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EXPERIMENT 3: INORGANIC QUALITATIVE ANALYSIS

OBJECTIVES

1. To understand and describe the procedures of qualitative analysis.

2. To know the difference between qualitative and quantitative analysis.

EXPERIMENTAL PROCEDURE

PART A

A. Appearance of compound

1. The colour and the shape of the solid iron (III) chloride (A), lead (II) nitrate (B) and
calcium carbonate (C) is identified.

B. Heating test

1. A half spatula of solid compound is put in a boiling tube. The compound is then
heated using Bunsen burner for about 10 to 15 minutes. The colour and the odour of
gas released is recorded.

C. Solubility with water

1. A half spatula of compound is placed in 2mL of distilled water in boiling tube and
shaken.

2. Another 3mL of distilled water is added if the compound does not dissolve. The
mixture is then shook and stirred.

3. If the amount is dissolved after a considerable stirring, the compound is soluble. If


some of the amount is dissolved, the compound is moderately soluble. If a very small
amount does not dissolve, the compound is considered as insoluble.
D. Reaction with nitric acid

1. A half spatula of solid compound is put in a boiling tube. 15 mL of nitric acid (1M)
is added to the compound and any reaction that occur is observed.

2. The mixture is kept for the reaction with sodium hydroxide and ammonia.

E. Reaction with sodium hydroxide

1. 1M of solution NaOH is added drop-wise to the solution. The mixture is shaken


until precipitate is formed. Any reaction happened is observed.

F. Reaction with ammonia

1. 3M of solution NH3 is added drop-wise to the solution. The mixture is shaken and
any reaction is observed.

PART B

The ions that present in the unknown compounds is predicted.

A. Cation identification test

Compound D

1. A half spatula of compound D is acidified with 2mL of acetic acid (6M).

2. 1 mL of 0.2M of sodium acetate solution is added.

3. 1 mL of dimethylgloxime solution is added and another 1 mL is added drop-wise.


Any colour changes is observed.
Compound E

1. A half spatula of compound E is acidified with 5 mL HNO3. The solution is tested


with litmus paper.

2. 0.1M NH4SCN solution is added drop-wise. Any changes of colour is observed.

B. Anion identification test

Compound F

1. A half spatula of compound F is acidified with 5 mL HNO3 (3M) in the test tube.
The solution is tested with litmus paper.

2. Half of the solution is poured in the centrifuge tube. 5 drops of 0.1M AgNO3 is
added until white precipitate is formed. The solution is then centrifuged and the
supernatant is removed.

3. 6M NH3 is added drop-wise to the precipitate with stirring until dissolved.

4. 6M HNO3 is added to the solution until white precipitate is formed.

Compound G

1. A half spatula of compound G is acidified with 10 mL H2SO4 (2M) in the boiling


tube.

2. One-half spatula full of solid FeSO4.7H2O is dissolved.

3. The solution is then cool with some ice for 20 minutes.

4. 0.5 mL of concentrated H2SO4 is added carefully by allowing it to flow down the


side of the tilted test tube.

5. The solution is allowed to sit undisturbed for 2 hours so that a definite layer is
formed by the sulphuric acid.
RESULT AND OBSERVATION

PART A

Qualitative Observation of compound

analysis A B C

Colour of Yellowish
White White
Appearance compound black

of compound Shape of
Powdery Crystal Fine powder
compound

Yellow gas is Orange gas is


Colour of gas No gas is
Heating test released released
released
Odour of gas Pungent smell Pungent smell

Solubility Moderately
Soluble Insoluble
with water soluble

No reaction No reaction Gas bubble is


Nitric acid
occur occur released

A crystal-like A powder-like
Sodium
No precipitate precipitate is precipitate is
Reaction with hydoxide
formed formed

White
Red precipitate
Ammonia precipitate is No precipitate
is formed
formed

PART B

Qualitative Observation
analysis D E F G

i) Blue
litmus paper
turns red
Green
colour of ii) Yellow
Cation
solution colour of
turns red solution
turns
reddish
brown

i) After
Identification
addition of
test i) Blue
concentrated
litmus
H2SO4, two
paper turns
layers of
red
solution is

Anion formed

ii) White iii) After 2


precipitate hours, the two
is formed layers become
after one
addition of light-brownish
HNO3 layer

DISCUSSION

In chemistry, qualitative analysis is the determination of the chemical


composition of a sample. It encompasses a set of techniques that provide
non-numerical information about a specimen. Qualitative analysis can tell whether an
atom, ion, functional group or compound is present or absent in a sample, but it does
not provide information about its quantity. Quantification of a sample is called
quantitative analysis. There are two main branches of qualitative analysis, which are
organic qualitative analysis and inorganic qualitative analysis. Organic analysis tends
to look at types of molecules, functional groups and chemical bonds, while inorganic
qualitative analysis focused on the elemental and ionic composition of a sample.

In this experiment, we held several tests on compounds that are known and
unknown. For known compounds, we held tests such as heating test,solubility with
water, reaction with nitric acid, sodium hyroxide and ammonia, whereas for the
unknown compound, there are two types of tests, which are cation and anion
identification test.

For the known compound, we put iron (III) chloride, lead(II) nitrate and calcium
carbonate into different boiling tube and conducted the test on the three compounds.
For heating test, all the compounds will form an oxide compound and release different
kind of gases. As for iron (III) chloride, it released yellow gas, which is chlorine gas
to form iron (III) oxide. As for lead (II) nitrate, it released orange gas, which is
nitrogen dioxide gas to form lead (II) oxide. While for calcium carbonate, it should
decompose into calcium oxide and carbon dioxide gas, but our sample had no changes
happened. For the solubility with water, iron (III) chloride is the most soluble in water,
followed by lead (II) nitrate which is moderately soluble, and calcium carbonate that
is insoluble in water. As for reaction with nitric acid, only calcium carbonate reacted,
with the release of gas bubbles, which is carbon dioxide gas. Next, reaction with
sodium hydroxide will produce hydroxide salt, which is an insoluble salt. Our
experiment resulted only iron (III) chloride and lead (II) nitrate that form precipitate
in the boiling tube. Lastly, reaction with ammonia resulted various result. For iron (III)
chloride, it produced red precipitate, which was iron (III) hydroxide whereas for lead
(II) nitrate, white precipitate formed, which was lead (II) hydroxide. As for calcium
carbonate, there was no precipitate because it produced calcium cyanide which is
soluble in water, that is why there were no precipitate formed.
Next, the cation identification test on compound D resulted the change of solution
colour from green to red after the addition of dimethlglyoxime solution. This indicates
that nickel ion is present in the compound. While for compound E, the yellow colour
solution changed to reddish brown after addition of ammonium thiocyanate that
indicates the presence of iron (III) ion.

Lastly, the anion identification for compound F resulted the formation of white
precipitate after the addition of nitric acid. This indicates the presence of chloride ion.
Whereas for compound G, the result of the experiment was a light brownish layer is
formed, that indicates that nitrate ion is present.

QUESTIONS

1. Write all the balance equations for each reaction and any observations.

PART A

A 4FeCl3 + 3O2 → 2Fe2O3 + 6Cl2

Heating test B 2Pb(NO3)2 → 2PbO +4NO2 +O2

C CaCO3 → CaO +CO2

A 2FeCl3 +3H2O → Fe2O3 + 6HCl

Solubility with B Pb(NO3)2 + H2O → Pb(OH)NO3 + HNO3


water
CaCO3 + H2O → no reaction
C
(insoluble in water)

A FeCl3 + HNO3 → no reaction

Reaction with
B Pb(NO3)2 + HNO3 → no reaction
nitric acid

C CaCO3 + 2HNO3 → Ca(NO3)2 + CO2 + H2O


A FeCl3 + 3NaOH → Fe(OH)3 +3NaCl
Reaction with
sodium B Pb(NO3)2 + 2NaOH → Pb(OH)2 +2NaNO3
hydroxide
C CaCO3 + 2NaOH → Ca(OH)2 +Na2CO3

A FeCl3 + NH3 + H2O → Fe(OH)3 + NH4Cl

Reaction with B Pb(NO3)2 +NH3 + H2O → Pb(OH)2 + NH4NO3


ammonia
CaCO3 +NH3 → CaCN2 + 3H2O
C
(soluble in water)

2. Identify the cations and anions for the unknown compounds.

PART B

Type of ion Compound Ions that present in the compound

D Nickel ion (Ni2+)


Cation
E Iron (II) ion (Fe3+)

F Chloride ion (Cl-)


Anion
G Nitrate ion (NO3-)

CONCLUSIONS

1. The procedures of qualitative analysis is understood and described, where quantity


is not something that measured.

2. The difference between qualitative and quantitative analysis is known, which is


quantity is not measured in the qualitative analysis.
REFERENCES

1. Helmenstine, A. M., (2017), Qualitative analysis definition,


https://www.thoughtco.com/definition-of-qualitative-analysis-604626

2. Wired Chemist, (2018), Qualitative analysis,


http://www.wiredchemist.com/chemistry/instructional/laboratory-tutorials/qualitative-
analysis