Grade 11/2023

Addu High School SEMESTER 2

Unit 3: Practical Skills in Chemistry I

Addu High School Chemistry - 2023
 Learning Objectives
Content overview
• Students are expected to develop experimental skills, and a
knowledge and understanding of experimental techniques, by
carrying out a range of practical experiments and investigations
while they study Units 1 and 2.
• This unit will assess students’ knowledge and understanding of
experimental procedures and techniques that were developed in
Units 1 and 2.

AS Level - Chemistry
 Learning Objectives
Assessment overview
• This paper may include short-open, open-response and calculation
questions.
• This paper will include a minimum of 6 marks that target
mathematics at Level 2 or above (see Appendix 6: Mathematical
skills and exemplifications).
• Students will be expected to apply their knowledge and
understanding of practical skills to familiar and unfamiliar
situations.
AS Level - Chemistry
 Core practicals
1. Measuring the molar volume of a gas
2. To determine the enthalpy change of a reaction using Hess’s Law
3. Finding the concentration of a solution of hydrochloric acid
4. Preparation of a standard solution from a solid acid and use it to
find the concentration of a solution of sodium hydroxide
5. Investigation of the rates of hydrolysis of halogenoalkanes
6. Chlorination of 2-methylpropan-2-ol with concentrated
hydrochloric acid
7. The oxidation of propan-1-ol to produce propanal and propanoic
acid
8. Analysis of some inorganic and organic unknowns
AS Level - Chemistry
 Chemical analysis - Inorganic analysis
Test for cations
Ammonium ion, NH4+
• Gently warm the solid or in solution by adding sodium hydroxide solution,
Ammonium salt given off ammonia gas.
• The presence of ammonia gas can be tested by placing a piece of damp red
litmus paper at the open end of the test tube. Ammonia gas reacts with
water to form an alkali, turning the red litmus paper blue.

NH4+ (aq) + OH− (aq) ⇌ NH3(aq) + H2O(l)

AS Level - Chemistry
 Chemical analysis - Inorganic analysis
Test for cations (group 1 and 2)
Flame tests
• To carry out a flame test, a clean nichrome wire is used to mix a
sample of a solid with a few drop of concentrated hydrochloric
acid. The wire is then held at the edge of a hot Bunsen flame
and the colour observed.
Flame test cannot be used on mixtures
containing two of these ions, (Li+, Na+, K+,
Ca2+, Sr2+, Ba2+) because the colour
produced by one of the ions will mask the
colour produced by the other metal ion.

AS Level - Chemistry
 Chemical analysis - Inorganic analysis
Test for cations (group 1 and 2) Flame tests
• Magnesium metal produces a white flame but Magnesium
compounds do not have colour in flame.

Flame colour Metal ion

yellow Sodium
lilac Potassium
Yellow-red Calcium
Pale green Barium
Red* Lithium, Strontium
* Further tests would
Red-violet Rubidium be needed to
distinguish these ions.
AS Level - Chemistry
 Chemical analysis - Inorganic analysis
Heating
• Gases or vapours may be given off on heating a solid inorganic compound.

Gas or vapour given off on

Possible compound
heating
Group 2 carbonates OR
carbon dioxide
lithium carbonate
Group 1 nitrates (except lithium
oxygen
nitrate)
Group 2 nitrates OR
oxygen and nitrogen dioxide
lithium nitrate
water Hydrated salts

AS Level - Chemistry
 Chemical analysis - Inorganic analysis
Test for Anions Carbonate, CO32-
• A small amount of dilute (acid) hydrochloric acid should be added to a test
tube containing carbonate solution.
• If it is a contain carbonate ion, CO2 will be given off.
• This is gas is tested by passing through lime water, which turns milky

Example:
Overall equation: 2HCl (aq) + Na2CO (aq) → 2NaCl (aq) + CO2 (g) + H2O (l)

Ionic equation: 2H+ (aq) + CO32- (aq) → CO2 (g) + H2O (l)

AS Level - Chemistry
 Chemical analysis - Inorganic analysis
Test for Anions Sulfate, SO42-
• 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

Example:
Overall equation: BaCl2 (aq) + Na2SO4 (aq) → 2NaCl (aq) + BaSO4 (s)

Ionic equation: Ba2+ (aq) + SO42- (aq) → BaSO4 (s)

AS Level - Chemistry
 Chemical analysis - Inorganic analysis
Test for Anions Sulfite, SO32-
• To the solution of sulfite ion, add Dilute HCl/ H2SO4 and warm the mixture.
• If sulfite ion is present, then SO2 gas will be given off.
• This gas will be tested by placing a piece of filter paper soaked in
potassium dichromate (VI) in the gas, which changes the colour from
orange to green

Example:
Ionic equation: 2H+ (aq) + SO32- (s) → SO2 (g) + H2O (l)

AS Level - Chemistry
 Chemical analysis - Inorganic analysis
Test for Anions Hydrogen carbonate, HCO3-
• Make a saturated solution of the unknown solid given, Hydrogen
carbonate decomposes with brisk effervescence, with CO2. the gas
The only
produced can be tested by passing it into lime water, which goes hydrogen
milky. carbonate that
• To the solution of CaCl2 add the unknown solution to be tested, exist as solids
Hydrogen carbonates do not give a precipitate because Ca(HCO3)2 is are those of
group 1
soluble, carbonates gives a white precipitates of CaCO3.
metals.
• Test the solution with pH paper, Carbonates have high pH, whereas
hydrogen carbonates are almost neutral.
Example:
Ionic equation: H+ (aq) + HCO3- (aq) → CO2 (g) + H2O (l)

AS Level - Chemistry
 Chemical analysis - Inorganic analysis
Silver nitrate solution
• Aqueous silver nitrate is used to test for the presence of halide ions in solution.
• Anions such as carbonate that would form precipitates with silver nitrate are
removed by adding dilute nitric acid before the aqueous silver nitrate.
• The identity of the halide may be confirmed by adding aqueous ammonia (both
dilute and concentrated) to the silver halide.
Precipitate Addition of aqueous ammonia
Anion
Colour Formula Dilute Concentrated
Chloride, Cl- White AgCl soluble X
Bromide, Br- Cream AgBr insoluble soluble
Iodide, I- Pale yellow AgI insoluble insoluble
AS Level - Chemistry
 Chemical analysis - Inorganic analysis
Barium chloride solution
• Aqueous barium chloride forms precipitates with a number of anions but is
usually used as the test for the sulfate(VI), SO42− anion.
• When dilute hydrochloric acid is added to the anion solution before the
addition of aqueous barium chloride then only the sulfate(VI) anion will
form a precipitate.

AS Level - Chemistry
 Chemical analysis - Inorganic analysis
Concentrated sulfuric acid
• When a few drops of concentrated sulfuric acid (H2SO4) are added to a
solid halide the observed reaction products may be used to identify the
particular halide ion present. This is a potentially hazardous reaction.
• It must be carried out on a small scale and in a fume cupboard.
• The gaseous products in brackets will not be observed since they are
colourless.
• No attempt should ever be made to detect these gases by smell.

AS Level - Chemistry
 Chemical analysis - Inorganic analysis
Concentrated sulfuric acid

AS Level - Chemistry
 Chemical analysis - Inorganic analysis
Displacement of halide ions
• When aqueous chlorine is added to a solution of a bromide or an iodide then
bromine or iodine is displaced.
• When aqueous bromine is added to a solution of an iodide then iodine is
displaced.
• The formation of aqueous solutions of bromine or iodine may be used as a
test for the bromide and iodide ions.
• If an organic solvent such as hexane is added to the reaction mixture the
bromine or iodine dissolves in the organic layer.

AS Level - Chemistry
 Chemical analysis - Inorganic analysis
Displacement of halide ions

AS Level - Chemistry
 Chemical analysis - Inorganic analysis
Test for gases

Bromine dissolves
in organic solvents
to form a brown
solution whereas
nitrogen dioxide is
insoluble.

AS Level - Chemistry
 Chemical analysis - Inorganic analysis
Test for gases

Gases Test Observation Equation

Burns with a
Hydrogen Ignite the gas H2 + ½ O2 → H2O
squeaky pop
Pass gas into Lime water turns CO2(g) + Ca(OH)2(aq) →
Carbon dioxide
lime water milky/ cloudy CaCO3 (s) + H2O (l)

Place a glowing
burns with the
oxygen wooden splint
splint
in the gas.

AS Level - Chemistry
 Chemical analysis - Inorganic analysis
Test for gases
Gases Test Observation

Place damp red litmus

Ammonia Litmus paper turns blue
in the gas

Nitrogen dioxide Observe the colour Brown vapour

Place the damp litmus

Chlorine Litmus paper bleaches
paper in the gas

AS Level - Chemistry
 Chemical analysis - Inorganic analysis
Test for gases
Gases Test Observation Equation
Steamy fumes
Test 1 that turn
Place damp blue litmus damp litmus
paper in the gas paper red
Hydrogen
Chloride /
Test 2
HCl(g)
Place the stopper from White srnoke HCl (g) + NH3 (g) → NH4Cl(s)
the bottle of Conc. (NH4Cl) is
Ammonia in the gas. formed.

AS Level - Chemistry
 Chemical analysis - Inorganic analysis
Test for gases

Gases Test Observation Equation

Place filter
paper soaked Colour changes 3S02 + Cr2072- + 2H+
Sulfur dioxide/
in K2Cr2O7, from orange to → 3SO42- + 2Cr3+ +
SO2
solution in green H20
the gas

AS Level - Chemistry
 Organic analysis
Ignition
• Igniting an organic compound on a crucible lid in a fume cupboard
may provide evidence for the identity of the compound.

AS Level - Chemistry
 Chemical analysis - Organic analysis
Chemical Test
Test Observations Inference

Shake with Yellow solution is

bromine water decolourised alkene

Warm with
aqueous, acidified Orange to green Primary or secondary
potassium solution alcohol, aldehyde
dichromate (VI)

AS Level - Chemistry
Chemical analysis - Organic analysis
Chemical Test
Test Observations Inference
Warm with White precipitate Chloroalkane
ethanol and
aqueous silver Cream precipitate Bromoalkane
nitrate Yellow precipitate Iodoalkane
Steamy fumes that
Phosphoric (v) O-H group in alcohols and
turn damp blue litmus
chloride carboxylic acid
paper red
 Chemical analysis - Organic analysis
Chemical Test
Test Observations Inference
Heat with
Fehling’s solution
or Benedict’s red precipitate aldehyde
solution
Warm with
Tollens’ reagent
silver mirror aldehyde
(ammoniacal silver
nitrate)

AS Level - Chemistry
 Chemical analysis - Organic analysis
Test for C=C
Test: Add bromine water
Observation: brown to colourless
Inference: showing the presence of the C=C group.

RCH=CH2 + Br2 + H2O → RCH(OH)CH2Br + HBr

AS Level - Chemistry
 Chemical analysis - Organic analysis
Test for C-OH
Test: Add PCl5
Observation: Steamy fumes which turns damp blue litmus red.
Inference: HCl gas evolved, showing the presence of the C–OH group
(alcohol and carboxylic acid).

ROH + PCl5 → RCl + POCl3 + HCl

• Do not state that this is a test for alcohols, If the compound gives a positive results
for a C-OH group, the determine whether it is a carboxylic acid or an alcohol.
• To distinguish between two, add sodium hydrogen carbonate solution and will give
brisk effervescence as CO2 with carboxylic acid , with an alcohol no reaction.

AS Level - Chemistry
 Chemical analysis - Organic analysis
Test for C-X (Halogen group)
Test: Warm the compound with aqueous NaOH and allow it to cool, Add
HNO3 and then add AgNO3. • The halogenoalkane is hydrolysed
R-X(aq) + OH-(aq) → R-OH + X- by the sodium hydroxide solution
to give halide ions in the solution,
X-(aq) + Ag+ (aq) → AgX which then reacts with silver ions
to form a precipitate.

Precipitate Addition of aqueous ammonia

Formula Colour Dilute Concentrated
AgCl White soluble X
AgBr Cream insoluble soluble
AgI Pale yellow insoluble insoluble

AS Level - Chemistry
 Organic Chemistry
Preparation of 1-bromobutane
1-bromobutane can be made from butan-1-ol and sodium bromide in 50%
sulfuric acid. Below is a standard preparation together with the reasons for
the various steps involved.
Step 1: Dissolve some sodium bromide in water and mix with butan-1-ol in a round-bottomed
flask. Fit a tap funnel to the flask via a still head. Place 25cm³ of concentrated sulfuric acid in
the tap funnel and allow the acid to fall drop by drop into the flask, keeping the contents well
shaken and cooling occasionally in an ice-water bath.

Why is the sulfuric acid added slowly? Why is cooling and shaking needed?
Sulfuric acid when diluted with water gives out a great deal of heat, enough sometimes
to raise steam, which would cause dangerous splashing. Hot 50% sulfuric acid (produced
in the fask) causes significant oxídation of the sodium bromide to bromine, which is
useless in this experiment. The yield of 1-bromobutane could therefore be reduced.

AS Level - Chemistry
 Organic Chemistry
Preparation of 1-bromobutane
1-bromobutane can be made from butan-1-ol and sodium bromide in 50%
sulfuric acid. Below is a standard preparation together with the reasons for
the various steps involved.
Step 2: When the addition is complete, replace the tap funnel and still head with a reflux
water condenser and gently boil the mixture over a sand bath, occasionally shaking the flask
gently.

Why is a sand bath used for heating?

The sand spreads the heating uniformly over the base of the flask. This reduces the
likelihood of cracking and of unwanted side reactions.
Why is the mixture heated?
Most organic reactions are slow because of the need to break strong covalent bonds the
activation energy for the reaction is high.

AS Level - Chemistry
 Organic Chemistry
Preparation of 1-bromobutane
1-bromobutane can be made from butan-1-ol and sodium bromide in 50%
sulfuric acid. Below is a standard preparation together with the reasons for
the various steps involved.

Step 3: Remove the reflux condenser and rearrange the apparatus for
distillation. Distil off the crude 1-bromobutane.

What impurities are present in the distillate?

The 1-bromobutane is contaminated with water, unchanged butan-
1-ol and some sulfuric acid.

AS Level - Chemistry
 Organic Chemistry
Preparation of 1-bromobutane
1-bromobutane can be made from butan-1-ol and sodium bromide in 50%
sulfuric acid. Below is a standard preparation together with the reasons for
the various steps involved.

Step 4: Shake the distillate with water in a separating funnel and run off the
lower layer of 1-bromobutane.

What does shaking with water achieve?

Water removes sulfuric acid and some of the butan-1-ol
How do you decide which layer is to be kept?
Because 1-bromobutane is denser than water.

AS Level - Chemistry
 Organic Chemistry
Preparation of 1-bromobutane
1-bromobutane can be made from butan-1-ol and sodium bromide in 50%
sulfuric acid. Below is a standard preparation together with the reasons for
the various steps involved.

Step 5: Return the 1-bromobutane to the funnel, add about half its volume of
concentrated hydrochloric acid and shake. Run off and discard the lower layer
of acid.
Why is concentrated hydrochloric acid added?
The acid protonates the butan-1-ol, giving an ionic species that is more
soluble in water than the alcohol itself:
CH3CH2CH2CH2OH + H+ → CH3CH2CH2CH2OH2+

AS Level - Chemistry
 Organic Chemistry
Preparation of 1-bromobutane
1-bromobutane can be made from butan-1-ol and sodium bromide in 50%
sulfuric acid. Below is a standard preparation together with the reasons for
the various steps involved.
Step 6: Shake the 1-bromobutane cautiously with dilute sodium carbonate solution, carefully
releasing the pressure at intervals
Why is the mixture shaken with sodium carbonate solution?
carbonate solution?
This removes hydrochloric acid dissolved in the 1-bromo-butane:
The mixture generates HBr which attacks the alcohol.
Na2CO3 + 2HCl → 2NaCl + CO2 + H20
Why must the pressure be periodically released?
To avoid the stopper being pushed out and product being lost and sprayed al over you.
The pressure is due to liberated carbon dioxide.
AS Level - Chemistry
 Organic Chemistry
Preparation of 1-bromobutane
1-bromobutane can be made from butan-1-ol and sodium bromide in 50%
sulfuric acid. Below is a standard preparation together with the reasons for
the various steps involved.
Step 7: Run off the lower layer of 1-bromobutane And add some granular
anhydrous calcium chloride. Swirl the mixture until the liquid is clear.

What is the function of the calcium chloride?

Calcium chloride is a drying agent.

AS Level - Chemistry
 Organic Chemistry
Preparation of 1-bromobutane
1-bromobutane can be made from butan-1-ol and sodium bromide in 50%
sulfuric acid. Below is a standard preparation together with the reasons for
the various steps involved.
Step 8: Filter the 1-bromobutane into a clean, dry flask and distil it,
collecting the fraction boiling between 99 °C and 102°C.

What is the significance of the temperatures quoted?

1-bromobutane has a boiling temperature of 101.5°C, so the range is narrow
enough to ensure that this is the distillate.
A similar reaction with Sodium chloride can be used to make 1-
chlorobutane, To make 1-iodobutane requires red phosphorus and
iodine instead of sulfuric acid and sodium iodide.

AS Level - Chemistry
 Organic Chemistry - Preparations
Preparation of ethanal by oxidation of ethanol
This standard preparation produces ethanal in aqueous solution It is invariably
contaminated with a small amount of ethanoic acid. The following table lists the steps
in the preparation.

Step 1: Place some water in a round-bottomed flask and add some

concentrated sulfuric acid slowly, with shaking. Add some anti-bumping granules.
Why must the sulfuric acid be added slowly, with shaking?
The reaction between concentrated sulfuric acid and water is dangerously
exothermic. If mixed rapidly so much heat will be produced that the mixture
will boil and spray out hot acidic solution.
What are anti-bumping granules and what is their purpose?
The granules are silicon dioxide. They Promote smooth or even boiling /
prevent the formation of large gas bubbles.
AS Level - Chemistry
 Organic Chemistry - Preparations
Preparation of ethanal by oxidation of ethanol
This standard preparation produces ethanal in aqueous solution It is invariably
contaminated with a small amount of ethanoic acid. The following table lists the steps
in the preparation.

Step 2: Assemble the flask containing the acid into a distillation apparatus.
The still head is fitted with a tap funnel instead of a thermometer. The
receiving flask is placed in an ice-water bath.

Why is the receiver surrounded by ice-water?

The boiling temperature of ethanal is 21°C, so the cooling reduces loss of
ethanal by evaporation.

AS Level - Chemistry
 Organic Chemistry - Preparations
Preparation of ethanal by oxidation of ethanol
This standard preparation produces ethanal in aqueous solution It is invariably
contaminated with a small amount of ethanoic acid. The following table lists the steps
in the preparation.

Step 3: Dissolve some sodium dichromate(VI) in water and add the ethanol.
Place the mixture in the tap funnel. Heat the contents of the round-bottomed
flask to almost boiling and turn off the flame.

Why isn't the ethanol oxidised by the dichromate(Vl) solution?

The oxidation requires H+ ions, and the mixture has not yet been acidified.

AS Level - Chemistry
 Organic Chemistry - Preparations
Preparation of ethanal by oxidation of ethanol
This standard preparation produces ethanal in aqueous solution It is invariably
contaminated with a small amount of ethanoic acid. The following table lists the steps
in the preparation.

Step 4: Slowly add the ethanol/ dichromate(VI) solution into the flask. A
vigorous reaction takes place and the ethanol is immediately boiled off and
condensed in the condenser. The solution turns green as Cr ions are
formed. The cooled receiver contains a mixture of ethanal and water plus a little
ethanoic acid and unreacted ethanol.
Why is the ethanol/dichromate(VI) mixture added slowly to the hot acid?
Rapid addition would lead to an excess of oxidizing agent and some of the
ethanal formed would be oxidised to ethanoic acid.
AS Level - Chemistry
 Organic Chemistry - Preparations
Experimental techniques
• Preparations can include some of the following laboratory
procedures:
• distillation
• heating under reflux
• filtration, including under reduced pressure
• purification by washing in a separating funnel
• solvent extraction

AS Level - Chemistry
Preparations and Purifications
Distilation
Example of diagram:
• Suitable flask (round-bottomed / pear
shaped flask) fitted with still head
containing mixture and heat and with
thermometer in correct position with bulb
opposite opening to condenser.(1)
• Condenser drawn downward with correct
water in and water out labelled (1)
• Collecting flask with vent in flask or in
connection to it.(1)
• Electrical heater(1)
Distilation
1. A student drew a diagram of the apparatus set up for distillation in Step 3.
There are three errors in the diagram. Assume the apparatus is clamped correctly and
an appropriate heat source is used.
Identify the three errors and how they should be corrected. (3)
Distilation
Distilation
2. Suggest why distillation is necessary. (1)
To separate volatile organic liquid substances from non-
volatile organic substances.

3. How could distillation apparatus be used to check the

purity of the product. (2)
• Measure the boiling temperature (1)
• Compare with the data / literature value (1)
Preparations and Purifications
Heat under reflux
• round-bottomed / pear shaped flask
Example of diagram: containing mixture and heat (1)
• vertical condenser with water jacket and
water flowing in the correct direction (1)
• no gaps and open condenser and apparatus
would work (1)

M1 Allow any indication of heat including an arrow or water bath

or electrical heater
Do not award conical flask/flask with no liquid in
Ignore anti bumping granules
M3 Ignore thermometer in the top of the condenser if it does
not seal the apparatus or through the side of a two necked flask
where it is sealed.
Ignore stirrer down condenser
Do not award if the condenser and flask are one piece of
apparatus
Heat under reflux
1. One student drew a diagram of the
apparatus used for reflux
Identify the three errors in the student’s
diagram.
Assume that the apparatus is clamped
correctly. (3)
Heat under reflux