Inorganic Chemistry Laboratory
Synthesis and Analysis of a Coordination Compound
Mr. *****
Department of Chemical Engineering and Chemistry, Mapua Institute of Technology
February 8, 2006
In this experiment, the compound was prepared to contain cobalt ion, ammonia, and chloride ions.
Our objective was to determine the umber of atoms using different methods for each ions. Our unknown
compound analyzed was Co1(NH3)5Cl3.
Introduction
One of the many interesting areas of
chemistry is the study of a class of substances
called coordination compounds or complexes.
These compounds are typically salts. One or both
of the ions in the salt can be composed of a
central metal atom, which is bonded to Lewis
bases. In this discipline of chemistry, the Lewis
bases are called ligands. In this experiment, a
compound was made that can have ion isomers.
In many reactions involving complex ion
formation the rate of reaction is very fast, so that
the thermodynamically stable form of the
complex is the one produced. By changing
ligand concentrations, one can quickly convert
from one complex to another. Those complexes
undergo rapid exchange with other Lewis bases
are referred to as labile; conversely, those
complexes that only exchange slowly with other
Lewis bases are referred to as inert.
Methodology
Preparation of Cox(NH3)yClz
Using a piece of weighing paper and a
top-loading balance, 10 g of ammonium chloride
was weighed. NH4Cl was poured into a 250-mL
beaker and 40 mL of distilled water was added.
To this, 8 g of cobalt (II) chloride hexahydrate,
CoCl2 · 6H20 and 0.8 g activated charcoal was
added. The mixture was heated to boiling point
with stirring to dissolve the soluble components.
The beaker was cooled in water, then in an ice
bath. Slowly, in a hood, 40 mL of 15 M NH3 was
added. After stirring, 50 mL of 10% H2O2,
hydrogen peroxide was added slowly, a few mL
at a time, while continuing to stir. When the
bubbling had stopped, the 250-mL beaker was
placed in a 600-mL beaker containing 100 mL of
water at about 60ºC. The beaker was left in the
water bath for 30 minutes, holding the
temperature of the bath at about 60ºC as long as
the liquid has a pink color. It was stirred
occasionally. When the 40 minutes were up, the
250-mL beaker was removed from the water
bath and cooled, first in a water bath and then in
an ice bath, until the liquid in the beaker had a
temperature below 5ºC for 5 minutes. The
Buchner funnel was setup and, with suction, the
mixture was filtered through the filter paper in
the funnel. The solid was scrapped from the filter
paper in the 250-mL beaker. 100 mL distilled
water was then added, and in a hood, 4 mL 12 M
HCl was also added. The mixture was heated to
boiling, with stirring, to dissolve the crystals.
The suction flask was rinsed with distilled water,
and the Buchner funnel was reassembled. The
hot mixture was then filtered through the paper
in the funnel, under suction. In this operation, the
charcoal was removed and placed on the filter
paper. The filtrate was transferred to the 250-mL
beaker and, in the hood, 15 mL 12 M HCl was
added. The beaker was placed in an ice bath and
was stirred for 5 minutes to promote formation
of the golden crystals of the product
Cox(NH3)yClz, 50 mL of nice-cold distilled water
was poured on to a piece of filter paper in the
Buchner funnel. The flask was then emptied and
the cold mixture was filtered containing the
product through the funnel, using suction. The
suction was turned off, and 20 mL 95% ethanol
was poured on to the crystals. The crystals was
transferred from the filter paper to the beaker and
stored.
Note: The methodology of the gravimetric
determination of chloride content and the
colorimetric determination of cobalt content will
not be discussed in this report since it was
performed by the other groups.
Volumetric Determination of Ammonia Content
In this part of the experiment the
complex was decomposed, releasing NH3 to the
solution. The NH3 was then distilled off into
another container, and was titrated against an
acid. The procedure is called a Kjeldahl analysis,
and is used for determining nitrogen content of
many organic and inorganic substances. The
distillation apparatus was assembled as shown in
the figure.
50 mL saturated boric acid solution was
inserted in the 125-mL receiving flask; with five
drops bromcresol green indicator, the level of the
flask was adjusted so that the latex tubing is well
under the liquid surface. 1 g of the compound
was weighted into a beaker and transferred in the
distilling flask using a funnel. The beaker was
rinsed several times with small portions of
distilled water. Distilled water was added to give
a final volume of about 50 mL. The flask was
stirred to dissolve the sample. A few boiling
chips and several pieces of granulated zinc was
added. 40 mL 6 M NaOH was poured with 50
mL distilled water into the flask and reconnected
to the distilling head. The plated was turn on.
Ammonia was recovered in the receiving flask.
Interpretation of Results
The synthesis of the unknown inorganic
compound followed this (unbalanced) equation:
CoCl2 · 6 H2O(s) + H2O + NH4Cl(s) + NH3 
Cox(NH3)zCly(s) + H2O(l)
Many, but by no means all, complexes
are labile. It exchanges ligands only very slowly
(inert). For such species, the preparation reaction
takes time, but once formed, the complex ion in
solution may resist change rather dramatically.
In the complex ion NH3 and Cl- may be ligands.
Some of the Cl- ions may be in the complex and
some may simply be anions in the crystal.
Cox(NH3)zCly(s) + OH-(aq)  Co3O4(s) + O2(g) +
NH3(aq) + H2O2 + Cl-
Co3O4(s) + SO32-(aq) + 6 H+(aq)  3 Co2+(aq) + SO42(aq)
+ 3 H2O(l)
When the compound is dissolved in
water, the free anions will go into solution, but
the ones in the complex will remain firmly
attached to cobalt. They neither will nor react
with a precipitating agent such as Ag+ ion,
which will tend to form AgCl with any free Cl-
ions. All of the NH3 molecules will be in the
complex ion, and will not react with added H+
ion, as they would if they were free. NH3 and
Cl- that is present in the compound was
destroyed attempting any analysis. The complete
analysis involves a gravimetric procedure for
chloride ion. A volumetric procedure for
ammonia was followed. The chemical reaction
for cobalt analysis which is a calorimetric
method is as follows:
Cox(NH3)zCly(s) + heat  CoCl2(s) + N2(g) +
NH4Cl(s) + NH3(g)
CoCl2(s) + water  3 Co2+(aq) (λ = 510 nm) + 2
Cl-
The calculations for the ions were as
follows:
Cobalt Content:
Molarity of Co ion = 0.0445 M
Molarity of Co in sample = (0.0445 M)(0.05L)
=2.225x10-3 mol
Mass of sample = (2.225x10-3 mol) / (0.5053 g)
= 4.4033x10-3 mol/g
Molarity of Co per 100 g sample = (4.4033 x10-3
mol/g)(100) = 0.4403 mol
Chloride Content:
Mass of AgCl = 1.5055 g
Mass of Cl- in AgCl = 1.5055 g (1 mol / 143.32 g
AgCl)(1 Cl- / 1 AgCl)(35 g / 1 Cl-) = 0.1210 g
Mass of Cl- per 100 g sample = (0.1210 g / employees.oneonta.edu/kotzjc/LAB/Complex_E
0.2307 g) x 100 = 52.4491 g xpt.pdf

Moles of Cl- per 100 g sample = 52.4491 g / 35 http://www.dit.ie/DIT/science/chemistry/rsccom

g/mol = 1.4794 mol p/competition00/distillation/labdistillation.JPG
Ammonia Content:

Moles of NH3 in 40 mL = (32.4 mL)(0.09533 M)

= 3.085x10-3 mol
Moles of NH3 in 250 mL = (3.085x10-3 mol)(250
/ 40) = 19.3x10-3
Molarity of NH3 per 100 g sample = (19.3x10-3)
(100) = 1.928 mol

From the calculations we can determine

the number of moles for each species present in a
mole of compound.

Moles cobalt / 100 g sample = 0.4403 mol

Moles chloride / 100 g sample = 1.4794 mol
Moles ammonia / 100 g sample = 1.928 mol

Because the mole ratio must equal the

atom or molecule ratio, we can determine the
formula of the compound.

x=1
y=3
z=5

Hence our unknown compound is

Co1(NH3)5Cl3(s)

Conclusion

Coordination compounds can be

prepared that have the same molecular formula
but different in the composition of ions.
The complete analysis involves a
gravimetric procedure for chloride ion, a
calorimetric method fro cobalt ion, and a
volumetric procedure for ammonia. Using these
methods of analysis the authors derive the
unknown inorganic compound which is
Co1(NH3)5Cl3.

References

www.accd.edu/nvc/areas/chem/ComDALab/Synt
handAnalofCoordinate.pdf

cod.edu/people/.../CHEM153/Syntheisi-
AnalysisCoordinationCompExp30.pdf