CHM 421 ANALYTICAL CHEMISTRY

EXPERIMENT 8 :

DETERMINATION OF FE IN A FERUM SOLUTION BY

GRAVIMETRIC ANALYSIS

NAME : OMMY MADINA BINTI ABDUL HALIM

STUDENT NUMBER : 2019295426

GROUP NUMBER : RAS2451A

LECTURER’S NAME : MOHD HAFIZ BIN YAAKOB

DATE EXPERIMENT : 11 NOVEMBER 2019

DATELINE EXPERIMENT : 02 DISEMBER 2019

Abstract :

The aim of this experiment is to determine the Fe in a Ferum Solution by gravimetric analysis.
The experiment need four parts which are preparing crucible, precipitation, filtering and
washing the precipitate and drying and weighing the precipitate.For Part A , the crucible
together with its lid was cleaned and heated it in furnace for 10 minutes. Cooled it in a
desiccators and weighted accurately.The next part is start with taking 25.0 mL ferum solution
given was pipette into a 400 ml beaker,25 mL distilled water and covered with watch glass. The
solution was heated to boiling. Then,1 ml of concentrated HNO 3 dropwisely was added.Continue
heating until the solution becomes clear. The solution was diluted to 200 mL with distilled water
and the solution was boiled again. Coutiously,the beaker was transferred to the fume cupboard
and added 1:1 NH4OH into the solution slowly and with stirring until it excess.In conclusion, the
mass of precipitate is 6.8421g which the percentage of analyte in the sample solution (%w/v) is
9.57 %.The Fe contain 2.393 g in 6.8421g Fe2O3 sample solution.

Objectives :

1.To Determine The Percentage Of Ferum In A Ferum Solution

Introduction:

Gravimetric analysis is a technique that can be considered as one of the most

accuratemethod analysis.It done from analyte (soluble form) to analyte ( insolute form) by
separated, dried and weighed which to determine the concentration of analyte in the exact
solution. In this experiment use precipitation method which one of the type of gravimetric
method.In precipitation method,analyte is converted to a sparingly soluble precipitate that is
filtered,wash free of impurities and convert to a product of known composition by suitable heat
treatment.Then this product will weighed.

The concentration of Fe can be determined when Fe(II) is oxidized to Fe(III) and then
precipitated as ferric oxide hydrates,Fe2O3.XH2O. To produce ferric oxide,Fe2O3,filtered,washed
and dried the precipitate. It can calculate the mass of Fe in the solution since Fe 2O3 is a stable
compound.

Method :

A.Preparing a Crucible

The crucible together with its lid was cleaned and heated it in furnace for 10 minutes.
Cooled it in a desiccators and weighted accurately.

B.Precipitation

25.0 mL ferum solution given was pipette into a 400 ml beaker,25 mL distilled water and
covered with watch glass. The solution was heated to boiling. Then,1 ml of concentrated HNO 3
dropwisely was added.Continue heating until the solution becomes clear. The solution was
diluted to 200 mL with distilled water and the solution was boiled again. Coutiously,the beaker
was transferred to the fume cupboard and added 1:1 NH 4OH into the solution slowly and with
stirring until it excess.

C. Filtering and Washing the Precipitate

The precipitation was filtered by decantation using filter paper no.41 without stirring the
solution to ensure that most of the precipitate will be left behind in the beaker. Then the
precipitate was washed with 30 mL warm 1% NH4OH solution. The solution was poured into the
filter funnel leaving behind most of the precipitate. Repeated this for two times and finally
transferred all the precipitate quantitatively into the funnel. Finally,the precipitate was washed
in the funnel using warm distilled water and the filtrate was tested for chloride with acidic silver
nitrate solution. If the test turn out positive,the washing process was repeated with more
distilled water.
D. Drying and Weighing the Precipitate

The filter paper was transferred containing all the precipitate into the crucible that have been
prepared earlier on. The crucible was heated using a Bunsen burner with a small flame at the
beginning until all the paper has burned. The flame was increased and continue heating for
another 20 minutes. The heating process was repeated until a constant mass is
obtained.Alternatively,if time does not permit,the crucible containing the precipitate was placed
and filter paper into muffle furnace. The position of your crucible on the piece of paper was
recorded at the furnace. The precipitate will be heated at 600° overnight. Once the crucible is
cooled, the mass of the crucible and the precipitate was weighed. The precipitate was poured
into a plastic wrap, folded and the plastic wrap was stapled at the top so as to contain the
precipitate inside the wrap.
Results :

Weight of empty crucible : 32.1565 g

Weight of crucible + precipitate = 38.9806 g

Weight of precipitate , g = 6.8241

Calculation :

Fe2+ Fe3+

Fe3+ + O2- Fe2O3xH2O

Analyte : Ferum

Precipitate : Ferum (II) Oxide (Fe2O3 )

Mass of precipitate = 6.8241 g

Moles of precipitate = 6.8241 g / 159.69 g mol -1

= 0.043 mol

1 mol of Fe2O3 = 1 mol of Fe

Mass of analyte = 0.043 mol (55.85 g mol-1 )

= 2.393 g

Percentage of analyte (%w/v) = Mass of analyte

X 100
Volume

= ( 2.939 g / 25 mL ) x 100

= 9.57 %
Discussion :

This experiment to determine the percentage of Ferum in Ferum solution using

gravimetric analysis.The experiment need 4 parts which are preparing crucible, precipitation,
filtering and washing the precipitate and drying and weighing the precipitate.This experiment
follow the Law of Conservation of Mass which state that the mattter can interchanged from one
form to another.Law of Conservation also statees that mixture can be separated and the pure
substances can be decomposed but the amount of mass remains .

This experiment which Iron (II) ion will oxidized to form Iron (III) ion to form
precipitate.The precipitate is ferric oxide hydrates which need to filtered, washed and dried to
produce Fe2O3.The colour is dark-brown when it reacts with NH 4OH which the function to
distinguish the colour so that the presence is much visible.

The mass of precipitate is 6.8421g which the percentage of analyte in the sample
solution (%w/v) is 9.57 %.The Fe contain 2.393 g in 6.8421g Fe 2O3 sample solution.In this
experiment got some errors make the results less accurate which is need to test the filtrate with
silver nitrate solution.If turn out positive,the washing process with more distilled water.

This experiment need to take with cautiously because the smell of NH 4OH will
distributed in laboratory room so it need to carried out in the fume cupboard.This experiment
need to followed strictly in a gravimetric analysis to minimize the desirable of the analysis and
more reliable.

Conclusion :

The Percentage of Ferum in a Ferum solution (%w/v) is 9.57 % has been determined
from the mass of precipitate which is 6.8421g that ferum is 2.393g in that ferum solution.
Reference :

Justin Marie (n.d) , CHM130 GRAVIMETRIC FULL REPORT.Retrieved December 12,2019 from
nnnnnnnnhttps://www.academia.edu/4117183/CHM130_GRAVIMETRIC_FULL_REPORT

Naz Helmi (July 22,2016), EXPERIMENT 8 : DETERMINATION OF Fe IN A FERUM SOLUTION BY

,,,,,,,,,,,,,GRAVIMETRIC ANALYSIS CHM42, Retrieved December 12,2019 from
https://www.scribd.com/document/318994222/EXPERIMENT-8-DETERMINATION-OF-Fe-IN-A-
FERUM-SOLUTION-BY-GRAVIMETRIC-ANALYSIS-CHM421