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    Qualitative Analysis

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    Carlo Joseph Moskito
    The document provides instructions for qualitative analysis of cations and anions in an unknown sample solution. The analysis involves multiple precipitation and filtration steps to sequentially separate the ions into groups based on solubility changes caused by changes in pH and addition of precipitating agents. Key reagents used include hydrochloric acid, ammonium hydroxide, sodium hydroxide and ammonium oxalate. Qualitative tests are then performed on the separated groups to identify the specific cations present.

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    Qualitative Analysis

    Uploaded by

    Carlo Joseph Moskito
    728 views10 pages
    The document provides instructions for qualitative analysis of cations and anions in an unknown sample solution. The analysis involves multiple precipitation and filtration steps to sequentially separate the ions into groups based on solubility changes caused by changes in pH and addition of precipitating agents. Key reagents used include hydrochloric acid, ammonium hydroxide, sodium hydroxide and ammonium oxalate. Qualitative tests are then performed on the separated groups to identify the specific cations present.

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    Qualitative Analysis()

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    The document provides instructions for qualitative analysis of cations and anions in an unknown sample solution. The analysis involves multiple precipitation and filtration steps to sequentially separate the ions into groups based on solubility changes caused by changes in pH and addition of precipitating agents. Key reagents used include hydrochloric acid, ammonium hydroxide, sodium hydroxide and ammonium oxalate. Qualitative tests are then performed on the separated groups to identify the specific cations present.

    Copyright:

    Attribution Non-Commercial (BY-NC)
    Download as PDF or read online from Scribd
    Download as pdf
    728 views10 pages

    Qualitative Analysis

    Uploaded by

    Carlo Joseph Moskito
    The document provides instructions for qualitative analysis of cations and anions in an unknown sample solution. The analysis involves multiple precipitation and filtration steps to sequentially separate the ions into groups based on solubility changes caused by changes in pH and addition of precipitating agents. Key reagents used include hydrochloric acid, ammonium hydroxide, sodium hydroxide and ammonium oxalate. Qualitative tests are then performed on the separated groups to identify the specific cations present.

    Copyright:

    Attribution Non-Commercial (BY-NC)
    Download as PDF or read online from Scribd
    Download as pdf
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    The document describes procedures for the qualitative analysis of cations and anions through a series of precipitation reactions and tests.

    The main steps involve adding reagents to precipitate out specific metal ions, separating the precipitates through centrifugation or filtration, and performing additional tests on the filtrates or precipitates to identify the present metals.

    Some common anion tests described include adding silver nitrate to test for halide ions, barium chloride to test for sulfate and sulfite, and iron(III) chloride to test for nitrite.

    SAMPLE SOLUTION

    6M HCl

    Precipitate: Group A Supernatant: Group B - E


    6M NH3
    pH 10

    Supernatant: Group C - E Precipitate: Group B

    6M (NH4)2C2O4

    Precipitate: Group C Supernatant: Group D - E


    ∆ to dryness
    conc. HNO3
    ∆ to dryness
    6M HCL
    Solution: Group D - E
    6M NaOH, 1M NaOH

    Precipitate: Group D Supernatant: Group E


    10 Drops of Sample Solution
    {Pb2+, Hg22+, Ag+}
    • Test for Complete Precipitation
    • Add 3 drops of 6M HCl
    • Centrifuge
    •Transfer centrifugate to a centrifuge tube

    PA1
    {White PbCl2, AgCl and Hg2Cl2}
    • Wash twice with 10 drops of COLD dH2O
    • Add 20 drops of dH2O CA1: Cations for other GROUPS
    • Heat in boiling water bath for 3 minutes
    with constant stirring.
    • Centrifuge quickly and decant
    supernatant liquid while HOT in a
    centrifuge tube

    PA2 CA2
    {White AgCl and Hg2Cl2} {Colorless: Pb2+}
    • Wash twice with 10 drops of HOT dH2O • Add 3 drops of 1M KI
    • Add 10 drops of 6M NH3.
    • Stir and centrifuge.
    • Decant supernatant liquid into a Yellow PbI2(s)
    centrifuge tube.

    PA3 CA3
    {Black Gray/White: HgNH2Cl(s)} {Colorless: Ag(NH3)2+
    {Black Hg(s)} • Add 6M HNO3 drop wise with
    stirring until acidic to litmus

    White AgCl(s)
    10 drops CA1 (Cations of Group B – E from
    Group A Analysis)
    • Add 6M NH3 drop wise until neutral
    • Add 12 drops 6M NH3 using a Pasteur Pipet.
    • Centrifuge and decant supernatant liquid into
    a centrifuge tube.

    PB1a {white Bi(OH)3, red brown Bi(OH)3,


    pale pink Mn(OH)2, Cr(OH)3}
    • Add 10 drops of 6M NaOH and 2 drops of 3% CB1: GROUPS C - E
    H2O2.
    • Stir thoroughly and allow solution to stand for
    two minutes.
    • Centrifuge. • Combine the centrifugates.
    • Decant supernatant liquid to a centrifuge tube • Label as CB2

    PB1b {Bi(OH)3, Bi(OH)3 MnO2}


    • Add 10 drops of 6M NaOH and 2 drops of 3% CB2 {CrO42-}
    H2O2. • Heat for 10 minutes in boiling
    • Stir thoroughly and allow solution to stand for water bath.
    two minutes. • Cool the content for two minutes
    • Centrifuge. in a cold water bath.
    • Decant supernatant liquid to a centrifuge tube • Add 6M HCl dropwise until acidic.
    • Add 1M NaHCO3 dropwise until
    neutral.
    PB2 {Bi(OH)3, Bi(OH)3 MnO2} •Discard any precipitate.
    • Add 2mL dH2O, stir and heat for 10 minutes in
    a boiling water bath.
    • Centrifuge. CB4 {Cr2O72-}
    • Decant and discard supernatant liquid. • Use 2 drops CB4
    • Wash with 2 mL dH2O. • Add 6M HCl dropwise until acidic.
    • Add 10 drops of 6M HCl. • Add 1 drop of 3% H2O2 while
    • Stir and heat for two minutes. observing a flash of color.
    • Discard any precipitate.

    CrO5 blue color that


    CB3 : Test Solution decomposes quickly
    {Bi3+, Mn4+, Fe3+}
    CB3 : Test Solution
    {Bi3+, Mn4+, Fe3+}

    4 drops of CB3 2 drops of CB3 2 drops of CB3


    • Add 2 drops of 2% H2O2 • Add 3 drops of 0.1M KSCN • Add 10 drops of 6M
    • Add a pinch of NaBiO3 or NaOH.
    a solution of it. • Add a pinch of SnCl2.
    • Centrifuge. • Agitate,.

    MnO4- FeSCN2+ Bi
    Purple Solutions Dark Red Brown Solution Black Precipitate
    10 drops CB1 (Cations for Group C – E from Analysis of Group B.
    • Add 8 drops of 0.5M Ammonium Oxalate
    • Stir thoroughly and centrifuge.

    PC1 CC1: GROUPS D - E


    {White: BaC2O4, CaC2O4, SrC2O4}
    {Light Pink: CoC2O4, }
    • Wash with 1mL dH2O
    • Transfer quantitatively using conc’d HNO3 into a
    clean evaporating dish.
    • Add 5 drops of conc’d HNO3
    • Heat to dryness under fumehood over low heat.
    • Cool for 5 mins then add 6 drops of conc’d HNO3 .
    • Heat to dryness again.
    • Cool for 5 minutes.
    • Transfer quantitatively using minimal amount of 12M
    HCl.
    • Add 6M KNO2 until precipitate forms.
    • Centrifuge.

    PC2
    CC2 {Ba2+, Ca2+, Sr2+} K3Co(NO2)6
    • Add 6M NH3 drop wise until basic. Yellow
    • Add 15 drops 3M (NH4)2CO3
    • Centrifuge.

    PC3 {BaCO3, CaCO3, SrCO3}


    • Wash with 10 drops of dH2O
    Discard Centrifugate. •Add 6M CH3COOH dropwise with stirring until dissolution
    (minimal drops)
    • Add equal number of drops of 6M CH3COOH in excess.
    • Dilute to 2 mL with dH2O
    • Add 5 drops of 0.1M K2CrO4
    • Mix and Centrifugate
    PC3 {BaCO3, CaCO3, SrCO3}
    • Wash with 10 drops of dH2O
    •Add 6M CH3COOH dropwise with stirring until dissolution
    (minimal drops)
    • Add equal number of drops of 6M CH3COOH in excess.
    • Dilute to 2 mL with dH2O
    • Add 5 drops of 0.1M K2CrO4
    • Mix and Centrifugate

    PC4 CC3 {Ca2+, Sr2+}


    BaCrO4 • Add 15M NH3 until basic.
    Yellow • Add 15 drops of 3M (NH4)2CO3
    • Centrifuge and discard centrifugate.
    • Wash ppt with 10 drops of dH2O
    • Dissolve ppt using 6M HCl dropwise.
    • Dilute to 2mL.
    • Add 10 drops of 1M (NH4)2SO4
    • Stand for 10 minutes and centrifuge.

    CC4 {Ca2+}
    • Add 2 drops of NH3
    • Add 5 drops of 0.5M (NH4)2C2O4 PC5
    • Centrifuge SrC2O4
    White

    CaC2O4,
    White
    10 drops CC1 (Cations for Group D – E from Analysis of Group C.
    • Heat the supernatant to dryness in low heat.
    • Cool for 5 mins and then add 6 drops of conc’d HNO3.
    • Heat to dryness again in low heat.
    • Cool for 5 minutes.
    • Dissolve the residue in 5 drops of 6M HCl.
    • Transfer quantitatively in a centrifuge tube using dH2O.

    CD1
    {Mg2+, Ni2+, Cu2+, Cd2+, Zn2+}

    1 drop of CD1 1 drop of CD1


    • Add 6M NH3 until neutral. •Add 6M NH3 with stirring until
    • Add 2 drops of 6M acetic acid to basic.
    make it slightly acidic. • Add 10 -15 drops
    • Add 3-4 drops of 0.1M K4Fe(CN)6 dimethylglyoxime (DMG)

    Cu2Fe(CN)6 Ni(DMG)2
    Maroon Cherry Red

    Remainder of CD1
    • Add 6M NH3 until neutral
    • Add 2 drops of 6M CH3COOH to make it
    slightly acidic.
    • Add 0.2 -0.3 g solid Na2S2O3.
    • Heat for 10 mins in boiling water bath.
    • Cool for 1 minute by swirling in cold temp.
    • Centrifuge.
    CD1

    CD2 {Mg2+} PD1 {CdS, ZnS, NiS, CuS}


    • Add 6M NH3 until basic. • Add 50 drops of 6M NaOH using
    • Add 6-8 drops of 0.1M Na2HPO4. Pasteur Pipet.
    • Allow to stand for several • Stir and centrifuge.
    minutes. • Quickly decant supernatant in a
    • Centrifuge. test tube.

    MgNH4PO4 (White Precipitate)

    CD3 {Zn2+} PD2 {CdS, NiS, CuS}


    • Add 12M HCl dropwise stirring until • Wash twice with 10 drops of dH2O.
    slightly acidic. • Add 6 drops of 6 HCl.
    • Add 4 drops of 0.1M K4Fe(CN)6 (do • Stir and centrifuge.
    this under the fumehood) • Quickly decant supernatant in a test
    tube.

    Zn2Fe(CN)6 (White Precipitate)

    PD4 {NiS, CuS}


    Discard

    CD4 {Cd2+}

    3 drops of CD4 {Cd2+} 3 drops of CD4 {Cd2+}


    • Add 6M NH3 until neutral. • Add 6 NH3 until neutral.
    • Add 2 drops of 6M CH3COOH to make • Add 5 drops of 0.2M Na2S.
    it slightly acidic.
    • Add 5 drops of 0.1M K4Fe(CN)6

    Cd2Fe(CN)6 CdS
    (White Precipitate) Yellow Precipitate
    Group E Cations

    Flame Test • Put 10 drops of the original solution


    in an evaporating dish.
    • Make alkaline with 6M NaOH, add 2
    more drops
    • Evaporate CC1 to two drops. • Cover dish with watch glass, on the
    • Discard any precipitate. underside of which is attached a wet
    • Add 1 drop conc’d HCl. red litmus paper.
    • Warm the solution but do not boil.
    Uniform (not spotted) change from red
    to blue of the litmus paper verifies
    presence of NH4+
    Na+ K+
    Intense Reddish
    Yellow Flame Violet
    NH4+
    Without With Blue
    Blue Filter Filter
    ANIONS (1 drop)

    1 drop 0.1M AgNO3

    AgI Ag2S2O3 Ag2S AgCl Ag2CO3 Ag3PO4 SO42-,


    AgBr AgSCN Ag2C2O4 SO32-,
    2 drops 2 drops NO3-
    2 drops 2 drops
    of 2M of 2M
    2 drops of 2M of 2M 2 drops
    HNO3 HNO3
    of 2M HNO3 HNO3 of 2M
    HNO3 HNO3
    Insoluble Insoluble Insoluble Colorless
    Solution
    Insoluble

    CO32- C2O42-

    1 drop 0.1M FeCl3

    SO42- C2O42- S2O32- NO2- FeSCN2+ FePO4


    SO32- S2-,
    NO3- CO32-
    Cl- ,Br- I-

    1 drop 0.1M BaCl2 plus 2 1 drop 0.1M FeSO4


    drops of 2M HNO3

    Fe(NO2)+ NO3-
    NO2- NO3- BaSO4
    BaSO3 1 drop
    of conc’d
    H2SO4

    NO2-

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