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    CHM 475 Inorganic Chemistry: (Experiment 5)

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    FAtma HAnys
    The document describes an experiment to synthesize potassium tris(oxalato) ferrate(III) trihydrate. The objective is to combine chemicals to form the new compound. Ferrous ammonium sulfate, oxalic acid, and potassium oxalate are reacted and heated to form the ferric complex salt. Filtration and washing yields 4.82 grams of the red product. The theoretical yield was calculated as 6.34 grams, so the percent yield was 76.03%. Sources of error that could explain the less than 100% yield are discussed.

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    CHM 475 Inorganic Chemistry: (Experiment 5)

    Uploaded by

    FAtma HAnys
    50 views7 pages
    The document describes an experiment to synthesize potassium tris(oxalato) ferrate(III) trihydrate. The objective is to combine chemicals to form the new compound. Ferrous ammonium sulfate, oxalic acid, and potassium oxalate are reacted and heated to form the ferric complex salt. Filtration and washing yields 4.82 grams of the red product. The theoretical yield was calculated as 6.34 grams, so the percent yield was 76.03%. Sources of error that could explain the less than 100% yield are discussed.

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    exp 5

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    The document describes an experiment to synthesize potassium tris(oxalato) ferrate(III) trihydrate. The objective is to combine chemicals to form the new compound. Ferrous ammonium sulfate, oxalic acid, and potassium oxalate are reacted and heated to form the ferric complex salt. Filtration and washing yields 4.82 grams of the red product. The theoretical yield was calculated as 6.34 grams, so the percent yield was 76.03%. Sources of error that could explain the less than 100% yield are discussed.

    Copyright:

    © All Rights Reserved
    Download as DOCX, PDF, TXT or read online from Scribd
    Download as docx, pdf, or txt
    50 views7 pages

    CHM 475 Inorganic Chemistry: (Experiment 5)

    Uploaded by

    FAtma HAnys
    The document describes an experiment to synthesize potassium tris(oxalato) ferrate(III) trihydrate. The objective is to combine chemicals to form the new compound. Ferrous ammonium sulfate, oxalic acid, and potassium oxalate are reacted and heated to form the ferric complex salt. Filtration and washing yields 4.82 grams of the red product. The theoretical yield was calculated as 6.34 grams, so the percent yield was 76.03%. Sources of error that could explain the less than 100% yield are discussed.

    Copyright:

    © All Rights Reserved
    Download as DOCX, PDF, TXT or read online from Scribd
    Download as docx, pdf, or txt
    of 7

    CHM 475

    INORGANIC CHEMISTRY
    (EXPERIMENT 5)

    Course Name : Bachelor in Education Science (Hons.) Chemistry


    Course Code : ED 260
    Title of experiment : Synthesis of Potassium Tris(oxalato)
    Ferrate(III) Trihydrate
    Name : Nur Fatma Hanis binti Abdullah Sani
    Matrix no : 2014665254
    Group Partner : Salmee Safina binti Mohd Yusuf
    Group : ED2602A
    Lecturer’s name : Dr Amalina binti Mohd Tajuddin
    Date of Submission : 10/04/2015
    EXPERIMENT 5

    OBJECTIVE

    The objective of this experiment is to synthesize potassium tris(oxalato) ferrate(III) trihydrate.

    INTRODUCTION

    Synthesis is process in which substances combine to form completely new substances. Ferrous
    ammonium sulphate was dissolved in a slightly acid solution, excess oxalic acid, H2C2O4 is
    added, and the balance chemical reaction that take place is Fe(NH 4)2(SO4)2.6H2O + H2C2O4 
    FeC2O4 + H2SO4 + (NH4)2SO4 + 6H2O. FeC2O4 precipitate was added with potassium oxalate
    which produces slightly basic solution for the oxidation of the ferrous ion to the ferric ion.
    Ferrous ion react with hydroxide ion to form ferric hydroxide that formed as brown precipitate.
    With the addition of excessive H2C2O4, the ferric hydroxide dissolve and the soluble complex
    formed. The balance chemical equation is : 3K 2C2O4 + 2Fe(OH)3 + 3H2C2O4 
    2K3[Fe(C2O4)3].3H2O + 3H2O.

    CHEMICAL AND APPARATUS

     Ferrous ammonium sulfate  Dilute sulfuric acid


     Distilled water  Beaker
     Weighing balance  Oxalic acid dehydrate
     Boiling water bath  6% H2O2
     Solid potassium oxalate monohydrate  95% Ethanol
     Buchner funnel  Suction filtration
     Cooled acetone  Funnel
    PROCEDURE.

    Procedure A.
    1. 5.00 g of ferrous ammonium sulfate was well-stirred in 20 ml of water containing 1 ml of
    dilute sulfuric acid in the beaker.
    2. 2.50 g of oxalic acid dihydrate was added in 25 ml of water.
    3. The oxalic acid solution was added to the ferrous ammonium sulfate solution.
    4. The mixture was heated slowly and yellow precipitate was formed. Supernatant was
    decant.
    5. 15 ml of hot water was added to the yellow precipitate and the supernatant was decant.
    Then 15 ml of hot water was added again to the mixture.
    6. 3.50 g solid potassium oxalate monohydrate was added to the mixture and it was heated
    approximately 40 ˚C.
    7. At 40 ˚C, 10 ml of 6% H2O2 was added to the mixture and was heated until boiling.
    8. A solution of 2.00 g of oxalic acid dihydrate in 30 ml of water in portions was added to
    the mixture.
    9. The clear solution was boiled and was filtered through a Buchner funnel.
    10. 30 ml of 95% ethanol was added slowly to the solution.
    11. The crystals was dissolved by heating.

    Procedure B.
    1. The crystals was obtained using suction filtration.
    2. The crystal was washed twice with a cooled 1:1 ethanol/water mixture and with cooled
    acetone.
    3. The crystal was dried in air and weighed.
    DATASHEET EXPERIMENT 5

    Name : Nur Fatma Hanis binti Abdullah Sani Date : 24/03/2015


    Student ID : 2014665254 Group : ED2602A

    Determination of limiting reactant.

    Chemical equation involved.

    1) Fe(NH4)2(SO4)2.6H2O + H2C2O4  FeC2O4 + H2SO4 + (NH4)2SO4 + 6H2O


    2) Fe3+ + 3OH-  Fe(OH)3

    Note that the number of mole of Fe(OH)3 is equal to the number of mole of
    Fe(NH4)2(SO4)2.6H2O.

    Balanced chemical equation

     3K2C2O4 + 2Fe(OH)3 + 3H2C2O4  2K3[Fe(C2O4)3].3H2O + 3H2O.

    The number of moles K2C2O4

     3.31 g / 166.22 gmol-1 = 0.0199 moles

    The number of moles H2C2O4

     2.67 g / 90.02 gmol-1 = 0.0297 moles

    The number of moles Fe(NH4)2(SO4)2.6H2O

     5.04 g / 392.01 gmol-1 = 0.0129 moles

    Since the number of mole of Fe(OH)3 is equal to the number of mole of Fe(NH4)2(SO4)2.6H2O, so
    the number of mole of Fe(OH)3 is 0.0129 moles.

     The limiting reactant is Fe(OH)3.


    1. Theoretical yield of K3[Fe(C2O4)3].3H2O

    2 mole of Fe(OH)3 = 2 moles of K3[Fe(C2O4)3].3H2O

    0.0129 moles of Fe(OH)3 x 2 moles of K3[Fe(C2O4)3].3H2O

    2 moles of Fe(OH)3

     0.0129 moles of K3[Fe(C2O4)3].3H2O

    0.0129 moles of K3[Fe(C2O4)3].3H2O x 491.21 gmol-1 = 6.34 g

     Theoretical yield of K3[Fe(C2O4)3].3H2O is 6.34 g

    2. Mass of K3[Fe(C2O4)3].3H2O obtained

     Mass of K3[Fe(C2O4)3].3H2O obtained is 4.82 g

    3. Percent yield of K3[Fe(C2O4)3].3H2O

    4.82 g x 100% = 76.03 %

    6.34 g

     The percentage yield of K3[Cr(C2O4)3].3H2O is 76.03 %.


    DISCUSSION

    A. Interpretation.
     Ferrous ammonium sulphate was dissolved in a slightly acid solution, excess oxalic acid,
    H2C2O4 is added, and the balance chemical reaction that take place is
    Fe(NH4)2(SO4)2.6H2O + H2C2O4  FeC2O4 + H2SO4 + (NH4)2SO4 + 6H2O.
     The brown precipitate formed due to the presence of ferric hydroxide that produce from
    reaction between hydroxide ion and ferrous ion.
     The balance chemical equation is : 3K2C2O4 + 2Fe(OH)3 + 3H2C2O4 
    2K3[Fe(C2O4)3].3H2O + 3H2O.
     The theoretical yield obtained is 6.34 gram and the mass of 2K 3[Fe(C2O4)3].3H2O
    obtained was 4.82 gram.
     The percentage yield obtained is not 100% due to some errors occur during the
    experiment. The error occurred were stated below.

    B. Error
     Using contaminated apparatus - we need to make sure our conical flask is cleaned before
    we are using it, this is important because the other substance may left in the conical flask
    and cause our product to contaminate.
     Period of heating – when there is heating process, limited working experiment may force
    the students shorten the heating period so the mixture cannot react completely or maybe
    the mixture was over heated.

    C. Safety Precaution
     We must wear gloves as a protection as we do not want to have direct contact with toxic
    chemicals.
    D. Suggestion Mark
     For an accurate result, we can carry out this experiment in the unlimited working time.
     We also must weigh accurately according to the actual weight that required in the lab
    manual.

    CONCLUSION

     The balance chemical equation is 3K2C2O4 + 2Fe(OH)3 + 3H2C2O4 


    2K3[Fe(C2O4)3].3H2O + 3H2O.
     The theoretical yield of K3[Fe(C2O4)3].3H2O is 6.34 gram.
     The mass of K3[Fe(C2O4)3].3H2O obtained is 4.82 gram.
     The percentage yield is 76.03%.
     The percentage error is 23.97%.

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