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Synthesis and Characterization of CR (III) Oxide (Cr2O3) : Lab Report (4a)

Chromium(III) oxide (Cr2O3) was prepared through the thermal decomposition of ammonium dichromate ((NH4)2Cr2O7). When ammonium dichromate is heated to 168-185°C, it decomposes to produce Cr2O3, nitrogen gas (N2), and water (H2O) vapor. The Cr2O3 product was characterized using UV-visible spectroscopy, ATR-FTIR spectroscopy, and XRD, which confirmed the formation of hexagonal α-Cr2O3. Safety precautions were outlined due to the toxic nature of ammonium dichromate and potential irritant properties of the products.

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Falak Naz
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241 views

Synthesis and Characterization of CR (III) Oxide (Cr2O3) : Lab Report (4a)

Chromium(III) oxide (Cr2O3) was prepared through the thermal decomposition of ammonium dichromate ((NH4)2Cr2O7). When ammonium dichromate is heated to 168-185°C, it decomposes to produce Cr2O3, nitrogen gas (N2), and water (H2O) vapor. The Cr2O3 product was characterized using UV-visible spectroscopy, ATR-FTIR spectroscopy, and XRD, which confirmed the formation of hexagonal α-Cr2O3. Safety precautions were outlined due to the toxic nature of ammonium dichromate and potential irritant properties of the products.

Uploaded by

Falak Naz
Copyright
© © All Rights Reserved
Available Formats
Download as DOCX, PDF, TXT or read online on Scribd
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Lab report (4a)

Synthesis and characterization of Cr(III) Oxide (Cr2O3)


 Apparatus
1-L Erlenmeyer flask
Ring stand, clamp, iron ring
Angel hair
Wire mesh
Bunsen burner
Glass wool
 Chemicals
10 g (NH4)2Cr2O7
 Principle
When ammonium dichromate is heated, its decomposition occur resulting in the formation of
Chrmoium(III) oxide, Cr2O3.
 Theory
In this experiment, Chromium(III) oxide, Cr2O3 is prepared by the thermal decomposition of
ammonium dichromate.
Ammonium dichromate
Ammonium dichromate is a flammable inorganic compound with the chemical formula
(NH4)2Cr2O7. It is orange-red needles produced during crystallization. It is used as an approved
pesticide and used as a mordant for dyeing, used as a pigment.

Chromium(III) oxide
Chromium(III) oxide is the inorganic compound of the formula Cr2O3 with chemical name
Chromic oxide. It is one of principal oxides of chromium and is used as a pigment. In nature,
it occurs as the rare mineral eskolaite. Chromium (III) oxide appears as a fine light to dark
green, hexagonal crystal.

Chromium(III) oxide is amphoteric. Although insoluble in water, it dissolves in acid to


produce hydrated chromium ions, [Cr(H2O)6]3+ which react with base to give salts of
[Cr(OH)6]3−.
ionic compound
Chromium trioxide (Cr2O3) is an ionic compound composed of 2 Cr3+ ions, and 3 (O)2-
ions. (That's an oxygen ion with a -2 charge). In the formation of this compound electrons are
not shared between the constituent ions, as they would be between atoms in a covalent bond.

Crystal structure hexagonal

Boiling point of Chromic oxide 4,000 °C

Melting point of Chromic oxide 2,435 °C

Colour Light to dark green

Uses

 In glasses, inks and paints.


 As the colorant in 'chrome green' and 'institutional green'
 Precursor to the magnetic pigment (chromium dioxide)
 In the process of stropping knives.

 Reaction

(NH4)2Cr2O7(s)  ——>  Cr2O3(s)  +  N2(g)  +  4H2O(g)

168-185°C.

 Mechanism
Ammonium dichromate (NH4)2Cr2O7, contains both reducing (NH4) and oxidizing (Cr2O7)
agents. During the thermal decomposition of ammonium dichromate, chromium is reduced from
+6 to +3 oxidation state and the dichromate ions oxidize ammonia to nitrogen gas and water.
Decomposition of ammonium dichromate is an exothermal process which produces sparks,
steam and nitrogen gas. The product Cr2O3 is an ash like compound. The chromium(III) oxide
crystals that are produced are "fluffier" than the original ammonium dichromate crystals, and
even though a lot of the mass of the starting materials escapes as vapor, the product looks like a
larger amount of material.  

 Procedure:

1. Clamp a 1-L Erlenmeyer flask to a ring stand, leaving enough room underneath for a Bunsen
burner. Carefully pour (NH4)2Cr2O7 into the center of the flask, forming a cone shaped pile.

2. Place glass wool in the top to cover the opening. Place wire mesh on top of the glass wool.
Secure another ring clamp on top of the wire mesh.

3. Light the Bunsen burner underneath. It should take less than a minute for the ammonium
dichromate to start to decompose. Sparks and smoke emanate from the cone, and Cr2O3 is
produced as a fluffy green solid.

 Characterization

Characterization by UV-Visible spectroscopy

The UV-visible absorption spectroscopy of Cr2O3 nanoparticles shows sharp absorption


peak in the visible region around 460 nm.
Nano-sized Cr2O3 particles show absorbance in the UV-visible region due to Surface
Plasmon Resonance, which originates due to the resonance of collective conduction electrons
with incident electromagnetic radiations.
Characterization of Cr2O3 by ATR-FTIR spectrum
Room temperature ATR-FTIR spectrum of the α-Cr2O3 nanoparticles annealed at 500°C for 2 h.

The ATR-FT-IR typical spectrum could be split into two regions, the first lying between the 400
and 800 cm−1 and the second between 2100 and 2700 cm−1 . The vibrational modes observed at
418, 558 and 643 cm−1 are typical of metal oxide single bonds in the bending mode. The
relatively weak absorption band at 418 cm−1 and the strong absorption band at 558 cm−1 can be
attributed to Cr–O bonds in the bending mode, while the strong absorption band at 643 cm−1 is a
clear evidence for the presence of crystalline α-Cr2O3. The broad band of low intensity at 1060
cm−1 can be attributed to surface Cr–O stretching vibrations.
Characterization by XRD
The major XRD peaks of the products, including (0 1 2), (1 0 4), (1 1 0), (1 1 3), (0 2 4), (1 1 6),
(2 1 4), (3 0 0), (1 1 9) and (2 2 0), can be indexed to α-Cr2O3, which is in agreement with the
standard value for the Cr2O3 phase (JCPDS card No. 1308-38-9, hexagonal close-packed,
a=4.958 Å, and c=13.59 Å).

 Discussion
1. Covering of Erlenmeyer flask
Before ignition the opening of the Erlenmeyer flask is covered with glass wool to prevent the
loss of Cr2O3 during the thermal decomposition.
2. Check for the Completion of reaction:
The colour of ammonium dichromate is bright orange red while its decomposition
product, Cr2O3 is light to dark green in colour. If bright orange red crystals are observed in the
final product, it indicate the presence of unreacted ammonium dichromate.
3. Colour
Basically, the light incident on the metal has two components, one which bounces off the
actual surface and one which passes through a thin film, in this case the oxide layer, and then
bounces back. The two wave components interfere with each other in such a way as to make
the crystal change color.
There is a hexagonal close packing in the Cr2O3 structure. And so, when incident light falls
on it, it reflects back from different layers and that leads to interference phenomenon (in
which light colour changes). That's why green color is observed in Cr2O3 oxide.

 Safety

Ammonium dichromate, like all chromium (VI) compounds, is highly toxic and a proven
carcinogen. It is also a strong irritant. Take off contaminated clothing and shoes immediately.
Wash off with soap and plenty of water.

Ammonium Dichromate may cause an asthma-like allergy. Ammonium dichromate


(explosive, very toxic, danger to the environment).

Chromium (III) Oxide may be regarded as essentially nontoxic. However, excessive exposure
may cause irritation to the eyes, skin or lungs.
 Comment

volcano reactions: While the ammonium dichromate decomposes, it gives off orange sparks and
throws the green chromium(III) oxide crystals into the air, producing an effect that looks like a
miniature volcanic eruption.

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