Qualitative Analysis of Cations

October 22, 2014
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 NH4OH, Na+, K+, Mg2+, Ca2+, Ba2+, Cu2+, Al3+,
Pb2+, Cr2+,Mn2+, Fe2+, Fe3+, Zn2+, NH4+
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
Observation: A lilac coloured flame was observed.
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.
Ca2+
Test: A clean nichrome wire was dipped in a white powdery salt and held over a Bunsen flame. The colour of
Observation: A red-orange coloured flame was observed.
to a lower quantum level. A red-orange flame is indicative of Ca2+ is visible in the electromagnetic spectrum
Ba2+
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October 22, 2014
Test: A clean nichrome wire was dipped in a white crystalline salt and held over a Bunsen flame. The colour of
Observation: A green flame was observed.
to a lower quantum level. A green flame is indicative of Ba2+ is visible in the electromagnetic spectrum with a
wavelength of approximately 450-560 nm.
Cu2+
Test: A clean nichrome wire was dipped in a blue crystalline salt and held over a Bunsen flame. The colour of
Observation: A blue-green flame was observed.
to a lower quantum level. A blue-green flame is indicative of Cu2+ is visible in the electromagnetic spectrum
Systematic Tests
Mg2+
Test with NaOH(aq)
Approximately 2cm3 of Mg2+(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 1st 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
Mg2+(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 NH4OH(aq)
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October 22, 2014
Approximately 2cm3 of Mg2+(aq) solution was poured in a test tube. Diluted NH4OH(aq)was added to the solution
dropwise to the solution, the test tube was gently shaken until a reaction was observed. NH4OH(aq)was then
Observation
Dropwise
At the 3rd drop of NH4OH(aq)a white precipitate (ppt) was observed. The ppt increased as the drops of
NH4OH(aq) increased.
Excess
Precipitate remained in excess of NH4OH(aq)
Interpretation
Mg2+(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 NH4OH(aq)
Ca2+
Test with NaOH(aq)
Approximately 2cm3 of Ca2+(aq) solution was poured in a test tube. Diluted NaOH(aq) was added to the solution
Observation
Dropwise
At the 1st drop of NaOH(aq) a white precipitate (ppt) was observed. The ppt increased as the drops of NaOH(aq)
increased.
Excess
Interpretation
Ca2+(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 NH4OH(aq)
Approximately 2cm3 of Ca2+(aq) solution was poured in a test tube. Diluted NH4OH(aq)was added to the solution
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October 22, 2014
Observation
Dropwise
At the 3rd drop of NH4OH(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 NH4OH(aq). Strong smell of ammonia observed.
Interpretation
Ca2+(aq) + 2OH-(aq) Ca(OH)2(aq)
No ppt suggests that Ca(OH)2(aq) is soluble in excess NH4OH(aq). The smell of Ammonia indicates that the
NH4+(g was being released as the CaOH was being formed.
Ba2+
Test with NaOH(aq)
Approximately 2cm3 of Ba2+(aq) solution was poured in a test tube. Diluted NaOH(aq) was added to the solution
Observation
Dropwise
At the 1st drop of NaOH(aq) no precipitate (ppt) was observed. At the 3rd drop a faint white ppt was formed.
Precipitate increased as the drops of NaOH(aq) increased.
Excess
Interpretation
Ba2+(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 NH4OH(aq)
Approximately 2cm3 of Ba2+(aq) solution was poured in a test tube. Diluted NH4OH(aq)was added to the solution
Observation
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October 22, 2014
Dropwise
No ppt was formed, no changes observed.
Excess
No ppt observed in excess of NH4OH(aq).
Interpretation
Ba2+(aq) + 2OH-(aq) Ba(OH)2(aq)
Barium is slightly unsoluble.
Al3+
Test with NaOH(aq)
Approximately 2cm3 of Al3+(aq) solution was poured in a test tube. Diluted NaOH(aq) was added to the solution
Observation
Dropwise
At the 1st 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
Al3+(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 NH4OH(aq)

Approximately 2cm3 of Al3+(aq) solution was poured in a test tube. Diluted NH4OH(aq)was added to the solution
Observation
Dropwise
At 1st drop a white ppt was formed. Precipitate remained as drops increased.
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October 22, 2014
Excess
Precipitate observed in excess of NH4OH(aq).
Interpretation
Al3+(aq) + 3OH- (aq) Al(OH)3(s)
Al(OH)3 is sparingly soluble in excess NH4OH(aq).
Test with dilute HCl(aq)

Approximately 2cm3 of Al3+(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 1st drop no change was observed. No change was observed as the drops were increased.
Excess
No change observed in excess dilute HCl(aq).
Interpretation
2Al3+(aq) + 6Cl-(aq) 2AlCl3(aq)
Al3+ is soluble in excess dilute HCl(aq).
Pb2+
Test with NaOH(aq)
Approximately 2cm3 of Pb2+(aq) solution was poured in a test tube. Diluted NaOH(aq) was added to the solution
Observation
Dropwise
NaOH(aq) increased.
Excess
Interpretation
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October 22, 2014
Pb2+(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 NH4OH(aq)

Approximately 2cm3 of Pb2+(aq) solution was poured in a test tube. Diluted NH4OH(aq)was added to the solution
Observation
Dropwise
At 1st drop a white ppt was formed. Precipitate remained as drops increased.
Excess
Interpretation
Pb2+(aq) + 2OH-(aq) Pb(OH)2(s)
Pb(OH)2 is sparingly soluble in excess NH4OH(aq).
Test with dilute HCl(aq)

Approximately 2cm3 of Pb2+(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 1st 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
Pb2+(aq) + 2Cl-(aq) PbCl2(aq)
Pb2+ is sparingly soluble in excess dilute HCl(aq).
October 22, 2014
Cr3+
Test with NaOH(aq)
Approximately 2cm3 of Cr3+(aq) solution was poured in a test tube. Diluted NaOH(aq) was added to the solution
Observation
Dropwise
At the 1st drop of NaOH(aq) a green-grey precipitate (ppt) was observed. Precipitate increased as the drops of
NaOH(aq) increased.
Excess
Interpretation
2Cr3+(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 NH4OH(aq)

Approximately 2cm3 of Cr3+(aq) solution was poured in a test tube. Diluted NH4OH(aq)was added to the solution
Observation
Dropwise
At 1st drop a grey-green ppt was formed. Precipitate increased as drops increased.
Excess
Interpretation
Cr3+(aq) + 3OH-(aq) Cr(OH)3(s)
Cr(OH)3 is sparingly soluble in excess NH4OH(aq).
Mn2+
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October 22, 2014
Test with NaOH(aq)

Approximately 2cm3 of Mn2+(aq) solution was poured in a test tube. Diluted NaOH(aq) was added to the solution
Observation
Dropwise
At the 1st 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
Mn2+(aq) + 2OH-(aq) Mn(OH)2(s)
MnOH is sparingly soluble in excess NaOH. The MnOH oxidized to Managanese (III) oxide to Mn2O3 and then
to Managanese (IV) Oxide MnO2.
Test with NH4OH(aq)

Approximately 2cm3 of Mn2+(aq) solution was poured in a test tube. Diluted NH4OH(aq)was added to the solution
Observation
Dropwise
At 1st drop a light brown ppt was formed. Precipitate increased as drops increased.
Excess
Precipitate observed in excess of NH4OH(aq). The ppt slowly turned darker the longer the solution remained in
the air.
Interpretation
Mn2+(aq) + 2OH-(aq) Mn(OH)2(s)
Mn(OH)2 is sparingly soluble in excess NH4OH(aq). The ppt turned darker due to oxidation taking place.
Fe2+
Test with NaOH(aq)
October 22, 2014
Approximately 2cm3 of Fe2+(aq) solution was poured in a test tube. Diluted NaOH(aq) was added to the solution
Observation
Dropwise
At the 1st 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
Fe2+(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 NH4OH(aq)

Approximately 2cm3 of Fe2+(aq) solution was poured in a test tube. Diluted NH4OH(aq)was added to the solution
Observation
Dropwise
At 1st drop no ppt was formed. By the 5th drop a green ppt started to form. Precipitate increased as drops
increased.
Excess
Brown ppt observed in excess of NH4OH(aq).
Interpretation
Fe(OH)2 is sparingly soluble in excess NH4OH(aq). The ppt turned darker due to oxidation taking place to form
Fe(OH)3.
Fe3+
Test with NaOH(aq)
Approximately 2cm3 of Fe3+(aq) solution was poured in a test tube. Diluted NaOH(aq) was added to the solution
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October 22, 2014
Observation
Dropwise
At the 1st 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
2Fe3+(aq) + 6OH-(aq) 2Fe(OH)3(s)
Fe(OH)3 is remains in excess NaOH indicating that the hydroxide is sparingly soluble.
Test with NH4OH(aq)

Approximately 2cm3 of Fe3+(aq) solution was poured in a test tube. Diluted NH4OH(aq)was added to the solution
Observation
Dropwise
At 1st drop a brown ppt was formed. Precipitate increased as drops increased.
Excess
Interpretation
Fe(OH)3 is sparingly soluble in excess NH4OH(aq).
Zn2+
Test with NaOH(aq)
Approximately 2cm3 of Zn2+(aq) solution was poured in a test tube. Diluted NaOH(aq) was added to the solution
Observation
Dropwise
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October 22, 2014
NaOH(aq).
Excess
Precipitate redissolves in excess of NaOH(aq). Colour change from white to transparent.
Interpretation
Zn2+(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 NH4OH(aq)
Approximately 2cm3 of Zn2+(aq) solution was poured in a test tube. Diluted NH4OH(aq)was added to the solution
Observation
Dropwise
At 1st drop a white ppt was formed. Precipitate increased as drops increased.
Excess
Precipitate redissolved in excess of NH4OH(aq). Colour changed from white to transparent.
Interpretation
Zn2+(aq) + 2OH-(aq) Zn(OH)2(s)
Zn(OH)2 redissolved in excess NH4OH(aq) indicating that the hydroxide is soluble and formed a complex ion.
Zn(OH)2(s) + 4NH3(aq) [Zn(NH3)4]2+(aq) + 2OHNH4+
Test with NaOH(aq)
Approximately 2cm3 of NH4+(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
NH4+(aq) + OH- Na(aq) + NH3 + H2O(l)
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October 22, 2014
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, Mg2+- white crystal, Ca2+-white powder, Ba2+- fine white crystals, Al3+ - medium white
crystals, Pb2+-white crystals, Cr3+- green powder, Mn2+- pink crystals, Fe2+-pale green crystals, Fe3+- orange
brown crystals, Zn3+- fine white crystals and NH4+- fine white crystals. This confirms that transition metals
have a coloured salt or a coloured aqueous solution (Cr3+, Mn2+, Fe2+ & Fe3+) 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 NH4OH. 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. Mg2+- white ppt, Cr2+ - grey-green ppt and Mn2+- 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. Mg2+ and Fe2+. Metallic ions that redissolved in excess of the reagents such as
Al3+ and Zn2+in NaOH exhibited amphoteric behaviour as both hydroxide dissolves in acids as well. Al3+ and
Pb2+ both form white ppt in NaOH(aq), the precipitates are soluble in excess, while in NH4(aq) they are insoluble
in excess. As can be seen, Al3+ and Pb2+ give the same results. So, to differentiate between them, another
reaction must be considered. Pb2+ will form a white precipitate with Cl- while Al3+ will not. Two other cations
form white precipitates. Zn2+ forms a white precipitate, which is soluble both in excess NaOH(aq) and NH4(aq)OH
and Ca2+ forms a white precipitate which is insoluble in excess NaOH but does not form a precipitate when
treated with NH4(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: Na2+, K+, Ca2+, Ba2+ and Cu2+. Using diluted NaOH and diluted NH4OH
as reagents the following metals could be confirmed: Mg2+, Ca2+, Ba2+, Cr3+, Mn2+, Fe2+, Fe3+ and Zn2+. A
further test with diluted HCl was able to confirm samples of Al3+ and Pb2+. A heat test could confirm the
presence of Ammonium ion using NaOH.
13

Qualitative Analysis of Cations

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Qualitative Analysis of Cations

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October 22, 2014

Topic: Qualitative Analysis

October 22, 2014

October 22, 2014

October 22, 2014

October 22, 2014

Test with NH4OH(aq)

October 22, 2014

Test with dilute HCl(aq)

October 22, 2014

Pb2+(aq) + 2OH(aq) Pb(OH)2(s)

Test with NH4OH(aq)

Test with dilute HCl(aq)

October 22, 2014

Test with NH4OH(aq)

October 22, 2014

Test with NaOH(aq)

Test with NH4OH(aq)

October 22, 2014

Test with NH4OH(aq)

October 22, 2014

Test with NH4OH(aq)

October 22, 2014

October 22, 2014

Sources of Error and Limitation

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