page 9 of 37
YOUR NOTES

Page 10 of 37
6.1.4 Finding Ka Values YOUR NOTES


Core Practical 11: Finding Ka for a Weak Acid
The Ka of a weak acid may be determined by finding the pH at the half equivalence point
At the half equivalence point Ka = [H+]
Key steps in the procedure

A pH probe or meter is calibrated before use
25 cm3 of 0.1 mol dm-3 ethanoic acid is pipetted into a conical flask and a few drops of
phenolphthalein indicator are added
A burette is filled with 0.1 mol dm-3 sodium hydroxide solution
The contents of the conical flask are titrated against the sodium hydroxide until the
indicator just turns pink
A further pipette containing 25 cm3 of the acid is then added to the flask and the pH is
measured
Specimen Results
pH at half equivalence point = 4.75
Analysis
After the addition of the second portion of acid, the solution is effectively a half-neutralised
sample of acid
This is the half-equivalence point at which the Ka = [H+]
By measuring the pH at that point you can convert it to [H+] and hence find the Ka of the acid
pH = 4.75
[H+] = 10-pH = 1.8 x 10-5 mol dm-3
∴ Ka = 1.8 x 10-5 mol dm-3
You can also say that the pKa = pH at the half-equivalence point
Page 11 of 37
YOUR NOTES

The pH at the half-equivalence point in a weak acid titration gives the pKa of the weak acid
 Exam Tip
The sources of uncertainty in this experiment include the measurements made by
the pipette and burette, and the judgement of the end-point of the titration.Be
careful, there is a single uncertainty in the pipette measurements as one reading was
taken but there is double the uncertainty for the burette reading as there was the
initial and final readings.
Page 12 of 37
6.1.5 Electrochemical Cells YOUR NOTES


Core Practical 12: Investigating Electrochemical Cells
Measuring the EMF of a cell
To measure a cell EMF you will need
Two small beakers, around 75 cm3 capacity
Strips of suitable metals such as copper, zinc, iron and silver
1.0 mol dm-3 solutions of the metal ions (nitrates, chlorides or sulfates depending on
their solubility)
A high resistance voltmeter (usually a digital multimeter has this)
Two sets of wires with crocodile clips
A salt bridge consisting of a strip of filter paper soaked in saturated potassium nitrate
The experimental set up for measuring the EMF of a cell made of two metal / metal ion half
cells
The strips of metals need to be freshly cleaned to remove any oxide coatings
This can be done with a piece of sandpaper
To support the metals, it is easiest to have long strips that can be folded over the side of the
beaker and held in place with the crocodile clips
Fill up the beakers to about two thirds of the way with the metal ion solutions
Page 13 of 37
Using tongs, dip a strip of filter paper into a beaker of saturated potassium nitrate solution YOUR NOTES
and then place it between the two beakers making sure the ends of the strip are well 
immersed in the solutions
Connect the crocodile clips to the voltmeter, wait for a steady reading and record the
measurement
Practical tips
If you don't get a positive reading on the voltmeter swap the terminals around
Voltmeters will have marked positive and negative terminals (usually in red and black,
respectively), so when you get a positive reading this tells you the relative polarity of the
metals in the cell
Change the salt bridge each time, to prevent cross contamination of ions between half
cells
Specimen Results
Here is a set of typical results for this experiment
Specimen EMF Results (theoretical values) Table
Analysis
It is unlikely you will get very close to the theoretical results as these would be obtained
under standard conditions which are hard to achieve in a school laboratory
However, the relative EMF of cells you construct should match the theoretical values
The higher the EMF, the larger the difference in reactivity ('electron pushing power')
between the metals
Page 14 of 37
6.2 Advanced Inorganic & Organic Chemistry Core Practicals YOUR NOTES

6.2.1 Redox Titration - Iron(II) & Manganate(VII)
Core Practical 13a: Iron(II) & Manganate(VII) Titration

Redox Titrations
In a titration, the concentration of a solution is determined by titrating with a solution of
known concentration.
In redox titrations, an oxidising agent is titrated against a reducing agent
Electrons are transferred from one species to the other
Indicators are sometimes used to show the endpoint of the titration
However, most transition metal ions naturally change colour when changing oxidation
state
There are two common redox titrations you should know about manganate(VII) titrations
and iodine-thiosulfate titrations
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
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
Page 15 of 37
with the Fe2+(aq) YOUR NOTES

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-
Page 16 of 37
Add the two half equations: YOUR NOTES

MnO4- (aq) + 8H+ (aq) + 5Fe2+ (aq) → Mn2+ (aq) + 4H2O (l) + 5Fe3+ (aq) 
Manganate(VII) titrations can be used to determine:

The percentage purity of iron supplements
mass of sample
Percentage purity = × 100
mass of impure sample
The formula of a sample of hydrated ethanedioic acid
 Worked Example
Analysis of iron tablets
An iron tablet, weighing 0.960 g was dissolved in dilute sulfuric acid. An average
titre of 28.50 cm3 of 0.0180 mol dm-3 potassium manganate(VII) solution was
needed to reach the endpoint.
What is the percentage by mass of iron in the tablet?
Answer:
MnO4- (aq) + 8H+ (aq) + 5Fe2+ → Mn2+ (aq) + 5Fe3+ (aq) + 4H2O (l)
1 : 5 ratio of MnO4- : Fe2+
0 . 0180 × 25. 0
Number of moles of MnO4- (aq) = = 5.13 x 10-4 moles
1000
Moles of iron(II) = 5 x 5.13 x 10-4 = 2.565 x 10-3 moles
Mass of iron(II) = 56.0 x 2.565 x 10-3 = 0.14364 g
0 . 14364
Percentage by mass = = × 100 = 15.0%
0 . 960
Page 17 of 37
6.2.2 Redox Titration -Thiosulfate & Iodine YOUR NOTES


Core Practical 13b: Thiosulfate & Iodine Titration
Iodine-Thiosulfate Titrations
A redox reaction occurs between iodine and thiosulfate ions:
2S2O32– (aq) + I2 (aq) → 2I–(aq) + S4O62– (aq)
The light brown/yellow colour of the iodine turns paler as it is converted to colourless iodide
ions
When the solution is a straw colour, starch is added to clarify the end point
The solution turns blue/black until all the iodine reacts, at which point the colour
disappears.
This titration can be used to determine the concentration of an oxidising agent, which
oxidises iodide ions to iodine molecules
The amount of iodine is determined from titration against a known quantity of sodium
thiosulfate solution
 Worked Example
Analysis of household bleach
Chlorate(I) ions, ClO-, are the active ingredient in many household bleaches.
10.0 cm3 of bleach was made up to 250.0 cm3. 25.0 cm3 of this solution had 10.0
cm3 of 1.0 mol dm-3 potassium iodide and then acidified with 1.0 mol dm-3
hydrochloric acid.
ClO- (aq) + 2I- (aq) + 2H+ (aq) → Cl- (aq) + I2 (aq) + H2O (l)
This was titrated with 0.05 mol dm-3 sodium thiosulfate solution giving an average
titre of 25.20 cm3.
2S2O32- (aq) + I2 (aq) → 2I- (aq) + S4O62- (aq)
What is the concentration of chlorate(I) ions in the bleach?
Answer:
One mole of ClO- (aq) produces one mole of I2 (aq) which reacts with two moles of 2S2O32-
(aq)
Therefore, 1 : 2 ratio of ClO- (aq) : S2O32- (aq)
0 . 05 × 25. 20
Number of moles of S2O32- (aq) = = 1.26 x 10-3 moles
1000
1 . 26 × 10−3
Number of moles of I2 (aq) and ClO- (aq) in 25.0 cm3 = = 6.30 x 10-4 moles
2
Number of moles of ClO- (aq) in 250.0 cm3 = 6.30 x 10-4 x 10 = 6.30 x 10-3 moles
The 250.0 cm3 was prepared from 10.0 cm3 bleach
10 cm3 bleach = 6.30 x 10-3 moles of ClO- ions
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1.0 dm3 bleach = 0.630 moles of ClO- ions YOUR NOTES

Therefore, the concentration of ClO- ions in the bleach is 0.630 mol dm-3 
 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
Page 19 of 37
6.2.3 Transition Metal Complexes YOUR NOTES


Core Practical 12: Preparing a Transition Metal Complex
Method
1. Weigh between 1.4 g and 1.6 g of copper(II) sulfate.
To do this you should weigh a test tube and record its mass.
Then add the copper(II) sulfate to the test tube, reweigh and record the mass.
The mass of the copper(II) sulfate is the difference between the two masses.
2. Add 4 cm3 of water to the test tube using a graduated pipette.
3. Prepare a water bath using hot water from a kettle in a 100 cm3 beaker and stand the test
tube in the water bath.
4. Stir gently to dissolve the copper(II) sulfate.
5. Remove the test tube containing copper(II) sulfate solution from the water bath.
6. Perform this step in the fume cupboard wearing gloves. Add, while stirring, 2 cm3 of
concentrated ammonia solution to the copper(II) sulfate solution.
7. Pour the contents of the test tube into 6 cm3 of ethanol that has been pipetted into a
beaker – mix well and then cool the mixture in an ice bath.
8. Using a Bϋchner funnel and flask, filter the crystals. Wash your test tube with cold ethanol
and add the washings to the Bϋchner funnel. Finally, rinse the crystals with cold ethanol.
9. Carefully scrape the crystals off the filter paper onto a fresh piece of filter paper. Cover the
crystals with a second piece of filter paper, Carefully pat the paper to dry the crystals. Note
that to get the crystals completely dry, you may need to repeatedly move the crystals to dry
parts of the filter paper.
10. Once dry, measure and record the mass of crystals
Buchner filtration set-up to filter crystals
Page 20 of 37
Exam Tip YOUR NOTES

 You may be asked about some of the steps in more detail.

The solution produced in step 6 is a dark blue solution due to the formation of the
[Cu(NH3)4(H2O)2]2+ complex ion.
Adding ethanol in step 7 causes the precipitation of dark blue Cu(NH3)4SO4•H2O
crystals. This is because ethanol is less polar than water and any ionic compounds
will be less soluble in it than they are in water. As ethanol is added, the solubility of
Cu(NH3)4SO4•H2O, decreases and crystals are formed.
In step 8, ethanol is added to remove any impurities. Cold ethanol is used as
Cu(NH3)4SO4•H2O is less soluble in cold ethanol - if hot ethanol were used,
Cu(NH3)4SO4•H2O would dissolve.
 Worked Example
A student carried out the method mentioned above and measured the final mass of
Cu(NH3)SO4·H2O after drying the crystals of 1.2 g.
1. Write an equation for this reaction
2. Calculate the relative formula masses of CuSO4·5H2O and Cu(NH3)SO4·H2O
3. Calculate the number of moles of copper(II) sulfate used in the reaction
(assume 1.5 g was used)
4. Use your answer to calculate the theoretical yield of tetraaminecopper(II)
sulfate-1-water your reaction should have produced
5. Calculate the percentage yield obtained in this reaction
Answers
1. CuSO4•5H2O + 4NH3 → Cu(NH3)4SO4•H2O +4H2O
2. Mr of CuSO4•5H2O: = 63.5 + 32.1 + (4 x 16.0) + 5 x ((2 x 1.0) + 16.0)
= 249.6
Mr of Cu(NH3)4SO4•H2O = 63.5 + (4 x (14.0 + 3 x 1.0) + 32.1 + (4 x 16.0) + (2 x 1.0) + 16.0

= 245.6
3. Moles of copper(II) sulfate used (based on 1.5 g of CuSO4•5H2O):
1. 5
moles = = 0.00601
249 . 6
4. Theoretical yield of Cu(NH3)4SO4•H2O:

As there is a molar ratio of 1:1 we know we will have 0.00601 moles of
Cu(NH3)4SO4•H2O
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The theoretical mass that we would expect to produce can then be calculated YOUR NOTES

mass = 0.00601 x 245.6 = 1.48 g
1. 2
5. Percentage yield = x 100 = 81%
1. 48
 Exam Tip
The percentage yield in this preparation is often calculated to be greater than 100%.
This is usually because the crystals have not been completely dried. This causes the
final mass to be greater than the actual value as it also includes the mass of the
water remaining.
Safety
ENVIRONMENTAL
TOXIC CORROSIVE FLAMMABLE
HAZARD
The hazard symbols associated with this experiment
Wear a lab coat and use eye protection.
Tie long hair back.
Concentrated ammonia solution is corrosive and dangerous to the environment. It must be
kept in the fume cupboard and handled wearing gloves. Ammonia gas can also be evolved
from the solution, which is toxic.
Copper salts are harmful and dangerous to the environment.
Ethanol is flammable and must be kept away from flames.
Errors
Losses could be from the reaction not going to completion and product staying in solution
(i.e. not crystallising out)
Gains could be from impure or wet crystals.
Page 22 of 37
6.2.4 A-Level Qualitative Analysis YOUR NOTES


Core Practical 15: Analysis of Inorganic and Organic Unknowns
Testing for positive ions
Simple test tube reactions can be done to identify the following positive ions:
Group 2 ions (M2+)
Ammonium ions (NH4+)
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 Metal ions
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 chloride 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
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The red litmus paper will change colour and become blue in the presence of ammonia gas YOUR NOTES

Damp red litmus paper turning blue in the presence of ammonia gas
Testing for negative ions
Simple test tube reactions can be done to identify the following negative ions:
Halide ions (X–)
Hydroxide ions (OH–)
Carbonate ions (CO32-)
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 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
The white precipitate is AgCl
The cream precipitate will form if bromide ions are present in the sample
The cream precipitate is AgBr
The yellow precipitate will form if iodide ions are present in the sample
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The yellow precipitate is AgI YOUR NOTES

Further test for halides using ammonia solution 
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
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
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The delivery tube should transfer the gas which is formed into a different test tube YOUR NOTES
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
Page 26 of 37
Exam Tip YOUR NOTES

 HCl is added first to remove any carbonates which may be present and would also

produce a precipitate and interfere with the results.
Testing for alkenes / saturation

Halogens can be used to test if a molecule is unsaturated (i.e. contain a double bond)
Br2 is an orange or 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 for alcohols
Phosphorus(V) chloride (PCl5) can be used as a qualitative test for the presence of an
alcoholic -OH group
This results in a vigorous reaction at room temperature and does not need heating
The evolution of steamy fumes (HCl gas) is a positive result for the presence of the -
OH group
Acidified potassium dichromate(VI) (K2Cr2O7) can be used to identify primary and
secondary alcohols from tertiary alcohols
Acidified potassium manganate(VII) (KMnO4) can also be used
Positive Test Result:
Primary and secondary alcohols are oxidised to aldehydes and ketones respectively (which
can be further tested)
Page 27 of 37
Primary and secondary alcohols will change acidified potassium dichromate(VI) solution YOUR NOTES
from orange to green 
They will also cause a colour change from purple to colourless with acidified
potassium manganate(VII) solution
The colour changes associated with testing for primary and secondary alcohols
Testing for carbonyls (general)
The carbonyl group undergoes a condensation reaction with 2,4-dinitrophenylhydrazine
The product formed when 2,4-DNPH is added to a solution that contains an aldehyde or
ketone is a deep-orange precipitate which can be purified by recrystallisation
Page 28 of 37
YOUR NOTES

The test tube on the left shows a negative 2,4-DNPH test and the tube on the right shows a
positive test
The melting point of the formed precipitate can then be measured and compared to
literature values to find out which specific aldehyde or ketone had reacted with 2,4-DNPH
Testing for Carbonyls (aldehyde / ketone specific)
Tollens' reagent, also known as ammoniacal silver nitrate, is a more specific test-tube
reaction that can distinguish between aldehydes and ketones
When Tollens' reagent is gently warmed with an aldehyde, the silver mirror is formed
This is the positive test result
When Tollens' reagent is gently warmed with a ketone, no silver mirror will be seen, as the
ketone cannot be oxidised by Tollens' reagent, so no reaction takes place
This is a negative test result
Page 29 of 37
TheAg+ ions in Tollens’ reagent areoxidising agents, oxidising the aldehyde to a carboxylic YOUR NOTES
acid and getting reduced themselves to silver atoms 
Fehling's solution (or Benedict's solution) is another specific test-tube reaction that can
distinguish between aldehydes and ketones
When Fehling's solution is gently warmed with an aldehyde, a brick-red precipitate is
formed
This is the positive test result
When Fehling's solution is gently warmed with a ketone, no brick-red precipitate will be
seen, as the ketone cannot be oxidised by Fehling's solution, so no reaction takes place
This is a negative test result
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
Testing for carboxylic acids
Solid sodium carbonate, Na2CO3 (s), or aqueous sodium hydrogen carbonate, NaHCO3
(aq), can be used to test for the presence of a carboxylic acid
Effervescence / bubbles of gas are seen as carbon dioxide is evolved
Page 30 of 37
6.2.5 Aspirin Preparation YOUR NOTES


Core Practical 16: Aspirin Preparation
This practical covers a number of key laboratory skills
use appropriate apparatus to record a range of measurements
use water bath or electric heater or sand bath for heating
use laboratory apparatus for a variety of experimental techniques
purify a solid product by recrystallisation
use melting point apparatus
safely and carefully handle solids and liquids
Synthesis of Aspirin
Key steps in the procedure
6.0 g of salicylic acid is added to a conical flask along with 10 cm3 of ethanoic anhydride
and 5 drops of concentrated sulfuric acid
The mixture is swirled and held in a warm water bath around 60 oC for about 20 minutes
The flask is then allowed to cool and the contents are added to 75 cm3 cold water in a
beaker at which point the aspirin crystallises out
The aspirin is recovered using Buchner filtration and left to dry
The preparation of aspirin using a hot water bath

Recrystallisation and melting point test
The impure aspirin is recrystalised using ethanol, and when the solid has dissolved the
solution is poured over 40 cm3 cold water and recovered using Buchner filtration as before
The melting point of pure aspirin is 135 oC, so the purity of the product can be assessed
Page 31 of 37
Recrystallisation YOUR NOTES

Recrystallisation is used to purify impure solids 
The principle is that a hot solvent is used to dissolve both the organic solid and the
impurities and then as the solution cools the solid crystallises out and leaves behind the
impurities in the solution
The key is using the minimum amount of solvent to dissolve the solid and avoid loss of the
product
If any solid impurities remain in the solution, a hot filtration can be carried out
Once the solution has cooled down to room temperature and crystallised then the product
crystals can be recovered by filtration
This is faster using Buchner apparatus in which filtration occurs under reduced pressure
Recrystallisation and Buchner filtration

After filtration the product is washed with fresh cold solvent and then allowed to dry on filter
paper
Page 32 of 37
Exam Tip YOUR NOTES

 Recrystallisation can be repeated more than once to ensure a very pure product, but

each time the yield of product will decrease. Slow cooling results in bigger well
defined crystals which are easier to filter and dry.
Melting point analysis

The melting point of a solid is indicative of its purity and identity
A melting point can be matched to a known substance as a means of identification or
confirmation of a desired product
The proximity of a melting point to the actual data book value can express purity
Impurities tend to lower the melting point of a solid
The melting point range also reveals the degree of purity
Pure substances have sharp well defined melting points
Impure substances have a broad melting point range, i.e. a large difference between
when the substance first melts until it completely melts
The skills needed in performing a melting point test are largely dependent on the specific
melting point apparatus you are using
However, there are some common key skills:
Correctly preparing the melting point tubes
Heating the tubes very slowly
Repeating to get a range of measurements (three would be normal)
The sample solid must be totally dry and finely powdered - this can be achieved by crushing
it with the back of a spatula onto some filter paper or the back of a white tile (this absorbs
any moisture)
Use the first tube to find the approximate melting point range and then repeat using a much
slower heating rate
Page 33 of 37
YOUR NOTES

Melting point test using an oil bath
Page 34 of 37
Melting point test using a Thiele tube YOUR NOTES


Melting point test using a melt station
 Exam Tip
Always quote a melting point as a range + or - and reference a data book value if you
have one.
Page 35 of 37
Page 36 of 37
Page 37 of 37

UNIT 6 - Practical Skills in Chemistry II

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6. Practical Skills in Chemistry II

6.1 Advanced Physical Chemistry Core Practicals YOUR NOTES

Core Practical 9a: Titrimetric Methods

This graph is a straight line graph

Concentration-time graphs of a zero-order reaction

6.1.2 Rates of Reaction - Clock Reaction YOUR NOTES

Iodine Clock Volume Compositions Table YOUR NOTES

A rate- concentration graph for the iodine clock reaction

6.1.3 Activation Energy YOUR NOTES

Graph plotted from data

6.1.4 Finding Ka Values YOUR NOTES

Key steps in the procedure

6.1.5 Electrochemical Cells YOUR NOTES

Core Practical 13a: Iron(II) & Manganate(VII) Titration

Indicator and end point

with the Fe2+(aq) YOUR NOTES

Add the two half equations: YOUR NOTES

Manganate(VII) titrations can be used to determine:

6.2.2 Redox Titration -Thiosulfate & Iodine YOUR NOTES

1.0 dm3 bleach = 0.630 moles of ClO- ions YOUR NOTES

6.2.3 Transition Metal Complexes YOUR NOTES

Buchner filtration set-up to filter crystals

Exam Tip YOUR NOTES

Mr of Cu(NH3)4SO4•H2O = 63.5 + (4 x (14.0 + 3 x 1.0) + 32.1 + (4 x 16.0) + (2 x 1.0) + 16.0

4. Theoretical yield of Cu(NH3)4SO4•H2O:

6.2.4 A-Level Qualitative Analysis YOUR NOTES

Testing for Ammonium Ions

The yellow precipitate is AgI YOUR NOTES

Exam Tip YOUR NOTES

Testing for alkenes / saturation

6.2.5 Aspirin Preparation YOUR NOTES

The preparation of aspirin using a hot water bath

Recrystallisation YOUR NOTES

Recrystallisation and Buchner filtration

Exam Tip YOUR NOTES

Melting point analysis

Melting point test using an oil bath

Melting point test using a Thiele tube YOUR NOTES

Melting point test using a melt station

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