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Uace Chem 3 Guiding Manual

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0% found this document useful (0 votes)

437 views53 pages

Uace Chem 3 Guiding Manual

For all chemistry students in Uganda who do chemistry as part of their combination.. this might be helpful to you

Uploaded by

masemvirgin

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Extract From JUSAN Advanced Level Practical Manual

 COMPLEX MIXTURES AND THE DOUBLE INDICATOR ANALYSIS TECHNIQUE

These are solution mixtures in which both components in the mixture react with the standard
solution titrated against.
Examples of complex mixtures include;
 NaOH and Na2CO3 titrated with HCl/ HNO3/H2SO4
 NaOH and NaHCO3 titrated with HCl/ HNO3/H2SO4
 Na2CO3 and NaHCO3 titrated with HCl/ HNO3/H2SO4
 KOH and K2CO3 titrated with HCl/ HNO3/H2SO4
 KOH and KHCO3 titrated with HCl/ HNO3/H2SO4
 K2CO3 and KHCO3 titrated with HCl/ HNO3/H2SO4
Theory for complex mixture titration.
These mixtures are analyzed using two indicators, methyl orange and phenolphthalein
indicators, hence, double indicator titration.
These two indicators have different working pH ranges (pH range over which the indicator
changes colour), therefore detect end points at different pH points.

ANALYSIS OF MIXTURE OF NaOH AND Na2CO3 WHEN TITRATED WITH HCl

While the reaction with NaOH takes place in one step
NaOH (aq) + HCl (aq) ⟶ NaCl (aq) + H2O (l).................................................... (i)
Reaction between HCl (aq) with Na2CO3 takes place in two stages:
Na2CO3 (aq) + HCl (aq) ⟶ NaHCO3 (aq) + NaCl (aq)........................................ (ii)
NaHCO3 (aq) + HCl (aq) ⟶ NaCl (aq) + H2O (l) + CO2 (g)................................... (iii)

HINT ON INDICATOR ACTION!

Solution mixture of reaction (i) at the endpoint point is neutral, that of reaction (ii) is alkaline
and that of reaction (iii) is acidic. Endpoints for reactions (i) and (ii) can be indicated by
phenolphthalein and that of reaction (ii) can be indicated by methyl orange.

Check! Do you realize that all the above reactions have a reaction ratio of 1: 1

THE TWO STEP/ DISCONTINOUS/ STEPWISE AND CONTINUOUS TITRATION

TECHNIQUES OF DOUBLE INDICATOR METHOD.
The analysis of the above mixture can be done by step wise titration or continuous titration, each
technique resulting in different titer values for each indicator. For convenience during
calculations, the volume of acid required to reach the phenolphthalein end point will be denoted
by Vp while that for the methyl orange end point will be denoted by Vm. The expressions for
determine the volume of acid required to neutralize the different components in the mixture can
be derived for the different techniques.

1. Stepwise/ discontinuous method, (using two indicators separately)

In this method, a fixed volume of the solution mixture containing sodium carbonate and
sodium hydroxide is pipette in the conical flask, 2-3 drops of phenolphthalein indicator are
added, then titrated against the standard acid in the burette to the endpoint. The volume Vp
cm3 is recorded in the result table 1; and average volume of standard acid used is calculated.
The resultant solution in conical flask is poured away; and a fresh fixed volume of the mixture/
aliquot is pipette into the conical flask, 2-3 drops methyl orange indicator are added, then

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Page 1 of 17
Extract From JUSAN Advanced Level Practical Manual

titrated against standard acid to the end point. The volume Vm cm3 is recorded in the result
table 2.

ANALYSIS OF VOLUMES FROM STEPWISE METHOD

The volume Vp cm3 will be for the reaction (i) and (ii) as below.
NaOH (aq) + HCl (aq) ⟶ NaCl (aq) + H2O (l)........................... (i)
Na2CO3 (aq) + HCl(aq) ⟶ NaHCO3 (aq) + NaCl (aq)....................(ii)
The volume Vm cm3 will be for all the reaction (i), (ii) and (iii) as below.
NaOH (aq) + HCl (aq) ⟶ NaCl (aq) + H2O (l)................................... (i)
Na2CO3 (aq) + HCl (aq)⟶ NaHCO3 (aq) + NaCl (aq)........................ (ii)
Remember reaction (i) and (ii) already exist when using phenolphthalein!
NaHCO3 (aq) + HCl (aq) ⟶NaCl (aq) + H2O (l) + CO2 (g)................ (iii)
Therefore:
 The volume of acid for reaction (iii) = (Vm – Vp) cm3, but this is half the volume required for
the complete neutralization of the Na2CO3 in the mixture to NaHCO3, hence the volume of
acid required to completely neutralize the Na 2CO3 = 2 (Vm – Vp) cm3
 Since the volume for reaction (iii) = volume for reaction (ii); reason being they are all half
neutralization reactions of Na2CO3. Therefore, the volume of acid required for neutralization
of NaOH = Vp – (Vm – Vp) cm3 = (2Vp – Vm) cm3
 The calculation follow the usual mole-concept and stoichiometry
 It should be noted therefore that for discontinuous/ step wise titration, Vm > Vp

1. SAMPLE P525/1&2 STRUCTURED QUESTION

25.0cm3 of solution containing sodium hydroxide, NaOH and sodium carbonate Na 2CO3;
required 17.0cm3 of 0.1M hydrochloric acid when using phenolphthalein indicator. 25.0cm 3 of
the solution required 22.0cm3 of the acid while using methyl orange indicator.
(a) Write equation(s) that took place when using;
(i) Phenolphthalein indicator. (2mark)
NaOH (aq) + HCl (aq) ⟶ NaCl (aq) + H2O (l) ✓
Na2CO3 (aq) + HCl (aq) ⟶ NaHCO3 (aq) + NaCl (aq) ✓
(ii) Methyl orange indicator. (3mark)
NaOH (aq) + HCl (aq) ⟶ NaCl (aq) + H2O (l). ✓
Na2CO3 (aq) + HCl (aq)⟶ NaHCO3 (aq) + NaCl (aq). ✓
NaHCO3 (aq) + HCl (aq) ⟶NaCl (aq) + H2O (l) + CO2 (g) ✓
(b) Determine the volume of hydrochloric acid required for complete neutralization of ,
(i) Sodium carbonate. (1mark)
Let the volume required when using phenolphthalein indicator be Vp = 22.00cm3
Let the volume required when using methyl orange indicator be Vm = 17.00cm 3
Volume of HCl required to neutralize Na2CO3 = 2(Vm- Vp) cm3
2 (22.00 – 17.00) cm3✓ = 10.00cm3✓
(ii) Sodium hydroxide. (1mark)
Volume of HCl required to neutralize NaOH = 2Vp- Vm cm3
2 (22.00 – 17.00) cm3✓
= 12.00cm3✓
(c) The concentration of sodium carbonate in the mixture in g/500cm3. (5½marks)
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Page 2 of 17
Extract From JUSAN Advanced Level Practical Manual

1000cm3 of solution contain 0.1 moles of HCl

moles of HCl✓
𝟎.𝟏 𝒙 𝟏𝟎.𝟎𝟎
10.00cm3 of solution contain
𝟏𝟎𝟎𝟎
= 0.001 moles of HCl ✓
From equation, Na2CO3 (aq) + 2HCl (aq) ⟶ 𝟐NaCl (aq) + H2O (l) + CO2 (g) ✓✓
2moles of HCl react with 1 moles of sodium carbonate
moles of sodium carbonate✓
𝟏 𝒙 𝟎.𝟎𝟎𝟏
0.001 moles of HCl react with
𝟐
= 0.0005 moles of sodium carbonate✓
3
25.0cm of solution contain 0.0005 moles of sodium carbonate
moles/ 500cm3✓
𝟎.𝟎𝟎𝟎𝟓 𝒙 𝟓𝟎𝟎
500cm3 of solution contain
𝟐𝟓.𝟎
= 0.01 moles/500cm3 of Na2CO3. ✓
From molar mass of Na2CO3 = (23x2) + (12x1) + (16 x3) = 106gmol-1✓
1 moles weighs 106g of Na2CO3
0.01moles weigh (106 x 0.01) g/500cm3 Na2CO3. ✓
= 1.06 g/500cm3 Na2CO3✓
(d) The concentration of sodium hydroxide in the mixture in g/dm3 (5½marks)
3
1000cm of solution contain 0.1 moles of HCl
moles of HCl✓
𝟎.𝟏 𝒙 𝟏𝟐.𝟎𝟎
12.00cm3 of solution contain
𝟏𝟎𝟎𝟎
= 0.0012 moles of HCl ✓
From equation, NaOH (aq) + HCl (aq) ⟶NaCl (aq) + H2O (l) ✓
1moles of HCl react with 1 moles of NaOH
0.0012 moles of HCl react with 0.0012 moles of NaOH ✓
= 0.0012 moles of NaOH✓
3
25.0cm of solution contain 0.0012 moles of NaOH
moldm-3✓
𝟎.𝟎𝟎𝟏𝟐 𝒙 𝟏𝟎𝟎𝟎
1000cm3 of solution contain
𝟐𝟓.𝟎
= 0.048 mol/dm3 of NaOH. ✓
From molar mass of NaOH= (23x1) + (1x1) + (16 x1) = 40gmol-1✓
1 moles weighs 40g of NaOH
0.01moles weigh (40 x 0.048) gdm-3 NaOH ✓
= 1.92 gdm3 NaOH✓

2. TRIAL P525/1&2 ESSAY QUESTTION

50.0cm3 of a solution containing sodium hydroxide and sodium carbonate was diluted to
250cm3 with distilled water. 25cm3 of the diluted solution required 15cm3 of 0.2M sulphuric
acid using phenolphthalein indicator, another 25cm3 of the diluted solution of the mixture
required 27.5cm3 of 0.2M sulphuric acid using methyl orange indicator.
(a) Write equation(s) that took place when using;
(iii) Phenolphthalein indicator. (2mark)
(iv) Methyl orange indicator. (3mark)
(b) Determine the volume of sulphuric acid required for complete neutralization of ,
(iii) Sodium carbonate. (1mark)
(iv) Sodium hydroxide. (1mark)
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Page 3 of 17
Extract From JUSAN Advanced Level Practical Manual

(c) Calculate in grams per litre.

(i) The concentration of sodium carbonate in the mixture. (5½marks)
(ii) The concentration of sodium hydroxide in the mixture. (5½marks)

EXPERIMENT 1:
You are provided with
FA3 which is a solution mixture of sodium hydroxide and sodium carbonate
FA4 is a standard solution of 0.1M hydrochloric acid.
You are required to determine to amount of sodium hydroxide and sodium carbonate in
a mixture using standard hydrochloric acid.
Procedure 1.
(i) Pipette 20 or 25cm3 of FA3 into a clean conical flask.
(ii) Titrate with FA4 using 2-3 drops of phenolphthalein indicator until the end point is attained.
(iii) Repeat the titration to obtain consistent results.
(iv) Record the results in the table 1 below.
Results.
Volume of Pipette……………………………………………………………..cm3. (½marks)
Table 1.
TITRATION NUMBER I II III

Final burette reading (cm3)

Initial burette reading (cm3)

Volume of FA4 used (cm3)

(4½marks)

Titre values used to calculate average volume of FA4 used are; (½marks)
and cm3

Therefore average volume of FA4 using phenolphthalein = cm3. (2½marks)

Procedure 2.
(i) Pipette 20 or 25cm3 of a fresh aliquot of FA3.
(ii) Titrate with FA4 using 2-3 drops of methyl orange indicator until the end point is attained.
(iii) Repeat the titration to obtain consistent results.
(iv) Record the results in the table below.
Results
Volume of Pipette………………………………………………………..cm 3. (½marks)
Table 2

TITRATION NUMBER I II III

Final burette reading (cm3)

Initial burette reading (cm3)

Volume of FA4 used (cm3)

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Page 4 of 17
Extract From JUSAN Advanced Level Practical Manual

(4½marks)

Titre values used to calculate average volume of FA4 used are; (½marks)
and cm3

Therefore average volume of FA4 using methyl orange = cm3. (2½marks)

(a) Write equation(s) that took place when using;
(i) Phenolphthalein indicator. (2mark)
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
(ii) Methyl orange indicator. (3mark)
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
(a) Determine the volume of sulphuric acid required for complete neutralization of ,
(i) Sodium carbonate. (1mark)
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
(ii) Sodium hydroxide. (1mark)
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
(b) Calculate the concentration in grams per litre of.
(i) Sodium carbonate in FA3. (5½marks)
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
(ii) Sodium hydroxide in FA3. (5½marks)

2. Continuous titration; (using two indicators co-currently)

In this method, a fixed volume/ an aliquot of the mixture is pipette into a clean conical flask;
2-3 drops of phenolphthalein indicator are added and then titrated against standard acid from
the burette until the end-point. The volume Vp cm3 required to reach endpoint is recorded
in the result table 1. Without pouring away the resultant solution in the conical flask, add 2-3
drops of methyl orange indicator and continue titrating to obtain a second end point, the
volume Vm cm3 is recorded in the result table 2.
ANALYISIS OF VOLUMES FROM CONTINUOUS METHOD
The volume of the acid Vp cm3 will be for reactions (i) and (ii)
NaOH (aq) + HCl (aq) ⟶ NaCl(aq) + H2O (l)............................................................... (i)
Na2CO3 (aq) + HCl (aq) ⟶ NaHCO3 (aq) + NaCl (aq).................................................. (ii)
Remember reaction (ii) is half neutralization of Na2CO3 which will be completed in
reaction (iii)
The volume Vm cm3 will be for only reaction (iii)
NaHCO3 (aq) (from initial Na2CO3) + HCl (aq) ⟶ NaCl (aq) + H2O (l) + CO2 (g)................ (iii)

Therefore
 Since the volume of the acid Vm for reaction (iii) = volume for reaction (ii) is for half
neutralization of Na2CO3 to NaHCO3, hence volume required to completely neutralize
Na2CO3 in the mixture = 2Vm cm3
 The volume of acid required to neutralize NaOH in the mixture = (Vp – Vm) cm3
 It should be noted that for continuous titration Vp >Vm

1. SAMPLE P525/1&2 STRUCTURED QUESTION

25.0cm3 of a solution mixture containing sodium hydroxide and sodium carbonate; required
30.00cm3 of a 0.1M hydrochloric acid using phenolphthalein indicator and further 12.50cm 3 of
the acid was required using methyl orange indicator. Calculate the concentration of;
(a) Write equation(s) that took place when using;
(i) Phenolphthalein indicator. (2mark)
NaOH (aq) + HCl (aq) ⟶ NaCl(aq) + H2O (l). ✓
Na2CO3 (aq) + HCl (aq) ⟶ NaHCO3 (aq) + NaCl (aq) ✓
(ii) Methyl orange indicator. (1mark)
NaHCO3 (aq) + HCl (aq) ⟶ NaCl (aq) + H2O (l) + CO2 (g) ✓
(b) Determine the volume of sulphuric acid required for complete neutralization of ,
(i) Sodium carbonate. (1mark)
Let the volume required when using phenolphthalein indicator be Vp = 30.00cm 3
Let the volume required when using methyl orange indicator be Vm = 12.50cm3
Volume of HCl required to neutralize Na2CO3 = 2Vm cm3
2 x 12.5 cm3✓
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Page 6 of 17
Extract From JUSAN Advanced Level Practical Manual

= 25.00cm3✓
(ii) Sodium hydroxide. (1mark)
3
Volume of HCl required to neutralize NaOH = (Vp – Vm) cm
(30.00- 12.50) cm3✓
= 17.50cm3✓
(c) Calculate in grams per litre.
(i) The concentration of sodium carbonate in the mixture. (5½marks
1000cm3 of solution contain 0.1 moles of HCl
moles of HCl✓
𝟎.𝟏 𝒙 𝟐𝟓.𝟎𝟎
25.00cm3 of solution contain
𝟏𝟎𝟎𝟎
= 0.0025 moles of HCl ✓
From equation, Na2CO3 (aq) + 2HCl (aq) ⟶ 𝟐NaCl (aq) + H2O (l) + CO2 (g) ✓✓
2moles of HCl react with 1 moles of sodium carbonate
moles of sodium carbonate✓
𝟏 𝒙 𝟎.𝟎𝟎𝟐𝟓
0.001 moles of HCl react with
𝟐
= 0.00125 moles of sodium carbonate✓
3
25.0cm of solution contain 0.00125 moles of sodium carbonate
moles/ 500cm3✓
𝟎.𝟎𝟏𝟐𝟓 𝒙 𝟏𝟎𝟎𝟎
1000cm3 of solution contain
𝟐𝟓.𝟎
= 0.05 moles/500cm3 of Na2CO3. ✓
From molar mass of Na2CO3 = (23x2) + (12x1) + (16 x3) = 106gmol-1✓
1 moles weighs 106g of Na2CO3
0.05moles weigh (106 x 0.01) g/dm3 Na2CO3. ✓
= 5.3 gl-1 Na2CO3✓
(ii) The concentration of sodium hydroxide in the mixture. (5marks)
1000cm3 of solution contain 0.1 moles of HCl
moles of HCl✓
𝟎.𝟏 𝒙 𝟏𝟕.𝟓𝟎
17.50cm3 of solution contain
𝟏𝟎𝟎𝟎
= 0.00175 moles of HCl ✓
From equation, NaOH (aq) + HCl (aq) ⟶NaCl (aq) + H2O (l) ✓
1moles of HCl react with 1 moles of NaOH
0.00175 moles of HCl react with 0.00175 moles of NaOH✓
= 0.00175 moles of NaOH✓

25.0cm3 of solution contain 0.00175 moles of NaOH

moldm-3✓
𝟎.𝟎𝟎𝟏𝟕𝟓𝒙 𝟏𝟎𝟎𝟎
1000cm3 of solution contain
𝟐𝟓.𝟎
= 0.07 mol/dm3 of NaOH. ✓
From molar mass of NaOH= (23x1) + (1x1) + (16 x1) = 40gmol-1✓
1 moles weighs 40g of NaOH
0.07 moles weigh (40 x 0.07) gdm-3 NaOH ✓
= 2.8 gl-1 NaOH✓

2. TRIAL P525/1&2 ESSAY QUESTION

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Page 7 of 17
Extract From JUSAN Advanced Level Practical Manual

25.0cm3 of a solution mixture containing sodium hydroxide and sodium carbonate required
23.10cm3 of a 0.2M hydrochloric acid using phenolphthalein indicator, and further 7.90cm 3 of
the acid using methyl orange indicator. Calculate the concentration of sodium hydroxide and
sodium carbonate in the mixture in g/250cm 3.
(a) Write equation(s) that took place when using;
(i) Phenolphthalein indicator. (2mark)
(ii) Methyl orange indicator. (1mark)
(b) Determine the volume of sulphuric acid required for complete neutralization of ,
(i) Sodium carbonate. (1mark)
(ii) Sodium hydroxide. (1mark)
(c) Calculate in grams per litre.
(i) The concentration of sodium carbonate in the mixture. (5½marks)
(ii) The concentration of sodium hydroxide in the mixture. (5marks)

EXPERIMENT 2:
You are provided with
FA1 which is a solution mixture containing sodium hydroxide and sodium carbonate.
FA2 is a standard solution of 0.2M hydrochloric acid.
You are required to determine the concentration of sodium hydroxide and sodium
carbonate in a mixture using standard hydrochloric.
Procedure
Pipette 20 or 25cm3 of FA1 into a conical flask and titrate with FA2 using 2-3 drops of
phenolphthalein indicator until the end point is attained.
Record the results in table 1
Without pouring away, the resultant solution in the conical flask, add 2-3 drops of methyl orange
indicator and continue to titrate with FA2 until the second end point is attained.
Record the results in table 2.
Repeat the procedure 2 more times to obtain consistent results.

Results.
Volume of Pipette……………………………………………………………..cm 3. (½marks)

Table 1: (Phenolphthalein indicator)

TITRATION NUMBER I II III

Final burette reading (cm3)

Initial burette reading (cm3)

Volume of FA2 used (cm3)

(4½marks)

Titre values used to calculate average volume of FA2 used are; (½marks)
and cm3

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Page 8 of 17
Extract From JUSAN Advanced Level Practical Manual

Therefore average volume of FA2 using phenolphthalein = cm3. (2½marks).

Table 2. (Methyl orange indicator)

TITRATION NUMBER I II III

Final burette reading (cm3)

Initial burette reading (cm3)

Volume of FA2 used (cm3)

(4½marks)

Titre values used to calculate average volume of FA2 used are; (½marks)
and cm3

Therefore average volume of FA2 using methyl orange = cm3. (2½marks)

(b) Write equation(s) that took place when using;

(iii)Phenolphthalein indicator. (2mark)
…………………………………………………………………………………………………………………

…………………………………………………………………………………………………………………

(iv) Methyl orange indicator. (1mark)

…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………

(c) Determine the volume of sulphuric acid required for complete neutralization of ,
(iii)Sodium carbonate. (1mark)
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
(iv) Sodium hydroxide. (1mark)

…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
(d) Calculate the concentration in grams per litre of.
(iii)Sodium carbonate in FA1. (5½marks)
…………………………………………………………………………………………………………………

…………………………………………………………………………………………………………………
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Page 9 of 17
Extract From JUSAN Advanced Level Practical Manual

…………………………………………………………………………………………………………………

(iv) Sodium hydroxide in FA1. (5marks)

ANALYSIS OF MIXTURE OF Na2CO3 AND NaHCO3 WHEN TITRATED WITH HCl

Neutralization of sodium carbonate Na2CO3 occurs in two steps as per the equations below.
Na2CO3 (aq) + HCl (aq) ⟶ NaHCO3 (aq) + NaCl (aq) ......................................... (i)
NaHCO3 (aq) + HCl(aq)⟶ NaCl(aq) + H2O(l) + CO2(g) .................................. (ii)
Neutralization of sodium hydrogen carbonate NaHCO 3 occurs in one step.
NaHCO3 (aq) + HCl (aq) ⟶ NaCl (aq) + H2O (l) + CO2 (g)........................................ (iii)

NOTE: The volume for reactions (ii) and (iii) may not necessarily be equal because the NaHCO 3
in equation (ii) is as a result of half neutralization of Na2CO3 in the mixture while the NaHCO3
in equation (iii) is actually the one originally dissolved in the mixture.

1. Stepwise/ discontinuous method, (using two indicators separately)

In this method, a fixed volume of the solution mixture containing sodium carbonate and
sodium hydrogen carbonate is pipetted in the conical flask, 2-3 drops of phenolphthalein
indicator are added, then titrated against the standard hydrochloric acid in the burette to the
endpoint. The volume Vp cm3 is recorded in the result table 1; and average volume of
standard acid used is calculated. The resultant solution in conical flask is poured away; and a
fresh fixed volume of the mixture/ aliquot is pipette into the conical flask, 2-3 drops methyl

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Page 10 of 17
Extract From JUSAN Advanced Level Practical Manual

orange indicator are added, then titrated against standard acid to the end point. The volume
Vm cm3 is recorded in the result table 2.
ANALYSIS OF VOLUMES FROM STEPWISE METHOD
The volume of HCl, Vp cm3 is for the reaction (i) only because phenolphthalein cannot detect
the end point for reactions (ii) and (iii).
Na2CO3( aq) + HCl(aq) ⟶ NaHCO3(aq) + NaCl(aq)..........................................(i)
The volume of HCl Vm cm3 is for all reactions (i), (ii) and (iii) since methyl orange can detect
both end-points
Na2CO3( aq) + HCl(aq) ⟶ NaHCO3(aq) + NaCl(aq)............................................(i)
NaHCO3(aq) + HCl(aq) ⟶ NaCl(aq) + H2O(l) + CO2(g).....................................(ii)
0riginalNaHCO3(aq) + HCl(aq) ⟶ NaCl(aq) + H2O(l) + CO2(g).........................(iii)

Therefore,
 the volume of HCl, Vp cm3 required to half neutralize Na 2CO3 to NaHCO3 in reaction (i) =
that neutralizing the resultant NaHCO3 in reaction (ii), hence volume for completely
neutralizing Na2CO3 in reaction (i) and (ii) = 2Vp cm3
 the volume of HCl required to completely neutralize original NaHCO 3 when using methyl
orange in reaction (iii) = (Vm – 2Vp) cm3 that is to say; volume for [(i)+(ii)+(iii)]-[(i)+(ii)]

1. TRIAL P525/1&2 ESSAY QUESTION

50.0cm3 of a solution containing sodium carbonate and sodium hydrogen carbonate was diluted
to 250cm3 with distilled water. 25cm3 of the diluted solution required 10.00cm3 of 0.2M sulphuric
acid using phenolphthalein indicator, another 25cm 3 of the diluted solution of the mixture
required 32.50cm3 of 0.2M sulphuric acid using methyl orange indicator.
(a) Write equation(s) that took place when using;
(i) Phenolphthalein indicator. (1mark)
(ii) Methyl orange indicator. (3mark)
(b) Determine the volume of sulphuric acid required for complete neutralization of ,
(i) Sodium carbonate. (1mark)
(ii) Sodium hydroxide. (1mark)
(c) Calculate in grams per litre.
(i) The concentration of sodium carbonate in the mixture. (5½marks)
(ii) The concentration of sodium hydroxide in the mixture. (5marks)

EXPERIMENT 2:
You are provided with the following
BA1 which is a solution mixture containing sodium carbonate and sodium hydrogen carbonate
solution.
BA2 which is 0.1M nitric acid.
Phenolphthalein and methyl orange indicator.
You are required to determine the concentration of Na2CO3 and NaHCO3 in the solution
mixture and hence the percentage of Na2CO3 in the mixture.
Procedure I
(i) Pipette 20 or 25cm3 of BA1 into a clean conical flask, add 2-3 drops of phenolphthalein
indicator and titrate with BA2 from the burette until the end point.
(ii) Repeat the titration until you obtain consistent results.
(iii) Record your result in the table 1 below.
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Extract From JUSAN Advanced Level Practical Manual

Results.
Volume of pipette used …………………………………………………………….. (½marks)

Table 1. With phenolphthalein indicator

EXPERIMENT I II III

Final burette reading (cm3)

Initial burette reading(cm3)
Volume of BA2 used (cm3)
(4½marks)

Titre values used to calculate average volume of BA2 used are; (½marks)

and cm3

Therefore average volume of BA2 using phenolphthalein = cm3. (2½marks)

Procedure II
(i) Pipette 20 or 25cm3 of BA1 into a clean conical flask. Add 2-3 drops of methyl orange
indicator and titrate with BA2 from the burette until the end point is reached.
(ii) Repeat the titration until you obtain consistent results.
(iii) Record your results in the table 2 below.

Volume of pipette used ……………………………………………………….……. (½marks)

Table 2. With methyl orange indicator.

EXPERIMENT I II III
Final burette reading (cm3)
Initial burette reading(cm3)

Volume of BA2 used (cm3)

(4½marks)

Titre values used to calculate average volume of BA2 used are; (½marks)

and cm3

Therefore average volume of BA2 using methyl orange = cm3. (2½marks)

(a) Write equation(s) that took place when using;

(i) Phenolphthalein indicator. (1mark)

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Extract From JUSAN Advanced Level Practical Manual

…………………………………………………………………………………………………………………
………………………………………………………………………………………………………………
(ii) Methyl orange indicator. (3mark)
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
(b) Determine the volume of nitric acid in BA2 required for the neutralization of;
(i) Sodium carbonate. (1mark)
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
(ii) Sodium hydrogen carbonate. (1mark)
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
(c) Calculate the concentration of sodium hydrogen carbonate in grams dm -3 in BA1
(5mark)
…………………………………………………………………………………………………………………

…………………………………………………………………………………………………………………

(d) Calculate the concentration of sodium carbonate in grams dm-3 in BA1. (5mark)
…………………………………………………………………………………………………………………

…………………………………………………………………………………………………………………

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Extract From JUSAN Advanced Level Practical Manual

…………………………………………………………………………………………………………………

(e) Determine percentage of sodium carbonate in the solution mixture. (1½mark)

…………………………………………………………………………………………………………………

2. Continuous titration; (using two indicators co-currently)

In this method, a fixed volume/ an aliquot of the mixture containing sodium carbonate and
sodium hydrogen carbonate is pipetted into a clean conical flask; 2-3 drops of phenolphthalein
indicator are added and then titrated against standard acid from the burette until the end-
point. The volume Vp cm3 required to reach endpoint is recorded in the result table 1.
Without pouring away the resultant solution in the conical flask, add 2-3 drops of methyl
orange indicator and continue titrating to obtain a second end point, the volume Vm cm3 is
recorded in the result table 2.

ANALYISIS OF VOLUMES FROM CONTINUOUS METHOD.

The volume of acid Vp cm3 will be for equation (i) only.
Na2CO3 (aq) + HCl (aq) ⟶ NaHCO3 (aq) + NaCl (aq).......................................... (i)
The volume Vm cm3 will be for equation (ii) and (iii) because its methyl orange that can detect
NaHCO3
NaHCO3 (aq) from (i) + HCl (aq) ⟶ NaCl (aq) + H2O (l) + CO2 (g)....................... (ii)
0riginalNaHCO3(aq) + HCl(aq) ⟶ NaCl(aq) + H2O(l) + CO2(g)......................(iii)

Therefore,
 The volume of acid Vp cm3 required to half neutralize Na2CO3 to NaHCO3 in reaction (i) =
volume required to neutralize the resultant NaHCO3 Na2CO3 to NaCl and CO2 in reaction
(ii), hence volume for complete neutralization of Na 2CO3 to NaCl and CO2 = 2Vp cm3. That
is to say, [volume (i) + volume (ii)].
 Since two reactions (i) and (ii) take place when using methyl orange, the first reaction (ii)
that completes the neutralization of the previously formed NaHCO3 required Vp cm3 of the
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Extract From JUSAN Advanced Level Practical Manual

acid hence, the volume required to completely neutralize the originally dissolved NaHCO 3 in
reaction (iii) = (Vm –Vp) cm3. That is to say, [volume (ii) + volume (iii)] – [volume (ii)]

EXPERIMENT 3:
You are provided with the following
BA1: solution of a mixture containing sodium carbonate and sodium hydrogen carbonate
BA2: 0.1M sulphuric acid solution
Phenolphthalein and methyl orange indicators
You are required to determine the concentration of Na2CO3 and NaHCO3 in the solution
mixture and hence the percentage of NaHCO3 in the mixture.
Procedure

(i) Pipette 20 cm3 of BA1 into a clean conical flask, add 3 drops of phenolphthalein indicator
and titrate with BA2 from the burette until the solution just turns colourless. Record your
result in the table 1 below.

(ii) Without pouring away the resultant colourless solution, add 3 drops of methyl orange
indicator and titrate until the solution just changes colour.
Record your result in table 2 below
(iii) Repeat the procedure to obtain consistent results

Results
Volume of pipette used …………………………….………………………..…cm 3. (½marks)
Table.
BURETTE READINGS Table 1 Table 2

With phenolphalein with methyl orange

Final burette reading (cm3)

Initial burette reading (cm3)

Volume of BA2 used (cm3)

(9marks)

Titre values used to calculate average volume of BA2 in table 1 used are; (½marks)

and cm3

Therefore average volume of BA2 using phenolphthalein = cm3. (2½marks)

Titre values used to calculate average volume of BA2 in table 2 used are; (½marks)

and cm3

Therefore average volume of BA2 using methyl orange = cm3. (2½marks)

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Extract From JUSAN Advanced Level Practical Manual

(a) Write equation(s) that took place when using;

(i) Phenolphthalein indicator. (1mark)
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
(ii) Methyl orange indicator. (2mark)
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
(b) Determine the volume of sulphuric acid in BA2 required for the neutralization of;
(iii) Sodium carbonate. (1mark)
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
(iv) Sodium hydrogen carbonate. (1mark)
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
(c) Calculate the concentration of sodium hydrogen carbonate in grams dm-3 in BA1.
(5mark)
…………………………………………………………………………………………………………………

…………………………………………………………………………………………………………………

(d) Calculate the concentration of sodium carbonate in grams dm-3 in BA1. (5mark)

…………………………………………………………………………………………………………………

…………………………………………………………………………………………………………………
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Extract From JUSAN Advanced Level Practical Manual

…………………………………………………………………………………………………………………

(e) Determine the percentage of sodium carbonate in the solution mixture. (1½mark)

…………………………………………………………………………………………………………………

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Page 17 of 17
Extract from JUSAN advanced level chemistry Manual

ACID-BASE TITRATION TECHNIQUES

There are several techniques in titration but the most important at this level are,
 Back titration
 Double indicator

 BACK TITRATION TECHNIQUE.

In this technique, the concentration of an analyte is determined by reacting it with a
known amount of excess reagent A. The remaining excess reagent A is then titrated with
another second reagent B. The titration results show how much of the excess standard reagent
A was used in the first titration and the original titrand’s / analyte’s concentration can then be
calculated. Back titration also useful if the reaction between the analyte and titrant is very slow
or when the analyte is an insoluble solid.
 Analyte + A (excess) ⟶ Product + unreacted of A
 Product + unreacted A + B (second reagent) ⟶ Products
Solutions A and B are standard solutions.

Note:
1. Calculations involve starting with the number of moles of the reactants used in the final
stages of the experiment followed by those of the reactants at the beginning of the
experiment.
2. During back titration, dilution is always done which simply means increasing the volume of
the solvent to the solution. It should be noted that dilution only changes the concentration of
the solution but not the number of moles of the compound in solution. Dilution is inversely
proportional to concentration.

Applications of back titration.

 Determination of relative atomic mass element in its carbonate. (JJEB P525/3:
2019)
 Analysis of ammonium salts. (UNEB: 2003 P525/2 No. 8) (JJEB P525/3: 2018)
 Determining percentage purity and impurity of;
(i) Samples such as chalk powder, limestone, egg shells containing calcium carbonate),
washing soda containing sodium carbonate among others.
(ii) Electropositive metals based on reaction with solution of suitable standard acid used in
excess.
(iii) Ores such as pyrulosite (manganese(IV), MnO 2) in redox titrations. See redox
titrations.
 Determining concentrations of oxalates, iodides, chromates etc. in redox reactions as
discussed in sub topic 7.

NOTE:
𝐦𝐚𝐬𝐬 𝐭𝐡𝐚𝐭 𝐫𝐞𝐚𝐜𝐭𝐬 (𝐩𝐮𝐫𝐞 𝐦𝐚𝐬𝐬 𝐨𝐫 𝐜𝐚𝐥𝐜𝐮𝐥𝐚𝐭𝐞𝐝 𝐦𝐚𝐬𝐬)
Percentage purity = x 100 %
𝐦𝐚𝐬𝐬 𝐨𝐟 𝐨𝐫𝐢𝐠𝐢𝐧𝐚𝐥 𝐬𝐚𝐦𝐩𝐥𝐞
𝐮𝐧𝐫𝐞𝐚𝐜𝐭𝐞𝐝 𝐦𝐚𝐬𝐬 (𝐨𝐫𝐢𝐠𝐢𝐧𝐚𝐥 𝐦𝐚𝐬𝐬−𝐦𝐚𝐬𝐬 𝐭𝐡𝐚𝐭 𝐫𝐞𝐚𝐜𝐭𝐬)
Percentage impurity = x 100 %
𝐨𝐫𝐢𝐠𝐢𝐧𝐚𝐥 𝐦𝐚𝐬𝐬 𝐨𝐟 𝐬𝐬𝐦𝐩𝐥𝐞
Or, percentage impurity = (100 – percentage purity) %

SAMPLE P525/1&2 STRUCTURED QUESTION ON BACK TITRATION.

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1. A sample containing ammonium chloride was warmed with 100cm 3 of 1.0moldm-3 of sodium
hydroxide solution. After all the ammonia had been driven off, the excess of sodium hydroxide
was titrated with 50.0cm3 of 0.25moldm-3 of sulphuric acid using phenolphthalein indicator.
What mass of ammonium chloride did the sample contain? (7marks)
Solution.
Initial moles of NaOH.
1000cm3 of solution contain 1.0moles of NaOH
moles of NaOH✓
𝟏.𝟎 ×𝟏𝟎𝟎
100cm3 of solution contain
𝟏𝟎𝟎𝟎
= 0.1 moles of NaOH✓
Moles of H2SO4 that neutralized the excess NaOH
1000cm3 of solution contain 0.25moles of H2SO4
𝟎.𝟐𝟓 ×𝟓𝟎
50.0cm3 of solution contain moles of H2SO4✓
𝟏𝟎𝟎𝟎
= 0.0125 moles of H2SO4✓
Moles of excess/ residual NaOH that reacted with the H2SO4.
From the reaction equation,
2NaOH (aq) + H2SO4 (aq) ⟶ Na2SO4 (aq) + H2O (l) ✓✓

2 moles of NaOH reacted with 1 moles of H2SO4

Therefore moles of excess NaOH = (2 x 0.0125) ✓
= 0.025. ✓
Moles of NaOH that reacted with NH 4Cl in the sample.
 (Initial moles – excess moles) = 0.075 moles. ✓
Moles of NH4Cl in the sample that reacted with NaOH.
From the reaction equation,
NH4Cl (aq) + NaOH (aq) ⟶ NaCl (aq) + NH3 (g) + H2O (l) + excess alkali. ✓
1mole of NH4Cl in the sample reacted with 1 mole of NaOH
Therefore moles of NH4Cl in the sample = 0.075. ✓
Mass of NH4Cl contained in the sample.
From molar mass of NH4Cl = (14x1) + (4x1) + (35.5x1) = 53.5gmol-1✓
1 mole of NH4Cl in the sample contains 53.5g
0.075 moles of NH4Cl in the sample contains (53.5x0.075) g✓
= 4.012g✓

TRIAL P525/1&2 STRUCTURED QUESTION ON BACK TITRATION.

2. A 0.50g sample of fertilizer contains ammonium sulphate was warmed with sodium
hydroxide solution, and the ammonia evolved was absorbed in 100cm 3 of 0.1moldm-3
hydrochloric acid. The excess hydrochloric acid required 55.9cm 3 of 0.1M sodium
hydroxide for complete neutralization. Calculate the percentage of ammonium sulphate in
the sample. (5marks)

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Extract from JUSAN advanced level chemistry Manual

3. 1.07g of a nitrogen compound was boiled with excess sodium hydroxide solution to produce
ammonia. The ammonia produced neutralized 200cm 3 of a 0.1M monobasic acid. Calculate
the percentage by mass of nitrogen in the compound. (3marks)
4. Manganese(IV) oxide occurs in pyrulosite, 2.5g of pyrulosite ore was boiled with excess
concentrated hydrochloric acid. The chlorine liberated was bubbled through excess
potassium iodide solution. The iodine liberated required 35.5cm 3 of 0.2M solution sodium
thiosulphate solution.
(a) Write equation(s) for the redox reactions that took place. (3marks)
(b) Calculate the percentage by mass of manganese(IV) oxide in the ore. (5marks)

EXPERIMENT 1:
Determination of the values of M in an insoluble carbonate MCO3 by titration.
You are provided with the following solutions
FA1 which is solution of 1M monobasic acid HA.
FA2 is 0.1M Sodium hydroxide solution
1.3g of insoluble carbonate MCO3.
Theory:
The insoluble metal carbonate reacts with excess acid added according to the equation below.
MCO3(s) + 2HA(aq) MA2(aq) + CO2(g) + H2O(l)
When the reaction above is complete, the excess acid HA left is then reacted with sodium
hydroxide solution as in equation below.
HA(aq) + NaOH(aq) NaA(aq) + H 2O(l)
Procedure
Weigh 1.0g of the metal carbonate MCO3 and place it in a beaker.
Add about 20cm3 of water followed by 40cm3 of FA1.
After effervescence is complete, transfer the resultant solution into a 250cm 3 volumetric flask
and add water up to the mark.
Pipette 20 or 25cm3 of this solution mixture and titrate with FA2 using methyl orange
indicator.
Repeat the titration to obtain consistent results.
Record the results in the table below.

Results
Mass of weighing bottle + metal carbonate =……………………………………g
Mass of weighing bottle =…………………………………….g
Mass of metal carbonate =…………………………………….g
Volume of pipette =………………………………………………………………….cm3

Titration number 1 2 3
Final burette reading (cm3)

Initial burette reading (cm3)

Volume of FA2 used (cm3)

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Page 3 of 12
Extract from JUSAN advanced level chemistry Manual

Titre values of FA2 used to calculate the average volume.

……………………………………………………………………………………………………………………
Average volume of FA2 used
……………………………………………………………………………………………………………………
.........................................................................................................................................

(a) Calculate the number of moles of excess acid HA

(ii) Number of moles of acid HA that reacted with the metal carbonate MCO3.

(c) Calculate the value of M in MCO3.

EXPERIMENT 2:
You are provided with the following
Solid M which is mixture of ammonium chloride and sodium chloride
FA1 which is a 0.2M sulphuric acid solution.
FA2 which is a solution of sodium hydroxide of unknown concentration.
FA3 which is a 0.05M hydrochloric acid solution
You are required to determine,

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Page 4 of 12
Extract from JUSAN advanced level chemistry Manual

(i) Standardize FA2 using the standard solution of FA1.

(ii) Concentration of sodium chloride.
(iii) Percentage composition by mass of sodium chloride in the mixture.
Part I
Procedure
Pipette 25cm3 of FA2 into a clean conical flask. Add 2-3 to three drops of phenolphalein indicator.
Titrate it against FA1 until the endpoint. Repeat the titration to obtain consistent results. Record
your results in the table below
Results
Volume of pipette used cm3 (½marks)
Table I
EXPERIMENT I II III

Final burette reading (cm3 )

Initial burette reading (cm3)

Volume of FA1 (cm3)

(4½marks)

Titre values used to calculate average volume of FA1 used are; (½marks)
and cm3

Therefore average volume of FA1 = cm3. (2½marks)

(a) Calculate the concentration sodium hydroxide in FA2 in moles per litre. (5½marks)
……………………………………………………………………………………………………………………
……………………………………………………………………………………………………………………
……………………………………………………………………………………………………………………
……………………………………………………………………………………………………………………
……………………………………………………………………………………………………………………
……………………………………………………………………………………………………………………
……………………………………………………………………………………………………………………
……………………………………………………………………………………………………………………
……………………………………………………………………………………………………………………

PART II:
Procedure II.
Weigh 1.2g of the solid mixture M, and transfer the sample into a clean conical flask. To weighed
sample in the conical flask, add 100cm3 of FA2 and boil for 5 minutes until no more ammonia is
driven off. Add distilled water to make up the residual volume to 250cm 3. Label it HA1.
Theory:
 The ammonium chloride in the mixture reacts with sodium hydroxide in FA2 according to the
equation. After the ammonia has been drive off, there remains excess/ residual sodium
hydroxide in the solution,

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Page 5 of 12
Extract from JUSAN advanced level chemistry Manual

NH4Cl (aq) + NaOH (aq) ⟶ NH3 (g) + H2O (l) + NaCl (aq)
 The sodium chloride in the mixture does not react with sodium hydroxide.
Pipette 20 or 25cm3 of HA1 (diluted residual sodium hydroxide solution), into a clean conical
flask. Add 2-3 drops of phenolphthalein indicator. And then titrate with FA3 in the burette until
the endpoint is reached. Repeat the titration to obtain consistent results. Record your results in
the table II below
Results.
Volume of pipette used cm3 (½marks)
Table II
EXPERIMENT I II III

Final burette reading (cm3)

Initial burette reading (cm3)

Volume of FA3 (cm3)

(4½marks)

Titre values used to calculate average volume of Fused are; (½marks)

and cm3

Therefore average volume of FA3 = cm3. (2½marks)

(b) Calculate the;

(i) Number of moles of sodium hydroxide in solution HA1. (3½marks)
………………………………………………………………………………………………………………………
………………………………………………………………………………………………………………………
………………………………………………………………………………………………………………………
………………………………………………………………………………………………………………………
………………………………………………………………………………………………………………………
………………………………………………………………………………………………………………………
………………………………………………………………………………………………………………………
(ii)Number moles of sodium hydroxide that reacted with ammonium chloride in the solid
mixture, M. (2½marks)
………………………………………………………………………………………………………………………
………………………………………………………………………………………………………………………
………………………………………………………………………………………………………………………
………………………………………………………………………………………………………………………

(iii) Percentage composition by mass sodium chloride in the solid mixture M. (4½marks)
………………………………………………………………………………………………………………………
………………………………………………………………………………………………………………………

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Page 6 of 12
Extract from JUSAN advanced level chemistry Manual

Procedure.
(i) Weigh accurately 1.5g of solid M into a clean conical flask.
(ii) Add 50cm3 of distilled water using a measuring cylinder and stir to form a paste; followed
by 50cm3 of HRA continue to stir until effervescence stops, shake the mixture until the
effervescence is over.
(iii) Transfer the contents to a 250cm3 volumetric flask; add distilled water to make the solution
to the 250cm3 mark. Label the solution HRC.
(iv) Pipette 20 or 25cm3 of HRB into a conical flask, add 2-3 drops of methyl orange indicator,
and titrate with solution HRC from the burette until the solution just changes colour.
Record the value in the table below.
(v) Repeat the titration to obtain consistent results.
Results.
Mass of container + M = g (½marks)

Mass of container alone = g (½marks)

Mass of M alone = g (½marks)

Volume of pipette used cm3 (½marks)

Table
EXPERIMENT I II II

Final burette reading (cm3)

Initial burette reading (cm3)

Volume of HRC used (cm3)

(4½marks)

Titre values used to calculate average volume of HRC used are; (½marks)
and cm3

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Page 7 of 12
Extract from JUSAN advanced level chemistry Manual

Therefore average volume of HRC = cm3 (2½marks)

(a) Calculate the:

(i) Number of moles of sodium hydroxide in HRB that reacted with hydrochloric acid in HRC.
(1marks)
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
(ii) Number of moles of excess hydrochloric acid in HRC that reacted with sodium hydroxide
in HRB. (1½marks)
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………

(iii) Number of moles of excess hydrochloric acid in 250cm 3 of HRC. (1marks)

…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
(iv) Number of moles of hydrochloric acid that reacted with calcium carbonate in chalk
powder. (2marks)
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………
…………………………………………………………………………………………………………………

(b) Determine the percentage;

(i) The percentage purity of calcium carbonate in chalk powder. (4marks)
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………

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Page 8 of 12
Extract from JUSAN advanced level chemistry Manual

……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
(ii) Impurity in chalk powder. (1marks)
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………

EXPERIMENT 4: (JJEB 2018)

You are provided with the following
GA1 which is a sodium hydroxide solution of unknown concentration
Solid W which is ethanedioic acid (oxalic acid crystals), H2C2O4, a dibasic acid.
Solid X which is impure ammonium chloride fertilizer.
Phenolphthalein indicator
You are required to standardize GA1 using ethanedioic acid and then use GA1 to
determine the percentage of ammonium chloride in the fertilizer.
You are required to determine the percentage purity of calcium carbonate in chalk
powder.
PROCEDURE I.

(a) Weigh accurately 1.5g to 1.6g of solid W into a clean beaker.

(b) Add a minimum of distilled water solution and stir well to dissolve. Transfer into a 250cm3
volumetric flask and make up to the mark with distilled water (solution GA2). Transfer GA2
into a clean beaker and wash the volumetric flask thoroughly for preparation of GA3.
(c) Run from burette exactly 23.5cm3 of GA1 into the 250cm3 volumetric flask. Add distilled
water to make up to the mark (solution GA3).
(d) Pipette 20.0 0r 25.0cm3 of GA3 into a clean conical flask. Add 2-3 drops of phenolphthalein
indicator and titrate with GA2 from the burette.
(e) Repeat the titration to obtain consistent results.
Results.

Mass of container + W = g (½marks)

Mass of container alone = g (½marks)

Mass of W alone = g (½marks)

Volume of pipette used cm3 (½marks)

Table 1.
Titration number I II II

Final burette reading (cm3)

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Initial burette reading (cm3)

Volume of GA2 used (cm3)

(4½marks)

Titre values used to calculate average volume of GA2 used are; (½marks)
and cm3

Therefore average volume of GA2 = cm3 (2½marks)

(a) Calculations:
(i) Determine the molar concentration (moldm-3) of GA2. (3marks)
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
(ii) Write an equation for the reaction between Ethanedioic acid (oxalic acid) and
sodium hydroxide solution. (1½marks)
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
(iii) Determine the molar concentration of GA3. (3marks)
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
(iv) Calculate the molar concentration of GA1. (2marks)
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………

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………………………………………………………………………………………………………
………………………………………………………………………………………………………
……………………………………………………………………………………………………….
PROCEDURE II:
(a) Excess of sodium hydroxide is reacted with the fertilizer X and the unreacted alkali
determined using GA2. Ammonia gas is given out in the course of heating the salt with alkali.
NH4+ (aq) + OH- (aq) ⟶ NH3 (g) + H2O (l)
(b) Weigh 2g of the fertilizer X into a conical flask. Using a measuring cylinder, add 50cm 3 of
GA1 into the flask. Transfer to a tripod and wire gauze and heat the mixture. Occasionally
add water to the flask to make up the loss due to evaporation. Continue heating until no
more recognizable smell of ammonia. Cool the mixture and transfer entirely to a 250cm3
volumetric flask. Make up to the mark using distilled water (solution GA4).
(c) Pipette 10cm3 of GA4 into a clean conical flask. Add phenolphthalein indicator and titrate
with GA2 from the burette.
(d) Repeat the procedures above to obtain consistent results.
Results.

Mass of container + X = g (½marks)

Mass of container alone = g (½marks)
Mass of X alone = g (½marks)
Volume of pipette used cm3 (½marks)
Table 2.
Titration number I II II

Final burette reading (cm3)

Initial burette reading (cm3)

Volume of GA2 used (cm3)

(4½marks)

Titre values used to calculate average volume of GA2 used are; (½marks)

and cm3

Therefore average volume of GA2 = cm3 (2½marks)

(b) Calculate
(i) Determine the concentration of GA4. (2½marks)
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………

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……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
(ii) Hence determine the moles of unreacted sodium hydroxide in GA4. (2½marks)
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
…………………………………………………………………………………………………………….
(iii) Calculate the moles of sodium hydroxide that reacted with X. (2½marks)
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
(iv) Calculate the moles of ammonium chloride that reacted. Hence determine the
percentage of ammonium chloride in the fertilizer. (2½marks)
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
……………………………………………………………………………………………………………
…………………………………………………………………………………………………………..

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CHAPTER 6: REDOX TITRATIONS WITH SODIUM THIOSULPHATE.

Most of the thiosulphate titrations involve use of standard iodine solution or iodine liberated from
a given chemical reaction. The titration is thus called iodimetry or iodometry.
Theory of reaction between Iodine solution and Sodium thiosulphate
Iodine is an oxidizing agent while the thiosulphate is a reducing agent. The thiosulphate is oxidized
to tetrathionate ions as in equation below.
2S2O32- (aq) ⟶S4O62- (aq) + 2e-………………………….. Equation. (i)
Iodine on the other hand is reduced to Iodine ions as in equation below.
I2 (aq) + 2e- ⟶ 2I- (aq)……………………………………. Equation (ii)
Adding equation (i) and (ii), the overall equation obtained is
2S2O32-(aq) + I2 (aq) ⟶ S4O62- (aq) + 2I- (aq)

(a) IODIMETRIC TITRATIONS:

These involve direct use an excess of standard solution of iodine in volumetric analysis. The
iodine solution acts as an oxidizing agent in iodimetry.
Question.
(a) Give two advantages of using iodine as a primary standard in volumetric analysis.
Iodine is obtained in a high state of purity. ✓
Iodine can be accurately used in making standard solutions. ✓
(b) Explain why iodine is not a good primary standard?
Iodine is highly volatile ✓ and this varies its concentration on standing, ✓ hence not
recommended for a primary standard.
Iodine has poor solubility in water. ✓
Question.
Iodine is dissolved in potassium iodide solution rather than water during iodimetry. Explain.
Iodine has a low water solubility ✓ but dissolves in moderately concentrated potassium
iodide solution due to the formation of a soluble triiodide ion complex, I3-(aq) ✓
Equation; I2 (aq) + I- (aq) ⇌ I3- (aq) ✓
Equilibrium attained between iodine and triiodide ions ensures that even when iodine
molecules are removed from the solution by a reaction, the triiodide ion readily
dissociate in solution ✓ and liberating more iodine molecules, ✓ so the dissolved iodine
behaves as if they are all free iodine. An explanation of Le Chatelier’s principle.

NOTE:
1. Iodine is standardized by titration with standard sodium thiosulphate solution.

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2. The thiosulphate is not a primary standard and is standardized by potassium permanganate

solution or potassium iodate or potassium dichromate.
3. Hydrochloric acid and nitric acid are not used to standardize sodium thiosulphate.
4. Acidified potassium dichromate is commonly associated with thiosulphate titrations.

Question.
Explain why,
(a) Sodium thiosulphate-5-water is not a good primary standard. (3marks)
Sodium thiosulphate-5-water contains water of crystallization✓ making its exact
concentration difficult to determine. ✓ This is because the composition depends on humidity
and temperature, that is to say, loses water of crystallization at high temperatures✓ and
absorbs water at high humidity✓ . Consequently affecting it absolute relative molecular
mass✓ and hence varying its concentration. ✓
(b) Titrations involving sodium thiosulphate should not be carried out in acid conditions.
(3½marks)
In acidic medium, hydrogen ions in solution easily react with the thiosulphate ions✓
depositing yellow precipitate of elemental sulphur, ✓ with bubbles of sulphur dioxide gas
and formation of water✓; depleting thiosulphate ions from solution✓.
Equations; S2O32- (aq) + 2H+ (aq) ⟶ S (s) + SO2 (g) + H2O (l) ✓ = 1½marks

(c) Sodium bicarbonate is added to analyte solution during iodimetry of sulphite ions with
standard thiosulphate solution. (7½marks)
During iodimetry; sulphite ions are oxidised sulphite ions with formation of hydrogen ions
in solution resulting to an acid medium. ✓
Equation, SO32- (aq) + H2O (l) + I2 (aq) ⟶ SO42- (aq) + 2I- (aq) + 2H+ (aq). ✓= 1½marks
Sodium bicarbonate added to quickly react with the hydrogen ions forming bubbles of a
colourless gas and water✓.
Equation;
HCO3- (aq) + H+ (aq) ⟶ CO2 (g) + H2O (l). ✓ = 1marks
This protects the thiosulphate ions from reacting with the hydrogen ions to deposit a yellow
solid of sulphur, sulphur dioxide and water✓, hence keeping them available to react with the
excess iodine in solution. ✓
Equation(s).
S2O32-(aq) + 2H+ (aq) ⟶ S(s) + SO2 (g) + H2O (l) ✓ = 1½marks
2S2O32-(aq) + I2 (aq) ⟶ S4O62- (aq) + 2I (aq) ✓
-
= 1½marks

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(d) Sodium thiosulphate solution becomes cloudy with formation of a yellow precipitate on
standing in air. (4marks)
When left exposed to air, sodium thiosulphate solution readily absorbs carbon dioxide from air this
forming weak carbonic acid. ✓ Carbonic acid formed, ionizes in producing hydrogen ions that
decompose the thiosulphate ions to deposit elemental sulphur, sulphur dioxide and water✓
which initially appears as a cloudy solution✓ but later settles as a yellow solid✓.
S2O32-(aq) + 2H+ (aq) ⟶ S(s) + SO2 (g) + H2O (l) ✓
Sodium thiosulphate solution absorbs atmospheric oxygen from air; ✓ hence easily oxidized
to sulphate. ✓
Atmospheric sulphur requiring bacteria may attack sodium thiosulphate solution causing
decomposition. ✓

(b) IODOMETRIC TITRATIONS:

These involve titration of standard solution of thiosulphate ions with iodine liberated from an
iodo-compound in given chemical reaction. (Iodo-compounds; containing excess iodide ions
for example, potassium iodide solution is usually used).
 Liberation of iodine in iodometry.
A known amount of suitable oxidizing agent in acid medium, reacted with excess potassium
solution. The iodide ions are reducing agents and they are therefore, oxidised to form aqueous
iodine (oxidant) which can then be titrated with a standard solution of the thiosulphate ions from
the burette.
 Common reactions that liberate aqueous iodine include;
(i) IO3- (aq) + 5I- (aq) + 6H+ (aq) ⟶ 3I2 (aq) + 3H2O (l)
(ii) ClO3- (aq) + 6I- (aq) + 6H+ (aq) ⟶ 3I2 (aq) + Cl- (aq) + 3H2O (l)
(iii) OCl- (aq) + 2I- (aq) + 2H+ (aq) ⟶ I2 (aq) + Cl- (aq) + 2H2O (l)
(iv) 2MnO4- (aq) + 10I- (aq) + 16H+ (aq) ⟶ 3I2 (aq) + 2Mn2+ (aq) + 8H2O (l)
(v) Cr2O72- (aq) + 6I- (aq) + 14H+ (aq) ⟶ 3I2 (aq) + 2Cr3+ (aq) + 7H2O (l)
(vi) H2O2 (aq) + 2I- (aq) + 2H+ (aq) ⟶ I2 (aq) + 2H2O (l)
(vii) 2Cu2+ (aq) + 4I- (aq) ⟶ I2 (aq) + Cu2I2 (s)
(viii) Cl2 (aq) + 2I- (aq) ⟶ I2 (aq) + 2Cl- (aq)

Detection of end point

The end point of all titrations involving thiosulphate ions and iodine is detected by the use of starch
solution as indicator.
Starch solution is added towards the end point and in the presence of free iodine. It produces a
deep blue solution. This blue colour is discharged as soon sufficient sodium thiosulphate is added
giving a colourless solution which serves as the end point.

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General procedure
Sodium thiosulphate solution in the burette is run into iodine solution in the conical flask until the
brown colour of solution turns pale yellow. At this point, about 3cm3 of starch is added producing
a blue coloured solution. Then the thiosulphate solution is then added drop by drop until the blue
solution just turns colourless at end point.
Question.
1.Why is starch indicator added close to the end point rather than at the beginning of the
experiment?
Adding starch close to the end point gives a sharp endpoint detection, while avoiding the
formation of excess starch iodine complex which would difficult to decompose
2.Why should the starch solution used in iodometry be freshly prepared?
Starch solution deteriorates quickly on standing.

SAMPLE P525/1&2 CALCULATION QUESTIONS ON IODOMETRY

1. 10.0cm3 of a sample of commercial bleach containing chlorine was diluted to 250cm 3 with
water. 25.0cm3 of this solution was transferred into a clean conical flask and potassium iodide
solution was added to liberate iodine. The iodine mixture required 23.2cm3 of a 0.1M sodium
thiosulphate solution for complete neutralization. Calculate the molar concentration of chlorine
in the commercial bleach. (UNEB 2015 P2 No.5). (3marks)
Solution.
Moles of sodium thiosulphate
1000cm3 of solution contain 0.1moles of sodium thiosulphate.
0.1𝑥23.2
23.5cm3 of solution contain ✓ = 0.00232molesof sodium thiosulphate. ✓
1000
Moles of liberated iodine.
From equation, 2S2O32-(aq) + I2 (aq) ⟶ S4O62- (aq) + 2I- (aq)
2moles of sodium thiosulphate reacted with 1mole of liberated iodine
0.00232𝑥1
0.00232moles of sodium thiosulphate reacted with ✓= 0.00116moles of iodine. ✓
2
Moles of chlorine in the bleach.
From equation, Cl2 (aq) + 2I- (aq) ⟶ I2 (aq) + 2Cl- (aq)
Or; OCl- (aq) + Cl- (aq) + 2H+ (aq) + 2I- (aq) ⟶ I2 (aq) + 2Cl- (aq) + H2O (l)
1mole of iodine was liberated by 1mole of chlorine in commercial bleach
0.00116molles of iodine were therefore liberated by 0.00116moles of chlorine in bleach. ✓
Molar concentration of chlorine in the commercial bleach.
25.0cm3 of solution contain 0.00116moles of chlorine.
0.00116 𝑥 1000
1000cm3 of solution contains 25.0
✓= 0.0454M Cl2 in commercial bleach. ✓

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TRIAL P525/1&2 QUESTIONS ON IODOMETRY

Answer in your revision book for submission.
2. 2.835g of iodine and 6g of potassium iodide are dissolved in distilled water and made up to
250cm3. A 25.0cm3 portion titrated against sodium thiosulphate solution required 17.5cm3 of
the solution. Calculate the concentration of the thiosulphate solution.
3. 1.015g of potassium iodate(V) are dissolved and made up to 250cm3. To a 25.0cm3 portion are
added an excess of potassium iodide and dilute sulphuric acid. The solution is titrated with a
solution of sodium thiosulphate, starch solution is being added near the end point. 29.8cm3 of
thiosulphate were required. Calculate the concentration of the thiosulphate solution.
4. A standard solution is made by dissolving 1.015g of potassium dichromate(VI) and making up
to 250cm3. A 25.0cm3 portion is added to excess potassium iodide and dilute sulphuric acid,
and the iodine liberated is titrated with sodium thiosulphate solution. 19.2cm3 of this solution
are needed. Find the concentration of the thiosulphate solution.
5. A domestic bleach in solution is diluted by pipetting 10.0cm3 and making this volume up to
250cm3. A 25cm3 portion of the solution is added to an excess of potassium iodide and ethanoic
acid and titrated against sodium thiosulphate solution of concentration 0.1moldm-3, using
starch indicator. The volume required is 21.3cm3. Calculate the percentage of available
chlorine in the bleach.

P525/3 QUESTIONS ON IODOMETRY

EXPERIMENT 15: UNEB 2018
You are provided with the following;
FA1 which is approximately 0.1M sodium thiosulphate solution.
FA2 which is a solution containing 2.5gdm-3 of potassium iodate.
Solid Y, which is a salt containing dichromate ions.
1M sulphuric acid solution.
5% potassium iodide solution.
Starch solution.
You are required to standardize FA1 and use it to determine the percentage by mass of Y.
In acid solution, iodate and dichromate ions (VI) ions react with potassium iodide to liberate iodine
according to the following equations.
IO3- (aq) + 5I- (aq) + 6H+ (aq) ⟶ 3I2 (aq) + 3H2O (l)
Cr2O72- (aq) + 6I- (aq) + 14H+ (aq) ⟶ 3I2 (aq) + 2Cr3+ (aq) + 7H2O (l)
The liberated iodine in both cases reacts with thiosulphate ions according to the equation.
2S2O32-(aq) + I2 (aq) ⟶ S4O62- (aq) + 2I- (aq)
PART 1
PROCEDURE:

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(a) Pipette 25.0 (or 20.0) cm of FA2 into a clean conical flask and add an equal volume of
0.1M sulphuric acid using a measuring cylinder, followed by 10cm3 of 5% potassium
iodide solution.
(b) Titrate the iodine liberated FA1, using starch indicator.
(c) Repeat the titration until you obtain consistent results.
(d) Record your results in the Table I below.
Results
Volume of pipette used cm3 (½marks)
Table I
BURETTE READINGS I II II
Final burette reading (cm3)
Initial burette reading (cm3)
Volume of FA1 used (cm3)
(4½marks)
Titre values used to calculate average volume of FA1 used are; (½marks)
3
and cm

Therefore average volume of FA1 used= cm3. (2½marks)

………………………………………………………………………………………………………
………………………………………………………………………………………………………
(a) Calculate the number of moles of iodine liberated by FA2. (2½ marks)
………………………………………………………………………………………………………
………………………………………………………………………………………………………
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………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
(b) Determine the concentration of FA1 in moldm-3 (2marks)
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
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PART 2
PROCEDURE:
(a) Weigh accurately about 1.2g of Y. dissolve it in minimum amount of distilled water and
transfer the solution into 250cm3 volumetric flask. Make the solution up to the mark with
distilled water and label it FA3.
(b) Pipette 25.0 (or 20.0) cm3 of FA3 into a clean conical flask and add an equal volume of
1M sulphuric acid using a measuring cylinder, followed by 10cm3 of 5% potassium iodide
solution. Titrate the iodine liberated with FA1 using starch indicator.
(c) Repeat the titration until you obtain consistent results.
(d) Record your results in the Table II below.
Results
Mass of weighing bottle + Y = g (½marks)
Mass of empty weighing bottle = g (½marks)
Mass of Y used = g (½marks)
Volume of pipette used cm3 (½marks)
Table II
BURETTE READINGS I II II
Final burette reading (cm3)
Initial burette reading (cm3)
Volume of FA1 used (cm3)
(4½marks)
Titre values used to calculate average volume of FA1 used are; (½marks)
3
and cm

Therefore average volume of FA1 used= cm3. (2½marks)

………………………………………………………………………………………………………
………………………………………………………………………………………………………
(a) Calculate the number of moles iodine liberated by FA3. (2marks)
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
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(b) Determine the :

(i) Concentration of FA3 in moldm-3. (2½marks)
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
(ii) Mass of chromium in Y and hence its percentage. (Cr = 52). (3½marks)
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
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………………………………………………………………………………………………………
………………………………………………………………………………………………………

EXPERIMENT 16: (ENTEBBE MOCK 2019)

You are provided with the following:
FA1; which is approximately 0.1 M sodium thiosulphate solution
FA2; which is a solution prepared by dissolving 1.0 g of potassium iodate(V) in 250 cm3 of distilled
water
Liquid X, which is a commercial bleaching agent containing sodium hypochlorite (sodium
chlorate(I))
You are required to standardize FA1 and use it to determine the percentage of chlorine in the
commercial bleaching agent.
Theory
In acid medium, iodate(V) ions react with iodide ions according to the following equation:
IO3- (aq) + 6H+ (aq) + 5 I– (aq) ⟶ 3 I2 (aq) + 3H2O (l)
In acid medium, hypochlorite ions react to produce chlorine which displaces iodine according to
the following equations:
OCl— (aq) + 2 H+ (aq) + 2 Cl— (aq) ⟶ Cl2 (aq) + H2O (l)
Cl2 (aq) + 2 I—(aq) ⟶ I2 (aq) + 2 Cl—(aq)
The liberated iodine reacts with thiosulphate ions according to the fooling equation:
2S2O32-(aq) + I2 (aq) ⟶ S4O62- (aq) + 2I- (aq)
Procedure A
(a) Pipette 10.0 cm3 of FA2 into a conical flask and add an equal volume of 1.0 M sulphuric acid
using a measuring cylinder followed by 10.0 cm3 of 0.5 M potassium iodide solution. Titrate
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the liberated iodine with FA1 from the burette until the mixture is pale yellow. Add 2 cm3 of
starch indicator and continue the titration until end point. Repeat the titration until you obtain
consistent results.
Record your observations in Table I below.
Results
Volume of pipette used cm3 (½marks)
Table I
BURETTE READINGS I II II
Final burette reading (cm3)
Initial burette reading (cm3)
Volume of FA1 used (cm3)
(4½marks)
Titre values used to calculate average volume of FA1 used are; (½marks)
3
and cm

Therefore average volume of FA1 used= cm3. (2½marks)

………………………………………………………………………………………………………
………………………………………………………………………………………………………
Questions:
(a) Calculate the concentration of FA1 in moldm-3. (6marks)
Procedure B
(a) Transfer 30.0 cm3 of liquid X into 250 cm3 volumetric flask. Add distilled water up to the
mark. Label the solution FA3.
Pipette 10.0 cm3 of FA3 into a conical flask and add an equal volume of 1.0 M sulphuric acid
using a measuring cylinder followed by 10 cm3 of 0.5 M potassium iodide solution. Titrate the
liberated iodine with FA1 from the burette until the mixture is pale yellow. Add starch indicator
and continue the titration until the end point. Repeat the titration to obtain consistent results.
Record your results in table II below.
Results
Volume of pipette used cm3 (½marks)
Table I
BURETTE READINGS I II II
Final burette reading (cm3)
Initial burette reading (cm3)

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Volume of FA1 used (cm3)

(4½marks)
Titre values used to calculate average volume of FA1 used are; (½marks)
3
and cm

Therefore average volume of FA1 used= cm3. (2½marks)

Questions:
(a) Calculate the number of moles of
(i) Sodium thiosulphate in FA1 that reacted. (1½ marks)
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
(ii) Iodine liberated by 10.0 cm3 of FA3. (1½ marks)
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
(iii) Aqueous chlorine in 30 cm3 of X. (2½ marks)
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
(b) Determine the
(i) mass of chlorine in 30 cm3 of X. (Cl = 35.5) (02 marks)
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
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Extract From Jusan A ‘level Practical Manual
Feb,2020

………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
(ii) Percentage by mass of chlorine in X. (01 mark)
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………

EXPERIMENT 17: (ASSHU-RWENZORI MOCK 2017)

You are provided with the following
FA1 which is approximately 0.1M sodium thiosulphate solution.
FA 2 which is a solution containing 3.5g per litre of potassium iodate.
Solid U which is a hydrated copper (II) salt.
10% potassium iodine solution 1M hydrochloric acid.
You are required to determine;
(a) the concentration of thiosulphate on FA1
(b) the percentage of copper in R.
Theory
In acidic solution potassium iodide, react with iodate ions according to the equation.
− + −
IO3(aq) + 6H(aq) + 5I(aq) → 3I2(aq) + 3H2 O(l)

Also copper (II) ions react with potassium iodide to form copper (I) iodide according to the
following equation.
2+ −
2CU(aq) + 4I(aq) → Cu2 I2(s) + I2(aq)

The iodine liberated on both reactions can be titrated with the thiosulphate according to the
equation.
2−
2S2 O3(aq) + I2(aq) → S4 O2− −
6(aq) + 2I(aq)

PROCEDURE (A)
Pipette 25cm3 or 20cm3 of FA2 into a conical flash add an equal volume of 1.0M hydrochloric
acid followed by about 10cm3 of 10% aqueous potassium iodide. Titrate the mixture with FA1
until the solution in the flask turns pale yellow. Add 3 – 4 drops of starch indicator and continue
the titration until the blue colour of the starch turns colourless. Repeat the titration to obtain
consistent results. Record your results in table 1 below.
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Results
Volume of pipette used cm3 (½marks)
Table I
BURETTE READINGS I II II
Final burette reading (cm3)
Initial burette reading (cm3)
Volume of FA1 used (cm3)
(4½marks)
Titre values used to calculate average volume of FA1 used are; (½marks)
3
and cm

Therefore average volume of FA1 used= cm3. (2½marks)

………………………………………………………………………………………………………
………………………………………………………………………………………………………
Calculate;
(i) the number of moles of iodate ions in FA2. (03 marks)
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
(ii) the molarity of the thiosulphate ions in FA1. (03 marks)
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………

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Feb,2020

PROCEDURE (B)
Weigh accurately about 6.0g of U and transfer it to a 250cm3 volumetric flash and add about
100cm3 of distilled water to dissolve, followed by sodium carbonate solution until there is a
slight precipitate formed. Add dilute ethanoic acid drop wise until the precipitate dissolves and
then make up the solution to the mass until distilled water, label the solutions FA3.
Pipette 25.0 (or 20.0) cm3 of FA3into a conical flash, and add 10cm3 of the potassium iodide
solution and titrate the mixture with FA1 until the solution is pale yellow. Add starch indicator
and continue the titrations until the blue colour of iodine turns colourless.
Repeat the titration to obtain consistent results. Record your results on table 2
Results
Mass of weighing bottle + U = g (½marks)
Mass of empty weighing bottle = g (½marks)
Mass of U used = g (½marks)
Volume of pipette used cm3 (½marks)
Table II
BURETTE READINGS I II II
Final burette reading (cm3)
Initial burette reading (cm3)
Volume of FA1 used (cm3)
(4½marks)
Titre values used to calculate average volume of FA1 used are; (½marks)
3
and cm

Therefore average volume of FA1 used= cm3. (2½marks)

………………………………………………………………………………………………………
………………………………………………………………………………………………………
Calculate;
(i) The number of moles of copper (II) ions in 250cm3 of FA3. (3½marks)
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
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Feb,2020

………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
(ii) The concentration of copper (II) ions in FA3 in mol/litre. (02marks)
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
(iii) the percentage of copper in U (Cu = 64) (2½marks)
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………
………………………………………………………………………………………………………

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Page 14 of 14
Extract from JUSAN advanced level practical Manual

ORGANIC QUALITATIVE ANALYSIS.

Question three of P525/3 is usually selected from organic chemistry and involves organic
qualitative analysis of identifying the nature of organic compounds.

APPROACH TO QUESTION THREE OF P525/3.

First ask yourself this question, “As a chemistry candidate, do I need the approach to
organic qualitative analysis?” If YES! Why do you need to analyze organic compounds?

The answer is here! Objectives for organic qualitative analysis:

1. To categorize organic compounds as either aliphatic or aromatic

2. To categorize organic compounds as either saturated or unsaturated
3. To determine the carbon to hydrogen ratio/ carbon content in organic compounds
4. To identify the functional group of organic compound under study
5. To determine class of organic compound, i.e. primary, secondary, tertiary

NOTE: It is from the above objectives that a candidate should derive the required comment
on the nature of the organic compound at the end of the analysis.

The above objectives are archived by two major tests which include;

(i) Preliminary tests, which give an overview/hint/clue of the physical nature of the compound
and these include physical state, appearance, and smell, solubility in water, pH and action of heat.
(ii) Confirmatory tests, which prove the chemical nature of the compound and its presence in the
sample under analysis; for example a yellow precipitate with Brady’s reagent indicates presence
of a carbonyl compound.

The above two tests will always enable candidates to comment on the nature of selected
commonly examined and analyzed organic compounds with the following functional group(s)
include;

 Hydroxyl group of alcohols and phenol; -OH

 Carbonyl groups of aldehydes and ketones; -CHO and –CO-
 Carboxylate group of carboxylic acids; -COOH
 Halocarboxylic acids; (UNEB 2015 SCCENARIO)

NATURE OF QUESTIONS

You are provided with an organic compound Q. You are require to carry out the following tests
below on Q .Record your observations and deductions in the table, and;

 Describe the nature of Q or

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 Comment on nature of Q or
 Identify nature of Q or
 Determine nature of Q and
 Identify any gases evolved/ liberated during the test.

Organic qualitative questions are organized in table format providing candidates with tests
requiring them to record observations and deductions.

Test Observation Deduction

Test: A chemical test is qualitative or quantitative procedure designed to identify, quantify or

characterize a chemical compound or chemical group. The chemical test may be a positive test
hence indicating the presence of a functional group or a negative test indicating absence of a
functional group in the sample under study. Usually candidates are provided with all the
necessary tests.

However, examiners are becoming more interested in instructing candidates to carry out specific
tests of their own choice to determine the presence or absence of a functional group. This
normally calls for confirmatory test after candidates have confirmed absence of other
compounds.

Sample test; to 1cm3 of Q in the test tube, add about 2cm3 of Ethanoic acid; ✓ shake well then
add 4 drops of concentrated sulphuric acid✓ and heat the mixture✓. Pour the product in a beaker
of cold water✓.

Observation: A good observation in organic qualitative analysis should capture; Color

followed by an appropriate technical term for example; yellow (color) precipitate (technical
term); violet/ purple solution; colourless solution; green solution; white crystalline solid; colorless
condensate; yellow oil; grey solid; silver mirror; white fumes; red precipitate; Bubbles/
effervescence of a colourless pungent/chocking gas; soluble/dissolves/miscible with water;
burns with a sooty/smoky flame; burns with a non-sooty/ non smoky flame; blue litmus.

Note: Candidate should always be careful when carrying the tests in order to record correct
observations, not reporting observations based on theory.

Deduction: This requires candidates to draw conclusions concerning the nature, presence or
absence of a particular organic compound based on the observations recorded from the test.
Deductions MUST be precise providing conclusive facts about the observations. For example;
phenol absent.

Comment on/ identification of/ description of nature of Q:

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This is a summarized statement of positive deductions about the nature of organic compound
present in the sample

(i) Q is an aliphatic;✓ saturated;✓ primary;✓ alcohol;✓ with a methyl group directly

attached on carbon carrying hydroxyl group; ✓ that is ethanol;
(ii) Q is an aliphatic,✓ primary;✓ alcohol;✓ of low carbon content;✓ of structure
CH3CH2OH;✓ that is ethanol;
(iii) Q is an aliphatic,✓ primary;✓ alcohol;✓ of a low carbon to hydrogen ratio;✓ of structure
CH3CH2OH;✓ that is ethanol;

HOW TO PRESENT POSSIBLE OBSERVATIONS AND DEDUCTIONS WHEN

ANSWERING QUESTION 3 OF P525/3

TEST OBSERVATION DEDUCTION

Burn a small amount Burns; with yellow non sooty Saturated aliphatic; compound of
on a spatula end or flame;✓ low carbon to hydrogen ratio;✓
porcelain dish
Aromatic; unsaturated aliphatic;
Burns; with yellow sooty flame;✓ saturated aliphatic; of high carbon
to hydrogen ratio;✓

Add sodium hydroxide Miscible in sodium hydroxide Acidic compound; ✓ aliphatic

solution solution✓ with no effervescence; carboxylic acid, phenol; present.✓

Miscible in sodium hydroxide

solution✓ with effervescence of Basic compound;✓ aliphatic amine
colourless gas that turns moist red present;✓ ammonium salt vapor
litmus blue; produced;

Solid dissolves/soluble✓ in
sodium hydroxide solution, to form Aromatic✓ carboxylic acid, phenol
a colourless solution on warming; present✓
with no effervescence;

Solid insoluble✓ in sodium

hydroxide solution; Aromatic✓ amine✓ present

Add bromine water Bromine water turns from brown Unsaturated compound;✓phenol;
to colourless✓ aniline;✓ present

Brown colour of bromine persists✓

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Saturated compound
present;✓(phenol, aniline absent) ✓

Shake with water; Miscible/ soluble✓ with cold water Polar compound;✓of low molecular
forming a colourless solution; mass;✓

Sparingly miscible/ soluble✓ in Polar compound;✓of high molecular

And test the resultant cold water forming a colourless mass;✓
solution with litmus or solution;
universal indicator.
Turns blue litmus red;✓ Acidic compound;✓carboxylic acid,
phenol;✓

Has no effect on litmus;✓

Neutral compound;✓alcohol,
carbonyl compound;✓

Add sodium Effervescence/ bubbles✓ Carbon dioxide gas;✓produced/

carbonate/ sodium Of a colourless gas; that turns lime evolved/ produced; Carboxylic acid
hydrogen carbonate water milky and moist/ dump blue present; ✓
(s/aq) litmus paper red.

No bubbles/ effervescence✓ Carboxylic acid absent; ✓

Add Brady’s reagent Yellow precipitate;✓ formed Carbonyl compound present;✓

aldehyde, ketone;✓

No yellow precipitate;✓ Carbonyl compound absent✓

Add Fehling’s reagent Red precipitate; is formed✓ Ketone absent; aldehyde confirmed
present;✓
No red precipitate;✓
Ketone confirmed present; aldehyde
absent;✓

Add neutral iron(iii) Violet/purple solution formed✓; Phenol confirmed present;✓

chloride solution
Violet/ purple solution not Phenol absent;✓
formed;✓

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Add Tollen’s reagent Silver mirror formed;✓ Ketone absent; aldehyde confirmed
present;✓
No silver mirror;✓
Ketone confirmed present; aldehyde
absent;✓

Add Orange solution turns to green; ✓ Reducing agent present;✓ primary

Acidified potassium alcohol, secondary alcohol,
dichromate solution aldehyde present;
and heat. No observable change; ✓
Reducing agent absent;✓ tertiary
alcohol, ketone, probably present;✓

Add purple solution turns colourless✓ Reducing agent present;✓ primary

Acidified potassium alcohol, secondary alcohol,
permanganate aldehyde present;✓
solution and warm No observable change;✓
Reducing agent absent; tertiary
alcohol, ketone, probably present;✓

Add Lucus reagent Cloudy solution✓ formed is formed Tertiary alcohol present;✓
immediately✓

Cloudy solution✓ within 5-10 Secondary alcohol present;✓

minutes✓
NB: candidates must specify the
actual value of time when
recording the observation not
stating the range.
Primary alcohol present;✓
No observable change✓ at room
temperature
Add excess iodine Yellow precipitate is formed;✓ with Alcohols, carbonyl compounds;
solution followed by antiseptic smell;✓ carboxylic acid; ✓ with a methyl
sodium hydroxide group (CH3-) ✓ directly attached to
solution drop wise carbon with functional group;
until solution turns present. CH3I (s) formed✓
pale yellow. Warm No Yellow precipitate ✓
gently and cool under
Alcohols, carbonyl compounds;
running tap water
carboxylic acid; ✓ without a methyl
group (CH3-) ✓ directly attached to

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carbon with functional group;

present.

Add sodium metal Effervescence✓ of a colourless gas Hydrogen gas produced;✓

that burns with a pop sound; Alcohol, phenol, carboxylic acid
present;✓

NB: candidates should master the composition of reagents incase trivial names such as
Lucus reagent, Fehling’s solution, Tollen’s reagent, Brady’s reagent, Iodoform reagent
are used in the question.

SAMPLE EXPERMENT: (ASSHU-RWENZORI MOCK 2017)

You are provided with an organic substance R. You are required to determine the nature of R.
Carryout the following test on R and record your observations and deductions in the table below.
(15 marks)

TESTS OBSERVATIONS DEDUCTION

(a) Heat a spatula endful of R on a White crystalline solid; Aromatic compound;✓
crucible. ✓ burns with a yellow Unsaturated
sooty flame✓ compound✓ with high
C: H ratio; ✓

(b) To two spatula endful of R in a clean Insoluble;✓ in cold R is an aromatic ✓

test tube, add about 5cm3 of distilled water but dissolves on carboxylic acid;✓
water. Shake vigorously and warm. warming, turns blue
Test the solution with litmus paper. litmus red, ✓ on
Divide the resultant solution into six cooling the solid
portions. reappears✓
(i) To the first portion of the solution, R dissolves;✓ in R is acidic;✓
add 3 drops of sodium hydroxide sodium hydroxide
and warm. solution
(ii) To the second portion of the No yellow precipitate Carbonyl
solutions, add 1cm3 of Brady’s formed;✓ group/aldehyde;✓ or
reagent. Ketone absent.

(iii) To the third portion of the solution, Brown precipitate PhCOO- formed, ✓
add 1cm3 of neutral iron (III) formed;✓ Benzoic acid present;✓
chloride.
(iv) To the fourth portion add 2cm3 of Sweet fruity smell;✓ Ester formed, ✓ -COOH
ethanol followed by 3 drops of present; ✓
concentrated sulphuric acid and
warm the mixture.
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(v) To the fifth portion, add 1cm3 of Effervescence of a CO2 evolved; ✓

sodium hydrogen carbonate colourless gas;✓ that -COOH group
solution. turns lime water confirmed;✓
milky;✓

(vi) To the sixth portion of the solution, Colourless gas✓ burns Aromatic carboxylic
add excess sodalime and heat the with a yellow sooty acid;✓ confirmed;✓
mixture. Place a burning splint on flame;✓
the mouth of the test tube.
(c) From your results above, deduce the nature of compound R.
R is an aromatic; ✓ carboxylic acid; ✓ Benzoic acid✓.

EXPERIMENT 1. (UNEB 2019)

You are required to carry out tests below on M and describe the nature of M and identify any
gases evolved. Record your observations and deductions in the table below.
(16 marks)

TESTS OBSERVATIONS DEDUCTIONS

(a) Burn a small amount of M on a

spatula end or in a dry porcelain
dish

(b) To about 2cm3 of M, add 3cm3 of

water, shake and divide the
mixture into three parts.

(i) To first part of the solution,

add 2-3 drops of neutral iron
(II) chloride solution.

(ii) To second part of the

solution, add 2-3 drops of
neutral iron (III) chloride
solution.

(iii) To third part of solution, add

2-3 drops of acidified
potassium dichromate (VI)
solution, warm.
(iv)

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(c) To 0.5cm3 of M in the test tube,

add 2-3 drops of Brady’s reagent.

(d) To about 1cm3 of M, add 2cm3 of

ethanoic acid followed by 3drops
of concentrated sulphuric acid
and heat. Pour the products in a
beaker of cold water.

(e) To 0.5cm3 of M, add 2cm3 of

sodium hydroxide solution
followed by aqueous iodine drop
wise until in excess. Warm the
mixture and leave to stand.

(f) To about 1cm3 of M, add 3cm3 of

Lucas reagent and shake, and
leave it to stand.

(g) Describe the nature of M.

…………………………………………………………………………………………………………………………

…………………………………………………………………………………………………………………………..

EXPERIMENT 2. (UNEB 2018)

You are provided with an organic compound W.
You are required to carry out tests below on W and describe the nature of W and identify any
gases evolved.
Record your observations and deductions in the table below. (18 marks)

TESTS OBSERVATIONS DEDUCTIONS

(a) Burn a small amount of w on

a spatula end or in a dry
porcelain dish

(b) To about 0.5cm3 of W, add

1cm3 of water, shake and test
the mixture with litmus paper

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(c) To about 1cm3 of W, add 3-4

drops of neutral iron(III)
chloride solution.

(d) To about 1cm3 of W, add 3-4

drops of Brady’s reagent.

(e) To about 2cm3 of W, add 4- 5

drops of acidified potassium
dichromate (VI) solution, heat,
allow to cool and use in part
(f).
(f) To the mixture from (e), add 3-
4 drops of Brady’s reagent.
(g) To about 2cm3 of Lucas
reagent, add 1cm3 of W.

Describe the nature of W.

…………………………………………………………………………………………………………………………

EXPERIMENT 3. (UMTA 2019)

You are provided with an organic compound Q. You are required to identify the nature of
compound Q and identify any gases evolved. Carry out the following tests on the compound and
record your observations and deductions in the table below. (17 marks)

TESTS OBSERVATIONS DEDUCTIONS

(a) Burn a small amount of Q on a
spatula end or in a dry porcelain
dish.

(b) To about 1cm3 of Q, add 2cm3 of

water, shake and test the mixture
with litmus.

(c) To about 0.5cm3 of Q, add 2-3 drops

of sodium carbonate solution.

(d) To about 0.5cm3 of Q, add 2-3 drops

of acidified potassium dichromate
solution and heat.
(e) To about 0.5cm3 of Q, add 2-3 drops
of Brady’s reagent.

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(f) To about 0.5cm3 of Q, add 2-3 drops

of acidified potassium dichromate
solution and heat. Then add ethanol
followed by 4-5 drops of
concentrated sulphuric acid. Pour
the mixture into a small beaker of
cold water.
(g) To about 0.5cm3 of Q, add 4cm3 of
iodine solution followed by sodium
hydroxide solution drop wise until
the brown color of iodine I just
discharged.
(h) To about 1cm3 of Q, add about
5drops of Tollen’s reagent and heat
gently.
Describe the nature of Q.

…………………………………………………………………………………………………………………………

EXPERIMENT 4.

ACCOMPLISHED CONTENT TO BE ACCESSED IN THE COMPLETE MANUAL.

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