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NAME: NURUL FATIN BINTI RAZAK

STUDENT ID: 2014983737


CLASS: AS2452D
COURSE: CHM 475
INORGANIC CHEMISTRY
LECTURERS NAME: DR. AMALINA MOHD
TAJUDDIN

EXPERIMENT 8:
SPECTROPHOTOMETRIC ANALYSIS OF TRANSITION METAL CATIONS

OBJECTIVE:
To determine the concentration of an unknown, copper(II) solution by spectrophotometric
analysis.

INTRODUCTION:
A spectrophotometer is an instrument that can measure intensity and the wavelength of the
light. The instrument measures quantitatively the fraction of the light passes through the
solution. Spectrophotometer detect as the light of the sample that absorbed and convert into
the numbes known as absorbance. The darker the colour of the solution, the more light will
absorb and the easier to get the absorbance value.
In this experiment, the absorbance value of the known Cu 2+ solution was determined by using
the spectrophotometer. Graph of absorbance versus concentration of the known solution was
plotted. This graph was explained about the relationship of the concentration and absorbance.
As the concentration of solution is increase, the absorbance value will become greater. It is
proved that the concentration is directly proportional to the absorbance.

PROCEDURE:
1. The spectrophotometers was switch on to warm up and the wavelength max was set at
645 nm.
2. Six test tubes were cleaned and numbers as 1-6.
3. 1 M HNO3 was transferred into the burette.
4. The six test tubes was filled with the following solution as listed in the table.
Test tube No.
1.
2.

Contents
10.0 mL of 1 M HNO3 from the burette
4.0 mL of standard Cu2+ solution and 6.0 mL of 1 M HNO 3

3.

from burette. Mixed well


7.0 mL of standard Cu2+ solution and 3.0 mL of 1 M HNO 3

4.
5.

from burette. Mixed well


10.0 mL of standard Cu2+ solution
0.05 g of unknown sample and 10.0 mL of 1 M HNO 3 form

6.

the burette. Mixed well


0.10 g of unknown sample and 10.0 mL of 1 M HNO 3 form
the burette. Mixed well

5. The contents in the test tubes was transferred into cuvettes and the absorbance of each
solution were measured at 645 nm.

RESULTS:
Test tube no.
1.
2.
3.
4.
5.
6.

Concentration (M)
0.000
0.060
0.140
0.200
0.102
0.009

Absorbance
0.087
0.270
0.430
0.598
0.348
0.111

CALCULATION:
Determination of concentration (M) of known Cu2+ solution.
Test tube No.
1.

Concentration
m1v1=m2v2
1

0.2 = 0.01 M

M = 0.000 M

81.9%
53.1%
37.2%
25.3%
44.3%
60.2%

m1v1=m2v2
2.

0.004 0.2 = 0.01 M


M = 0.080 M
m1v1=m2v2

3.

0.007 0.2 = 0.01 M


M = 0.140 M
m1v1=m2v2

4.

5.
6.

0.010 0.2 = M
M = 0.200 M
(0.348 0.087) 2.555
= 0.102 M
(0.111 0.087) 2.555
= 0.009 M

Y = mx + c
At point of (0.000, 0.087)
1.87 = (0.000 m) + c
c = 0.087
At point (0.200, 0.598)
0.598 = m (0.200) + 0.087
m = 2.555
Therefore, the equation is Y = 2.555x + c

DISCUSSION:
Spectrophotometer was used in this experiment to determine the concentration of the
unknown copper(II) solution. The spectrophotometer is very sensitive because it cannot
detect any solution than contain too low concentration of the solution. The colour of the
solution was very important so that spectrophotometer can absorbed the light and convert into
the value of absorbance. The absorbance value helped to determine the concentration of the
unknown copper(II) solution.

Based on the experiment, standard Cu2+ solution and unknown sample solution were
prepared. At 645 nm of the wavelength, the absorbance of all the solution were measured.
The absorbance value increased due to the increased of the concentration of the known
solution. Spectrophotometer also helped to determine the concentration of the unknown
solution. The concentration was determine through the calibration curve absorbance versus
the concentration. Based on the graph drawn, the gradient is 2.555 as the y-intercept is 0.087.
The formula of the graph is written base on Y = mx + c. the concentration was calculated
through the formula; Y = 2.555x + c. The absorbance of the first unknown solution in the test
tube 5 is 0.348 and the concentration is 0.102 M. the absorbance of the second unknown
solution in the test tube 6 is 0.111 and the concentration is small which is 0.009 M.

QUESTIONS:
1. Plot a graph of absorbance versus concentration (calibration curve) of known Cu 2+
solution.

Graph of Absorbance versus Concentration Of Known Cu2+ Solution


0.7
0.6
0.5
0.4

absorbance

0.3
0.2
0.1
0

0.05

0.1

0.15

0.2

0.25

concentration (M)

2. Determine the concentration of the unknown from the calibration curve.


The concentration of the unknown are 0.1M and 0.01 M.
3. What is the general relationship between concentration and absorbance?
The relationship between the concentration and the absorbance is as the concentration
increasing, the value of the absorbance become greater. The concentration is directly
proportional to the absorbance.

4. Explain how the concentration of the unknown is determined.


The concentration of the unknown is determine using the formula Y = mx + c. The
value of c is determine on the y axis. The m is the gradient of the graph. So, the
concentration is calculated which is the x.

CONCLUSION:
The concentration of the known Cu2+ solution was determined by using spectrophotometer.
The concentration is 0.102 M and 0.009 M.

REFERENCES:
1. Raymond Chang and Kenneth A. Golsby, Chemistry, eleventh edition published by
Mc. Graw Hill copyright 2013.

EXPERIMENT 9:
COMPLEX IONS AND THE SPECTROCHEMICAL SERIES

OBJECTIVE:
To generate the spectrochemical series of ligand by observing the colours of several complex
ions
INTRODUCTION:

Complex ion contain metal ion at the centre with number of the other of the molecules or
ions. The ions or molecules attached to the central by co-ordinate bonds. The spectrochemical
series is a list of ligands that sequences on the ligand strength and the oxidation number of
the metal ions. Ligands modify the difference in energy between the d-orbital called the
crysta-field splitting parameter. The parameter is reflected the differences in color of the
ligand complexes. In this experiment, different ligands were reacts with copper(II) solution
and cobalt(II) solution. The complex ion was formed and different of observation on each of
the ligands. There are 10 ligands which is hydrochloric acid, ammonia, sodium thiosulphate,
oxalic acid, tartaric acid, acetic acid, EDTA, sodium bromide and dimethylglyoxime in 1%
ethyl alcohol.

PROCEDURE:
1. 11 test tubes were cleaned and labelled as 1 to 11.
2. 1 mL of copper(II) solution was measured and transferred into the 11 test tubes.
3. The pH of the saturated solution of oxalic acid and tartaric acid is adjusted by adding
small amount of ammonia solution. The pH paper was used to determine the pH
value.
4. Test tube 1 was set as control. Several drops of ligands were added to the 10 test tubes
containing copper(II) solution and mix. There are the ligands that were used:

Test tube No.


1.
2.
3.
4.
5.
6.
7.
8.
9.

Ligands
Hydrochloric acid
Sodium thiosulphate
Ammonia
Oxalic acid (saturated solution)
Tartaric acid (saturated solution)
Sodium bromide
Dimethyglyoxime in 1% ethyl alcohol solution
Acetic acid
EDTA

5. The change after addition of ligands were observed. Continue to add ligands until a
noticeable colour changes occurred. The ligands solution were compared with the
control.
6. The step 1 to 5 were repeated with the cobalt(II) solution.

RESULT:
Table 1: Observation of complexes solution when ligands were added.
Test
tube

Observation
Ligands

Copper(II) solution

Cobalt(II) solution

Blue solution

Pale pink solution

No change
Blue milky blue

No change

No.
Control (without
1.

ligands)
Hydrochloric acid

2.

Ammonia

3.

Sodium thiosulphate

dark blue solution and

Pale pink blue solution


and precipitate

precipitate
Blue green yellow

Pale pink purple

colourless solution

solution

4.

Oxalic acid

Blue milky blue


solution
Blue milky blue

5.
6.
7.
8.
9.

Tartaric acid
Acetic acid
EDTA
Sodium bromide
Dimethylglyoxime in
1% ethyl alcohol

blue solution and

Pale pink cloudy pink


pink solution and
precipitate
Pale pink purple
solution

precipitate
No change
No change
No change

No change
No change
No change

No change

No change

DISCUSSION:
Based on the experiment, two of complexes were used to react with different types of
ligands. The complexes are copper(II) solution and cobalt(II) solution. The colour of
copper(II) solution is blue solution while the cobalt(II) solution is pink solution. The
experiment is started with copper(II) solution and cobalt(II) solution to reacted with
hydrochloric acid. There is no change of the colour solution for both of the complexes. there
is also no observation on both of the complexes when reacted with acetic acid, EDTA,
sodium bromide and dimethylglyoxime in 1% ethyl alcohol. As ligand, ammonia is added to
the copper(II) solution, the solution slowly turn into milky blue solution and turn into dark
blue solution at the end of the reaction. Blue solution with precipitate was formed as the
ammonia solution was added. There is observation when ligand of sodium thiosulphate
reacted with complexes. The copper(II) solution turned from blue solution into colourless
solution. During the reaction, the blue solution slowly turn from green and yellow solution
before completely turn into colourless solution. Cobalt(II) solution changed colour from pink
to purple solution when sodium thiosulphate was added. Oxalic acid and tartaric acid ligands
were mixed with ammonia solution to become neutral solution before reacted with the

complexes. During the test of the neutralization on the ligands, precaution must be aware so
that the result will not affected. The solution was tested using pH paper until and the addition
of ammonia must be dropwise. Oxalic acid that reacted with copper(II) is observed no
change. Same goes to cobalt(II), the solution are not changing. Last but not least, the
copper(II) complex was reacted with tartaric acid anf formed milky blue with precipitate
solution. The cobalt(II) solution change from pink to purple solution when tartaric acid is
added.

CONCLUSION:
As the conclusion, the spectrochemical series of ligand is generated and the colour of the
several complex ions are observed.
REFERENCES:
1. Raymond Chang and Kenneth A. Golsby, Chemistry, eleventh edition published by
Mc. Graw Hill copyright 2013.