Preparation and Analysis

of K3[Fe(C2O4)3]·3H2O

Aylin ÇOBAN - 2507960

Session 1

20 Aralık 2021

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 PURPOSE:

In this experiment, we will learn how to prepare the complex

trioxalatoferrate(III) anion and isolate it as potassium trioxalatoferrate(III)

trihydrate. We will also learn about the photochemical reduction reactions
by investigating the interactions of potassium trioxalatoferrate(III) trihydrate
with light.

THEORY:
Photochemical reaction, a chemical reaction initiated by the absorption
of energy in the form of light. The consequence of molecules’ absorbing light
is the creation of transient excited states whose chemical and physical
properties di er greatly from the original molecules. These new chemical
species can fall apart, change to new structures, combine with each other or
other molecules, or transfer electrons, hydrogen atoms, protons, or their
electronic excitation energy to other molecules. Excited states are stronger
acids and stronger reductants than the original ground states.

Radiant energy can be characterized by two variables:its wavelength and

its frequency which are related to another by the relation;

C=V.λ

C is the speed of light, 3.00 x 10⁸ meters per second.

V is the frequency of electromagnetic waves.
λ Lambda is the wavelength of electromagnetic waves.

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 Wavelength is the distance from crest to crest and frequency is the
number of waves passing through a point in a time interval.

When matter interacts with radiant energy various processes such as

transmittance, re lection, absorption and scattering may take place.
Absorption of light by a species results in rotational, vibrational transitions or
electronic excitation in the energy levels of the molecule. The amount of
energy absorbed, E, is de ined as

E=h.V
Where h is the Planck’s constant.

A sample can absorb radiation if the energy of the radiation is equal to

the energy di erence between the energy states. When a molecule absorbs
radiation, it becomes excited. The excited species may lose the excess
energy by various processes, such as emission, radiation less relaxations etc.

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 A chemical change may also occur as a result. Photochemistry is the
study of chemical reactions produced by light, such as ionization,
isomerization, dissociation or direct reaction etc., that may be brought about
by the absorption of light.

Potassium trioxalatoferrate(III) trihydrate is a green crystalline salt,

soluble in hot water but rather insoluble in cold water. It can be prepared by
the reaction of K2C2O4.H2O with FeCl3.6H20 according to the reaction
given below.

3K2C2O4.6H20(aq) + FeCl3.6H2O(aq) ———> K3[Fe(C2O4)3].3H2O(aq) + 3KCl(aq) + 6H2O(aq)

MATERIALS:

Chemicals Apparatus

Iron(III) chloride hexahydrate Beakers (250 mL)

Light source

Potassium oxalate monohydrate Filter paper

Opaque Objects
Pipette

0.1 M potassiumferricyanide solution Glass rod

2 M hydrochloric acid solution Test Tube

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 PROCEDURE:
A. Preparation of trioxalatoferrate(III) trihydrate
1) Weighed approximately 9.0 g of hydrated potassium oxalate into a
250 mL beaker.
2) Added 30.0 mL of water into the beaker wit K2C2O4.H2O. Using the
bunsen burner, heated my solution in the beaker gently until the solid
dissolved.
3) Weighed 4.4 g of Iron(III) chloride hexahydrate in a new beaker.
4) Dissolved the solid in 10 mL of cold water using a stirring rod.
5) Added the cold solution to the warm oxalate solution while stirring
gently with a glass rod. Placed the beaker into an ice-water mixture, away
from the sunlight and allow let the mixture cool down.
6) When the solution cooled down, collected the potassium
trioxalatoferrate(III) trihydrate by decantation.

Separation by decantation

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 B. Blueprinting
1) Transferred approximately 1/3 of potassium trioxalateferrate(III)
trihydrate crystals we obtained in part A to a test tube. Tried to dissolve
the crystals in minimum amount of cold water using a stirring rod.
2) Wet a ilter paper with the potassium trioxalateferrate(III) trihydrate
solution.
3) Placed the wet ilter paper in an oven to dry for a few minutes.
4) When the ilter paper is dry, placed an eraser on it.
5) Irradiated the paper for a few minutes using a light source.
6) Wet the ilter paper with potassium ferricyanide solution in sink using
a pipette.
7) Took the ilter paper and dip into a beaker illed with distilled water to
wash o the excess ferricyanide solution.

C. Photochemical Reaction
1) Dissolved the remaining potassium trioxalateferrate(III) trihydrate
crystals in 50 mL water in a clean beaker. Added 3.0 mL of 2.0 M
hydrochloric acid and swirled the beaker.
2) Took three clean test tubes, and labeled them as 1, 2 and 3. To each of
three labeled test tubes, transferred 10.0 mL of potassium
trioxalateferrate(III) trihydrate solution.
3) Took one of the tubes and put it in the cabinet under the bench away
from the right. Took the other tubes and irradiated them with the light
source for 5 and 15 minutes.
4) Added 1 mL of 0.1 M potassium ferricyanide solution to all three test
tubes and mixed the solutions well using a stirring rod.

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 RESULTS:
After carefully washing the ilter paper with potassium ferricyanide
solution, which we irst wetted and then dried, and then kept under the light
source in one of the stages of the experiment, we observed that the part that
did not see the light was of a di erent color(dark blue) and the part that saw
the light was of a di erent color(green). In part C, I observed that my 1st
sample is light green, my 2nd sample is green and my 3rd sample is dark
blue.

Dark Blue

Green

DISCUSSION:
First of all, there was no di erence between the expected and obtained
results in this experiment. for example, in the last step we achieved the
expected color tones in the test tubes. At the same time, we learned the
e ect of light on chemistry, how to experience it and its properties in this
experiment. Also, reusing the decantation technique in this experiment
allowed us to improve our simple laboratory techniques. If there was a
margin of error in the experiment, it could have been due to the inadequacy
of the light source or the solutions used.

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 REFERENCES:
- METU General Chemistry Lab Manual Textbook
- www.britannica.com
- www.radio2space.com
- https://qknowbooks.gitbooks.io/class_5_science-mixtures/content/
decantation.html

- https://string ixer.com/tr/Photochemistry
- http://www.quantumphysicslady.org/glossary/frequency-and-
wavelength/

- www.physicsforums.com

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