A Level Practical Manual-final 2023
A Level Practical Manual-final 2023
DEPARTMENT OF CHEMISTRY
Student’s Name……………………………………………………………...……
Combination……………………………………………………………..………….
A’ level chemistry examinations consist of three papers i.e. P525/1, P525/2 and P525/3.
Paper 3 (P525/3) is usually practical paper which is done in 3 hours. This paper consists of
three questions which are set from the three branches of chemistry as below;
This simplified workbook consists of two parts i.e. inorganic and organic qualitative
analysis with worked examples and exercise questions. It also contains short explained and
guiding notes which a student should read and understand.
For equations, refer to notes of theory and construct them in the spaces provided.
A good student does research and reads beyond what has been given in class; so be one but
not a master of complaints always.
Introduction
Qualitative analysis is branch of practical chemistry which deals with the identification of ions that
are present in a substance by carrying out several chemical tests on it. There are two types of ions
in ionic or electrovalent compound i.e. cations and anions.
Cations
These are positively charged ions. They are categorised into two major groups i.e. non-transition
metal ions (non- coloured cations) and transitional metal ions (coloured cations).
Anions
These are negatively charged ions. They include;
Others include;
Important to note
In qualitative analysis experiments, there is always a table which consists of three columns.
Test/procedure being the first column followed by observation and then conclusion/deduction/
inference as illustrated below.
Tests: These are instructions given to the students stating what to do on the unknown
substances or its solution in order to identify the ions present in it.
NB; In case the student is asked to carry out a test of his/her own choice to identify or
confirm an anion or a cation present in the unknown compound, the student has to write
the test he or she has performed to identify or confirm the ion asked.
Observation: This is what is seen or identified by a student during and after carrying out
a test. Observations should be short statements that are well summarized.
Deduction/conclusion/inference: These are facts derived from observations and can lead
to the correct identification of the ions present in the unknown substance. The deductions
should correspond to the stated observations that is should follow the order in which
observations are written.
NB: No correct deduction(s) is/are awarded any mark(s) if the corresponding
observation(s) is/are wrong.
PRELIMINARY TESTS
These are tests that give us a clue/hint or general guidelines on the nature of the substance being
analysed. Preliminary tests are majorly based on the following aspects i.e.
In terms of colour, the solid may be white, green, blue, pick/red, brown, yellow or orange, purple,
violet, etc. If the solid is white, then it consists of non-transition metal ions. However, if the solid
is coloured, then it consists of transition metal ions with its specific colour
Colour Deductions
White Non-transitional metal ions
Green Fe2+, Cu2+, Ni2+, Cr3+.
Blue Hydrated Cu2+ salt.
Brown Fe2+ or Fe3+
Black Cu2+ or Ni2+ or Fe2+ or Mn2+
Pink (not visible in solution) Mn2+
Violet Cr3+
Note;
1. In case the solid is crystalline, it has got water of crystallisation and this should be reflected
in that part of heating because water is given off.
2. In case of making deductions about the colour of any unknown solid given, ALWAYS
write cations because they (cations) are the ones that influence the colour of the solid.
A student may be asked to dissolve a sample of the solid given in water and he or she is expected
to make some observations and deductions. The sample may not dissolve in water but dissolves in
acid. Soluble and insoluble salts are given below.
Procedure
Dissolve a little of the substance provided e.g. a spatula endful in about 5 or 10 cm3 of water.
Shake the test tube well until the substance dissolves. The solution obtained is now your test
solution.
1. All soluble white compounds dissolve in water to form colourless solutions whereas
soluble coloured (transition) compounds form solutions corresponding to their colours
when dissolved in water.
2. Dilute nitric acid, sulphuric acid or hydrochloric acid can be used to dissolve insoluble salts
and they also form solutions depending on the colour of the solid given.
3. If the substance is insoluble or partially soluble then filtering may be done. When filtering
is performed, the colour of residue and filtrate must be stated with respective deduction(s).
i) Evolution of a gas;
Gases may be evolved and can be identified using their smell, action on a glowing splint, effect on
litmus paper or any specific reagent for that particular gas given off.
Identification of gases
Gases are normally given off when substances are heated or when acids are added to substances.
A learner can know that a gas is given off through;
Effervescence (rapid emission of bubbles) occurs. This is only seen when an acid is added
to a solid.
Colour. A few gases possess noticeable colours e.g. brown fumes for nitrogen dioxide.
Smell. Some gases have got distinctive smells and they are usually unpleasant. E.g.
ammonia (choking smell) and hydrogen sulphide (smell of rotten eggs).
After knowing that a gas is given off, it can then be identified using a chemical test.
Observation Deduction
Colourless vapour condenses on the cooler parts of the water of crystallization
test tube to form a colourless liquid that turns white :. Hydrated compound
anhydrous copper(II) sulphate blue or blue cobalt(II)
chloride paper pink.
A colourless gas is given off that turns moist/damp blue CO2 gas evolved
litmus paper red/pink and lime water milky. .: HCO3- or CO32- or CH3COO- or C2O42-
A colourless gas with a chocking/irritating smell is given NH3 gas produced
off that turns moist red litmus paper blue and forms dense :. NH4+
white fumes with concentrated hydrochloric
acid/hydrogen chloride gas.
A colourless gas with an irritating smell is given off that SO2 gas evolved
turns damp blue litmus paper red and orange potassium :. SO42- or SO32-
dichromate(VI) solution green.
Reddish brown or brown gas with an irritating smell is NO2 and O2 gases evolved
given off that turns moist blue litmus paper red and a :. NO3-
colourless gas that relights a glowing splint.
Brown vapour that turns moist blue litmus paper red and Br2 gas evolved
bleaches it. :. Br-
Purple vapour that turns moist blue litmus paper red and I2 gas evolved
sublimes to form a black or purple or purplish-black solid :. I-
A greenish yellow gas with an irritating smell, turns Cl2 gas produced
damp blue litmus paper red and then bleaches it. :. Cl-
A colourless gas with an irritating smell, fumes in moist HCl gas evolved
air, turns moist blue litmus paper red and forms dense :. Cl-
white fumes with concentrated ammonia.
White fumes with sweet odour that forms white CH3COCH3 gas evolved
precipitate with Brady’s reagent :. CH3COO-
White fumes that that moist blue litmus paper red and SO3 gas evolved
forms white precipitate with barium nitrate solution :. SO42-
Note: Students are advised to test for gases whenever they
Residue is a solid that remains in a glass tube after heating or on the filter paper after filtering a
mixture of a solid and a liquid. The colour of the residue helps to identify the Cation in the
unknown substance and therefore needs to be carefully observed.
Observation Deduction
Residue is black CuO or FeO or Fe3O4 or NiO or MnO2
:. Cu2+ or Fe2+ or Fe3+ orNi2+ or Mn2+
Residue is white. MgO or CaO or Al2O3 or BaO
:. Mg2+ or Ca2+ or Al3+ or Ba2+
White sublimate. NH4+
Procedure
- To a small portion of the test solution, add a few drops of NaOH(aq) or NH3(aq) and shake the
mixture. Check if precipitate is formed and note its colour.
- Add more sodium hydroxide solution or NH3(aq) until in excess and then shake the solution.
Note whether the precipitate formed is soluble in excess alkali or insoluble in excess alkali.
NB. In case no precipitate appears after adding sodium hydroxide solution, warm the mixture
gently and test for ammonium ions if present or not.
Below is a summary of observations and deductions for reactions between the common cations
and sodium hydroxide solution or aqueous ammonia
Write ionic equation(s) (if any) for the reaction(s) between the metal ions and sodium hydroxide
solution and aqueous ammonia.
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Observations Deductions
White precipitate insoluble in excess Zn2+ or Pb2+ or Sn2+ or Mg2+or Ba2+
White precipitate insoluble in excess with effervescence of a Al3+
colourless gas that turns lime water milky
White precipitate insoluble in excess but turns brown on Mn2+
standing
A green or blue precipitate insoluble in excess Cu2+
A dirty green precipitate insoluble in excess Fe2+
A brown precipitate insoluble in excess with effervescence of Fe3+
a colourless gas that turns lime water milky
Pale green precipitate insoluble in excess Ni2+
No observable change NH4+
Assignment 2
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These are tests that prove beyond doubt that indeed a particular ion is present in the given sample.
The table below summarizes the confirmatory tests for cations.
To the test solution, add a few drops of hydrogen A dark brown ppt with rapid
peroxide solution followed by dilute sodium effervescence of a colourless gas
hydroxide drop wise until in excess. that relights a glowing splint
Fe2+ To the test solution, add 3-4 drops of potassium A dark blue precipitate is formed
hexacyanoferrate(III) solution.
To the test solution, add hydrogen peroxide solution Pale green solution turns to brown
and warm
To the test solution, add concentrated nitric acid and Green solution turns to brown
warm
Fe3+ To the test solution, add 3-4 drops of potassium A dark blue precipitate is formed
hexacyanoferrate(II) solution.
To the test solution, add ammonium or potassium A deep red solution is formed
thiocyanate solution
Cr3+ To the test solution, add dilute sodium hydroxide A green precipitate soluble in
solution drop wise until in excess followed by excess NaOH forming a green
hydrogen peroxide and warm solution and turns to yellow on
addition of hydrogen peroxide
To the test solution, add lead(II) nitrate or ethanoate A yellow precipitate
solution followed by dilute sodium hydroxide
This is done by adding dilute mineral acid such as dilute nitric acid to the filtrate obtained after
adding sodium hydroxide solution or ammonia solution and filtering. This differentiates
amphoteric cations and non-amphoteric cations.
During addition of an acid, a precipitate is formed and when it dissolves, the addition is stopped
and the solution is said to be ’just acidic’.
Explanation
During the reaction the amphoteric cation with sodium hydroxide, a precipitate is formed which
dissolves in excess to form a complex solution e.g.
During filtration the colourless solution (tetrahydroxoaluminate(III) ions) remain in the filtrate and
to make them free, an acid has to be add to the filtrate until it is just acidic. Then the aluminium
ions are free in solution. The reactions which occur are;
Washing the residue with distilled water and then dissolving in acid
This is done by pouring water on the residue through the filter paper in a funnel times. This
removes any traces of the soluble cations which might be trapped in the residue. The wash residue
is the dried between filter papers and carefully transferred to the test tube.
A dilute acid normally hydrochloric acid or nitric acid is then added to the residue until there is no
further change. Watch what happens and the write your observations and deductions as illustrated
below
Observations Deductions
The white residue dissolves with effervescence CO2 evolved
of a colourless gas that turns moist blue litmus CO32- confirmed
paper red and lime water milky.
The resultant solution is colourless Non transition metal ions present
Identification of anions
To the test solution, add few White precipitate insoluble in Cl- confirmed
drops of silver nitrate acid
followed by dilute nitric acid A pale yellow precipitate I-
A white precipitate soluble in CO2 evolved
the acid with effervescence of C2O42-, CO32-
a colourless gas that turns
moist blue litmus paper red
and lime water milky
Sample question
You are provided with substance K which contains two cations and two anions. You are required
to carry out the following tests on K to identify the cations and anions in K. Identify any gas(es)
evolved. Record your observations and deductions in the table below.
Tests Observations Deductions
a) Heat a spatula endful of 𝑲 -White crystalline solid Non-transition metal ions
in a dry test tube strongly -A colourless condensate which turns Water of crystallization
until there is no further white anhydrous copper(II) sulphate to Hydrated salt
change. blue
-A colourless vapour with a sweet fruity Propanone vapour evolved
smell and forms a yellow precipitate CH3COO-
with Brady’s reagent
-A colorless gas that turns lime water CO2 evolved
milky and moist blue litmus paper red C2O42- or CO32-
-Brown fumes of a gas which turns NO2 evolved
moist blue litmus paper red NO3-
-A brown residue when hot and yellow PbO
on cooling Pb2+
b) To a spatula endful of 𝑲, - White fumes with a vinegar smell Ethanoic acid fumes
add 3-5 drops of and turns moist blue litmus paper evolved
concentrated sulphuric acid red. ∴ CH3COO-
and warm gently. - Brown fumes which turn moist blue NO2(g) evolved
litmus paper red. ∴ NO3−
c) To two spatula endfuls of - White crystalline solid dissolves to Ba2+, Ca2+ or Mg2+
K, add distilled water and form a colourless solution
shake to dissolve. To the - White precipitate insoluble in Pb2+ or Al3+ or Mg2+
resultant solution, add dilute excess.
ammonia solution drop wise - Colourless filtrate. Zn2+ or Ca2+
until in excess and filter. - White solid residue. Pb2+or Al3+
drops of concentrated
sulphuric acid and warm.
Pour the mixture into a
beaker of cold water.
vi) To the sixth portion, add A colourless gas which turns moist red NH3(g) evolved.
zinc metal powder followed litmus paper blue and forms dense white ∴ NO3− confirmed
by excess sodium hydroxide fumes with hydrogen chloride gas.
solution and warm.
f) Wash the residue obtained White solid residue dissolves to form a Pb2+ or Al3+or Mg2+
in (c) with water and dissolve colourless solution
it in dilute nitric acid. Divide
the resultant solution into
four portions.
i) To the first part, add dilute White precipitate soluble in excess to Pb2+ or Al3+
sodium hydroxide solution form a colourless solution.
drop wise until in excess.
ii) To the second portion, add White precipitate insoluble in excess Pb2+ or Al3+
dilute ammonia solution drop
wise until in excess.
iii) To the third portion, add White precipitate Pb2+
dilute sulphuric acid.
iv) To the fourth portion, add Yellow precipitate soluble in excess to Pb2+
potassium chromate solution form a yellow solution
followed by sodium
hydroxide solution drop wise
until in excess.
BRAIN CHECK.
1. You are provided with substance Q which contains two cations and two anions. You are required
to carry out the following tests on Q to identify the cations and anions present. Identify any gas(es)
evolved. Record your observations and deductions in the table below.
Q [FeSO4.7H2O + ZnCO3]
d) Identify the
i) Cations in Q………………………………………………………………………………………
ii) Anions in Q………………………………………………………………………………………
3. You are provided with substance W which contains two cations and two anions. You are
required to carry out the following tests on W to identify the cations and anions present.
Identify any gas(es) evolved. Record your observations and deductions in the table below.
W [(CH3COO)2Pb + ZnCl2.6 H2O]
Tests Observations Deductions
a) Heat a spatula endful of W in
a dry test tube strongly until there
is no further change.
d) Identify the
i) Cations in W………………………………………………………………………………………
ii) Anions in W……………...………………………………………………………………………
4. You are provided with substance X which contains two cations and two anions. You are
required to carry out the following tests on X to identify the cations and anions present.
Identify any gas(es) evolved. Record your observations and deductions in the table below.
[NiCl2.6H2O + ZnCO3]
TESTS OBSERVATIONS DEDUCTIONS
a) Heat a spatula endful of X in a
dry test tube first gently, then
strongly until there is no further
change.
Allow it to cool
4. You are provided with substance T which contains two cations and two anions. You are
required to carry out the following tests on T to identify the cations and anions present.
Identify any gas(es) evolved. Record your observations and deductions in the table below.
TESTS OBSERVATIONS DEDUCTIONS
a) Heat a spatula endful of T in a
dry test tube first gently, then
strongly until there is no further
change.
d) Identify the;
i) Cations in T………………………………………………………………………………………
5. You are provided with substance H which contains two cations and two anions. You are
required to determine the ions in H.
Carry out the following tests and identify any gas(es) evolved. Record your observations
and deductions in table III below.
Tests Observations Deductions
Test
a) Identify the
i) Cations in H ……………………………………… and ……………………………
ii) Anions in H ……………………………………… and ……………………………
6. You are provided with substance X, which contains two cations and two anions. You are
required to carry out the following tests on X to identify the cations and anions in X.
Identify any gases evolved.
You are provided with an organic compound M. You are required to carry out the following
tests on M. Record your observations and deductions in the table below and describe the
/comment on the nature of M.
Organic questions are usually organized in a table format (as below) requiring candidates to
write observations and deductions after performing the given tests. However, examiners can
ask learners to carry out tests of their own choice to identify the organic compound given.
The objectives are above are achieved by carrying out preliminary and confirmatory tests on
the given organic substance
a) Preliminary tests
1. Physical appearance
This gives an over view of the nature of the organic compound
Observation Deduction
A colourless liquid Lower aliphatic compound e.g. alcohol,
aldehydes, ketones, carboxylic acids, esters
Solid compound Aromatic compound or higher aliphatic
compound e.g. salts of carboxylic acids,
phenol, dicarboxylic acids and
carbohydrates.
2. The flame test
Unlike inorganic compounds, flame test is vital in analyzing organic compounds.
This is important in
Categorizing organic compounds as either aliphatic or aromatic.
Determining carbon to hydrogen ratio (carbon content) in organic compounds
Categorizing organic compounds as either saturated or unsaturated.
Test Observation Deduction
Burn a small amount Burns with a yellow non- Aliphatic, saturated compound with
of the organic sooty flame a low carbon content
compound on a Burns with a yellow sooty Aromatic or unsaturated aliphatic
spatula end or flame compound with a high carbon content
crucible Does not burn Alkyl halide or nitrogen containing
compound or salt of carboxylic acid.
3. Smell. The smell of the compound can be a guide but not a sure test
4. Solubility in Water
The solubility of organic compounds decreases with increasing molecular mass of the
compounds in a given series.
Therefore, if the substance readily dissolves in water, then the sample is likely to be a low
molecular compound.
Usually the solution formed with water is tested with litmus (blue and red) or
universal indicator to ascertain whether it is neutral, basic or acidic.
Phenol and aromatic carboxylic acids do not easily dissolve in cold water, but
soluble in hot water, and their solutions turn blue litmus paper red.
5. Use of indicator
Litmus paper Litmus solution Universal indicator Deduction
solution
Has no effect on both Has no effect on litmus Solution remains green Neutral compound;
blue and red litmus solution Alcohols or carbonyl or
paper ester present
Blue litmus paper turns Blue litmus solution Solutions turn to red or Acidic compound;
to red or pink turns to red pink or orange Carboxylic acid or
phenol present
Red litmus paper turns Red litmus solution Solution turns blue Basic compound
blue turns blue Amines or salt of
carboxylic acid present
b) Confirmatory tests
Test Observation Deduction
Add a few drops of Brady’s reagent Yellow precipitate Carbonyl
or 2-3 drops of Compound;
2,4-dinitrophenylhydrazine (ketone or aldehyde)
Note: Conc. HCl can be added
followed by warming No observable change Carbonyl compound absent
Add acidified potassium dichromate Orange solution turns to Primary or secondary alcohol,
solution and heat green Aldehyde present
1. You are provided with an organic substance Y. Carry out the following tests on Y and
record your observations and deductions in the table below.
b) Add 1cm3 of Y to 1cm3 of Miscible with water forming a Polar aliphatic compound of
water in a test tube and shake. colourless solution; lower molecular.
Test the mixture with litmus. Resultant solution has no effect Neutral compound;
Divide the resultant solution on litmus Alcohol or carbonyl
into three parts. compound.
i) To the first part, add 2-3 drops No observable change Carboxylic acid absent
of sodium carbonate solution
ii) To the second part, add 2cm3 No observable change Carbonyl compound absent;
of Brady’s reagent alcohol present.
iii) To the third part, add 2cm3 of Yellow precipitate CHI3 formed
iodine solution followed by Alcohol with a methyl group
sodium hydroxide solution directly attached to the carbon
dropwise until the colour of atom with the functional
iodine is discharged. group present.
c) Add 2cm3 of acidified The purple solution turns to Primary or secondary alcohol
potassium permanganate colourless oxidised
solution to 3cm3 of Y in a
boiling tube heat the mixture.
Divide the solution into two
parts
ii) To the second part, add Effervescence of a colourless gas Carbon dioxide evolved
sodium carbonate solution that turns lime water milky and Carboxylic acid from
moist blue litmus paper red oxidation of primary alcohol
d) Deduce the nature of Y.
Y is a polar aliphatic saturated primary alcohol with a methyl group directly attached
to the carbon atom with the functional group.
2. You are provided with solid T. you are required to carry out the following tests to
determine the nature of T
Tests Observations Deductions
a) Burn a little of T on a spatula T burns with a yellow sooty Aromatic compound
end flame
i) To the first part add sodium Effervescence of a colourless Carbon dioxide evolved
carbonate solution gas that turns lime water milky Carboxylic acid
and moist blue litmus paper
ii) To the second part, add neutral Purple or violet solution is Phenol present
iron(III) chloride solution formed
iii) To the third part, add Brady’s No observable change Carbonyl compound absent
reagent
iv) To the fourth part add sodium Colourless sweet fruity Esterification reaction
hydroxide solution followed by few smelling compound Ester formed
drops of concentrated sulphuric acid Phenol present
followed by ethanoic acid
v) To the fifth part, add equal volume Colourless sweet fruity Ester formed
of ethanol followed by three drops of smelling compound T is Carboxylic acid
concentrated sulphuric acid and warm.
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3. You are provided with an organic compound R. carry out the following tests on R to
identify its nature. Record your observations and deductions in the table below
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3. You are provided with an organic compound Q. carry out the following tests on Q to identify
nature.
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4. You are provided with substance Y which is an organic compound. Carry out the following tests
to identify its nature
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5. You are provided with substance K which is an organic compound. Carry out the following tests
on K to identify its functional group.
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6. You are provided with an organic compound W. You are required to carry out the tests below
on W to identify its nature. Identify any gas(es) evolved. Record your observations and deductions
in the table below
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7. You are provided substance M which is an organic compound. You are required to
determine the nature of M. carry out the following tests and identify any gas(es) evolved
Record your observations and deductions in the table below
Tests Observations Deductions
a) Burn a small amount of M on
a spatula
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8. You are provided substance L which is an organic compound. You are required to determine
the nature of L. carry out the following tests and identify any gas(es) evolved. Record your
observations and deductions in the table below
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9. You are provided with an organic compound H. You are required to determine the nature of H.
carry out the following tests and identify any gas(es) evolved
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THE END