PRACTICAL 3

Purpose: To determine the cation and anion in an unknown salts

Materials: Substance Y, distilled water, litmus paper, wooden splint, matches,
barium nitrate solution, dilute nitric acid, sodium hydroxide solution,
ammonia solution, dilute sulphuric acid, ferum (II) sulphate, potassium
hexacyanoferrate(II) solution.
Apparatus: 100 cm3 beaker, glass rod, test tube, test tube rack, boiling tube,
spatula, bunsen burner, dropper, litmus paper, wooden splint
Procedure: Y is a soluble salts. Carry out the following test on Y. Record the
observations and inferences in Table 1. Indentify one cation and anion
in Y.

Observation and Inference:

Table 1: Observation and inference based on tests conducted on Y
Test Observation Inference
a  No reaction  Dissolved salts
Mix a small amount of Y mixture  Produced
with distilled water in a test tube. colourless mixture
Divide the solution to four
portions
i) Add the first portion with  Colourless  Nitrate ion might
barium nitrate, followed by  No change presence
dilute nitric acid.  No reaction

ii) Add the second portion with  White precipitate  Zinc ion is
sodium hydroxide solution  Dissolve in excess presence
 Colourless when  Zn(OH4)2- formed
excess  Heat produced

iii) Add to the third portion with  Cloudy  Aluminium ion,

ammonia solution  Turn colourless in Lead ion is no
excess presence
 Zinc ion is
presence
 Tetraaminezinc(II)
formed
iv) Add to the forth portion with  White precipitate  Zinc ion presence
potassium hexacyanoferrate formed
(II) solution

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 b Heat a small amout of substance  White and yellow  Its shows acidic
Y in a boiling tube. solution formed gas nature
 Brown gas with a  Nitrogen and
Test any gas release from the pungent smell oxygen were
reaction produced presence
 Lighting wooden
splinter burned
 Moist blue litmus
paper turned into
red
c Add dilute sulphuric acid and  When H2SO4 was  Nitrate ion was
iron (II) sulphate to a solution of added, there was presence
substance Y no change  Nitrosonium
Then add concentrated sulphuric  When FeSO4 was complex
slowly added, two layer [Fe(H2O)5NO]SO4
was formed was formed
 Then, when
concentrated
H2SO4 was added
brown ring was
formed

Disscusion:
This experiment was conducted to identify the cation and anion of
substance Y. Before the experiment, substance Y was mix with distilled water and
stir in order to dissolved substance Y. Then mixture Y is divided into 4 portion.

For the first test, barium nitrate was added and followed by adding dilute nitric
acid. The observation for the first test is there is no change occurs and no precipitate
formed inside the the test tube. Dilute nitric acid was added to acidify the test
solution. Nitric might presence in mixture Y.

Next, the second experiment, sodium hydroxide is added. Based on the

observation, a white precipitate is formed.

Zn2+ + 2 OH− → Zn(OH)2.

Zn2+(OH2)4(aq) + OH−(aq) → Zn2+(OH2)3OH−(aq) + H2O(l)

But when excess of sodium hydroxide was added, the white precipitate gone and
became colourless. The reaction produce heat.

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 Zn(OH)2 + 2 OH− → Zn(OH)42−.

When the white precipitate formed, this shows that there sign of zinc ion presence in
substance Y. Zincate ion was formed when excess sodium hydroxide solution was
added into the test tube. The heat produced is because it is an exothermic reaction.

The third portion was test by adding ammonia solution into the test tube. The
solution inside the test tube turn cloudy but when ammonia was added in excess, the
solution turn to colourless.

Zn2+(aq) + 2 NH3(aq) + 2 H2O(l)   Zn(OH)2(s) + 2 NH4+(aq)

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

(when excess ammonia is added)

Based on the observation, its shows that aluminium ion and lead ion is not presence
in the solution. But zinc ion was presence due to the formation of
Tetraamminezinc(II), [Zn(NH3)4]2+.

The fourth experiment was undergo by adding potassium hexacyanoferrate

(II) solution into the test tube. A white precipitate was formed when the potassium
hexacyanoferrate (II) solution was added. It can be conclude that zinc ion was
presence because zinc(II) is precipitated by potassium hexacyanoferrate ions as
K2Zn[Fe(CN)6] (white precipitate)

3Zn(NO3)2 + 2K4[Fe(CN)6] → K2Zn3[Fe(CN)6]2 + 6KNO3

For experiment B, substance Y was boil inside a boiling tube. Substance Y
turn to white and yellow solution. A brown gas with a pungent smell was release
during the boiling process. When the gas is test with a lighting wooden splinter, the
wooden splinter burned. Blue litmus paper was used to measure the acidic level of
the gas. The blue litmus paper turn to red. Based on the observation, the lighting
wooden splinter was used to determine the presence of oxygen gas and other basic
gas. When the lighting wooden splinter burned, it shows that oxygen and nitrogen is
presence. This is because nitrogen is an inert gas while oxygen react with the flame
to make it continue burning. If the flame extinguishes, then there is no oxygen in the
tube, and the gas is one without any reactivity to fire, for example, nitrogen. Nitrogen

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gas has no reactivity to fire because it is inert. The blue litmus paper that change to
red shows that it has an acidic properties.

For the last experiment , dilute sulphuric acid and iron (II) sulphate was added
solution of substance then concentrated sulphuric was added slowly. When dilute
sulphuric acid, no reaction occur while iron(II) sulphate was added two layer of
solution of substance Y was formed. Then when concentrated sulphuric acid was
added, a brown ring was formed.

2HNO3+ 3H2SO4 + 6FeSO4 --->> 3Fe2(SO4)3 + 2NO + 4H2O

[Fe(H2O)6]SO4 + NO = [Fe(H2O)5(NO)]SO4+ H2O

The brown ring indicate the presence of nitrate ion. The overall reaction is the
reduction of the nitrate ion by iron(II) which is oxidised to iron(III) and formation of a
nitrosonium complex. Plus due to the sulphuric acid being denser than the solution in
which the acid of the concentrated sulphuric acid will sinks to the bottom of the
mixture of iron(II) sulphate and a suspected nitrate solution. The brown ring is due to
the formation of iron(ii) suplhate - nitrogen (ii) complex, FeSO4.NO or Nitroso iron(ii)
complex.

Question:

1) Write a balanced ionic equation for the reaction involved in test (a) (iv)?
3Zn(NO3)2 + 2K4[Fe(CN)6] → K2Zn3[Fe(CN)6]2 + 6KNO3

2) Explain why substance Y needs to be heated in test (b)?

Substance Y was heated in test (b) is to change it state into gas state so the gas
produce can be test to detect the presence of basic gas and oxygen. As the
temperature increase, the molecule in solid state gain more energy and break it
chains to became liquid and further same goes to the process from liquid to gas.

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3) Explain how gas released in test (b) can be tested ?
The gas released was test (b) by putting a lighting wooden splinter at the mouth
of the boiling tube. Oxygen gas is a combustion gas. So a lighting wooden
splinter was place at the mouth of the test tube. While for nitrogen gas, it can be
detected by presence of brown gas with a pungent smell

4) Explain why concentrated sulphuric acid need to be add slowly ?

Concentrated sulphuric acid was needed to be add slowly because to allowed the
sulphuric acid to formed a layer under the aqueous solution without disturbing
solution of substance Y
5) Predict what will happen in a solution of substance Y is added sodium
carbonate? Write a balanced ionic equation for the reaction involved.
The reaction of substance Y when reacts with sodium carbonate is will produced
a white precipitate of sodium nitrate and zinc carbonate.
Na2CO3 (aq) + Zn(NO3)2 (aq) --> 2NaNO3(aq) + ZnCO3 (s)

Precaution Steps:

a) All apparatus is rinsed with distilled water first before starting the experiment.
b) Be careful when handling with concentrated sulphuric acid .
c) Wash our hand after finishing the experiment to avoid any injured or poisoning
occur to ourself
d) Do not inhale the nitrogen gas release because it is toxic.

Conclusion:

In conclusion, the unknow salts Y is a soluble zinc nitrate salts

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References

Ooi Yong Seang & Darric Lim. (2014). Spotlight Galaksi SPM : Kimia. Selangor : Pan
Asia Publications Sdn. Bhd.

Rowley, S. P. (2011). General Chemistry I Laboratory Manual (2nd ed.). Kendall

Hunt.

Yeap Tok Kheng. (2012). Esensi Kimia SPM. Kuala Lumpur : Pearson Sdn. Bhd.

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Appendix

(Formation fo Brown Ring test (c))

(Solution of substance Y became cloudy in test (a)(iii))

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( In test a)((iii), the solution became colourless after excess ammonia is added)

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(All of the test tube of experiment A)