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Name: DIONGCO, MARC ANGELO V. Date Performed: 23 June 2016

MANALO, JEAN LOUISE B. Date Submitted:

Experiment 2
GRAVIMETRIC DETERMINATION OF IRON

I. INTRODUCTION

Gravimetry is any method in which the signal is a mass or change in mass. There are four kinds: precipitation
gravimetry, electrogravimetry, volatilization gravimetry and particulate gravimetry (Harvey, 2000). Gravimetric
determination of iron is an example of precipitation gravimetry. It is based on the formation of an insoluble
compound after the addition of a precipitating reagent, called a precipitant, to a solution of the analyte (Harvey,
2000). In this experiment, iron in the form of Fe3⁺, is precipitated as hydrous ferric oxide from a slightly acidic,
slightly basic or neutral medium (Harris, 2010):

Fe3⁺ + 3 OH¯ + n H2O ⇌ Fe(OH)3 • nH2O

ferric ion

The precipitate formed is gelatinous due to presence of water. However, the iron precipitated as hydrous ferric
acid is not complete if the form of iron present is not in its Fe3⁺ form. The ferrous iron, Fe2⁺, present in the
medium can be oxidized to Fe3⁺ using bromine water or nitric acid before precipitation occurs (Harris, 2010).

3 Fe2⁺ + NO3¯ + 4 H3O⁺ ⇌ 3 Fe3⁺ + NO + 6 H2O

ferrous ion ferric ion

Formation of FeSO4•NO complex can be observed as the solution starts to darkens, and as the oxidation of Fe2⁺ to
Fe3⁺ progresses, the color changes to the bright yellow color of the ferric ion (Harris, 2010).

Based on solubility rules, insoluble hydroxides are formed from every metallic ion other than from alkali metal
ions in basic solution (Chang and Overby, 2011). Therefore, in order for selective precipitation of Fe(OH)3 to
occur, the concentration of hydroxide ions, OH¯, must be controlled, and this can be done by controlling the pH of
the solution medium. Instead of using strong bases, weak bases are very useful in limiting the OH¯ concentration
(Harris, 2010). In this exercise, aqueous ammonia, a weak base, is used as precipitant.

To turn the precipitated hydrous ferric oxide to its anhydrous pure form, Fe(OH)3, the hydrous form is subjected
to high temperatures to obtain the anhydrous form. This anhydrous ferric oxide is in its definite composition and
can be weighed (Harris, 2010).

2 Fe(OH)3 • nH2O → 3 Fe2O3 + (2n+3) H2O

This experiment aims to show the concepts, principles and techniques involved in precipitation gravimetry. It also
aims to apply techniques such as precipitation, filtration, washing and ignition in the quantitative determination
of iron and to determine the amount of iron present in a given unknown sample.
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II. SCHEMATIC DIAGRAM OF PROCEDURE

A. Taring of Crucible

B. Gravimetric Determination of Iron

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III. DATA AND RESULTS

Unknown Code/Number: _______

Table 2.1. Taring of crucibles

Trial 1 Trial 2

Weight of crucible, g

Constant weight of crucible, g

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Table 2.2. Gravimetric determination of iron

Trial 1 Trial 2
Weight of sample container + sample, g
Weight of sample container – sample, g
Weight of sample used, g

Weight of crucible + Fe2O3, g

Constant weight of crucible + Fe2O3, g

Weight of Fe2O3, g
% Fe2O3
±d
% Fe
±d

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