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    Scheme Group III Cations

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    analytical chemistry

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    Scheme Group III Cations

    Uploaded by

    demro channel
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    analytical chemistry

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    Scheme Group III cations

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    analytical chemistry

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    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    8 views2 pages

    Scheme Group III Cations

    Uploaded by

    demro channel
    analytical chemistry

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
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    Scheme for Analysis of Group III (Fe3+, Cr3+, Al3+& Mn2+)

    To the centrifugate obtained from group II:


    1-! Boil to expel all H2S – test with lead acetate paper.
    2-! Add 1ml conc HNO3, boil 2 min, cool.
    3-! Add solid NH4Cl + excess conc.NH4OH till ammonia odor, boil, centrifuge

    Re Precipitate Centrifugate
    Group III Hydroxides:(White gel: Al(OH)3 ↓, dirty green: Cr(OH)3↓, (Groups: IV-VI)
    reddish brown: Fe(OH)3↓)&(Brown ppt: MnO2from Group IV)

    + Excess NaOH + 2 drops H2O2[O]


    Boil, centrifuge

    Reddish Brown ppt Fe(OH)3↓ Centrifugate


    2-
    + Brown ppt MnO2↓ CrO4 (Yellow Chromate)
    AlO2- (Colorless Aluminate)
    Dissolve in conc HNO3 → Fe3+, Mn2+
    Divide into 3 parts

    Test for Fe3+ Test for Mn2+ Divide


    1- Add SCN- → [FeSCN]2+ Add H+ + Pb3O4 (red lead) into 2 parts
    Blood red color ↓boil
    4-
    2- Add [Fe(CN)6] →Fe4[Fe(CN)6]3↓ Purple color of permanganate
    Prussian blue ppt (MnO4-) + Pb2+ + H2O

    Test for AlO2- Test for CrO42-


    Add excess NH4Cl + H2O
    Boil, cool Divide

    White gel ppt + Acetic acid +2H+→ Cr2O72- + H2O


    Al(OH)3↓ + Lead acetate Then add H2O2
    + NH3 + Cl- + ether

    Yellow ppt Blue color of per-chromate


    PbCrO4 in ether layer
    CrO83-
    + H2O + H+
    Why is NH4Cl added to NH4OH ?
    NH4Cl ⇋ NH4+ + Cl-
    NH4OH ⇋ NH4+ + OH-
    (This reaction will be shifted backward)
    NH4Cl forms a common ion effect with NH4OH leading to shifting the ionization reaction of NH4OH backward
    producing limited amount of hydroxide just sufficient to precipitate group III not group IV& Magnesium as
    Hydroxides.

    Why is concentrated HNO3 added?


    HNO3 oxidizes Fe2+ into Fe3+ before precipitation as hydroxide because Fe(OH)2 is not completely
    precipitated (has high Ksp).

    The centrifugate obtained from group II should be boiled off …..why ?


    Boiling is necessary to expel H2S to prevent precipitation of group IV as sulfides in alkaline medium.

    Excess ammonium hydroxide should be removed by boiling…..why?


    To prevent solubility of Cr(OH)3 in excess NH4OH forming ammine complex.
    Cr(OH)3 + 6NH4OH [Cr(NH3)6](OH)3 soluble + 6H2O

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