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Issue No.2
August 6, 2014
ABSTRACT
Electrogravimetry is a method to determine the amount of metal present in the analyte using electroplating at the
electrode. This experiment aimed to apply electrogravimetric technique in determining the amount of metal in
aqueous solutions of their divalent salts and to separate metals from its mixture. The chlorine ion of the salts NiCl 2,
CuCl2 and CoCl2 were removed and reagents such as H2SO4 and NH4OH were added to produce analytes of pure Ni,
Cu and Co, and mixture of Ni-Cu and Co-Cu. These were subjected to Eberbach Electroanalyzer where the change
in weight of electrodes was equal to the amount of metal after electroanalysing with the aide of air and oven drying.
The amount of pure Ni and Cu were observed near to their actual value while the amount of Cu in the mixture was
greater than the actual value. After performing the experiment, the two purposes were obtained.
INTRODUCTION
Electroanalytical chemistry is composed of methods
that are based upon the electrical properties of a
solution of the analyte when it is made part of an
electrochemical cell.
Electrogravimetry is one of the two electroanalytical
methods. The product of electrogravimetry is
deposited quantitatively on an electrode by an
electrolytic reaction and the amount of product is
determined by weighing the electrode before and
after electrolysis. Electroplating is done at the
negative electrode or the cathode, where reduction
takes place. When the electrode gains weight, the
amount of the metal can be calculated. The goal of
electrogravimetry is to electroplate 100% of the
desired analyte of the solution.
There are two types of electrogravimetry; controlledpotential and controlled-current. In controlledpotential, the potential at the electrode is kept
constant while plating out all the analyte. The current
decreases as the metal is plated out. This type is
effective when 2 or more metals are plated out where
the metal ion that is more easily reduced can be
plated out quantitatively without the involvement of
the other. In controlled-current, large amount of
voltage is needed to sustain a constant current to flow
throughout the cell.
EXPERIMENTAL SECTION
The reagents used were 85% hydrazine hydrate,
concentrated H2SO4 and NH4OH, CuCl2, NiCl2 and
CoCl2 samples. The main instrument used was the
Eberbach Electroanalyzer. For the solution to be
prepared, the glasswares and apparatus used were
pipet, beakers, thermometer, watch glass, stirring rod,
wash bottle, Bunsen burner and hot plate.
Average wt. of
metal
0.616 0.0135
0.1827 0.1537
0.616 5.0576
x 10-3
Average time
consumed
30 1.6859
35.84 11.23
30 1.6859
%
error
4.6%
74%
3.2%
Average wt. of
metal
0.168 0.094
0.3243 0.4561
Average time
consumed
30.32 1.997
29 1.6859
%
error
76%
54%
CONCLUSION
After performing the experiment, the two objectives
were successfully obtained. For the first objective,
the researcher had successfully measured the amount
of nickel, copper, and cobalt present in the respective
analytes which were close to the true value of the
metal. The amounts of Nickel-Copper and CobaltCopper were also measured though the percent errors
are very high due to some sources such as confusion
in procedure and incomplete drying. For the second
objective, the metals in mixture were separated by
REFERENCES
1. Skoog, D. A., Holler, F. J., and Nieman, T. A.
(1998) Principles of Instrumental Analysis, 5th Ed.,
Thomas Learning, Inc.
2. Skoog, D. A., Holler, F. J., West, D. M., and
Crouch, S. R. (2011) Fundamentals of Analytical
Chemistry, 8th Ed., Cengage Learning.
3. Owen, J. F., Patterson, C. S., and Rice, G. S.
(1983), Electrogravimetric Determination of Cobalt,
Nickel and Copper in Presence of Chlorine Ion,
Analytic Chemistry, 990-992, ACS Publication.
4. Skoog, D. A., Holler, F. J., and Crouch, S. R.
(2011) Principles of Instrumental Analysis, 6th Ed.,
Thomas Learning, Inc.
5. Habib, M. A. (1988) Electrogravimetric
characterization of the electrochromic polyaniline
film surface, Langmuir, 1302-1304, ACS Publication.
Website:
1.
http://staff.tanta.edu.eg/uploads/unit_5_electrogr
avimetry_and_coulometry.pdf