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    Experiment 2 Synthesis of Potassium Tris (Oxalato) Ferrate (III) Trihydrate (K (Fe (C O) ) .3H O) Objectives

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    nathirahjaini
    The document describes an experiment to synthesize the coordination compound potassium tris(oxalato)ferrate(III) trihydrate (K3[Fe(C2O4)3].3H2O) through a series of reaction steps. Ferrous ammonium sulfate is reacted with oxalic acid to form ferrous oxalate precipitate, which is then oxidized to ferric ions using potassium oxalate and hydrogen peroxide. Additional oxalic acid causes the ferric ions to complex with oxalate, forming the desired product, which precipitates upon addition of ethanol. Safety precautions are outlined for working with the toxic, flammable, and corrosive chemicals involved

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    Experiment 2 Synthesis of Potassium Tris (Oxalato) Ferrate (III) Trihydrate (K (Fe (C O) ) .3H O) Objectives

    Uploaded by

    nathirahjaini
    333 views4 pages
    The document describes an experiment to synthesize the coordination compound potassium tris(oxalato)ferrate(III) trihydrate (K3[Fe(C2O4)3].3H2O) through a series of reaction steps. Ferrous ammonium sulfate is reacted with oxalic acid to form ferrous oxalate precipitate, which is then oxidized to ferric ions using potassium oxalate and hydrogen peroxide. Additional oxalic acid causes the ferric ions to complex with oxalate, forming the desired product, which precipitates upon addition of ethanol. Safety precautions are outlined for working with the toxic, flammable, and corrosive chemicals involved

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    The document describes an experiment to synthesize the coordination compound potassium tris(oxalato)ferrate(III) trihydrate (K3[Fe(C2O4)3].3H2O) through a series of reaction steps. Ferrous ammonium sulfate is reacted with oxalic acid to form ferrous oxalate precipitate, which is then oxidized to ferric ions using potassium oxalate and hydrogen peroxide. Additional oxalic acid causes the ferric ions to complex with oxalate, forming the desired product, which precipitates upon addition of ethanol. Safety precautions are outlined for working with the toxic, flammable, and corrosive chemicals involved

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    © All Rights Reserved
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    333 views4 pages

    Experiment 2 Synthesis of Potassium Tris (Oxalato) Ferrate (III) Trihydrate (K (Fe (C O) ) .3H O) Objectives

    Uploaded by

    nathirahjaini
    The document describes an experiment to synthesize the coordination compound potassium tris(oxalato)ferrate(III) trihydrate (K3[Fe(C2O4)3].3H2O) through a series of reaction steps. Ferrous ammonium sulfate is reacted with oxalic acid to form ferrous oxalate precipitate, which is then oxidized to ferric ions using potassium oxalate and hydrogen peroxide. Additional oxalic acid causes the ferric ions to complex with oxalate, forming the desired product, which precipitates upon addition of ethanol. Safety precautions are outlined for working with the toxic, flammable, and corrosive chemicals involved

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    of 4

    EXPERIMENT 2

    Synthesis of Potassium Tris(oxalato)ferrate(III) Trihydrate (K3[Fe(C2O4)3].3H2O)

    Objectives

    To synthesis a coordination compound, potassium tris(oxalato)ferrate(III) trihydrate


    under carefully controlled conditions.

    Introduction

    Synthesis is a useful technique in all areas of chemistry. This technique is important


    because it is the basis for developing new compounds, which may be useful for
    animals and vegetation. Most developments in the pharmaceutical industry as well as
    the introduction of new and less harmful pesticides are made possible because the
    chemicals involved are synthesised and tested in the laboratory. In addition, many
    chemical compounds used in everyday life are synthesised from simpler materials.

    This experiment involves preparing a substance by reacting known quantities


    of chemicals. The expected product is potassium tris(oxalato)ferrate(III) trihydrate,
    K3[Fe(C2O4)3]·3H2O. The preparation of this compound involves several steps. Firstly,
    ferrous ammonium sulphate, Fe(NH3)2(SO4)2.6H2O, is dissolved in distilled water to
    which excess oxalic acid, H2C2O4, is added to make it slightly acidic and the following
    reaction occurs.

    The preparation of this compound involves several steps. Firstly, ferrous


    ammonium sulphate, Fe(NH3)2(SO4)2.6H2O, is dissolved in distilled water to which
    excess oxalic acid, H2C2O4, is added to make it slightly acidic and the following
    reaction occurs.

    Fe(NH4)2(SO4)2.6H2O (aq) + H2C2O4 (aq) → FeC2O4 (s) + H2SO4 (aq) + (NH4)2SO4 (aq)
    + 6H2O (l) ..............(Eq 1)

    Ferrous oxalate, FeC2O4, is a finely divided precipitate and tends to be colloidal.


    However, heating the solution causes it to coagulate and facilitates separating the
    precipitate from the solution.

    Next, potassium oxalate solution, K2C2O4(aq), is added to the FeC2O4


    precipitate which produces a slightly basic solution to facilitate the oxidation of ferrous
    ion to ferric ion by hydrogen peroxide, H2O2. The following reaction takes place:

    [Oxidation / 2 electrons lost] 2Fe2+ → 2Fe3+ + 2e−


    [Reduction / 2 electrons gained] H2O + HO2− + 2e− → 3OH−
    [Overall net reaction] 2Fe2+ + H2O + HO2− → 2Fe3+ + 3OH− ..........(Eq 2)

    Note that FeC2O4 is the source of Fe2+ ions in Eq. 2.

    The OH− ion concentration of the solution is high enough so that some of the
    Fe3+ ions react with OH− ions to form ferric hydroxide (brown precipitate) as follows:

    Fe3+ + 3OH− → Fe(OH)3 (s)..........(Eq 3)

    With the addition of more H2C2O4, Fe(OH)3 dissolves and the soluble complex
    K3[Fe(C2O4)3].3H2O is formed according to:

    3K2C2O4 (aq) + 2Fe(OH)3 (s) + 3H2C2O4 (aq) →2K3[Fe(C2O4)3].3H2O (aq) + 3H2O (l)
    ……….(Eq.4)

    Alcohol is added to the solution to cause the complex iron salt to precipitate
    since it is less soluble in alcohol than in water.

    The complexity of the series of reactions described in equations 1 – 4 may be


    greatly simplified by following the Fe2+/ Fe3+ ion throughout. It can be seen that for
    every mole of Fe(NH3)2(SO4)2.6H2O used as the starting material, one mole of
    K3[Fe(C2O4)3].3H2O will be obtained as the final product.

    Fe(NH4)2(SO4)2.6H2O (aq) + H2C2O4 (aq) → FeC2O4 (s) + ...etc (see Eq.1)

    FeC2O4 + K2C2O4 + H2O2 → Fe(OH)3(s) + ...etc (see Eq.2 & 3)


    (Fe2+ = Fe3+)

    Fe(OH)3 + H2O2 + K2C2O4 → K3[Fe(C2O4)3].3H2O (aq) + ...etc (Eq.4)

    Safety precautions
    All chemicals are toxic. The organic solvents are highly flammable and can be irritating
    to body tissues and respiratory tract. Acids are corrosive. Work with care and wear
    safety goggles. Wash hands thoroughly with soap and water before leaving the
    laboratory.

    Apparatus
    Balance
    125 mL Erlenmeyer flask
    Measuring cylinder, 50 mL (2 pieces)
    Beakers (100 mL, 3 pieces)
    Beaker, 400 mL
    Glass rod
    Ice bath
    Bunsen burner
    Tripod stand
    Thermometer
    Buchner funnel
    Vacuum filtration apparatus
    Filter paper

    Chemicals
    Ferrous ammonium sulphate, Fe(NH4)2(SO4)2.6H2O
    0.5 M oxalic acid, H2C2O4 (aq)
    1 M potassium oxalate monohydrate, K2C2O4·H2O (aq)
    3 M sulphuric acid, H2SO4
    6% hydrogen peroxide, H2O2
    Ethanol
    1:1 ethanol/water solution
    Deionised water

    Procedure

    1. Weigh out about 5 g ferrous ammonium sulphate salt. Record the actual weight
    used. Put this into a 125 mL Erlenmeyer flask. Dissolve this compound with 15 mL
    of distilled water and add 5 drops of 3M sulphuric acid.
    2. Add 50 mL of 0.5 M oxalic acid to this solution and heat it to boiling, stirring
    constantly to prevent bumping.
    3. Remove the Erlenmeyer flask from the heat and allow the yellow precipitate of
    FeC2O4 to settle. Decant the supernatant liquid and wash the precipitate using 20
    mL of hot distilled water. Swirl the mixture and allow the precipitate to settle;
    decant and repeat the washing once more.
    4. Add 20 mL of 1M K2C2O4 to the precipitate, stir and heat to 40oC. While the
    temperature is at 40oC, immediately add 10 mL of 6% H2O2 dropwise and stir
    continuously. Make sure the temperature does not go below 40 oC and not above
    50oC during the addition of hydrogen peroxide. Some brown precipitate of Fe(OH)3
    may form at this time.
    5. Heat the resulting solution to boiling. Add in 20 mL of 0.5 M H2C2O4 all at once
    while maintaining the temperature near boiling. The solution should turn clear
    green. If some brown residue remains, add more 0.5 M H2C2O4 dropwise while
    the solution is boiling, until it turns clear green. However, if the remaining residue
    is yellow, it is probably unreacted FeC2O4 and more H2O2 should be added
    carefully.
    6. If the solution is cloudy, gravity filter it into a clean 125 mL Erlenmeyer flask. If it
    is clear, no flitration is necessary. Then while swirling constantly, slowly add 15
    mL of ethanol to the solution. Allow to cool in an ice bath prepared in a 400 mL
    beaker. Immerse the bottom portion of the flask in the ice bath and slowly stir the
    solution until crystals begin to form. Stop stirring and allow the solution to
    stand in the ice bath for 20 minutes. A good crop of crystals should have formed
    before the solution is filtered.
    7. Prepare the vacuum filtration apparatus.
    8. Decant the supernatant liquid away from the green crystals. With the aid of a clean
    glass rod, transfer the crystals to the Buchner funnel and apply suction for about
    2 minutes.
    9. Stop the suction and add 10 mL of the 1:1 ethanol/water solution. Wait for 30
    seconds and then apply suction for 2 minutes. Repeat this washing process. After
    the final wash, allow the suction to continue for a further 2 minutes.
    10. Transfer the crystals to a preweighed labelled dry 50 mL beaker. Discard the
    wash solutions.

    Note: The complex is photosensitive and should not be exposed to light.


    Store in a sample bottle/vial wrapped in foil. Keep the crystals for the next
    experiment

    Useful Molar Masses


    K2C2O4 = 166.22 g/mol
    Fe(NH4)2(SO4)2.6H2O = 392.13 g/mol
    K3[Fe(C2O4)3].3H2O = 491.24 g/mol

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