EXPERIMENT NO.

6:
GRAVIMETRIC DETERMINATION
OF IRON

ABARRO, JUSTINE MARIE E.

APEGO, JAN-MICHAEL V.
BS CHEMICAL ENGINEERING

CHM141L-A01
A.Y. 2013-2014 1ST TERM
July 2, 2013

I. Introduction
The evolution of scientific knowledge owes its pace to the intelligence of mankind that
paved techniques to be passed to one generation after another, from the discovery of the nature of
atom, to Mendeleevs creation of the periodic table, leading to T.W. Richards and his students
determination of the atomic masses of certain elements. The nature of Analytical Chemistry is
the identification of composition of materials, either through quantitative analysis or qualitative
analysis. The latter involves a method called Gravimetric Analysis that plays significant role in
the determination of the amount of species in a material through the conversion of that species to
a product that can be isolated completely and weighed (Gammon, 2011). Most traditional
gravimetric methods require the knowledge of stoichiometric reactions, solubility rules and the
calculation of mass of substance. A chemical reaction for gravimetric analysis is

where a moles of analyte A contained in the sample reacts with r moles of the
reagent R to form the precipitate AaRr, noted as solid phase (s) in the reaction.
Reference: http://ion.chem.usu.edu/~sbialkow/Classes/3600/overheads/Gravimetry/gravimetric.html

Gravimetry is comprised of sub-procedures such as precipitating the sample, filtering the

solution, washing the precipitate free of contaminants, igniting the precipitate and finally
weighing the precipitate and determining its mass by difference. Precipitation is a process in
which the sample is reacted with another sample to form an insoluble product which is called the
precipitate while the manner of separating the precipitate from the mother liquor is filtration. It is
necessary to assure that the precipitate is free from impurities within, large enough to filter and
negligibly soluble. Washing of precipitate with liquid removes all soluble impurities sticking
with the precipitates (Hage et. al, 2011). After separation, the substance must undergo ignition
before weighing by heating up the precipitate to drive off excess solvent and volatile electrolytes
but it is subjected to change the chemical composition of the precipitate.
An advantage of gravimetric analysis is that identifying the mass of a substance is one of
the most accurate measurements that can be made with errors of less than 0.2% (Hage et. al,
2011). This method of analysis has a real life applications such as the determination of chemicals
in contaminated water, amount of fat a food may contain, chemical analysis of ores and other

industrial materials, in the calibration of instruments, and in the elemental analysis of inorganic
compounds and measurement of the essential elements in plant foods. Although the process is
time-consuming and tedious, the method guarantees an accurate result.
In this experiment, the Gravimetric Determination of Iron, the purpose is to define the
principles and standard techniques involved in precipitation and gravimetric analysis. It aims to
obtain the percent composition of the analyte, which is Iron, in an unknown sample using
gravimetric data. Gravimetric factor is defined to be the algebraic expression that converts grams
of a compound into grams of a single element. It is the ratio of the formula weight of the
substance being sought to that of the substance weighed. The formula for gravimetric factor is:
(m * FW (Sough Substance)) divided by (n * FW (Substance Weight)) where m and n are molar
masses.
It is designed to measure whether the techniques in precipitation and gravimetric analysis were
properly performed by the analysts in order to yield an accurate outcome. Thus, in this
experiment, one will analyze the amount of an iron in an unknown sample by precipitating, from
basic solution, the hydrated Iron Oxide. The reaction is immediately followed by a dehydrated
reaction to produce the solid Fe2O3. The reaction for this experiment is as follows:
Fe3+ + 3H2O FeOOHH2O (s) + 3H
900C

2 FeOOHH2O

Fe2O3 (s) + 2 H2O

Reference: http://students.ycp.edu/~tcummin2/Quant/experiement%20data/quant%20lab%20experiment%202%20info.pdf

The gelatinous hydrous oxide can block impurities. Therefore, the initial precipitate is
dissolved in acid and re-precipitated. Because the concentration of impurities is lower during the
second precipitation, occlusion is diminished (Harris, 2003). The expected percentage value of
Iron in the sample must be around 30%.

II. Methodology
Constant Mass of the Crucible
In the beginning of the process, two crucibles were labeled as crucible A and
crucible B. Both crucibles were weighed so that the initial mass can be bases of comparison to
the mass of the crucibles when heated. The crucible A should be heated in a way of bringing
the flame in and out every two seconds. When the crucible glowed orange, the heating
continued for 10 more minutes while the ceramic supports on the clay triangle also glowed.
After heating, the set-up was cooled until the crucible was at room temperature. The crucible
was placed in a dessicator which was then brought to the balance room. The crucible was taken
out of the dessicator and was weighed in an analytical balance. After recording the mass, the
crucible was placed back in the dessicator to keep the crucible dry. If the crucible were not
placed in the dessicator it is subjected to moisture and, therefore, can make the mass of the
crucible heavier since what was weighed was the mass of the crucible plus moisture. The steps
done with crucible A were repeated with crucible B. Alternately, while crucible B was being
cooled down, the 2nd trial for crucible A was being performed. The process was continued until
the 2nd trial for crucible B was performed. Successive weighing must agree within 0.3 mg.
Gravimetric Determination of Iron
Two trials were performed in this part of experiment. In the first trial, the obtained
mass of the sample, named sample A, was 0.546g and then placed in a 400-mL beaker. For the
second trial, sample B with a mass of 0.606g was also placed in a 400-mL beaker. Both
samples were added with 15-mL water and 10-mL of 3M HCl. Both samples were not filtered
and, therefore, was added with 5-mL of 6M HNO3 to the solution and boiled for a few minutes
until the solution becomes clear yellow. Both samples were diluted to 200-mL distilled water
and were added with 3M of NH3. The solutions were constantly stirred until it was basic. The
basicity was determined through the use of litmus paper. The precipitate was then digested by

boiling for 5 minutes. Since both samples did not boil, the solutions were heated vigorously for
25 minutes and then allowed the precipitate to settle.
In filtering both solutions, an ashless filter paper was used to each in order to
avoid contamination of the sample. Note that sample A and sample B were not filtered
simultaneously due to unavailability of equipments. The ashless filter paper was wetted to
make it stick to the funnel. The supernatant liquid of both solutions were decanted not higher
than 1 cm from the top of the funnel. All solid from the beaker were quantitatively transferred
to the filter paper through the use of rubber policeman and hot 1% (w/w) NH 4NO3. The filter
paper that contained the precipitate was drained thoroughly until it was ready to lift out of the
funnel. The filter paper was folded in a manner in which it must be flatten, the edges were
folded then the top and finally placed inside the crucible with point pushed against bottom. The
crucibles were properly labeled with sample A and sample B.
The crucibles that each contained the samples were left in a container for two
nights. The experiment was then continued, starting with the process of ignition. Each
uncovered crucible was subjected to heating with full heat coming out from the burner to
completely burn the filter paper. Through the use of crucible tongs, the cover was placed on the
crucible, which contained the precipitate formed in sample A, every time the filter paper inside
the crucible was caught with flame. However, the cover was also removed every after a few
seconds to have access to air to avoid turning the carbon into graphite or to avoid reduction of
iron. Moreover, the crucible was also moved every once in a while so that the heat was not
concentrated on one side of the base. By the time, the filter paper was charred, the position of
the crucible was moved in a manner that the flame evenly touches the surface of its base. It was
subjected to full heat for about 15 minutes to ensure complete ignition of the Iron Oxide. When
ignition was completed, the crucible was cooled in air until it reached room temperature level
before it was transferred to the dessicator. The crucible and the lid were individually weighed.
The sum of the recorded mass of crucible and lid was then subtracted to the constant mass of
the heated crucible A without the precipitate and the difference was the mass of Iron Oxide.
The process was repeated for the second trial of crucible A, first trial of crucible B and second
trial of crucible B with both trials in crucible B containing the precipitate were each subtracted
to the constant mass of the heated crucible B without the precipitate. After the weight percent
of iron in each sample was obtained, the average and average deviation were then calculated.

IV. References
Hage, David S. and James D. Carr. 2011. Analytical chemistry and quantitative analysis. New
Jersey: Pearson Prentice Hall.
Harris, Daniel C. 2003. Quantitative chemical analysis. (6th ed). New York: W. H. Freeman and
Company.
Chang, Raymond, and Ken A. Goldsby. Chemistry. 11th ed. 1221 Avenue of the Americas, New
York, NY: McGraw-Hill Companies, 2010.
Davis, Raymond E., M. Larry Peck, and George G. Stanley. "Chapter 3: Chemical Equations and
Reaction Stoichiometry." Chemistry. By Kenneth W. Whitten. Eighth ed.
Belmont,
California: David Harris, 2007.

http://ion.chem.usu.edu/~sbialkow/Classes/3600/overheads/Gravimetry/gravimetric.html