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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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