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October 22, 2014

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Topic: Qualitative Analysis
Title: Cation Analysis
Aim: To identify cations in a solution
Apparatus:
Test tubes, test tube holders, beakers, droppers, Bunsen burner, nichrome wire, test tube washer, tongs
Materials:
Diluted HCl, Conc. HCl, 3M Aqueous NaOH, 3M Aqueous NH
4
OH, Na
+
, K
+
, Mg
2+
, Ca
2+
, Ba
2+
, Cu
2+
, Al
3+
,
Pb
2+
, Cr
2+
,Mn
2+
, Fe
2+
, Fe
3+
, Zn
2+
, NH
4
+

Flame Test
Na
+

Test: A clean nichrome wire was dipped in a white crystalline salt and held over a Bunsen flame. The colour of
the flame was observed.
Observation: A bright yellow-orange coloured flame was observed.
Interpretation: As the metal is heated valence electrons absorb the energy and is promote to move from a
lower quantum (energy) level to a higher quantum level and then radiation is emitted as the electron falls back
to a lower quantum level. A bright yellow flame is indicative of Na
+
is visible in the electromagnetic spectrum
with a wavelength of approximately 560-600 nm.
K
+
Test: A clean nichrome wire was dipped in a white powdery salt and held over a Bunsen flame. The colour of
the flame was observed.
Observation: A lilac coloured flame was observed.
Interpretation: As the metal is heated valence electrons absorb the energy and is promote to move from a
lower quantum (energy) level to a higher quantum level and then radiation is emitted as the electron falls back
to a lower quantum level. A lilac flame is indicative of K
+
is visible in the electromagnetic spectrum with a
wavelength of approximately 450-480 nm.
Ca
2+

Test: A clean nichrome wire was dipped in a white powdery salt and held over a Bunsen flame. The colour of
the flame was observed.
Observation: A red-orange coloured flame was observed.
Interpretation: As the metal is heated valence electrons absorb the energy and is promote to move from a
lower quantum (energy) level to a higher quantum level and then radiation is emitted as the electron falls back
to a lower quantum level. A red-orange flame is indicative of Ca
2+
is visible in the electromagnetic spectrum
with a wavelength of approximately 600-700 nm.
Ba
2+

October 22, 2014

2

Test: A clean nichrome wire was dipped in a white crystalline salt and held over a Bunsen flame. The colour of
the flame was observed.
Observation: A green flame was observed.
Interpretation: As the metal is heated valence electrons absorb the energy and is promote to move from a
lower quantum (energy) level to a higher quantum level and then radiation is emitted as the electron falls back
to a lower quantum level. A green flame is indicative of Ba
2+
is visible in the electromagnetic spectrum with a
wavelength of approximately 450-560 nm.
Cu
2+

Test: A clean nichrome wire was dipped in a blue crystalline salt and held over a Bunsen flame. The colour of
the flame was observed.
Observation: A blue-green flame was observed.
Interpretation: As the metal is heated valence electrons absorb the energy and is promote to move from a
lower quantum (energy) level to a higher quantum level and then radiation is emitted as the electron falls back
to a lower quantum level. A blue-green flame is indicative of Cu
2+
is visible in the electromagnetic spectrum
with a wavelength of approximately 480-560 nm.

Systematic Tests
Mg
2+

Test with NaOH
(aq)

Approximately 2cm
3
of Mg
2+
(aq)
solution was poured in a test tube. Diluted NaOH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NaOH
(aq)
was then
added in excess and reaction observed.
Observation
Dropwise
At the 1
st
drop of NaOH
(aq)
a white precipitate (ppt) was observed. The ppt increased as the drops of NaOH
(aq)

increased.
Excess
Precipitate remained in excess of NaOH
(aq)

Interpretation
Mg
2+
(aq)
+ 2OH
-

(aq)
Mg(OH)
2(s)


The presence of the white ppt is indicative of a sparingly soluble Mg(OH)
2(s)
. Mg(OH)
2(s)
is not amphoteric
which is why it did not dissolve in excess NaOH
(aq).

Test with NH
4
OH
(aq)
October 22, 2014

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Approximately 2cm
3
of Mg
2+
(aq)
solution was poured in a test tube. Diluted NH
4
OH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NH
4
OH
(aq)
was then
added in excess and reaction observed.
Observation
Dropwise
At the 3
rd


drop of NH
4
OH
(aq)
a white precipitate (ppt) was observed. The ppt increased as the drops of
NH
4
OH
(aq)
increased.
Excess
Precipitate remained in excess of NH
4
OH
(aq)

Interpretation
Mg
2+
(aq)
+ 2OH
-
(aq)
Mg(OH)
2(s)

The presence of the white ppt is indicative of a sparingly soluble Mg(OH)
2(s)
. Mg(OH)
2(s)
is not amphoteric
which is why it did not dissolve in excess NH
4
OH
(aq)


Ca
2+
Test with NaOH
(aq)

Approximately 2cm
3
of Ca
2+
(aq)
solution was poured in a test tube. Diluted NaOH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NaOH
(aq)
was then
added in excess and reaction observed.
Observation
Dropwise
At the 1
st
drop of NaOH
(aq)
a white precipitate (ppt) was observed. The ppt increased as the drops of NaOH
(aq)

increased.
Excess
Precipitate remained in excess of NaOH
(aq)

Interpretation
Ca
2+
(aq)
+ 2OH
-

(aq)
Ca(OH)
2(s)


The presence of the white ppt is indicative of a sparingly soluble Ca(OH)
2(s)
. Ca(OH)
2(s)
is not amphoteric
which is why it did not dissolve in excess NaOH
(aq).

Test with NH
4
OH
(aq)
Approximately 2cm
3
of Ca
2+
(aq)
solution was poured in a test tube. Diluted NH
4
OH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NH
4
OH
(aq)
was then
added in excess and reaction observed.
October 22, 2014

4

Observation
Dropwise
At the 3
rd


drop of NH
4
OH
(aq)
a smell of ammonia was noted, no ppt was observed. There was no ppt was
observed as the drops increased.
Excess
No ppt observed in excess of NH
4
OH
(aq)
. Strong smell of ammonia observed.

Interpretation
Ca
2+
(aq)
+ 2OH
-
(aq)
Ca(OH)
2(aq)

No ppt suggests that Ca(OH)
2(aq)
is soluble in excess NH
4
OH
(aq)
. The smell of Ammonia indicates that the
NH
4
+
(g
was being released as the CaOH was being formed.

Ba
2+
Test with NaOH
(aq)

Approximately 2cm
3
of Ba
2+
(aq)
solution was poured in a test tube. Diluted NaOH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NaOH
(aq)
was then
added in excess and reaction observed.
Observation
Dropwise
At the 1
st
drop of NaOH
(aq)
no precipitate (ppt) was observed. At the 3
rd
drop a faint white ppt was formed.
Precipitate increased as the drops of NaOH
(aq)
increased.
Excess
Precipitate remained in excess of NaOH
(aq)

Interpretation
Ba
2+
(aq)
+ 2OH
-
(aq)
Ba(OH)
2(s)


Barium has a slightly unsoluble hydroxide, which is why it took much longer for a precipitate to be formed in
the NaOH
(aq)
Test with NH
4
OH
(aq)
Approximately 2cm
3
of Ba
2+
(aq)
solution was poured in a test tube. Diluted NH
4
OH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NH
4
OH
(aq)
was then
added in excess and reaction observed.
Observation
October 22, 2014

5

Dropwise
No ppt was formed, no changes observed.
Excess
No ppt observed in excess of NH
4
OH
(aq)
.
Interpretation
Ba
2+
(aq)
+ 2OH
-
(aq)
Ba(OH)
2(aq)


Barium is slightly unsoluble.
Al
3+

Test with NaOH
(aq)

Approximately 2cm
3
of Al
3+
(aq)
solution was poured in a test tube. Diluted NaOH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NaOH
(aq)
was then
added in excess and reaction observed.
Observation
Dropwise
At the 1
st
drop of NaOH
(aq)
a white precipitate (ppt) was observed. Precipitate increased as the drops of
NaOH
(aq)
increased.
Excess
Precipitate dissolves in excess of NaOH
(aq)

Interpretation
Al
3+
(aq)
+ 3OH
-
(aq)
Al(OH)
3(s)

Aluminium is redissolves in excess NaOH to form a complex ion Al(OH)
-
4
.
Al(OH)
3(s)
+ OH

(aq)
[Al(OH)
4
]

(aq)

This indicates that the Aluminium hydroxide displayed amphoteric behaviour.


Test with NH
4
OH
(aq)
Approximately 2cm
3
of Al
3+
(aq)
solution was poured in a test tube. Diluted NH
4
OH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NH
4
OH
(aq)
was then
added in excess and reaction observed.
Observation
Dropwise
At 1
st
drop a white ppt was formed. Precipitate remained as drops increased.
October 22, 2014

6

Excess
Precipitate observed in excess of NH
4
OH
(aq)
.
Interpretation
Al
3+
(aq)
+ 3OH
-
(aq)
Al(OH)
3(s)


Al(OH)
3
is sparingly soluble in excess NH
4
OH
(aq)
.

Test with dilute HCl
(aq)
Approximately 2cm
3
of Al
3+
(aq)
solution was poured in a test tube. Diluted HCl
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. HCl
(aq)
was then added in
excess and reaction observed.
Observation
Dropwise
At 1
st
drop no change was observed. No change was observed as the drops were increased.
Excess
No change observed in excess dilute HCl
(aq)
.
Interpretation
2Al
3+
(aq)
+ 6Cl
-
(aq)
2AlCl
3(aq)


Al
3+

is soluble in excess dilute HCl
(aq).


Pb
2+
Test with NaOH
(aq)

Approximately 2cm
3
of Pb
2+
(aq)
solution was poured in a test tube. Diluted NaOH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NaOH
(aq)
was then
added in excess and reaction observed.
Observation
Dropwise
At the 1
st
drop of NaOH
(aq)
a white precipitate (ppt) was observed. Precipitate increased as the drops of
NaOH
(aq)
increased.
Excess
Precipitate dissolves in excess of NaOH
(aq)

Interpretation
October 22, 2014

7

Pb
2+
(aq)
+ 2OH
(aq)
Pb(OH)
2(s)


Lead is redissolves in excess NaOH to form a complex ion Pb(OH)
2
-2
.
Pb(OH)
2(s
+ OH

(aq)
[Pb(OH)
2
]
2
(aq)

This indicates that the Lead hydroxide displayed amphoteric behaviour.


Test with NH
4
OH
(aq)
Approximately 2cm
3
of Pb
2+
(aq)
solution was poured in a test tube. Diluted NH
4
OH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NH
4
OH
(aq)
was then
added in excess and reaction observed.
Observation
Dropwise
At 1
st
drop a white ppt was formed. Precipitate remained as drops increased.
Excess
Precipitate observed in excess of NH
4
OH
(aq)
.
Interpretation
Pb
2+
(aq)
+ 2OH
-
(aq)
Pb(OH)
2(s)


Pb(OH)
2
is sparingly soluble in excess NH
4
OH
(aq)
.

Test with dilute HCl
(aq)
Approximately 2cm
3
of Pb
2+
(aq)
solution was poured in a test tube. Diluted HCl
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. HCl
(aq)
was then added in
excess and reaction observed.
Observation
Dropwise
At 1
st
drop white ppt. Precipitate increased as the drops were increased.
Excess
White ppt observed in excess dilute HCl
(aq)
.When left alone the ppt settled at the base of the test tube.
Interpretation
Pb
2+
(aq)
+ 2Cl
-
(aq)
PbCl
2(aq)


Pb
2+

is sparingly soluble in excess dilute HCl
(aq).


October 22, 2014

8

Cr
3+
Test with NaOH
(aq)

Approximately 2cm
3
of Cr
3+
(aq)
solution was poured in a test tube. Diluted NaOH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NaOH
(aq)
was then
added in excess and reaction observed.
Observation
Dropwise
At the 1
st
drop of NaOH
(aq)
a green-grey precipitate (ppt) was observed. Precipitate increased as the drops of
NaOH
(aq)
increased.
Excess
Precipitate dissolves in excess of NaOH
(aq)

Interpretation
2Cr
3+
(aq)
+ 6OH
-
(aq)
2Cr(OH)
3(s)


Cr(OH) is redissolves in excess NaOH to form a complex ion [Cr(OH)
6
]
-3
.
Cr(OH)
3(s)
+ 3OH
-
(aq)
[Cr(OH)
6
]
-3
(aq)

This indicates that the Cr(OH) displayed amphoteric behaviour.


Test with NH
4
OH
(aq)
Approximately 2cm
3
of Cr
3+
(aq)
solution was poured in a test tube. Diluted NH
4
OH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NH
4
OH
(aq)
was then
added in excess and reaction observed.
Observation
Dropwise
At 1
st
drop a grey-green ppt was formed. Precipitate increased as drops increased.
Excess
Precipitate observed in excess of NH
4
OH
(aq)
.
Interpretation
Cr
3+
(aq)
+ 3OH
-
(aq)
Cr(OH)
3(s)

Cr(OH)
3
is sparingly soluble in excess NH
4
OH
(aq)
.

Mn
2+
October 22, 2014

9

Test with NaOH
(aq)

Approximately 2cm
3
of Mn
2+
(aq)
solution was poured in a test tube. Diluted NaOH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NaOH
(aq)
was then
added in excess and reaction observed.
Observation
Dropwise
At the 1
st
drop of NaOH
(aq)
an off-white precipitate (ppt) was observed. Precipitate increased as the drops of
NaOH
(aq)
increased.
Excess
Precipitate remains in excess of NaOH
(aq)
. Precipitate quickly turned brown and then dark brown.
Interpretation
Mn
2+
(aq)
+ 2OH
-
(aq)
Mn(OH)
2(s)

MnOH is sparingly soluble in excess NaOH. The MnOH oxidized to Managanese (III) oxide to Mn
2
O
3
and then
to Managanese (IV) Oxide MnO
2
.

Test with NH
4
OH
(aq)
Approximately 2cm
3
of Mn
2+
(aq)
solution was poured in a test tube. Diluted NH
4
OH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NH
4
OH
(aq)
was then
added in excess and reaction observed.
Observation
Dropwise
At 1
st
drop a light brown ppt was formed. Precipitate increased as drops increased.
Excess
Precipitate observed in excess of NH
4
OH
(aq)
. The ppt slowly turned darker the longer the solution remained in
the air.
Interpretation
Mn
2+
(aq)
+ 2OH
-
(aq)
Mn(OH)
2(s)

Mn(OH)
2
is sparingly soluble in excess NH
4
OH
(aq)
. The ppt turned darker due to oxidation taking place.

Fe
2+
Test with NaOH
(aq)

October 22, 2014

10

Approximately 2cm
3
of Fe
2+
(aq)
solution was poured in a test tube. Diluted NaOH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NaOH
(aq)
was then
added in excess and reaction observed.
Observation
Dropwise
At the 1
st
drop of NaOH
(aq)
an green precipitate (ppt) was observed. Precipitate increased as the drops of
NaOH
(aq)
increased.
Excess
Precipitate became darker and was slightly gel-like in excess of NaOH
(aq)
.
Interpretation
Fe
2+
(aq)
+ 2OH
-
(aq)
Fe(OH)
2(s)


Fe(OH)
2(s)
is sparingly soluble in excess NaOH. The Fe(OH)
2(s)
oxidized to form Fe(OH)
3
which resulted in
the ppt becoming darker and gel-like.

Test with NH
4
OH
(aq)
Approximately 2cm
3
of Fe
2+
(aq)
solution was poured in a test tube. Diluted NH
4
OH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NH
4
OH
(aq)
was then
added in excess and reaction observed.
Observation
Dropwise
At 1
st
drop no ppt was formed. By the 5
th
drop a green ppt started to form. Precipitate increased as drops
increased.
Excess
Brown ppt observed in excess of NH
4
OH
(aq)
.
Interpretation
Fe
2+
(aq)
+ 2OH
-
(aq)
Fe(OH)
2(s)

Fe(OH)
2
is sparingly soluble in excess NH
4
OH
(aq)
. The ppt turned darker due to oxidation taking place to form
Fe(OH)
3
.
Fe
3+
Test with NaOH
(aq)

Approximately 2cm
3
of Fe
3+
(aq)
solution was poured in a test tube. Diluted NaOH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NaOH
(aq)
was then
added in excess and reaction observed.
October 22, 2014

11

Observation
Dropwise
At the 1
st
drop of NaOH
(aq)
a dark brown precipitate (ppt) was observed. Precipitate increased as the drops of
NaOH
(aq)
increased to give a gel-like red-brown ppt.
Excess
Precipitate remains in excess of NaOH
(aq)

Interpretation
2Fe
3+
(aq)
+ 6OH
-
(aq)
2Fe(OH)
3(s)


Fe(OH)
3
is remains in excess NaOH indicating that the hydroxide is sparingly soluble.


Test with NH
4
OH
(aq)
Approximately 2cm
3
of Fe
3+
(aq)
solution was poured in a test tube. Diluted NH
4
OH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NH
4
OH
(aq)
was then
added in excess and reaction observed.
Observation
Dropwise
At 1
st
drop a brown ppt was formed. Precipitate increased as drops increased.
Excess
Precipitate observed in excess of NH
4
OH
(aq)
.
Interpretation
Fe
3+
(aq)
+ 3OH
-
(aq)
Fe(OH)
3(s)

Fe(OH)
3
is sparingly soluble in excess NH
4
OH
(aq)
.

Zn
2+
Test with NaOH
(aq)

Approximately 2cm
3
of Zn
2+
(aq)
solution was poured in a test tube. Diluted NaOH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NaOH
(aq)
was then
added in excess and reaction observed.
Observation
Dropwise
October 22, 2014

12

At the 1
st
drop of NaOH
(aq)
a white precipitate (ppt) was observed. Precipitate increased as the drops of
NaOH
(aq)
.
Excess
Precipitate redissolves in excess of NaOH
(aq)
. Colour change from white to transparent.
Interpretation
Zn
2+
(aq)
+ 2OH
-
(aq)
Zn(OH)
2(s)


Zn(OH)
2
dissolves in excess NaOH indicating that the hydroxide is soluble and formed a complex ion.

Zn(OH)
2(s)
+ 2OH

(aq)
[Zn(OH)
4
]
-2
(aq)

Test with NH
4
OH
(aq)
Approximately 2cm
3
of Zn
2+
(aq)
solution was poured in a test tube. Diluted NH
4
OH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NH
4
OH
(aq)
was then
added in excess and reaction observed.
Observation
Dropwise
At 1
st
drop a white ppt was formed. Precipitate increased as drops increased.
Excess
Precipitate redissolved in excess of NH
4
OH
(aq)
. Colour changed from white to transparent.
Interpretation
Zn
2+
(aq)
+ 2OH
-
(aq)
Zn(OH)
2(s)

Zn(OH)
2
redissolved in excess NH
4
OH
(aq)
indicating that the hydroxide is soluble and formed a complex ion.

Zn(OH)
2(s)
+ 4NH
3

(aq)
[Zn(NH
3
)
4
]
2+
(aq)
+ 2OH
-
NH
4
+
Test with NaOH
(aq)

Approximately 2cm
3
of NH
4
+
(aq)
solution was poured in a test tube. Diluted NaOH
(aq)
was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NaOH
(aq)
was then added
in excess and reaction observed. The combined solution was then heated until a reaction occurred.
Observation
No change was observed as the NaOH
(aq)
was added to the solution dropwise or in excess. As the solution was
heated a colourless gas was observed.
Interpretation
NH
4
+
(aq)
+ OH
-
Na
(aq)
+ NH
3
+ H
2
O
(l)

October 22, 2014

13


Sources of Error and Limitation
1. An exact measurement of each sample was not used.
2. Small amount of droplets of water were present in some test-tubes as they were washed after each cation
test.

Discussion
Qualitative analysis is used to identify the elements present in a substance. The compounds of the following
salts were tested, Mg
2+
- white crystal, Ca
2+
-white powder, Ba
2+
- fine white crystals, Al
3+
- medium white
crystals, Pb
2+
-white crystals, Cr
3+
- green powder, Mn
2+
- pink crystals, Fe
2+
-pale green crystals, Fe
3+
- orange
brown crystals, Zn
3+
- fine white crystals and NH
4
+
- fine white crystals. This confirms that transition metals
have a coloured salt or a coloured aqueous solution (Cr
3+
, Mn
2+
, Fe
2+
& Fe
3+
) For the Flame tests carried out the
presence of a flame colour is due to excitation of valence-shell electrons upon heating, followed by return of the
electrons with the emission of light to lower energy levels. Flame tests cannot be used for all elements, as not all
elements yield a measurable spectrum. Most metallic elements can be qualitatively analysed by using aqueous
NaOH and aqueous NH
4
OH. Precipitates in each reaction during the drop applications confirms the presence of
an insoluble (sparingly soluble) metal ion, the evidence of colour changes and smells are further indication of
which cation we are working with. For e.g. Mg
2+
- white ppt, Cr
2+
- grey-green ppt and Mn
2+
- light brown ppt to
name a few. The presence of precipitates in excess of the reagents indicates that the metal ion is neither
amphoteric nor soluble. For e.g. Mg
2+
and Fe
2+
. Metallic ions that redissolved in excess of the reagents such as
Al
3+
and Zn
2+
in NaOH exhibited amphoteric behaviour as both hydroxide dissolves in acids as well. Al
3+
and
Pb
2+
both form white ppt in NaOH
(aq)
, the precipitates are soluble in excess, while in NH
4(aq)
they are insoluble
in excess. As can be seen, Al
3+
and Pb
2+
give the same results. So, to differentiate between them, another
reaction must be considered. Pb
2+
will form a white precipitate with Cl
-
while Al
3+
will not. Two other cations
form white precipitates. Zn
2+
forms a white precipitate, which is soluble both in excess NaOH
(aq)
and NH
4(aq)
OH
and Ca
2+
forms a white precipitate which is insoluble in excess NaOH but does not form a precipitate when
treated with NH
4(aq)
OH. It should also be noted that the tests with HCl were exothermic reactions and all others
were endothermic.

Conclusion
It can be concluded that the aim of this experiment was achieved as it was possible to confirm the cations that
were present by using a Flame test for: Na
2+
, K
+
, Ca
2+
, Ba
2+
and Cu
2+
. Using diluted NaOH and diluted NH
4
OH
as reagents the following metals could be confirmed: Mg
2+
, Ca
2+
, Ba
2+
, Cr
3+
, Mn
2+
, Fe
2+
, Fe
3+
and Zn
2+
. A
further test with diluted HCl was able to confirm samples of Al
3+
and Pb
2+
. A heat test could confirm the
presence of Ammonium ion using NaOH.