Preparation
of iron oxide nanoparticles (NPs)
Theory:
The co-precipitation method involves the
precipitation of iron hydroxide from iron salts in the presence of a base. In
this case, the FeCl3 and FeSO4 salts are used to provide
Fe+2 ions for the reaction. By gradually adding NH4OH as
the base, the pH of the solution increases, leading to the formation of iron
hydroxide. The iron hydroxide precipitate can then be further processed to
obtain iron oxide nanoparticles.
Chemicals
Required:
- Iron (III) chloride (FeCl3) solution, 0.2 M
- Iron (II) sulfate (FeSO4) solution, 0.1 M
- Ammonium hydroxide (NH4OH) solution
- Solvent: Water or appropriate organic solvent
Materials
Required:
- Reaction vessel or flask
- Magnetic stirrer or mechanical stirrer
- pH meter
- Centrifuge
- Drying equipment (e.g., vacuum oven or desiccator)
Procedure:
- Prepare a reaction vessel and add the FeCl3 solution (50 ml, 0.2 M) and the FeSO4 solution (50 ml, 0.1 M) to it.
- Start stirring the mixture using a magnetic or mechanical stirrer for 15 minutes to ensure proper mixing.
- Gradually add NH4OH dropwise to the reaction mixture while monitoring the pH using a pH meter.
- Continue stirring the mixture for an additional 20 minutes or until the pH reaches 11. The pH adjustment to 11 promotes the formation of iron hydroxide precipitates.
- Once the reaction time is complete, stop the stirring and allow the precipitate to settle.
- Separate the precipitate from the solution using a centrifuge. Discard the supernatant.
- Wash the obtained precipitate several times with water or a suitable solvent to remove any impurities or unreacted reagents.
- Dry the washed precipitate using a vacuum oven or desiccator to remove any residual moisture.
- The resulting dried material will likely consist of iron oxide nanoparticles, which can be characterized using various techniques such as X-ray diffraction (XRD), transmission electron microscopy (TEM), or Fourier-transform infrared spectroscopy (FTIR).
Alternating
method for synthesis of Iron Oxide Nanoparticles by using ammonia:
Theory:
Iron oxide nanoparticles are commonly
synthesized through a precipitation method using iron chloride and iron sulfate
solutions. The addition of ammonia helps in the formation of iron hydroxide,
which is subsequently transformed into iron oxide nanoparticles through heat
treatment or aging.
Formation
of iron hydroxide:
FeCl2 + 2NaOH → Fe(OH)2 +
2NaCl
FeSO4 + 2NaOH → Fe(OH)2 + Na2SO4
Conversion
of iron hydroxide to iron oxide:
2Fe(OH) 2 → Fe2O3 +
2H2O
Overall
reaction:
2FeCl2 + 4NaOH → Fe2O3
+ 4NaCl + 2H2O
2FeSO4 + 4NaOH → Fe2O3
+ 2Na2SO4 + 2H2O
Procedure:
- Prepare a 0.2 M solution of iron chloride (FeCl2) by dissolving the appropriate amount of iron chloride in 50 ml of distilled water.
- Prepare a 0.1 M solution of iron sulfate (FeSO4) by dissolving the appropriate amount of iron sulfate in 50 ml of distilled water.
- Mix both solutions (0.2 M FeCl2 and 0.1 M FeSO4) in a glass beaker.
- Stir the mixture for approximately 15 minutes to ensure thorough mixing. Apparatus required: Magnetic stirrer, stir bar.
- Add 40 ml of ammonia (NH3) to the mixture while continuing to stir.
- Continue stirring the mixture until the formation of iron oxide nanoparticles.
Note:
The stirring time required for nanoparticle formation may vary depending on the desired size and properties of the nanoparticles. Further heat treatment or aging may be necessary to complete the transformation.
Calculations:
Molar mass of FeCl3 = 55.845
g/mol + 106.359 g/mol = 162.204 g/mol
To prepare a 0.2 M solution of FeCl3
in 50 ml water:
Molarity (M) = moles of solute / volume
of solution (L)
0.2 M = moles of FeCl3 / 0.05
L (50 ml = 0.05 L)
Moles of FeCl3 = 0.2 M x 0.05
L = 0.01 moles
Mass of FeCl3 = Moles of FeCl3
x Molar mass of FeCl3
Mass of FeCl3 = 0.01 moles x
162.204 g/mol
Therefore, the mass of FeCl3 required
is 1.62204 grams.
Similarly, for FeSO4:
Molar mass of FeSO4 = 55.845
g/mol + 32.06 g/mol + 63.996 g/mol = 151.901
g/mol
To prepare a 0.1 M solution of FeSO4
in 50 ml water:
Molarity (M) = moles of solute / volume
of solution (L)
0.1 M = moles of FeSO4 / 0.05
L (50 ml = 0.05 L)
Moles of FeSO4 = 0.1 M x 0.05
L = 0.005 moles
Safety Precautions:
- Wear appropriate personal protective equipment, such as gloves and safety goggles, when handling chemicals.
- Work in a well-ventilated area or under a fume hood to avoid inhalation of fumes.
- Handle ammonia with care, as it is a corrosive substance. Avoid direct contact with skin and eyes.
- Follow proper waste disposal protocols for chemicals used in the synthesis.