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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 et.
al, 2009). Most traditional gravimetric methods require the knowledge of stoichiometric
reactions, solubility rules and the calculation of mass of substance.

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
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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:



,where m and n are molar masses.

On the other hand, the formula for the percentage of an element in a sample is given as:




where,


(

)
(

)





The experiment 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 a given sample by
precipitating, from basic solution, the hydrated Iron Oxide. The reaction is immediately followed
by a dehydrated reaction to produce the solid Fe
2
O
3.
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).







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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 2
nd
trial for crucible A was being performed. The process was continued until
the 2
nd
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 HNO
3
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 NH
3
. 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
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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
4
NO
3
. 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.




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III. Results and Discussion
The initial part of the experiment focused on the weighing of two crucibles until constant
mass was achieved. When the difference of the two mass
of each crucible from the first trial and the second trial
does not lie within the range of 0.3 mg, the procedure
must then be repeated until successive weighings become
constant in order to draw out all the volatiles and
moisture of the sample.

CRUCIBLE A CRUCIBLE B
INITIAL MASS 26.635 g 26.633 g
1
ST
HEATING 39.424 g 38.299 g
2
ND
HEATING 39.424 g 38.299 g
Figure 6.1 Mass of two crucibles at initial condition and when heated.
On the second-half of the experiment which focuses on the Gravimetric determination of
Iron from the sample, the principle of gravimetric analysis in which one measures the mass of a
material formed in the reaction of the analyte with the
reagent was employed. General procedures included
in gravimetric analysis are precipitation, filtration,
washing, and ignition.
When the sample was added with H
2
O, the product
of the reaction was then added with HCl. Nitric acid
plays an important role when added to the solution to
convert Fe
2+
to Fe
3+
. The solution was heated, diluted
and added with 3M of ammonia until the solution was
basic, which was determined through the use of
litmus paper. Prolonged digestion was then performed
The solution of the unknown sample, added with
H
2
O, HCl, HNO
3
, diluted, added with 3M NH
3
then finally digested, was being cooled down.
Each of the crucibles was heated through the
use of Bunsen Burner.
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on the solution when the precipitate is left to rest in contact with the hot or cold solution for a
period of time. In this process, coagulation for solids is formed. There are factors needed to be
considered while performing the precipitation method. First, precipitates must be unbounded
from soluble impurities and it must insoluble in solution. Precipitates must be readily separated
from the solution by filtration.
By the time the precipitate has settled, the solution was filtered with the use of ashless
filter paper. Using an ashless filter paper, one can avoid improper measurement and get an
accurate mass of the unknown sample without contaminating the sample because it will not
leave ashes behind after combustion. Size and diameter of filter paper should be taken
recognition and must be in accord to the bulk of the precipitates. Moreover, pores of filter must
be smaller than the size of the particle of the precipitates. Filtration of a gelatinous precipitate
done while the solution is still hot because it helps coagulation which means, solvent can pass
smoothly when filtrated.
In washing the precipitate, the properties of ideal
washing liquids should be taken consideration of in
which there is no solvent action on precipitates but must
removes all foreign impurities. It should not form any
volatile product with precipitates, should easily volatile
on ignition, should have no dispersive action on the
precipitates and should not interfere with precipitates
(Gammon et. al, 2009). The precipitate was then subjected to ignition through the use of
Bunsen burner. Ignition of the precipitate was a time-consuming process since the filter paper
in the crucible must be completely dry for faster burning. After ignition, the crucibles were
then placed in a dessicator. The dessicator
contains silica gel beads that remove water
from the precipitate. The crucibles should
immediately be placed inside the
dessicator when it reached room
temperature. If it were not placed in the
dessicator, it is subjected to moisture since
the material used for crucible is porous.
The precipitate obtained from the filtered
solution being ignited through Bunsen burner.
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MASS OF CRUCIBLE MASS OF LID
MASS OF IRON OXIDE
Trial 1 26.638 g 14.457 g 0.272 g
Trial 2 26.638g 14.457 g 0.004 g
Fig.6.2 Mass of Iron Oxide from the difference of the mass of crucible A and its lid.


MASS OF CRUCIBLE MASS OF LID MASS OF IRON OXIDE
Trial 1 28.318 g 10.521 g 0.54 g
Trial 2 28.318 g 10.522 g 0.541 g
Fig.6.3 Mass of Iron Oxide from the difference of the mass of crucible B and its lid.

To compute for the percentage of Fe, the formula below was used,

The following was the computation for the percentage of Fe in the sample in crucible A,

The following was the computation for the percentage of Fe in the sample in crucible B,
The ignited precipitate left black stains on
the inside of the crucible lid.
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The following presents the computation for the expected amount of Fe
2
O
3
that would
precipitate when 0.6094g of FeCl
3
is used:


Using gravimetric factor,

Using stoichiometry for elaboration and details,

Thus, the mass of

obtained is 0.2999 g.
In calculating the percent Fe in the iron (III) oxide, the following calculation was done,

x 100 % = 69.95% of Fe in Iron(III) Oxide.

With the equation of percent relative error,

and a mean of,

= 42.265%
the percent relative error, using the expected result, may be calculated as,

x 100%= 39.58%

In this result, it is proper to say that there is a random error. One error is that the crucibles
used in the experiment were mixed with other crucibles and there is uncertainty whether the
crucible obtained for ignition is still the same crucible. This can be a factor because every
crucible used doesnt have an equal weight. Another error is that, not all of the ashless paper is
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incinerated. There is a few amount of paper when we weighed the sample leaving it to lower or
higher percentage from the theoretical value.

IV. Conclusion
Through gravimetric analysis we were able to determine the percent composition of Fe in
the unknown sample. One of the most important sources of error in this experiment would have
to be the nature of the precipitate was in colloidal form. The form of colloidal precipitation is
caused by adding the precipitant in a hasty manner instead of slowly which is the reason why the
solution in the beaker does not clearly distinguish the separation of the solvent to the precipitate.
Moreover, using high concentrations of analyte and precipitant can also lead to form a not-so-
good precipitate. To achieve a good precipitate, it is important to digest the colloidal sample by
heating. Another error accounted was that the crucibles left in the dessicator were switched to
another group, thus, leaving a hunch that the walls of crucibles were contaminated if the person
who held it with bare hands. If fingerprints were left on the walls of the crucible, it could add
more mass to the crucible when weighed in an analytical balance. Furthermore, when crucibles
were not immediately placed in the dessicator after cooling, the moisture absorbed by the
crucible can also add more weight compared to the original. Crucibles are made in materials that
are porous and can, therefore, easily absorb moisture. The ashless filter paper also took some
time to burn completely. However, in the experiment performed the filter paper was not
completely incinerated.
Judging by the computed result, the experiment performed did not yield great accuracy
because of systematic errors. However, if errors were minimized, the experiment could have
proved that Gravimetric Analysis through the determination of Iron in an unknown sample can
really yield accurate result as much as stoichiometric methods can.






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V. References
Ebbing, Darrell D. and Gammon, Steven D. 2009. General Chemistry. New York:
Cengage Learning.
Hage, David S. and Carr, James D. 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.