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University Teknologi MARA

Sabah Branch
Faculty of Applied Sciences
Diploma in Sciences

CHM 260 LABORATORY REPORT


Experiment Number: 03
Title: Qualitative Analysis of Group III Cations
Lab Partners Name:
1.
2.
3.
4.

Ramona binti Masri


Siti Nurajjar binti Jami (2010673706)
Suliana binti Salim
Yusliana binti Yusof

Lecturers Name: PM. Gan Gin Hoon


Date of Submission: 23rd JANUARY 2013

1.0 TITLE:
1.1 Qualitative analysis of Group III cations: Fe2+, Fe3+ Al3+, Cr3+, Co2+, Ni2+,
Mn2+,Zn2+.
2.0 OBJECTIVE:
2.1 To identify the group III cations in solutions.
3.0 INTRODUCTION:
Qualitative analysis is useful in detecting the presence of specific ions in an aqueous
solution. It is an analysis that falls under the general category of analytical chemistry, which
will make it able to answer the question of; "What is in a sample?". The basis for a qualitative
analysis is the fact that ions will undergo specific chemical reactions with certain reagents to
yield observable products. For example, silver ion can be precipitated with hydrochloric acid
to yield solid silver chloride. Because many cations will not react with hydrochloric acid in
this way, this simple reaction can be used to separate ions that form insoluble chlorides from
those that do not. In fact, the qualitative detection of ions in a mixture is commonly
accomplished by a system of analysis in which precipitation reactions play a major role.
In addition, acid-base reactions, oxidation-reduction reactions, and the formation of
complex ions are often used in a systematic way for either separating ions or for determining
the presence of specific ions. The qualitative analysis of ions in a mixture must follow a
scheme that can be summarized as follows:
(i)

Add reagents that exploit the more general properties of ions to separate

(ii)

major groups of ions;


Separate major groups into subgroups with reactions that will distinguish

(iii)

less general properties; and


Add reagents that will specifically confirm the presence of individual ions.

For a successful qualitative analysis, the order of reagent addition is crucial and
should follow the order of; group I first, group II second, and so on. For example, addition of
carbonate first would precipitate everything but the group V ions or addition of basic H2S
first would precipitate all group II and group III ions.

4.0 CHEMICALS:
4.1 Solutions of Fe2+, Fe3+ Al3+, Cr3+, Co2+, Ni2+, Mn2+ and Zn2+.
4.2 NH3
4.3 NaOH
4.4 K2CrO4
4.5 KSCN
4.6 K4Fe(CN)6
4.7 PbO2 powder
4.8 HNO3 (concentrated)
4.9 Solution C
5.0 PROCEDURE
5.1 Part A: Reactions of Group III cations.
5.1.1
5.1.2

5.1.3
5.1.4
5.1.5
5.1.6

5.1.7

5.1.8

Apart from Fe3+, all other elements were dissolved to become solutions
first before being tested.
The first test was using the NH3 solution as the reagent. A small
amount of NH3 solution was added into the sample, and then followed
by an excess amount of the reagent.
Next, a small amount of NaOH solution was added into the sample,
followed by an excess amount of the reagent.
For the third test, some potassium thiocyanate, KSCN solution was
added into the sample.
Some potassium hexacyanoferrate (III), K4Fe(CN)6 solution was added
into the sample.
The final test was to add small amount of potassium cyanide, K2CrO4
solution into the sample, and then followed by an excess amount of the
reagent.
But for Mn2+, there was a sixth test, which was some PbO2 powder was
added first into the solution. Then, some concentrated HNO3 was
added into the mixture. After that, the solution was heated to boil. The
colour change was observed.
All of the observations were recorded in a table.

5.2 Part B: Identification of the cations present in unknown samples.


5.2.1 All tests in Part A were carried out on Solution C, including the sixth
test.
5.2.2 The cation present in Solution C was identified.

7.0 DISCUSSION:
When NaOH added to Fe2+ solution which is already prepared in five test tube, the
mixture turn from light green to dark green and there was form a precipitate. Whereas for
KSCN solution, when we added it into test tube filled with Fe 2+, the mixture turn from
light green into light orange and when we added in excess, there is no changes. As we
added NH3 solution, as based on our observation, we found the mixture was turn from
light green into dirty green and as we added in excess there is no changes. Besides, when
we added K2CRO4 solution, we found the mixture turn from light green to dark brown
and when we added in excess, there was no change. When we added K 4Fe(CN)6 solution
into test tube filled with Fe2+ solution, we found the mixture in the test tube turn from
light green to dark blue.
When we added NaOH into test tube filled with Fe 3+, we found the mixture was
turn from orange into brown and the precipitate was formed. When we added in excess
the mixture was not dissolve. When we added KSCN solution into test tube filled with
Fe3+ solution, the mixture turn from orange to dark brown. For NH 3,when we added it into
test tube filled with Fe3+,the mixture turn from orange into brown and its was form a
precipitate. When we added K2CRO4 into the test tube filled with Fe 3+,the mixture turn
from orange to dark orange. When we added K 4Fe(CN)6 solution into test tube filled with
Fe3+ solution we found the mixture turn the orange colour into dark blue.
When Cr3+ which is green in colour was added with drop wise NH 3 which white in
colour, the solution turned to greenish. When NH3 added in excess, the solution then
turned from greenish to greyish blue in colour. Next, the Cr 3+ was added with drop wise
NaOH which is also white in colour and the mixed solution turned to light green and
when it is added in excess, the light green colour of the solution remain constant. After
that, Cr3+ was added with KSCN which white in colour and it was observed that no
reaction occurs. The green colour of the Cr3+ remains constant. Then, yellow in colour of
K3Fe(CN)5 was added to Cr3+ and it was observed that no changes occur. Lastly, Cr 3+ was
added with drop wise K2CrO4 which is also yellow in colour resulting the solution colour
changes from green to yellowish green in colour. Then, when it was added in excess, the
solution turned from yellowish green to dark yellowish green in colour.
When drop wise NH3 solution was added to Co2+, blue precipitate was formed.
After that, when NH3 was added in excess, the precipitate do not dissolved. Next, blue
precipitate also formed when drop wise of NaOH was added into Co 2+. However, the blue

solution turned colour from blue to pale pink when NaOH was added in excess and the
precipitate do not dissolved. When dropwise of KSCN added to Co 2+, no changes occur
same when it was added in excess. Dirty green precipitate formed when K 3Fe(CN)5 was
added into Co2+ in dropwise while in excess, the precipitate formed do not dissolved.
After that, when Co2+ added with K2CrO4, the solution turned to orange and no precipitate
formed. While when excess K2CrO4 added, the orange solution change colour to brown.
Dropwise NH3 added to Mn2+ resulting white precipitate formed and more
precipitate formed and the precipitate do not dissolved when NH 3 added in excess into
Mn2+. After that, dropwise NaOH added into Mn2+ causing white precipitate to form and
the precipitate do not dissolved when NaOH added in excess into Mn 2+. Next, when
KSCN was added into Mn2+, no changes occur and the solution remains colourless. Then,
Mn2+ added with K3Fe(CN)5 and white precipitate formed. The solution of Mn 2+ turned
from colourless to yellow when added with dropwise K 2CrO4 and when it was added in
excess, the solution turned from yellow to dark yellow. Lastly, the Mn 2+ added with PbO2
and black precipitate formed. Then the solution added with HNO 3, resulting the
precipitate to dissolved. After that, the solution heated and the black solution turned to
dark purple in colour.
When Zn2+ was mixed with a little of ammonia NH3, white crystal precipitate was
formed and the precipitate was dissolved when an excess of ammonia mixed to the
solution of Zn2+. When a little of sodium hydroxide , NaOH was added to the solution of
Zn2+, white crystal precipitate is formed and it dissolved when an excess of it added to the
Zn2+ solution. There is no reaction formed when KSCN was added to Zn 2+ solution which
is the colour of the solution remained constant. A white precipitate is formed when
K4Fe(CN)6 was added into Zn2+. The colour of the Zn2+ solution change from colourless to
light yellow and the colour of the solution is change from light yellow to bright yellow
when an excess of K2CrO4 was added to the solution.
A white precipitate is formed when a little of NH3 is added into the solution of
Al3+ and not dissolved when an excess of it was mixed to the solution. When NaOH is
added the solution of Al3+ , white precipitate is formed and it is dissolved when an excess
of NaOH is mixed with the solution. There is no reaction when KSCN is added to the
solution. When K4Fe(CN)6 is mixed to the solution of Al3+ , the colour of the solution
change to greenish grey and light blue colour was formed when an excess of K 4Fe(CN)6 is
added to the solution. A milky light yellow of colour was formed when K2CrO4.
The colour of the solution change from green to greenish blue when NH 3 is added
to the solution of Ni+ and blue precipitate is formed. When an excess of NH 3 is added to

the solution, the colour change from greenish blue to blue and the precipitate is dissolved.
The colour of the solution is unchanged and pale green precipitate is formed when NaOH
is added with Ni+ and the mixture showed no reaction when an excess of the NaOH is
added to the Ni+ solution. When KSCN is added to the Ni+ solution, the colour of the
solution remains unchanged and no reaction occur when an excess of KSCN is added to
the solution. A pale green precipitate is formed and the precipitate is not dissolve when an
excess of K4Fe(CN)6 is added into the solution. The colour of the solution changes from
green to yellowish green when K2CrO4 is added into Ni+ solution. It showed no reaction
when an excess of K2CrO4 is mixed to the solution.
In part B, identification of the cation present in unknown samples. This is carried
out by adding up NH3, NaOH, KSCN, K4Fe(CN)6, K2CrO4 into 4 test tube containing
solution C. When we add 3 drops of NH3 solution into the solution C, we found the
solution C formed white gelatinous precipitate and when we added in excess, there is no
change. Whereas for NaOH, when we added 3 drops into it solution C we observe that the
solution C form a gelatinous precipitate. When we added in excess there was no change.
KSCN solution, when we added in 3 drop into solution C, we found there is no change on
the mixture. When we added K4Fe(CN)6 solution into the solution C, we found the
colourless solution turn to bright blue. When we added in excess, there is no change.
K2CrO4 solution, when we added it in 3 drops into the solution C, we found the solution
turn from colourless into yellow oranges. When added in excess the yellow gelatinous
precipitate formed. HNO3 and PbO3 solution, when we added in 3 drops both of it into
solution C, we found the black colour form after poured with both of HNO3 and PbO3
and after it is boiled, there was no changes occurred.

8.0 QUESTIONS:
8.1 Write the equation of the following reactions:
8.1.1 Reaction between copper (II) ion and ammonia (limited and excess).

2++2 NH 3 Cu+2 NH 4

Cu
2+
2++4 NH 3 Cu(NH 3 )4
Cu
8.1.2

Reaction between iron (III) ion and KSCN.

K 3 Fe (SCN )6

+SCN

3++K
Fe
8.1.3

Reaction between cobalt (II) ion and potassium cyanide (limited and
excess)

3 K 3 Co(NO 2 )6
++Co(NO2 )6

3K
8.1.4

Reaction that occurs when the mixture of Mn2+, PbO2 and HNO3
(concentrated) is heated.

2++4 H 2 O
Mn
+e
+8 H

MnO4
9.0 CONCLUSION:

9.1 Solution C has identified as Aluminium, Al3+ ion.