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    Fe (NO), Co (NO), Ni (NO), Al (NO), ZN (NO) : Analysis of Group Iii Cations

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    jude
    The document provides instructions for analyzing an unknown solution containing Group III cations (iron, cobalt, nickel, aluminum, and zinc ions). The procedure involves precipitating the cations from solution, separating the precipitates, and testing filtrates and residues to identify each cation. Direct tests are also described to identify nickel, iron, cobalt, and zinc ions without fully separating the cations.

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    Fe (NO), Co (NO), Ni (NO), Al (NO), ZN (NO) : Analysis of Group Iii Cations

    Uploaded by

    jude
    29 views3 pages
    The document provides instructions for analyzing an unknown solution containing Group III cations (iron, cobalt, nickel, aluminum, and zinc ions). The procedure involves precipitating the cations from solution, separating the precipitates, and testing filtrates and residues to identify each cation. Direct tests are also described to identify nickel, iron, cobalt, and zinc ions without fully separating the cations.

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    The document provides instructions for analyzing an unknown solution containing Group III cations (iron, cobalt, nickel, aluminum, and zinc ions). The procedure involves precipitating the cations from solution, separating the precipitates, and testing filtrates and residues to identify each cation. Direct tests are also described to identify nickel, iron, cobalt, and zinc ions without fully separating the cations.

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    © All Rights Reserved
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    Download as docx, pdf, or txt
    29 views3 pages

    Fe (NO), Co (NO), Ni (NO), Al (NO), ZN (NO) : Analysis of Group Iii Cations

    Uploaded by

    jude
    The document provides instructions for analyzing an unknown solution containing Group III cations (iron, cobalt, nickel, aluminum, and zinc ions). The procedure involves precipitating the cations from solution, separating the precipitates, and testing filtrates and residues to identify each cation. Direct tests are also described to identify nickel, iron, cobalt, and zinc ions without fully separating the cations.

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    ANALYSIS OF GROUP III CATIONS

    Prepare a known Solution by mixing approximately 1 ml each of ferric nitrate, cobalt nitrate, nickel nitrate, aluminum
    nitrate, and zinc nitrate.

    Dilute with water to make approximately 10 ml of solution. (5ml of distilled water)

    Analyze as a practice unknown by the following procedure:

    Fe(NO3)3, Co(NO3)2, Ni(NO3)2, Al(NO3)3, Zn(NO3)2


    Precipitation of Group III Cations:
    1. To 3 ml of the unknown solution,
    2. Add 1 ml of 5 M NH4Cl.
    3. Add drop by drop of 15 M NH4OH until basic plus 5 drops in excess.
    4. Then 10 drops of 1 M thioacetamide solution.
    5. Mix thoroughly and heat the tube in a water bath for 7 to 10 minutes.
    6. Centrifuge.
    7. Decant the supernatant liquid into another tube.
    8. Test for complete precipitation, by adding 5 drops of thioacetamide .
    9. Heat for 5 to 10 minutes.
    10. Should a ppt. form, return the suspension to the test tube with the ppt.
    11. Centrifuge again. Repeat the test for complete precipitation.
    12. Wash the ppt. with a mixture of 4 drops of 5 M NH4N03 and 2 ml of water.
    13. Centrifuge.
    14. Discard the washings.

    Ppt. of groups: Al(OH)3, Fe2S3, CoS, NiS, ZnS

    Separation of the Aluminum Group from the Iron Group :


    1. To the solution E-F-1 add 6 M NaOH until basic then 8 drops in excess.
    2. Add 5 drops of 3% H202
    3. Boil until bubbles of oxygen are no longer evolved from the hot solution.
    4. Centrifuge
    5. Decent the supernatant liquid through a filter.
    6. Label the filtrate F-1.
    7. Wash the ppt. by warming it with 10 drops 6 M HCI and treat this solution according to E-2.

    Ppt: Fe(OH)3, Co(OH)3, Ni(OH)2 Sol’n: AlO2- or Al(OH)4-, ZnO2-2 or Zn(OH)2-4

    Separation and Test for Ferric Ion:


    1. Dilute the solution E-2 to 2 ml with water.
    2. Add 6 M NH4OH until alkaline. then 5 drops in excess.
    3. If there is no ppt. ferric ion is absent and this solution
    4. Should then be divided into two equal portions for E3 and E4.
    5. If a ppt forms, centrifuge.
    6. Decant and divide the supernatant into halves: label one E-3 and the other E-4.

    Ppt: Fe(OH)3 Sol’n: Co(NH3)62+, Ni(NH3)2+

    7. Wash the ppt. with 1 ml water,


    8. Centrifuge.
    9. Discard washings.
    Fe3+
    10. Dissolve the residue in 5 drops of 6 M HCI,dilute to 2 ml.

    11. Add 5 drops of 1 M KSCN solution.


    Sol’n: Co(NH3)62+, Ni(NH3)2+
    FeSCN2+(Deep Red)
    Test for Cobalt Ion:

    1. To the solution E-3 add 6 M HAc until acidic then 3 drops in excess.
    2. Add 1 ml of 6 M KNO2.
    3. Warm the solution and allow to stand for a few minutes.
    4. A yellow or olive colored ppt. indicates the presence of cobalt ion.
    5. If no ppt. is observed,
    6. Add 3 to 5 drops additional HAc and
    7. Warm again before concluding that cobalt is absent.

    Ppt: K3Co(NO2)6 (Yellow)

    Test for Nickel Ion:

    1. To the solution E-4 add 4 drops of 1% dimethylglyoxime solution.


    2. A red or pink ppt. is a positive test for nickel ion.
    3. If cobalt is present, the first few drops of dimethylglyoxime reagent may react with the cobalt to
    give a brown solution.
    4. If the brown solution is observed, add 10 additional drops of dimethylglyoxime.
    5. Centrifuge.
    6. Decant the supernatant liquid.

    Ppt: Ni(DMG)2 (Red)

    Sol’n: AlO2- or Al(OH)4-, ZnO2-2 or Zn(OH)2-4


    Test for Aluminum Ion:

    1. To the solution F-1 add 1 ml of 5 M NH4N03


    2. Mix and heat for 5 minutes in a water bath.
    3. A white gelatinous ppt. indicates the presence of aluminum ion.

    Ppt: Al(OH)3 Sol’n.: ZnO22-

    4. Filter and label the filtrate F-2.


    5. Wash the filter with 20 drops of water or until the yellow color of chromate, if present, is removed
    from the filter.
    6. Discard the washings.
    7. Dissolve any aluminum hydroxide on the filter in 5 drops of 6M HCI.
    8. Wash the acid through the filter with 20 drops of water, catching the water in the same tube with
    the acid.
    Al(OH)4-

    9. Add 3 drops of aluminum reagent and 20 drops of 3 M NH4Ac.


    10. Warm allow to stand for 5 minutes and examine carefully.
    A red ppt. confirms aluminum.

    Ppt.: Al(OH)3 (Red)

    Sol’n.: ZnO22-

    Test for Zinc Ion:

    1. To the solution F-3 add drops of thioacetamide.


    2. Heat the tube for 5 minutes in a water bath.

    Ppt.: ZnS (White)


    Name: Gacho, Stephen Jude D. BSMT-1F Analytical Chemistry
    Lecturer: Mrs. Gemma Cabanilla
    DIRECT TESTS

    Under certain conditions some Group III ions may be tested directly from the original unknown solution without
    following the lengthy procedure:

    Test for Nickel Ion:


    1. To 5 drops of the unknown, add 5 drops water,
    2. 6 M NH4OH dropwise until the ppt first formed dissolves (or until the solution smells of ammonia).
    3. Centrifuge.
    4. To the clear supernatant add a few drops of dimethylglyoxime.

    A red ppt. Indicates nickel.

    Test for Ferric Ion:


    1. To 5 drops of the unknown add 6 M HCI until acidic.
    2. Add KSCN dropwise.

    A deep red color indicates ferric ion.

    If a ppt. forms upon addition of KSCN add excess of the reagent until complete precipitation.

    Test for Cobalt Ion:


    1. lf ferric is present, remove it as follows:
    2. To 10 drops of the unknown solution
    3. Add 6 M HCI until acidic, then add SnCl2 solution dropwise until the solution is almost color less (or light green).
    4. To test for cobalt, add KSCN and acetone to the solution.

    A deep blue color indicates the presence of cobalt.

    Test for Zinc:


    1. To a few drops of the unknown, add 6 M HAc until acidic.
    2. 5 drops of thlioacetamide.
    3. Heat in a water bath.

    A white ppt. indicates zinc ion.

    (Note: Remove Group 1 and Group II ions before performing the test). '

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