Inorganic Chemistry

Experiment 5

Lab A: Wednesday at 14:00 Name: Avril Watson (14302674)

Demonstrator: Harrison
Analysis of a Solid Complex of

2+

Cu

Introduction:
Objectives:
The objectives for the practical for this week was to analyse the copper
amine complex that was made last week. Also, to determine the value x
2+ .
which is the number of ligands attached the C u
Theory:
When ammonia is added to metal ions it has an interesting affect. It can
act in two ways, either as a base or a possible ligand which can replace
water molecules around a central metal ion. When it does act as a ligand
in this manner it is in the form of a Lewis base. Ammonia is used as a

source of O H . When only a few drops of ammonia is added to a metal

ion, hydroxide forms as precipitate in the solution. However, when
ammonia is added is excess, it acts as a ligand and dissolves the
precipitate. Sometimes excess ammonia does not dissolve the precipitate.
This is due to the interaction of two equilibria. The one where ammonia
acts as a base and the other where ammonia acts as a ligand. To get the
precipitate to dissolve, the ligand exchange equilibria needs to lie far on
the right but you need the acid-base equilibrium to be easy to pull back to
the left.
2+
This method is used to determine the value of x in the complex of C u
where the

N H3

molecules in the complex are acting as ligands and are

attached to the central metal ion. The excess HCl added to the complex
displaces the N H 3 and a back titration is performed to determine the
value of x.
Back titrations are used to determine the unknown concentration of a
solution. Its determined by reacting the solution with a known amount of
excess reagent. The left over excess reagent is then titrated with another
second reagent. The second titrations results show how much of the
excess reagent was used in the first titration and thus the unknown
concentration of the solution can be calculated.

Avril Watson

Inorganic Experiment 4Student number: 14302674

Experimental Procedure:
The experiment for this week was split up into two parts:
(i)

1 cm

of

Qualitative Test:
2+
2+N i
2+ , Z n
2+ , M n
C u

were each placed into a test tube. Dilute ammonia

solution was added to each ion dropwise until a colour change was noted.
After an initial colour change, excess ammonia was added to halfway up
the test tube to see if there were any further changes. All results were
then recorded.
(ii)

Analysis

0.5g of the compound prepared in last weeks practical was accurately

weighed using the analytical top balance. The weighed compound was
3
added to a 250 c m conical flask. The weight boat containing the sample
was then reweighed so the accurate weight of the copper complex could
be determined.
A little bit of deionised water was added to the copper complex in the
3
conical flask. Then 50 c m of HCl (0.2M) was pipetted in also. 2-3 drops
of bromophenol blue was added as an indicator also. This solution was
then titrated with NaOH (0.02M) until the first colour change of green to
blue occurred.
This analysis was repeated again and the results for both titrations were
recorded. The necessarily calculations were completed to determine the
value of x in the amminated copper complex. Finally, the percentage yield
was calculated.
Results:
Part one:
Initial
Colour:
2+

Mn

Colourless

Effect of a few
drops of
ammonia:
Cloudy orange

2+
N i

Light green

Cloudy blue

Blue

2+

Cu

Blue

Cloudy blue

Dark blue

2+

Colourless

Cloudy

Colourless

Avril Watson
Zn

Effect of
excess
ammonia:
Cloudy orange

Inorganic Experiment 4Student number: 14302674

NH 3

appears to displace O H

in the

2+
M n ,

2+
N i and

2+
C u . The

correlates well with their positions on the transition metal series. The

metals to the left tend to have O H displaced easier than those towards
the right.
Part two: Analysis
Experiment
1:
0.3713

Experiment
2:
0.3515

Initial:

Final:

10.7

10.6

Titre:

10.7

10.6

(i)Weight of sample in
grams:
Titration Readings in ml

Calculations for Experiment 1:

Concentration of HCl used is 0.2M
3
Volume of HCl used is 50 c m

Total number of moles of HCl added is 0.01mol

From the titre, the number of moles of NaOH used is

Number of moles of HCl that reacted with the complex is

7.86 103 mol
The molar mass of N H 3 is 17.03g/mol.

The mass of

2.14 10

N H3

in the complex is 0.13g.

The mass of CuS O 4 . H 2 O in the sample is 0.2413g
3
The moles of CuS O4 . H 2 O in the sample is 1.36 10 mol

X = 5.58

mol

Calculations for Experiment 2:

Concentration of HCl used is 0.2M
3
Volume of HCl used is 50 c m

Total number of moles of HCl added is 0.01mol

From the titre, the number of moles of NaOH is

Avril Watson

2.12 10

mol

Inorganic Experiment 4Student number: 14302674

Number of moles of HCl that reacted with the complex is

7.88 103 mol
The molar mass of N H 3 is 17.01g/mol.

The mass of

N H3

in the complex is 0.1342g

The mass of CuS O 4 . H 2 O is 0.2173g
3
The moles of CuS O4 . H 2 O in the sample is 1.22 10 mol

X = 6.459
Average value of X = 6.1195 6

Moles of

Percentage yield in the preparation is 71%

[ Cu ( N H 3 ) x ] . S O4 . H 2 O

made in week 6: 0.02mol

Discussion:
The experiment was fairly straight forward in my opinion and there was
little room for error. The use of the analytical top balance ensured that the
correct amount of the copper complex was taken for the back-titration.
The exact weight was calculated by adding the complex to a weigh boat
on the scales and measuring it up to 5g. Then when the complex had
been added to the conical flask, the weigh boat was weighed again to find
the weight of the boat on its own and also any residue left on the weigh
boat. However, the first time we did this, some of the residue of the
complex got on our hands which resulted in us getting an inaccurate value
for the weight of the copper complex. In future, it is important to hold the
weigh boat flat and not put any fingers into the boat.
For the first titration, we stopped titrating too late which gave us a
deviation in the true value of NaOH used to indicate a colour change. This
meant we had to repeat the experiment to get a more accurate value. In
future, it is important to keep an eye on the solution and the colour
changes instead of the burette and how much NaOH is used.
The calculations were easy enough to do. We ended up with a percentage
yield of 71% which I was happy about. I feel it was a success.
Conclusion:
The experiment was relatively straight forward and all the objectives for
the practical were achieved. The average value of x was 9.33mol and the
percentage yield was 71%. This experiment furthered my knowledge on
the transition metal series and metal complexes as well as enabling me to
practise further titrations.

Post Practical Questions:

Avril Watson

Inorganic Experiment 4Student number: 14302674

1. Give a definition and an example of each of the following:

-

an octahedral transition metal complex (with diagram)

An octahedral transition metal complex has six ligands
symmetrically arranged around a central metal atom. The shape
defines the vertices of an octahedron. An example of this is
[ Co ( N H 3 ) 6)
3+
. It is not octahedral in the mathematic sense but its

shape is octahedral.
When two or more types of ligands are attached to an octahedral
metal centre, the complex can appear as different isomers.

a ligand substitution reaction

A ligand substitution involves the exchange of one ligand for
another. This has no effect on the oxidation state of the metal
centre. Incoming or outgoing ligands may be either L or X type.
Although the oxidation state doesnt change, the charge of the
complex changes if the ligand changes. If you swap X for L, the
charge decreases by 1. If you swap L for X, the charge increases by
1. The charges are always conserved.

a bidentalate ligand

Avril Watson

Inorganic Experiment 4Student number: 14302674