Analytical Chemistry Laboratory 2

Electrogravimetric Determination of Copper

Mr. *****

Department of Chemical Engineering and Chemistry, Mapua Institute of Technology

Electrogravimetric analysis is an easy and accurate method for determining metal

concentrations using electrochemistry. The element copper that was determined was deposited as
a solid on a pre-weighed electrode throughout the reduction process, and was measured by the
weight gained by the electrode. The experiment was performed in two trials using sample # 2.
The average percentage of copper in the solution was 17.72%.

complete. After the solution was heated, it

Objective was then cooled and diluted to 100 mL. This

The main purpose of this
experiment is to determine the percentage of
copper in the solution by electrogravimetric
analysis.
Discussion
Overview
In electrogravimetry, a metal ion is
quantitatively (>99.9%) electroplated onto a
preweighed “working” electrode almost
always as the solid metal. This takes place at
the negative electrode or cathode, which is
defined as that electrode at which reduction
takes place. From the gain in mass of the
electrode, the amount of metal in the sample
can be calculated – assuming no interferants
are also electroplated onto the electrode. A
few metal ions can be deposited in some
chemical form onto the anode, the electrode
at which oxidation takes place.
The unknown sample containing
copper was prepared by weighing (to the
nearest 0.1 mg) 1-g samples into a 250-mL
beaker. 25 mL of water was added, followed
by 4 mL H2SO4 and 1 mL HNO3. It was then
heated below boiling until solution is
procedure was repeated again for the second
trial.
Copper (Cu) is a heavy metal whose
unbound ions are toxic. Copper salts are
irritants to the skin, eyes, and mucous
membranes. Ingestion of copper salts may
cause vomiting, diarrhoea, hemorragic
gastritis, and excessive salivation. Toxicity
is primarily due to accidental and suicidal
attempts, and results in intravascular
hemolysis, methemogloninemia, renal
failure and often death. Vineyard sprayers
using a solution containing aqueous copper
sulphate developed granulomatous and
fibrotic lung lesions. Inhalation of copper
dust and fume results in irritation of the
respiratory tract, ulceration and perforation
of nasal septum, metallic or sweet taste, and
in some instances, discoloration of the skin
and hair. The inhalation of metal fumes
produced at high temperature, such as
welding, may cause "metal fume fever", an
influenza-like (benign) illness. High copper
content in drinking water and food may
contribute to the development of severe liver
damage in infants.
As with all of the other industrial
activities, copper production is highly
subject to environmental regulation related
to air quality. The main pollutant of concern
that results from the copper smelting process
is sulfur dioxide. Uncontrolled copper
smelting processes emit large quantities of
this, which can have major impacts on
human health. Because of the consequences
evolving from these processes, The Clean
Air Act was established, setting standards to
regulate the “criteria pollutants”. In addition
to the air quality concern with the mining
and mineral processing of copper, there are
also many impacts on the environment
dealing with the water quality and waste
disposal. These adverse water quality
impacts are caused primarily by land
disposal practices that fail to contain wastes,
by run-on and run-off controls that are
inadequate to prevent surface water from
flowing through impoundments, or by
groundwater infiltrating surface
impoundments. These open-pit mining
methods also can cause disturbances that can
lower the water table in an area, causing
water shortages, land subsidence, and
fracturing. In response to these effects, the
EPA administered four major programs to
help control the water quality and waste
disposal practices at domestic copper mining
operations. The first program was The Clean
Water Act, which imposes limitations on
point sources and requires permits from the
National Pollutant Discharge Elimination
System for any discharge of pollutants. The
next program was the Resource
Conservation and Recovery Act, regulating
the generation, transport, and disposal of
hazardous and solid wastes. Another
program was the Superfund, which designs
priorities for and oversees the clean up of
these polluted sites. The fourth program was
the Safe Drinking Water Act, designed to
protect the quality of public drinking water
supplies. As for the adverse impacts on
copper wastes, waste management practices
have been established to set acceptable
levels to control areas such as the
minimization, collection, and treatment of
mine drainage, mill process water, and
contaminated surface damage. These areas
of control are also for handling, storage,
ultimate disposal of tailings and waste rock,
and reclamation of the site to minimize long
term environmental effects once active
mining has ceased.
Methodology
Preparation of Electrodes.
The platinum electrodes were
immersed in hot 6 M HNO3 for about 5
minutes. It was then washed with distilled
water and rinsed with several small portions
of ethanol, and was dried in an oven at
110ºC for 2 to 3 minutes. It was then cooled.
Electrolysis.
The cathode was attached to the
negative terminal and the anode to the
positive terminal of the electrolysis
apparatus. The samples were placed in the
beaker and the electrode was immersed in it.
The electrolysis was then commenced
maintaining a current of 0.5 A (2 V) with
stirring operating for about 30 minutes.
After the duration, the completeness of the
electrolysis was tested by removing one
drop of the solution with a medicine
dropper, and was mixed with a few drops of
NH3(aq) in a small test tube. The mixture
did’t turned blue therefore electrolysis was
complete. The cathodes were dried for about
3 minutes at 110ºC, and were cooled in air
before weighing them.
Instrumentation
With this electrolysis apparatus, the
cathode absorbs the copper ions in the
solution.
Interpretation
 The data obtained for sample # 2 co-deposition is unlikely when the right
were as follows. conditions are established.
The copper metal formed by this
Trial 1: process adheres to the platinum surface. The
cathode becomes plated with copper. In
Weight of sample 1.0048 g effect the passage of current removes Cu 2+
Weight of electrode 38.2712 g from the aqueous solution, and the
Weight of electrode with Cu 38.4418 g calculated average value of Cu2+ present in
Weight of Cu 0.1706 g the solution was 17.72 %.
% Cu 16.98%
References
Trial 2:
1. Christian, G.D., Analytical Chemistry, 6th
Weight of sample 1.0006 g edition, New Jersey, John Wiley, 2004.
Weight of electrode 38.2819 g
Weight of electrode with Cu 38.4665 g
Weight of Cu 0.1706 g 2. Skoog, D. A., and Leary, J. J., Principles
% Cu 18.45% of Instrumental Analysis, 4th edition,
Saunders, New York 1992.
A dilute, acidified solution of
copper ion was plated onto a pre-weighed 3. Harris, D.C., Quantitative Chemical
platinum electrode: Analysis, 3rd edition, Freeman, New York,
Cu2+(aq) + 2e- → Cu(s) 1991.
The weight of the copper was
calculated by subtracting the initial weight 4. U.S. Congress, Office of Technology
of the electrode from the final weigh of the Assessment. “Environmental Aspects of
electrode. The result was divided by the Copper Production.” Copper: Technology
weight of the sample multiple by one and Competitiveness. September 1988.
hundred, to get the % Cu. The average
percentage of copper was calculated by
addin the % Cu of the two trial divided by 2.
The resulting value was 17.72 %.
The margin of error was fairly large.
One possible answer was that during the
preparation of sample, the solution was not
evaporated to 5 mL as it should be.
The nitrate ion in this experiment
acts as a "cathode depolarizer". If it were not
present, H+ ions in the solution would be
reduced at the cathode and form H2 gas. This
would prevent the element (copper) from
adhering properly, resulting in a porous and
poorly adherent copper plate. Small pieces
would fall off and ruin the analysis.

Conclusion

Gravimetric analysis is one of the

most accurate and precise methods of
macroquantitative analysis. Its main
advantages are that filtration is avoided and