UTAR

FHSC1134 Inorganic Chemistry

Trimester 2/3

Experiment 1
________________________________________________________________________
Title: Properties of Period 3 Oxides

Aim:
To examine the oxides of Period 3 elements and describe their structure and bonding.

Introduction:
Generally, there are oxides of metals and non-metals. Metals burn in oxygen to form basic
oxides while non-metals form acidic oxides. Structurally, they are covalent or ionic
compounds. You are to do some simple observations and tests, to find out the differences
between the types of oxides provided and to account for these differences.

Apparatus:
Test tubes Test tube rack
Measuring cylinders Thermometer
Wooden splinter Glass rod

Materials:
Sodium peroxide Magnesium oxide
Silicon(IV) oxide Phosphorus pentoxide
Universal indicator solution Litmus paper

Safety measures:
Safety goggles

**Warning:
Phosphorus(V) oxide is corrosive and irritates eyes, skin and lungs.
Sodium peroxide is also corrosive and a powerful oxidant.

Procedure:
Part A: Appearance:
Examine your oxide samples, and in Table 1, note for the physical states at room
temperature:
(a) whether it is solid, liquid or gas,
(b) its color (if any)

Part B: On mixing with water:

1. Set up 4 test tubes, side by side.
2. Into each test tube pour about 5 cm3 of distilled water.
3. In the test tube, place a thermometer.
a. Note the temperature.
b. Add half a spatula-tip of sodium peroxide and stir carefully with the glass rod.
c. Note after one minute, (i) the temperature, (ii) whether the solid has dissolved and
(iii) anything else you see. For example, is gas evolved at any time? If so, is the gas
acidic? Can you identify it using a simple test?
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d. Add 2 -4 drops of universal indicator solution, compare the color with the chart
provided, and note the pH indicated or use a piece of pH paper.
4. Repeat the above steps 3 (a) – (d), using, in turn, magnesium oxide, silicon(IV) oxide
and phosphorus(V) oxide.
5. Measure the pH of the water in the fifth test tube by adding 2-4 drops of universal
indicator solution for comparison with the above.

Results:

Table 1
Na2O2 MgO SiO2 P4O10
Appearance

Initial temperature/ºC

Final temperature/ºC

Solubility

pH of solution

Other observation(s)

Questions:
1. Use your experimental results and your test books (if necessary) to complete a larger
copy of Table 2.

Table 2
Formula of oxide
Na2O2 MgO Al2O3 SiO2 P4O10 Cl2O
Melting-point/ oC

Boiling-point/ oC

State at s.t.p.

Action of water

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pH of aqueous
solution

Acid/base nature

Conductivity of
liquid
Solubility in hexane
Structure

Bonding

2. Write equations for any reactions which took place when you add the oxides to water.

3. Comment on the change in structure and bonding in the oxides of the elements in the
period between sodium and chlorine.

4. How does the acid-base nature of the oxides of the elements in Period 3 change with
increasing atomic number?

5. Can you relate this change in structure and bonding that take place along the period?

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Experiment 2
________________________________________________________________________
Title: The Solubility of Salts of Group II Elements

Aim:
To study the solubility of the sulphates, sulphites and hydroxides of Group II elements.

Introduction:
In this experiment, you add each of the anion solutions to 1 cm3 of each cation solution
provided, drop by drop, until the first sign of a precipitate appears. For each salt, the
solubility is proportional to the number of drops of anion added.

Apparatus:
Test tubes Test tubes racks
Graduated pipette Pasteur pipette
Beaker (50ml)

Materials:
0.1 M solution of the following cations: Mg2+, Ca2+, Ba2+
1.0 M solution of OH-
0.5 M solution of SO42-
0.5 M solution of SO32-

Procedure:
1. Set up three rows of three test tubes each.
2. For each row, label the 1st test tube Mg2+, the 2nd test tube Ca2+, and 3rd test tube Ba2+.
3. Add 1 cm3 of the appropriate cation solution to each test tube by using a 1 cm3
graduated pipette.
4. To each test tube in the first row, add OH- solution drop by drop and shake until the
first sign of precipitate appears.
5. Record the number of drops of OH- solution used in Table 1.
6. If a precipitate is produced, classify the precipitate as slight (s) or heavy (h).
7. If no precipitate is produced after forty drops, then write ‘40+’ and assign the salt as
soluble.
8. Repeat steps 4 to 7 by replacing OH- with SO42- and SO32- to the 2nd and 3rd rows of
test tubes respectively.

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Results:

Table 1
Cation Number of drops of anion solution added to form a precipitate
Solution
OH- SO32- SO42-
2+
Mg

Ca2+

Ba2+

Questions:
1. For Group II, what are the solubility trends of the salts listed below:
(a) Hydroxides (b) Sulphites (c) Sulphates

2. Explain your answer for (1).

3. Use Table 2 to answer the following questions.

Table 2: Solubility of Group II compound in water at 298 K

Singly-charged anions Doubly-charged anions
Solubility Solubility
Compound /mol per 100 g Compound /mol per 100g
of water of water
-1
MgCl2 5.6 x 10 MgCO3 1.8 x 10-4
-1
CaCl2 5.4 x 10 CaCO3 0.13 x 10-4
-1
SrCl2 3.5 x 10 SrCO3 0.07 x 10-4
BaCl2 1.5 x 10-1 BaCO3 0.09 x 10-4
Mg (NO3)2 4.9 x 10-1 MgSO4 3600 x 10-4
-1
Ca (NO3)2 6.2 x 10 CaSO4 11 x 10-4
Sr (NO3)2 1.6 x 10-1 SrSO4 0.62 x 10-4
-1
Ba (NO3)2 0.4 x 10 BaSO4 0.009 x 10-4
Mg (OH)2 0.020 x 10-3 MgCrO4 8500 x 10-4
-3
Ca(OH)2 1.5 x 10 CaCrO4 870 x 10-4
Sr (OH)2 3.4 x 10-3 SrCrO4 5.9 x 10-4
-3
Ba (OH)2 15 x 10 BaCrO4 0.011 x 10-4

(a) Identify the group trends in solubility for each type of salt listed in Table 2.
(b) Does the solubility listed above for carbonates, sulphates and hydroxides match
with your findings in this experiment. If no, why?
(c) Which anions give more soluble compounds, singly-charged or doubly-charged
anions?
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Experiment 3
________________________________________________________________________
Title: Properties of Aluminium and Its Compounds

Aim:
To investigate the properties of aluminium and its compounds.

Introduction:
Aluminium is the most abundant metal in the earth’s surface (7.5% by mass). The
abundance of Al, coupled with its attractive combination of physical and chemical
properties, accounts for the fact that it is one of the principal industrial raw materials used
by industrialized societies.

Aluminium has more metallic character compared to boron, which is in the same group in
the Periodic Table. It forms trivalent compounds due to the 3 electrons in its valence shell.
Generally, aluminium compounds are ionic in nature but many compounds of aluminium
show both ionic and covalent character. In this experiment, we will investigate the
properties of aluminium and some of its salts.

Apparatus:
Test tube Glass dropper
Beaker Watch glass
Bunsen burner Glass rod

Materials:
Aluminium strips Filter paper
Aluminium foil Litmus paper
Sand paper Diluted sodium hydroxide
Diluted hydrochloric acid 20% aluminium sulphate
Diluted nitric acid Diluted sulphuric acid
Diluted ammonium hydroxide Distilled water
Concentrated sodium hydroxide

Safety measures:
Wear safety goggles. Wear gloves when using concentrated acid and base.

Procedure:
Part A: Reaction with air
1. Heat a small piece of aluminium foil using a bunsen burner. State the observation.

Part B: Reaction with acids

1. Put three small pieces of aluminium (clean with sand paper) into three separate test
tubes, each containing 5 cm3 of diluted hydrochloric acid, diluted nitric acid and diluted
sulphuric acid respectively.
2. Heat the solutions when necessary. Which acid reacts faster with aluminium?

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Part C: Reactions with alkali

1. Add 5 cm3 of concentrated sodium hydroxide solution into a test tube containing a piece
of aluminium.
2. Identify the gas released.

Part D: Aluminium hydroxide and aluminium sulphate

1. Fill in about 10 cm3 of 20% aluminium sulphate solution into a small beaker, and then
add 10 cm3 of diluted ammonium hydroxide solution.
2. Boil the mixture and filter it. Wash the aluminium hydroxide collected on the filter
paper with water.
3. Transfer a portion of the aluminium hydroxide prepared in step (2) on to a watch glass.
Using a glass dropper, add 6 drops of diluted hydrochloric acid.
4. Put a small amount of aluminium hydroxide from step (2) into a test tube. Add four
drops of sodium hydroxide solution, one drop at a time. Shake the test tube after adding
each drop and observe carefully for the appearance and disappearance of any
precipitate.
5. Test the pH of a small amount of aluminium sulphate solution using litmus paper and
record your observations.
6. Pour 5 cm3 of aluminium sulphate solution into a small beaker and add drop wise
sodium hydroxide solution slowly with stirring. Observe the reaction when excess
sodium hydroxide is added to the mixture.

Results:

Experiment Observation
A. Reaction with air

B. Reaction with acids

C. Reaction with alkali

D. Aluminium hydroxide and

aluminium sulphate

Question:
1. Write down all the chemical equations involved in this experiment.

2. Why must we use clean aluminium foil for this experiment?

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Experiment 4
________________________________________________________________________
Title: The Synthesis of Potassium Aluminium Sulfate (Alum)

Aim(s):
To prepare common aluminium complexes, alum, KAl(SO4)2.12H2O.

Introduction:
Aluminium occurs naturally as mineral bauxite (primarily a mixture of Al2O3.3H2O, Fe2O3
and SiO2), and it is purified in the following process:

Step 1: Purification of raw materials

Bauxite is firstly mined, crushed and then washed to remove water soluble impurities. The
remaining material is then dissolved in NaOH and heated up. Al2O3 is selectively dissolved
due to its properties of amphoteric oxide. The reaction is shown as below.

Al2O3 + 6NaOH + 3 H2O → 2Na3Al(OH)6

However, some of the crystalline forms of SiO2 can also be dissolved under the same
reaction. The equation is given as below.

SiO2 + 4NaOH → Na4SiO4 +2H2O

Both of these species are soluble, but Fe2O3 is a basic oxide and hence it is insoluble in
NaOH solution and can be filtered out. Over time the Na3Al(OH)6 decomposes to Al(OH)3
(an insoluble species), which can also be filtered out.

Na3Al(OH)6 + 2H2O → 3NaOH + Al(OH)3 .2H2O

This is then decomposed by heating to temperatures above 1000 °C to give alumina, Al2O3.

Al(OH)3 .2H2O → Al2O3 + 9 H2O

Step 2: Reduction of the alumina

The resultant alumina (Al2O3 ) is dissolved in molten cryolite (Na3AlF6), forming an ionic
and electrically conductive solution. This is decomposed by electrolysis later by using a
consumable carbon as anode with two concurrent reactions proceeding according to the
following equations:

Al2O3 + 3C → 2Al + 3CO

2 Al2O3 + 3C → 4Al + 3CO2

The use of consumable carbon anode lowers the required voltage by 1.0 V at the operating
temperature of 950-980 °C.

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Figure 1: Electrolysis process on extracting aluminium.

The environmental impact on extracting aluminium from its natural source (bauxite) is
quite high. Yet, the need for aluminium continues to grow due to its attractive properties.
Recycling aluminium products is one of the alternatives on saving environmental cost due
to its highly cost from the extraction process. Aluminium recycled from beverage cans only
requires 5 percent of energy if compared to the production of aluminium from ores. In the
year 2000, it was estimated that nearly 63 billion aluminium cans were recycled in the
United States. The commercial recycling of aluminium is a melting or purification process
that keeps the aluminium as aluminium metal. However, it needs to dissolve aluminium in
hot KOH in this experiment and use the dissolved aluminium to make crystals of potassium
aluminium sulphate dodecahydrate, KAl(SO4)2.12H2O. This compound belongs to a family
of metal sulphates called alums.

In this experiment, you will be recycling aluminium scrap in a very unusual way, and you
will produce two products which are potentially very useful: hydrogen gas (H 2) and very
pure potassium aluminium sulphate (KAl(SO4)2.12H2O or alum). Hydrogen gas has great
potential use as fuel, if some of its dangerous properties can be controlled (mixtures of H 2
and air are highly explosive). Hot aqueous hydroxide solution used in this experiment will
quickly remove the oxide layer on the aluminium surface and then dissolve the aluminium
metal by converting aluminium atoms to Al3+. There are a number of Al3+ species formed
in an aqueous environment, depending on the abundances of OH - and H+ ions (the pH of
the solution). Adding the H2SO4 to the mixture can lead to the desired KAl(SO4)2.12H2O
alum product.

Apparatus and Equipment:

Beaker, 250ml Measuring cylinder
Butchner funnel Pasteur pipette
Filtration flask Sandpaper
Filter paper Glass rod
Ice bath

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Materials:
Aluminium beverage can
Boiling chips
Distilled water
Ethanol
2 M Potassium hydroxide, KOH
9 M Sulphuric acid, H2SO4

Safety measures:
Protective gloves
Safety goggles
Hydrogen gas produced is very explosive.
Therefore, you MUST:
ENSURE THAT YOU ONLY HEAT THE BOTTOM OF THE BEAKER AND
NOT LETTING THE FLAME GET NEAR THE TOP.

Concentrated sulphuric acid is very corrosive and reacts vigorously with water.
Therefore, you MUST:
WEAR GLOVES AND SAFETY GOGGLES.
DISPOSE UNWANTED ACID BY COOLING AND POURING SLOWLY INTO
AN EXCESS OF WATER.

Ethanol is very flammable.

Therefore, you MUST:
KEEP THE BOTTLE CLOSED ALWAYS.
KEEP THE BOTTLE AWAY FROM FLAMES.
WEAR SAFETY GOGGLES.

Potassium hydroxide is very harmful if swallowed and causes severe burns.

Therefore, you MUST:
WEAR APPROPIATE PROTECTIVE CLOTHING.

Procedure:
Part A: Dissolution of the aluminium
1. Cut about 2 x 5 cm2 of aluminium strip from aluminium can provided. Scrap off
thoroughly any paint and/or plastic coating from both sides by using a piece of
sandpaper.
2. Weigh out approximately 1.0 g of the scrap aluminium strip into a 250 cm3 beaker.
Record the mass.
3. Cut the weighted aluminium strip into small pieces and place the pieces in a clean
beaker, followed by the addition of 50 cm3 of 2 M KOH into the beaker. Perform this
operation in the fume hood.
4. Heat the mixture very gently on a hot plate if the reaction is proceeding too slowly.

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5. Bubbles should form from the reaction between aluminium and aqueous potassium
hydroxide. Add distilled water to maintain the volume at approximately 25 cm3 (if the
liquid level in the beaker drops to less than half of its original volume). The reaction is
complete when the gas evolution ceases and without any trace of aluminium pieces.
6. Vacuum filter the solution (if the solution contains any remaining solid). Use a small
amount of water (not more than 200 cm3) to rinse the beaker and funnel.
7. Allow the filtrate to cool down to room temperature.

Part B: Formation of Al(OH)3 and removal of OH-

1. Transfer 20 cm3 of 9 M H2SO4 to the filtrate.
2. Add 20 cm3 of 9 M H2SO4 drop wise to the filtrate slowly and with stirring.
3. White precipitate will form upon the addition of sulphuric acid and will dissolve when
excess of sulphuric acid is added into the beaker.
(Note: There may be a small amount of undissolved white precipitate. Add 2 or 3
boiling chips (if necessary) and heat the solution gently until the solution becomes
clear.)

Part C: Precipitation of alum crystals

1. Prepare a half-full ice bath and add water until the bowl is three quarters full.
2. Cool the solution in Part B to room temperature and then place the beaker in the ice
bath. Crystals of alum should form. Allow it to cool for 15 minutes.
3. Vacuum filter the product and wash with 10– 20 cm3 of ethanol/water solution (1:1).
4. Allow the product to dry for a few minutes, remove the boiling chips and record the
weigh.
5. Calculate the percentage yield of alum obtained.

Results:
Part A: Observation(s)

Table 1: Observation(s) for each part of experiment

Observation(s)
(A) Dissolving the aluminium

(B) Formation of Al(OH)3

(C) Precipitating alum crystals

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Part B: Calculation

Table 2: Mass of aluminium

Mass of empty beaker (g)

Mass of beaker + aluminium strips (g)
Mass of aluminium strips used (g)

Table3: Mass of alum

Mass of filter paper (g)

Mass of filter paper + alum (g)
Mass of alum (g)

Questions:
1. Identify the gas released during the reaction of aluminium beverage can and potassium
hydroxide.

2. What is the white precipitate formed during the addition of concentrated sulphuric acid?
Write down the balanced equation that involved.

3. Why the white precipitate disappears when excess of sulphuric acid is added? Write
down the balanced equation that involved.

4. Write down the complete balanced equation of aluminium hydroxide, Al(OH)3, to form
alum, KAl(SO4)2.12H2O.

5. What is the theoretical yield of alum, in grams, obtained from the experiment?

6. What is the percentage yield of alum obtained from the experiment?

actual yield ( g )
Percentage yield =  100 %
theoretical yield ( g )

7. List out several common usages of aluminium.

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Experiment 5
________________________________________________________________________
Title: Reaction of Tin and its Common Ions

Aim:
To shows the reactions of tin with acids and to carry out some of the common reactions of
Sn2+ (aq).

Introduction:
In this experiment you will find out if the metallic character of tin is evident from its
reactions with acids. You treat the elements with two acids: an oxidizing agent (nitric acid)
and a non-oxidizing acid (hydrochloric acid). In each case you attempt to identify any gases
evolved.
The reactions of the divalent ions are included here to demonstrate the relative stability of
the +2 state in tin.

Apparatus:
Test tubes Test tube rack
Bunsen burner Test tube holder/ clamp
Asbestos sheet Beaker
Graduated pipette wooden splinter

Materials:
Diluted hydrochloric acid (2 M) Concentrated hydrochloric acid
Concentrated nitric acid 2 M NaOH solution
2.0 M ammonia solution 0.1 M K2CrO4
0.02 M Na2S solution 0.1 M KI solution
Tin (small pieces/granule) 0.1 M solution of Sn2+ ions (in diluted HCl acid)
0.01 M KMnO4 (in diluted ethanoic acid)

Safety measures:
Safety goggles

**Warning:
Sodium sulphide is toxic and corrosive and evolves highly poisonous hydrogen sulphide
gas on contact with acids.
Concentrated hydrochloric acid is very corrosive.
Concentrated nitric acid is very corrosive and a powerful oxidant.

WEAR PROTECTIVE GLOVES AND SAFETY GOGGLES.

USE SODIUM SULPHIDE IN THE FUME-CUPBOARD.

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Procedure:
1. Place a small piece of tin in each of three test tubes.
2. To one test tube add about 2 cm3 of diluted hydrochloric acid and heat gently.
Can you see or detect a gas? If not, repeat the experiment carefully using about 2 cm3
of concentrated hydrochloric acid.
3. In the remaining test tube add about 2 cm3 of concentrated nitric acid to the tin and heat
gently.
4. Record your results in a larger copy of Table 1.
5. Add approximately 2 cm3 of the Sn2+ solution to each of seven test tubes.
6. Add each of the following reagents to Sn2+:
(a) Diluted sodium hydroxide solution, initially drop-by-drop, and then to excess;
(b) Ammonia solution, initially drop-by-drop, and then to excess;
(c) About 2 cm3 of diluted hydrochloric acid, heat the mixtures and then cool them
under running cold water;
(d) About 2 cm3 of acidified potassium manganate (VII) solution;
(e) About 1 cm3 of potassium chromate (VI) solution;
(f) 5 drops of sodium sulphide solution (do this in the fume-cupboard and dispose of
the mixture by pouring into the fume-cupboard sink);
(g) About 2 cm3 of aqueous potassium iodide.
7. Record your observations in a larger copy of results Table 2.

Result:

Table 1: Reaction of Tin granules with acids:

Acid Observations
Diluted hydrochloric acid
Concentrated hydrochloric acid
Concentrated nitric acid

Table 2: Reaction of acidified Sn2+ (aq) with other reagents:

Reagent Observations
a) Sodium hydroxide solution
b) Ammonia solution
c) Diluted hydrochloric acid
d) Acidified potassium manganate(VII)
solution
e) Potassium chromate(VI)
f) Sodium sulphide solution
g) Potassium iodide solution
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Questions:
1. Complete the following equations:

Sn(s) + HCl(aq.) →

2. Are the reactions between the elements and hydrochloric acid typical of metals?
Explain your answer.

3. Reactions with nitric acid tend to be complex and equations are not generally required.
The questions illustrate some general points.
(a) Which gas did you detect when nitric acid reacted with tin?
(b) Do other metals behave in similar way with nitric acid? Give one example.
(c) Why does nitric acid behave differently from hydrochloric acid?

4. Use your text-book(s) to complete and balance the equations in Table 3.

In the comments column you should describe the type of chemical reaction occurring
and any other important feature(s).

Table 3:
Equations Comments

Sn2+ (aq) + OH-(aq) → The precipitate dissolves in excess NaOH to

Sn (OH)2 (s) + OH-(aq) → form a stannate(II) ion2 , Sn (OH)64-

2MnO4-(aq) + 16H+ (aq) + 5Sn2+ (aq) →

Cr2O72-(aq)** + H+ (aq) + Sn2+(aq) →
Sn2+(aq) + S2- (aq) →
* Various formulae have been proposed for the stannate(II) ion ranging from SnO22- for the anhydrous
form to Sn(OH)42- and Sn(OH)64- for the hydrated forms. Sn(OH)64- seems the most probable.
** Chromate(VI) (CrO42-) changes to dichromate (VI) (Cr2O72-) when acidified
[2CrO42-(aq) + 2H+ (aq) → Cr2O72-(aq) + H2O (1)]

5. In the experiment, potassium manganate(VII) solution was acidified with diluted

ethanoic acid and hot, as is usual, diluted hydrochloric acid or diluted sulphuric acid.
With the aid of your text-book (s), explain why you think this change was made. Give
any relevant equations in your answer and state what you would observe if the MnO 4-
solution were acidified with HCl (aq) or H2SO4 (aq).

6. Predict the reaction between aqueous tin (II) ions and a solution of mercury(II) chloride.
What do you think you would observe in this reaction?

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Experiment 6
________________________________________________________________________
Title: Halogen-Halide Reactions in Aqueous Solution

Aim:
To investigate the order of oxidizing ability of the halogens Cl2, Br2 and I2 in aqueous
solution.

Introduction:
You mix each of the aqueous solutions with halide ion solutions, C1- (aq), Br - (aq), and I-
(aq) in turn, and see whether a reaction takes place. The addition of cyclohexane to the
halogen-halide mixture enables you to recognize the halogen molecules present. The
halogen which oxidizes most of the other halide ions will clearly be the strongest oxidizing
agent.

Apparatus:
Test tubes fitted with cork Test tube rack
Graduated pipettes

Materials:
Bromine water, Br2 (aq) --------------- Chlorine water, C12 (aq) --------------------------------
Iodine solution, I2 in KI (aq) Potassium bromide solution, KBr
Potassium chloride solution, KC1 Potassium iodide solution, KI
Cyclohexane, C6H12 ----------------------------------------------------------------------------------------------------------------

Safety measures:
Safety goggles
Hazard warning
KEEP CYCLOHEXANE WELL STOPPERED AND AWAY FROM FLAMES
Halogen and organic vapors must not be inhaled.
THE LABORATORY MUST BE WELL VENTILATED AND REAGENT
BOTTLES AND TEST TUBES STOPPERED AS MUCH AS POSSIBLE.

Procedure:
1. Reaction (if any) of iodide with chlorine and bromine:
(a) To each of two test tubes add about 1 cm3 of potassium iodide solution.
(b) To one of those tubes, add about the same volume of chlorine water, and to the
other add the same volume of bromine water.
(c) Cork and shake the tubes and note the colour change (if any).
(d) To each tube add about 1 cm3 of cyclohexane. Cork and shake, allow it to settle.
Note the colour of each layer.
(e) Decide which reactions have taken place, and complete Table 1.
2. Reaction (if any) of bromide with chlorine and iodine.
Repeat the above steps, 1 (a) – (e), using potassium bromide with chlorine water and
iodine solution.

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3. Reaction (if any) of chloride with bromine and iodine

Repeat steps 1 (a) – (e) using potassium chloride with bromine water and iodine
solution.

Results:
Table 1
Chlorine Bromine Iodine
water water solution
Initial colour
Colour after shaking with KI solution

Colour of each layer Upper

1. after shaking with
cyclohexane Lower

Conclusion

Colour after shaking with KBr solution

Colour of each layer Upper

2. after shaking with
cyclohexane Lower

Conclusion

Colour after shaking with KCl solution

Colour of each layer Upper

3. after shaking with
cyclohexane Lower

Conclusion

Questions:
1. From the results:
(a) Does I2 (aq KI) oxidize Cl – (aq) and Br – (aq)?
(b) Does Br2 (aq) oxidize Cl – (aq) and I- (aq)?
(c) Does Cl2 (aq) oxidize Br – (aq) and I – (aq)?

2. Explain your answer for question (1).

3. State the purpose of using cyclohexane in this experiment.

4. Write ionic equations for the reactions that have taken place.
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Experiment 7
________________________________________________________________________
Title: Reactions of Halides in Solution

Aim:
To find out whether the ions, Cl-, Br- and I-, react in solution with certain reagents and
identify the products formed in the reactions.

Introduction:
In this experiment, you will add various reagents to separate samples of solutions
containing the Cl-, Br- and I- ions. In many of the reactions, precipitates are formed. Where
you are asked to add another reagent to excess, you should look carefully to see if any of
the precipitate dissolves.

Apparatus:
15 test tubes with corks Test tube racks
Pasteur pipettes

Materials:
Potassium bromide solution, KBr Potassium chloride solution, KCl
Potassium iodine solution, KI Silver nitrate solution, AgNO3
Diluted nitric acid, HNO3 Ammonia solution, NH3
Hydrogen peroxide solution, H2O2 Diluted sulphuric acid, H2SO4

Procedure:
Add the following reagents to 1 cm3 of the chloride, bromide and iodide solutions in turn,
and record your observations in Table 1.
1. Add approximately 1 cm3 of silver nitrate solution and shake gently. State the
observation. Move the three test tubes to a dark cupboard and leave them there till the
end of the lesson and note their appearance again.
2. Add silver nitrate solution as in (1). Leave these test tubes in their racks until the end
of the lesson, noting their appearance every 10-15 minutes.
3. Add approximately 1 cm3 of silver nitrate solution followed by excess (e.g. 5 cm3)
diluted nitric acid. Cork the test–tubes and shake vigorously.
4. Add approximately 1 cm3 of silver nitrate solution followed by excess (e.g. 5cm3)
ammonia solution. Cork the test tubes and shake.
5. Add approximately 1 cm3 of hydrogen peroxide solution followed by approximately 1
cm3 of diluted sulphuric acid. Cork these test tubes and allow them to stand. Add any
further reagent (s) which you think will help you to decide what has happened.

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Results:

Table 1:
Test Chloride Bromide Iodide

Action of AgNO3 (aq)

Effect of standing in
(a) dark
(b) light
Action of AgNO3(aq)
followed by diluted HNO3

Action of AgNO3 (aq)

followed by NH3 (aq)

Action of H2O2 (aq) and

diluted H2SO4 (aq)

Question:
1. Write ionic equations for the reactions between each of the three halide solutions and
silver nitrate solution.

2. Suggest chemical tests that can be used to distinguish between:

(a) Cl-(aq) and Br-(aq),
(b) Br-(aq) and I-(aq).

3. Write an ionic equation for the reaction between aqueous iodine and acidified hydrogen
peroxide.

4. Why do you think there is no reaction occurs between acidified hydrogen peroxide and
the other halide ions?

5. Suggest a reason for the darkening effect of light on the silver chloride and silver
bromide precipitates.

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Experiment 8
________________________________________________________________________
Title: Complex Formation and Precipitation

Aim:
To investigate complex formation and precipitation reactions.

Introduction:
Complex formation and precipitation reactions are the basis of qualitative inorganic
analysis. The reactions involve the manipulation of chemical equilibria by either adding
specific ions or adjusting their concentrations, in order to cause a precipitate to form or to
dissolve.
Substances that show conductivities proportional to their concentrations in aqueous
solution are classified as strong electrolytes. Strong electrolytes will dissociate completely
into ions in aqueous solution. Examples of salts are Li, Na, K, all nitrates, many metallic
chloride salts, all hydroxides, HCl, HNO3, and HClO4. In the present study the ions Na+,
K+, and NO3- can be regarded as spectator ions, not taking part in the reactions.

Complex formation
Addition of ammonia or sodium hydroxide to aqueous solutions of metal ions will often
cause precipitation of the metal hydroxide, eg:

Sn2+(aq) + 2OH-(aq) Sn(OH)2(s)

However, on addition of excess ammonia, or hydroxide ion, some metal hydroxides

dissolve by forming complex ions.

Zn(OH)2(s) + 4NH3(aq) [Zn(NH3)4]2+ (aq) + 2OH-(aq)

Sn(OH)2(s) + 3OH-(aq) + 3H2O(l) [Sn(H2O)3(OH)3-](aq)

The metal ions Zn2+, Cu2+ and Pb2+ form complexes in solution with a coordination number
of 4. This means that four ligands are joined to the central metal ion to form complex ion
such as [Cu(NH3)4]2+. Zn2+ and Pb2+ can also form six-coordinate complexes.

Precipitation Reaction
Almost all salts of the alkali metals are soluble in water and strong electrolytes, but anions
such as phosphate, carbonate or oxalate form insoluble salts with most other cations. Some
such precipitates can be made to dissolve by changing the pH or by adding suitable ligands,
soluble complexes can be formed whose large formation constant overwhelms the small
solubility product of the original salt.
Silver halides are insoluble in water. They can be distinguished by the differing actions of
dilute and concentrated ammonia solutions, thereby furnishing tests for the presence of
halide ions.

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Apparatus:
Test tubes Droppers
Red litmus paper Pipette

Materials:
1 M hydrochloric acid Potassium chloride
4 M ammonia solution Manganese(II) chloride
2 M sodium hydroxide Magnesium chloride
Zinc nitrate Calcium chloride
Copper(II) sulphate Trisodium phosphate

Caution:
Cleanliness of test tubes is essential.

Procedures:
Part A: Complex formation
1. Label two test tubes and add 4 M ammonia solution into respective test tubes of 0.5
cm3 of dilute zinc nitrate and copper(II) sulphate solutions drop wise until each is just
alkaline (test with red litmus paper).
2. Add more ammonia solution, and observe if there is any precipitate dissolves.
3. Repeat step 1 and 2 by using 2 M sodium hydroxide in place of ammonia solution.

Part B: Phosphate precipitation reaction

1. Label five test tubes and add 1 cm3 of each solution (potassium chloride, manganese(II)
chloride, magnesium chloride, calcium chloride and copper(II) sulphate) into
respective test tubes.
2. Add 1 cm3 of trisodium phosphate solution to each of the test tubes and shake. Observe
for any precipitation and record in the table.
3. Add a few drops of 1 M HCl to any test tube with precipitate formed and shake.
Note: The precipitates are not necessarily phosphates. Some precipitates are due to
hydrolysis of the anion in solution.

Results:

Part A: Complex formation

Observations

Limited NH3 Excess NH3

Zn(NO3)2

CuSO4

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Observations

Limited NaOH Excess NaOH

Zn(NO3)2

CuSO4

Part B: Phosphate precipitation reaction

Observations

KCl

MnCl2

MgCl2

CaCl2

CuSO4

Questions:
1. Explain briefly each of the reactions involved.

2. Write down appropriate equation(s) to describe your observations.

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Experiment 9
________________________________________________________________________
Title: Identification of Unknown Metal Ions

Aim:
To identify the presence of unknown metal ions in series of solutions.

Introduction:
Common metallic cations can be separated from one another and identified by using
qualitative analysis. During analysis, inferences can be made on the colour, solubility, the
effect of heat on the salt, the type of gas given out, reaction with other reagents and
confirmatory test. When the unknown cation has been identified, equations should be
added to support the conclusions.

Colours of common cation solutions:

Colourless Blue Yellow Pink Green

Ag , Pb , Ca Ba , Cu2+
+ 2+ 2+, 2+ Fe3+, Cr3+ Co2+, Mn2+ Ni2+, Fe2+
Zn2+, Mg2+, Cd2+ (very pale) (pale)

The cations supplied belong to four main groups:

Group 1: Cations whose chlorides are relatively insoluble

Group 2: Cations whose sulfates are relatively insoluble

Group 3: Cations which form soluble amine complexes in excess ammonia (at a pH of
approximately 10)

Group 4: Cations which form insoluble metal hydroxides in a solution of excess ammonia
at pH10

Apparatus:
Test tubes Dropper
Centrifuge tubes Centrifuge
Water bath

Materials:
6 M ammonia solution Silver nitrate, AgNO3
6 M hydrochloric acid Barium nitrate, Ba(NO3)2
6 M sulphuric acid Iron(III) nitrate, Fe(NO3)3
1 M hydrogen peroxide Chromium(III) nitrate, Cr(NO3)3
Ethanol Copper(II) nitrate, Cu(NO3)2

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Safety Precautions:
• Safety glasses must be worn at all times.
• Most of the metal ions used are poisonous. Do not throw residues containing metal ions
or sulfides down the sink. Containers are provided in the fume cupboards for such
residues.
• When heating any acid always heat cautiously and do not allow any vigorous reaction
to occur.
• Do not take the test tubes away from fume hood until the reaction has ceased
completely.
• All test tubes used for tests should be cleaned thoroughly.

Procedures:
1. In a set of 5 clean test tubes, add each of them with 1 cm3 of one unknown solutions.
Label the test tubes A - E.
2. Add 4 drops of 6 M HCl to each test tube. Mix the solutions thoroughly. Record your
observations about precipitation (if any) and colors.
3. Follow the flow chart illustrated in the next page for further investigations.

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Unknown metal ions

(Ag+, Ba2+, Fe3+, Cr3+, Cu2+)

Add 4 drops of 6 M HCl

and mix thoroughly

Precipitate Solution
Insoluble Chloride Add 1cm3 of ethanol, 2 drops of 6 M
H2SO4 and stand for 5 minutes.
Group: Ag+
Group: Ba2+, Fe3+, Cr3+, Cu2+

Precipitate Solution
Insoluble sulphate - Boil (in water bath) to expel ethanol.
- Add 2 cm3 of 6 M NH3.
Group: Ba2+
Subgroup: Fe3+, Cr3+, Cu2+

Precipitate Solution
Insoluble hydroxide Soluble amine

Subgroup: Fe3+, Cr3+ Subgroup: Cu2+

- Centrifuge and discard supernatant.

- Add 6 drops – 1 cm3 of 1 M H2O2. Stir
thoroughly and place in a boiling water
bath for 5 – 10 minutes.

Some or all precipitate dissolves to Precipitate remains, no colour change.

give a yellow supernatant solution. Fe present
Cr present as H2CrO4

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Results:

Qualitative Tests for the Individual Ion Solutions – Observations

Ion Chloride test Ethanol test NH3 test H2O2 test Possible ion
(HCl)
A

Questions:
1. Write down all the balanced equations involved.

2. Describe briefly the reactions involved.

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Mini Project
________________________________________________________________________
Poster Presentation (Nitrogen and its Compounds)

Objective:
To conduct a poster presentation on topics related to the element nitrogen and its
compounds.

Description:
The poster presentation is to be carried out in a group of 5 members. Students are required
to select a title based on issues/ research findings/ innovations, etc. related to nitrogen and/
or its compounds. Students are encouraged to look into topics beyond what is discussed in
the lecture notes. Students are required to register their title with their lecturer to avoid an
overlap within the class.

The titles selected must be related to nitrogen and/ or its compounds. Some examples are
listed below:
1. Uses of nitrogen
2. Forms of nitrogen in soil
3. Nitrogenous fertilisers
4. Nitrogen compounds as pollutants
5. How do nitrates and phosphates affect water quality?
6. Food products made with liquid nitrogen

Each group is tasked to prepare a A3 sized poster (landscape or portrait orientation) on the
title selected. Font type is Times New Roman (justified) and font size is 24. Students
should provide at least three (3) references from different sources. Wikipedia is not reliable
source to cite in scientific academic writing.

Students are required to present their poster by conducting a 15 minutes presentation (10
minutes for presentation and 5 minutes for Q&A). Students will be penalised if plagiarism
is detected.

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Learning outcome:
The learning outcomes that can be evaluated through this assessment include:
(i) To show coherent understanding and appreciation of nitrogen and its compounds
by articulating scientific knowledge on the particular topic.
(ii) To analyse and evaluate scientific information from a wide range of
sources/references.
(iii) To design scientific poster by use of electronic equipment and design software.
(iv) To demonstrate scientific presentation skills by communicating information and
responding effectively.
(v) To practice teamwork and complementary skills of collaborative learning.

Task Schedule:
Time (Week) Activities
2 Briefing and forming group by lecturer
3 Registration of title with lecturer
4-6 Preparation of Poster
5 Draft (optional)
7 Submission of poster
10 Poster Presentation

Marking Scheme Guideline:

Group Assessment (Total: 18 marks)
Poster:
Content
Visual Clarity & Appeal
Scientific Terms & Language
Originality & Creativity of Topic
Presentation:
Organisation
Audience Impact
Time Management & Teamwork

Individual Assessment (Total: 12 marks)

Content Knowledge
Scientific Terms & Language
Voice

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