Objective

Upon completion of this experiment, students should be able to:

1. understand and describe the procedures of qualitative analysis
2. know the difference between qualitative and quantitative analysis
Procedure
Part A
a. Appearance of compound
1. We identified the colour and shape of the solid iron (III) chloride (A), lead (II) nitrate (B)
and calcium carbonate (C).
b. Heating Test
1. A half spatula of solid compound has been put in boiling tube. The compound was heat
using Bunsen burner (about 10 to 15 minutes). When a gas is given off, note the colour
and odour of the gas.
c. Solubility with water
1. A half spatula of compound was placed in 2 ml of distilled water in boiling tube and
shake.
2. We added another 3 ml of distilled water when the compound does not dissolve. We
shake and stir the mixture.
3. If the compound is soluble this amount will dissolve after considerable stirring. If the
compound is moderately soluble, some of this amount will dissolve. If the compound
is insoluble, even a very small amount will not dissolve.
d. Reaction with nitric acid
1. A half spatula of solid compound was placed in boiling tube. Then we add 15 ml of
nitric acid (1M) to the compound and we observed any reaction that occurs
2. We didnt throw the mixture. We keep the solution for the reaction with sodium
hydroxide and ammonia.
e. Reaction with sodium hydroxide
1. 1 M of solution NaOH drop wise was added to the solution (used solution from test
tube in reaction with nitric acid), we can stir or shake the solution until precipitate form.
We observed any reactions happen.
f. Reaction with ammonia
1. 3 M of solution NH3 drop wise was added to the solution (used solution from test tube
in reaction with sodium hydroxide), we stir or shake the solution and we observed any
reaction. We observe any reactions happen.
PART B:
i. Cation Identification Test
Compound D
1. A half spatula of compound D was acidifed with 2 ml of acetic acid (6 M).
2. 1 ml of 0.2 M of sodium acetate solution was added.
3. 1 ml of dimethylglyoxime solution was added and another 1 ml drop wise also added.
We observe any changes colour.
Compound E
1. A half spatula of compound E acidified with 5 ml HNO3 (3 M). The solution was tested
with litmus paper.
2. 0.1 M NH4SCN solution drop wise was added. We observe any changes colour.
ii. Anion Identification Test
Compound F
1. A half spatula of compound F with 5 ml HNO3 (3 M) was acidify in the test tube.T he
solution was tested with litmus paper.
2. A half of the above solution was poured in the centrifuge tube. Several drops of 0.1 M
AgNO3 was added until white precipitate forms. We centrifuge and remove the
supernatant.
3. A drop wise 6 M NH3 was added to the precipitate with stirring until dissolved.
4. 6 M HNO3 was added to the solution until white precipitate forms.
Compound G
1. A half spatula of compound G was added with 10 ml H2SO4 (2 M) in the boiling tube.
2. One-half spatula full of solid FeSO4.7H2O was dissolved.
3. We cool the solution with some ice for 20 minutes.
4. Carefully 0.5 ml of concentrated H2SO4 was added by allowing it to flow down the side
of the tilted test tube.
5. We allow the solution to sit undisturbed for 2 hours so that the sulphuric acid forms a
definite layer.
Result
Part A
a) Appearance of compound
Compound Observation
Iron(III) Chloride (A) Black powder and shiny
Lead(II) Nitrate (B) White crystals, solid, shine
Calcium carbonate (C) White powder

b) Heating Test
Compound Observation
A Gas release with brown colour
B Gas release with yellow colour
C No gas release
No reaction

c) Solubility in water
Compound Observation
A Not dissolve
B Moderately soluble
C Not dissolve

d) Reaction with nitric acid

Compound Observation
A No change(No reaction)
Colour change to light yellow
B Dissolve, High pressure, Low reaction
C Soluble

e) Reaction with sodium hydroxide

Compound Observation
A Precipitate formed but when shake its gone
B No reaction occur
C White precipitate cloudy

f) Reaction with ammonia

Compound Observation
A Precipitate formed
B No reaction occur
C No reaction occur
PART B
Cation Identification Test
Compound D Compound E
3 layer formed. (precipitate formed) different Orange solution formed.
colour

Anion Identification Test

Compound Red Litmus Paper Blue Litmus Paper Precipitate
F No change Change to red White precipitate
formed
G No change Change to red Dark green solution
formed
Question
1. Write all the balance equations for each reaction and any observations.
a) Appearance of compound
Compound Observation
Iron(III) Chloride (A) Black powder and shiny
Lead(II) Nitrate (B) White crystals, solid, shine
Calcium carbonate (C) White powder

b) Heating Test
Compound Observation
A Gas release with brown colour
B Gas release with yellow colour
C No gas release
No reaction

c) Solubility in water
Compound Chemical Equation
A 2FeCl3 + 3H2O → Fe2O3 + 6HCl
B Pb(NO3)2 + H2O → Pb(OH)NO3 + HNO3
C CaCO3 + H2O ↔ Ca(OH)2 + CO2

d) Reaction with nitric acid

Compound Observation
A FeCl2 + 4HNO3 → Fe(NO3)3 + NO2 + 2HCl + H2O
B Dissolve, High pressure, Low reaction
C FeCl2 + 4HNO3 → Fe(NO3)3 + NO2 + 2HCl + H2O
e) Reaction with sodium hydroxide
Compound Observation
A 3NaOH + FeCl3 → Fe(OH)3 + 3NaCl
B Pb(NO3)2 + 2 NaOH → Pb(OH)2 + 2 NaNO3
C 2NaOH+CaCO3 →CaOH+Na2CO3

f) Reaction with ammonia

Compound Observation
A FeCl3 + 3NH3 + 3H2O → Fe(OH)3 + 3NH4Cl
Source:
B 2 NH4OH + Pb(NO3)2 → Pb(OH)2 + 2 NH4NO3
C CaCO3 + 2NH3 CaCN2 + 3H2O

PART B
Cation Identification Test
Compound D Compound E
3 layer formed. (precipitate formed) different Orange solution formed.
colour

Anion Identification Test

Compound Red Litmus Paper Blue Litmus Paper Precipitate
F No change Change to red White precipitate
formed
G No change Change to red Dark green solution
formed
2. Identify the cations and anions for the unknown compounds.
Compound D can be predicted as Barium Ions since its produced 3 layer formed. The reaction
which add with dimetyhlglyoxime solution, that formed a red precipitate in the buffered acid
solution is Nickel (II) ion. The Fe3+ ion is readily identified in a dilute nitric acid solution
through the blood red color of its thiocyanate complex. A large excess of reagent should be
avoided.Compound E can be predicted as Fe3+ since its produced orange colour.
Fe3+ + SCN- ↔ FeSCN2+
Furthermore, chloride anion form in soluble silver salt. The colour of the precipitate is difficult
to observe and confirmatory test are necessary. Silver chloride the most soluble, dissolve as
readily in 6 M NH3 solution because of formation of the ammonia complex. When the solution
of the ammonia complex is acidified, AgCl reprecipitates.
Cl- (aq) + Ag+ (aq) AgCl(s)
AgCl (s) + 2NH3(aq) Ag(NH3)2+ (aq) + Cl- (.aq)
Ag(NH3)2+ (aq) + Cl- (aq) + 2H+ (aq) AgCl (s) + 2NH4+ (aq)
So, we can conclude that compound F is chloride ion.
Compound G can be predicted as nitrite ion which formed of colour Dark green solution
formed.
Discussion
In this experiment the formation of the precipitate in the solution after added precipitate reagent
showed the positive reaction of the metal cation .But there is also invisible product of reaction
occurred where we can also detect the presence of it in solution. There is some precaution that
should be aware .Firstly, when handling the chemicals the gloves must ware because the acid
used is a strong acid of HCl. Then , make sure the test tubes are clean from any other
contamination because it will make chemical reaction slow and incomplete .Don’t pour the
excess chemical back into its bottle because it might be contaminated.
Conclusion
As a conclusion the precipitation method is one way of qualitative analysis to identify the ion
present in the solution .The precipitation of salt gave various color especially for the transition
element because it have more than one oxidation number

Reference

(n.d.). Retrieved from https://www.sciencedirect.com/topics/chemistry/inorganic-anion

(n.d.). Retrieved from https://chemiday.com/en/reaction/3-1-0-1492

Comprehensive Experimental Chemistry. (1997).