Objective:

Gain familiarity with some of the acid-base, oxidation-reduction and complexion reaction
of the elements of the first transition series.

Introduction:

Transition metal is an element which forms at least one ion with an incomplete d
subshell containing at least one electron. The transition elements are characterized by
the formation of coloured complexes. In this series of tests, will see how the ions of the
most common oxidation states of certain first row transition elements behave in various
standard conditions and also learn one or two unique reactions of each ion.

Chemicals:

0.5 M chrome alum, KCr(SO4)2.12H2O

0.5 M chromium (III) chloride, CrCl3.6H2O
0.25 M potassium dichromate, K2Cr2O7
2 M sodium hydroxide, NaOH
4 M sodium hydroxide, NaOH
6% hydrogen peroxide
2 M aqueous ammonia
4 M aqueous ammonia
1 M sodium carbonate, NaCO3
4 M sodium carbonate, NaCO3
6 M hydrochloric acid, HCl
Granular of zinc
Saturated zinc sulfate
2 M sulphuric acid, H2SO4
0.1 M barium chloride, BaCl2
0.5 M cobalt(II) chloride
Water
2 M potassium thiocyanate solution
Saturated sulphate solution
Pyridine
Acetic acid
Solid potassium nitrite
0.5 M nickel(II) chloride solution
Apparatus:

Test tubes
Graduated measuring cylinder
Dropper
Test tube rack
Hot plate
Beaker
Test tube holder
pH paper

PROCEDURE:

A. Reaction of chromium

Concentration of the chemicals used:

0.5 M chrome alum, KCr(SO4)2.12H2O
0.5 M Chromium (III) chloride, CrCl3.6H2O
0.25 M potassium dichromate, K2Cr2O7

1. Excess of 2 M NaOH are added to 2 ml of chrome alum solution. The, 2 ml of 6% of

hydrogen peroxide are added and warmed. Observed.

2. 2 M of NaOH are added slowly to 2 ml of chrome alum solution. Observed.

3. Excess 1 M sodium carbonate solution are added to 2 ml of chrome alum solution.

This experiment is compared with experiment from steps 1 and 2.

4. 2 ml of 6 M HCl (concentrated) and granular zinc are added to 2 ml of chromium(III)

chloride solution. The mixture is warmed and observed the changes. The liquid is poured
quickly into 4 ml of a saturated solution of sodium acetate. Observed.

5. 2 ml of the chromium (III) chloride solution, 2 ml of 6 HCl (concentrated) and a

granular of zinc are mixed together and warmed The solution is cooled and the test tube is
rotated . Observed.

6. A few drops of 2 M of sulphuric acid are added to 2 ml of potassium dichromate

solution until the pH is 4. Then, a few drops of 2 M NaOH are added until the pH is 9.
Then, 2 M of sulphuric acid are added to bring the pH back to 4. Observed.

7. A few drops of 1.0 M BaCl2 solution are added to 2 ml of potassium dichromate

solution. All observation are recorded.
B. Reaction of Cobalt

Concentration of chemical used:

0.5 M cobalt(II) chloride

1. 4 ml of water and 4 ml of 2 M NaOH solution are added slowly to 2 ml of the cobalt

(II) solution.

2. 4 ml of NaOH solution are added slowly to 2 ml of cobalt(II) chloride solution. The

result is compared with step 1.

3. 4 ml of 1 M sodium carbonate solution are added to 2 ml cobalt(II) chloride solution.

The result is compared with steps 1 and 2.

4. 4 ml of 4 M aqueous ammonia are added slowly to 2 ml of cobalt(II) chloride

solution. The result is compared with steps 1 to 3. Then, 4 drops of 6% of hydrogen
peroxide and 2 ml of 2 M NaOH are added immediately and boiled gently.

5. a) 1 ml of 2 M potassium thiocyanate and pyridine are added to 1 ml of cobalt(II)

chloride solution.

b) 1 ml of 2 M potassium thiocyanate and pyridine are added to 1 ml of saturated

zinc sulfate solution.

c) 1 ml of 2 M potassium thiocyanate and pyridine are added to a mixture of 1 ml of

cobalt (II) chloride solution and 1 ml of saturated zinc sulfate solution.

6. 1 ml of cobalt(II) chloride is acidified 1 with acetic acid and spatula of solid

potassium nitrite are added to the 4 solution. All observation are recorded.

C. Reactions of Nickel

Concentration of chemical used:

0.5 M nickel (II) chloride solution.

1. 4 ml of 2 M NaOH are added to 2 ml of nickel (II) chloride solution.

2. 4 ml of 4 M aqueous ammonia are slowly added to 2 ml of nickel (II) solution.

Result is compared with the first part of experiment 1. About 4 drops of 6%
hydrogen peroxide and 4 ml of 2 M NaOH are added. The mixture is boiled gently.
The experiment is compared with corresponding reaction of cobalt(II)

3. 4 ml of 1 M sodium carbonate solution are added to 2 ml of nickel(II)solution . The

results are compared with those of the first parts of experiments 1 and 2 .

4. 2 ml of 2 M potassium thiocyanate solution are added to 2 ml of nickel (II) solution.

A few drops of pyridine are added.
RESULT:
EXPERIMENT OBSERVATION
CHROMIUM COBALT NICKEL
(red solution) (green solution)

1 Green solution turns to Form two layers of Before heating:

emerald green clear solution and Light green
precipitate blue-grey precipitate precipitate is
formed

After heating:
Form two layers of
clear solution and
light green
precipitate

2 Dark green solution Form two layers of The solution turns to

turns to green-grey clear solution and cloudy.
precipitate pink precipitate
After heating:
Form two layers of
clear solution and
light green
precipitate.

3 Green solution turns to Form two layers of Green precipitate is

grey precipitate clear solution and formed.
purple precipitate

4 Dark green solution Turns to pink Green solution turns

turns to dark purple precipitate. to concentrated
milky blue solution.
Turns to blue
precipitate after
NaOH and 6%
hydrogen peroxide
was added.

After heating:
Form two layers of
clear solution and
brownish-purple
precipitate.
5 Dark green solution a) Turns to purple
turn to grey-green solution and
precipitate then
concentrated
milky pink
solution after
pyridine is
added

b) Turns to purple
solution and
then
concentrated
milky pink
solution after
pyridine is
added

c) Pink and blue

precipitate is
formed

6 Orange solution turns Cobalt with acetic

to light orange acid turns to red-
brick colour.
It turns to yellow-
green after
potassium nitrate is
added.

Blue litmus paper

turns to red.

7 Orange solution turns

to yellow precipitate
DISCUSSION

Reaction of chromium:

Chrome alum with NaOH and 6% hydrogen peroxide:

Strong bases such as NaOH also precipitate Cr(OH)3, but the green precipitate dissolves
in excess hydroxide.

Cr3+(aq) + 3OH-(aq) Cr(OH)3(s)

Cr(OH)3(s) + OH-(aq) Cr(OH)4-(aq)

Chrome alum with ammonia:

Ammonia reacts with chromium(III) ion to precipitate grey-green chromium(III)

hydroxide:

Cr3+(aq) + 3NH3(aq) + 3H2O(l) Cr(OH)3(s) + 3NH4+(aq)

Chrome alum with carbonate ions:

If sodium carbonate solution is added to a solution of chrome alum, you get exactly the
same precipitate as if you added sodium hydroxide solution or ammonia solution. The
carbonate ions which remove hydrogen ions from the hexaaqua ion and produce the
neutral complex.
Depending on the proportions of carbonate ions to hexaaqua ions, you will get either
hydrogencarbonate ions formed or carbon dioxide gas from the reaction between the
hydrogen ions and carbonate ions. The more usually quoted equation shows the formation
of carbon dioxide.

Chrome alum with ammonia solution:

The ammonia acts as both a base and a ligand. With a small amount of ammonia,
hydrogen ions are pulled off the hexaaqua ion exactly as in the hydroxide ion case to give
the same neutral complex.

That precipitate dissolves to some extent if excess of ammonia is added. The ammonia
replaces water as a ligand to give hexaamminechromium(III) ions.
Chromium (III) chloride solution with HCl and Zinc:

Chromium (III) ions reduced to chromium (II) ions using zinc and hydrochloric acid.
Hydrogen is produced from sid reaction between zinc and acid.

2Cr3+ + Zn 2Cr2+ + Zn2+

Potassium dichromate with sulfuric acid and NaOH:

The orange dichromate(VI) ion, Cr2O72-. If dilute sulfuric acid is added to the yellow
solution it turns orange. If sodium hydroxide solution is added to the orange solution it
turns yellow.

Potassium dichromate with BaCl2 :

The Barium is taken out of solution leaving K+, Cr6+and Cl- in solution. Well Cl- is very
pale green in solution and K+ forms a clear solution so the only colouring ion in solution
is Cr6+, which is orange.
Reaction of cobalt:

Cobalt(II) with NaOH:

Sodium hydroxide solution remove hydrogen ions from the water ligands attached to the
cobalt ion. Once a hydrogen ion has been removed from two of the water molecules, you
are left with a complex with no charge - a neutral complex. This is insoluble in water and
a precipitate is formed.

[Co(H2O)6 ]2+ + 2OH- Co(H2O)4(OH)2 + 2H2O

Cobalt(II) with aqueous ammonia and 6% hydrogen peroxide:

The ammonia acts as both a base and a ligand. With a small amount of ammonia,
hydrogen ions are pulled off the hexaaqua ion exactly as in the hydroxide ion case to give
the same neutral complex.

That precipitate dissolves if you add an excess of ammonia. The ammonia replaces water
as a ligand to give hexaamminecobalt(II) ions.

It will get the variably coloured precipitate of the cobalt(II) hydroxide complex when the
sodium hydroxide solution is added. Addition of hydrogen peroxide produces lots of
bubbles of oxygen and a brown precipitate.

Cobalt(II) with sodium carbonate:

Precipitation of cobalt(II) carbonate

Reaction of nickel:

Nickel with NaOH:

Sodium hydroxide precipitates nickel(II) hydroxide:

Ni2+(aq) + 2OH-(aq) Ni(OH)2(s)

Nickel with aqueous ammonia:

Aqueous ammonia precipitates green gelatinous Ni(OH)2:

Ni2+(aq) + 2NH3(aq) + 2H2O(l) Ni(OH)2(s) + 2NH4+(aq)

Some of the tests carried out have not obtained the expected result. It may have a few
error that have effected the results. One of the error is the volume of chemicals used are
qualitative. So the volumes are not accurate, some tests may have an excess substance
that can effect the result. The observer also can make any mistake such as didnt aware
about colour changes and gas released. The mixtures also are not shake very well. The
accurate results can be obtained if the observer shake the mixture very well and
concentrated while carried out the experiment. Graduated measuring cylinder can be
used to make the volume of chemicals are accurately measured.
 QUESTIONS

1. What are the common oxidation states of chromium, cobalt and nickel? What the d-
electron configurations of these oxidation states respectively?

Chromium (III) is the most stable oxidation state of this element in aqueous solution,
but the +6 state is also found in the well known chromate oxidizing agents, CrO42- , and
the dichromate Cr2O72-, ions. Cobalt, +3 state is most stable but it is strongly oxidizing
when the ligands are water molecules. Oxidation states of nickel other than +2 are quite
difficult to obtain although a nickel (III) oxide. d-electron configuration of chromium(III)
is, [Ar] 3d3. For cobalt , [Ar] 3d5 . For nickel, [Ar] 3d8 .

2. Interpret the results of the reactions carried out, write balance equations whenever
possible.

Experiment Balance equation

Chromium Cobalt Nickel
1 2NaOH + CoCl2 2NaCl NiCl2 + NaOH NaCl +NiOH2
+ Co(OH)2

2 Cr3+(aq) + 3NH3(aq) + 3H2O(l) 2NaOH + CoCl2 2NaCl Ni2+(aq) + 2NH3(aq) + 2H2O(l)

Cr(OH)3(s) + 3NH4+(aq) + Co(OH)2 Ni(OH)2(s)+ 2NH4+(aq)

3 Na2CO3 + CoCl2 CoCO3 NiCl2 + NaCO3 NaCl +

+ 2NaCl Ni(CO3)2
4 CoCl2 +6NH3
[Co(NH3)6]Cl2

[Co(NH3)6]Cl2 + H2O2
[Co(NH3)6]Cl3 +2OH-(aq)
5 2CrCl3 + Zn 2 CrCl2 + ZnCl2

6 K2Cr2O7 + 2H2SO4 2CrO3 +

2KHSO4 +H2O
7 BaCl2 + K2Cr2O7 BaCrO7 +
2KCl
CONCLUSION

Nickel reactions show the most familiarity than other reactions. While others, certain
result are almost same but not really same. So, some of the acid-base, oxidation-
reduction, complexion reactions show same result and some of them not.

REFERENCE

Books:

Peter Atkins, Tina Overton, Jonathan Rourke, Mark Weller, Fraser Armstrong, Shriver &
Atkins Inorganic Chemistry, Fifth Edition, 2010, Macmillan Publishing Solutions, Great
Clarendon Street, Oxford OX2 6DP.

James ONG, Definitions and Formulae In Chemistry, 1998, Golden Books Centre Sdn.
Bhd., 149 Jalan Masjid India, 50100 Kuala Lumpur.

David Nicholls, Complexes and First Row Transition Elements, 1974, Kedai buku
Koperatif Bhd, 11800 USM, Pulau Pinang, Malaysia.

Web:

http://www.chemguide.co.uk/inorganic/transition/cobalt.html

http://www.chemguide.co.uk/inorganic/transition/chromium.html