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Objectives: FIGURE A: Example of Coordination Compounds

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OBJECTIVES

1. To synthesize chloropentaamminecobalt (III) chloride.


2. To identify whether chloride atom is coordinated to cobalt or not.

INTRODUCTION
What is coordination compound? Coordination compound is when non metal atoms known as
ligands surround the central metal atom by chemical bonds [ CITATION Jac \l 17417 ]. Plus, it
can be also known as transition metal. Then, coordination compound can be differentiated
with complex ions by the presence of counter ions. For example, tetracyanonickelate (II) ion
is a complex ion while tetraaquadibromocobalt(III) nitrate is a coordination compound.
Therefore, coordination compounds consist of metal atom, ligand and counter ion.

FIGURE A: Example of Coordination Compounds

Then, coordination compound can be synthesized. For example, chloropentaamminecobalt


(III) chloride. The characteristics of this compound, is that it is red-violet, diamagnetic and
water-soluble salt. There are differences between cobalt +2 and cobalt +3 is their stability.
Therefore, cobalt+2 is known to have higher stability than cobalt +3. Consequently, cobalt+2
will have higher oxidation state compared to cobalt +3. The equation for preparation of this
compound can be seen in Figure B.

FIGURE B: Equation of preparation of chloropentaamminecobalt (III) chloride

The application of synthesizing chloropentaamminecobalt (III) chloride in our daily lives is


that it is used in electrical appliances with high temperatures and also in microporous hybrid
material with organic and donors when combine with other compounds [ CITATION Syn17 \l
17417 ].

APPARATUS

1. Googles
2. Fume hood
3. 100 ml graduated cylinder
4. Electronic balance
5. Filter paper
6. Magnetic stirring plate
7. Burner
8. Funnel
9. Aluminium foil

CHEMICALS

1. Ammonium chloride
2. Concentrated aqueous ammonia
3. CoCl2.6H2O
4. 30% hydrogen peroxide
5. Conc. HCl
6. Ethanol
7. Distilled water

PROCEDURE

1. In a fume hood, 5 g of ammonium chloride was added to 30 ml concentrated aqueous


ammonia in a 250 ml Erlenmeyer flask.
2. The ammonium chloride solution was stirred vigorously using a magnetic stirring
plate while 10 g of finely divided CoCl2.6H2O was added in small portions.
3. 8 ml 30% hydrogen peroxide was added to the brown Co slurry using a burette that
had been set up in the hood and filled by the laboratory assistant. An addition rate of 2
drops per second was sufficient, but to avoid excessive effervescent in this exothermic
reaction, this step was taken carefully.
4. When the effervescent had ceased, 30 ml conc. HCL was added with continuous
stirring, and 1-2 ml was poured at a time. At this point, the reaction had been removed
from the hood.
5. The solution was heated to 60 ℃ using a heater with occasional stirring. The
temperature was held between 55℃ and 65 ℃ for 15 minutes, which this incubation
period was necessary to allow complete displacement of all aqua ligands.
6. 25 ml of distilled water was added, and the solution was allowed to cool to room
temperature.
7. The purple product was collected by filtration through a Buchner funnel; washed three
times with 7.5 ml cold distilled water and twice with 7.5 ml ice-cold ethanol.
8. The product the transferred to crystallizing dish, loosely covered with aluminium foil,
and was allowed to dry.

RESULT

1 Mass of CoCl2.6H2O used 10.0003

2 Moles of CoCl2.6H2 O used 0.0420 mol

3 Theoretical yield of [Co(NH3)5Cl]Cl2 moles 0.0420 mol

4 Theoretical yield of [Co(NH3)5Cl]Cl2 mass 10.5257 g

5 Mass of [Co(NH3)5Cl]Cl2 obtained 4.9082 g

6 Percent yield of [Co(NH3)5Cl]Cl2 46.62%

2) Moles of CoCl2.6H2 O used

m
n=
M

10.0003
=
237.9309
=0.0420 mol

3) Theoretical yield of [Co(NH3)5Cl]Cl2 moles

2CoCl2 6H2O + 2NH4Cl + 8NH3 +H2O2 2[Co(NH3)5H2OCl] Cl2 + H2O

2 moles CoCl2.6H2 O = 2 moles [Co(NH3)5Cl]Cl2

Ratio 2:2

0.0420 mol = 0.0420 mol

Theoretical yield moles = 0.0420 mol

4) Theoretical yield of [Co(NH3)5Cl]Cl2 mass

10.0003 1 molCoCl 26 H 2O 2mol 2[Co( NH 3)5 H 2 OCl]Cl 2


= x x x
1 237.9 g CoCl 2 6 H 2 O 2mol CoCl 2. 6 H 2O
250.4 g 2[Co( NH 3)5 H 2 OCl]Cl 2
1 mol

=10.5257 g2[Co(NH3)5H2OCl] Cl2

5) Mass of [Co(NH3)5Cl]Cl2 obtained

5.3755 – 0.4673 = 4.9082 g

6) Percent Yield

actual yield
= x 100%
theoretical

4.9082 g
= x 100%
10.5257 g

=46.62%
DISCUSSION

The aim of this experiment was to synthesize chloropentaamminecobalt(III) chloride. The


apparatus that we used in this experiment were goggles, fume hood, 100 ml graduated
cylinder, electronic balance, filter paper, magnetic stirring plate, burner, funnel and
aluminium foil. In this experiment, magnetic stirring plate was used to ensure the solution
was homogenous in consistency at certain temperature. Magnetic stirring plate consists of
rotating magnet that creates rotating magnetic field. Therefore, by using this, solution was
quickly spin and mixing the solution will be a lot easier [ CITATION Mar151 \l 17417 ]. The
chemicals that we used in this experiment were ammonium chloride, concentrated aqueous
ammonia, CoCl2.6h2O, 30% hydrogen peroxide, concentrated HCl, ethanol and distilled
water. As the chemicals were highly concentrated, the procedure was ran in the fume hood
for safety.

Firstly, 5g of ammonium chloride was added to 30 ml concentrated ammonia in a


250ml of Erlenmeyer flask. This step was all done in a fume hood. Then, the ammonium
chloride solution was placed on a magnetic stirring plate while adding 10.003g of
CoCl2.6H2O. It must be stirred ]vigorously to make an efficient mixing [ CITATION Ali19 \l
17417 ]. After that, 8 ml of 30% hydrogen peroxide was added in 2 drops per second to the
Erlenmeyer flask that contained brown Co slurry by using a burette in the fume hood. Next,
when the bubbles have stopped 30 ml of concentrated HCl was added into the flask while
continuing stirring and pouring 1-2 ml at a time. After that, the solution was heated to 60°C
on a hot plate. For 15 minutes, the temperature must be in between 55°C to 65°C to allow
complete displacement of ligands. Then, the flask was added with 25ml distilled water and
then was allowed to cool in room temperature. As soon as the solution achieved the room
temperature, we use Buchner funnel to collect purple product by using filter paper on top of it
for filtration. The function of Buchner funnel is a device used for pressure assisted filtration.
A vacuum underneath the filter allows atmospheric pressure on the product to force the liquid
through the filter paper. [ CITATION Ohl19 \l 17417 ] . The product in the flask was poured to the
Buchner funnel and was washed for 3 times with 7.5 ml cold distilled water, and twice with
7.5 ml ice-cold ethanol. When the filtration was over, the product was transferred to as
crystallizing dish covered with aluminium foil and was allowed to dry. After several hour, the
product [Co(NH3)5Cl] Cl2 has been dried and it was taken to the analytical electronic balance
to weigh the mass of product obtained.

As for the results, the mass of CoCl 2.6H2O that was used was 10.003g. Therefore, by
using a formula of mass divided by formula mass, the moles of CoCl 2.6H2O that was used,
was 0.0420 mol. Next, theoretical yield was known as a theory of result of the product from a
perfect chemical reaction [ CITATION Ann192 \l 17417 ]. The theoretical yield of [Co(NH3)5Cl]
Cl2 moles was 0.0420mol while the theoretical yield mass was 10.5257g. The theoretical
mole was obtained from the equation (Figure A) where the ratio was 2:2.

FIGURE A: Equation of chloropentaamminecobalt (III) chloride

After that,the mass of [Co(NH3)5Cl]Cl2 was 4.9082g. By having the values needed, we were
able to obtain the percent yield. Percent yield was defined as the ratio of the actual yield and
the theoretical yield, where the formula was actual yield divided by theoretical yield and
multiplied by 100% [ CITATION Ann191 \l 17417 ] . Therefore, the percent yield of
[Co(NH3)5Cl]Cl2 was 46.62%. The result obtained was not 100% may due to incomplete
reactions or other factors that had influenced the chemical reaction in [Co(NH3)5Cl]Cl2.

Some errors can be occurred while preparing the sample such that the eyes is not
parallel to the pipet and measuring cylinder and the wrong measurement when took the
readings. The experiment must be in a fume hood because we use ammonia that is a
concentrated basic reagent with a strong odor. Be careful to not spill or spatter this reagent on
your skin and use gloves to handle it. Next, try to avoid spilling, as this stuff makes a mess. If
you spill any, clean it up immediately with a wet paper towel, before it stains someone’s
clothes. After the experiment, discard the filtrate (liquid) in the aqueous cobalt waste
container.

Conclusion
The experiment was successful and the purpose of the experiment is to synthesize
chloropentaamminecobalt (III) chloride and whether the chloride atom is coordinated to
cobalt or not was achieved. The purple coloured complex compound of
chloropentaamminecobalt (III) [Co (NH3)5Cl] Cl2 was synthesized and the percentage yield is
46.62%.

References
college, O. (2019). Buchner Funnel. Retrieved November 21, 2019, from Ohlone College:
http://www2.ohlone.edu.labs.buchner

Frontier, A. (2019). Tips and Tricks : Stirring. Retrieved November 21, 2019, from Tips and Tricks :
http://chem,chem.roschester.edu

Halpren, J. (n.d.). Coordination Compound. Retrieved from Encyclopaedia Britannica:


https://www.britannica.com/science/coordination-compound

Helmenstine, A. M. (2019, July 7). Percent Yield Definition and Formula. Retrieved from ThoughtCo:
https://www.thoughtco.com/definition-of-percent-yield-605899

Helmenstine, A. M. (2019, July 14). Theoretical Yield Definition in Chemistry. Retrieved from
ThoughtCo.: https://www.thoughtco.com/theoretical-yield-definition-602125

Loos, M. (2015). Magnetic Stirrer. Retrieved from ScienceDirect:


https://www.sciencedirect.com/topics/engineering/magnetic-stirrer

Synthesis of Chloropentaamminecobalt (II) Chloride: Characterization and study of its Application.


(2017, May 17). Retrieved from inslideshare:
https://www.slideshare.net/saimkhalid04/synthesis-of-chloropentaamminecobaltiii-chloride

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