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qualitative analysis of cations and anions

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DAY 2: Reactants (Color) Na2SO4 (clear)Na2CO3 (clear) NaCH3COO (clear) NaCl (clear) KMnO 4 (violet) CuSO 4 (blue) CuSO4 (blue) DAY 3:

Observations Precipitate formationGas formation

Predicted Product BaSO4 NaClH2CO3 NaCl

Net Ionic Equation Ba2+ (aq) + SO42- (aq)

Type of interionic reactionPrecipitate

BaCl2 (clear)HCl (clear) HCl (clear) KNO3 (clear) FeSO4 (orange)

BaSo 4 (s) + (aq) + CO 2- (aq) H 2H 3 2CO3 (s) + (aq) + CH H 3COO (aq) CH3COOH (aq) no net ionic equation

Gas

Vinegar smell

CH3COOH NaCl + Cl- K+ NO Na 3

Odor Ion formation

No visible reaction

Red -> Iron precipitate

FeO4 + MnO K 4

Little NH3 (clear) Excess NH3 (clear)

Less cloudy (blue)

Cloudy (blue)

Cu(OH)2 + SO 22NH4 4 2+ [Cu(NH3)4]

MnO - (aq) + 8 H+ (aq) + 5 Fe2+ 4 (aq) Mn2+ (aq) + 4 H 2O (l) + 5 3+ (aq) Fe Cu2+ (aq) + 2 OH- (aq) Cu(OH) 2 (s) Cu2+ (aq) + 4 HN

Redox

Precipitate Complex

3 (aq) 2+ (aq) Cu(NH3)4

Ba(NO 3)2 (colorless) Ba(NO3)2 (colorless) Na2SO4 (colorless) FeCl3 (orange) White ppt (Ba SO4) Orange (NR)

Na2SO4 (colorless) White ppt (Ba SO4)

FeCl3 (orange) Orange (NR) Light Yellow (Fe(SO4)3)

Pb(NO3)2 (colorless) Clear (NR) Milky White (PbSO4) Glassy String

KSCN (colorless) Clear (NR) Clear (NR) Black

K2Cr2O7 (orange) Milky Yellow (BaCr2O7) Clear Yellow

K2CrO4 (yellow-green) Milky Yellow (BaCrO4) Clear Yellow

Fe(SO4)3 (Light Yellow)

Dark Orange w/ppt (Fe2(Cr2O7)3)

Dark Orange w/ppt (Fe2(CrO4)3) Pastel Yellow w/ppt (PbCrO4) Clear Yellow

Pb(NO3)2 (colorless)

Clear (NR)

Milky White (PbSO4)

Glassy String

Clear (Pb(SCN)2)

Pastel Yellow w/ppt (PbCr2O7)

KSCN (colorless) K2Cr2O7 (orange)

Clear (NR) Milky Yellow (BaCr2O7)

Clear (NR) Clear Yellow

Black

Clear (Pb(SCN)2)

Light Orange

Dark Orange w/ppt (Fe2(Cr2O7)3)

Pastel Yellow w/ppt (PbCr2O7) Pastel Yellow w/ppt (PbCrO4)

Light Orange

Light Orange

K2CrO4 (yellow-green)

Milky Yellow (BaCrO4)

Clear Yellow

Pastel Yellow w/ppt (PbCrO4)

Clear Yellow

Light Orange

DAY 4-5: CATIO N 2+ Zn Al3+ COLOR NaOH (little: 2 drops) Clear Clear + + NaOH (excess: 3 drops) ++NH 3 (little: 2 drops) + + NH3 (excess: 3 drops) +++ HCl H2SO4 KSCN (NH4)2S + + CH3CSNH2 + -

Ba2+ Ni2+

Clear Clear Green

+ +

++ ++

+ +

++ +-

-

+ -

-

+

-

Ag+ Ca2+ Mg2+ Sr2+ Fe3+ Mn2+ Na+ K+ NH + 4 Cu2+

Clear Clear Clear Clear Orange Clear Pink Clear Clear Clear Clear Blue

+ + + + + +

++ ++ ++ ++ ++ ++

+ + + + + +

+++ ++ ++ ++ +-

+ -

+ -

+ -

+ + + +

+ + +

DAY 6:

Cation Zn2+ Ba2+ Ni2+ Ca2+ Sr2+ Fe3+ Mn2+ Na+ K+ NH + 4 Cu2+

Observation White Green (Bluish Green) Green (Pale/Apple Green)

Yellow (Brick Red) Crimson Red (Crimson) Yellow (Gold) Violet (Yellowish Green) Yellow (Intense Yellow) Violet (Lilac) Green Green (Blue-Green:Halide ; Green:Non-halide)

Cations With color: Cu(blue), Ni(green), Fe(red/orange), Mn(brown) ++: Ba, Ca, Mg, Sr +-: Zn, Ag, Al -: K, Na, NH 4 => verify through flame test

DAY 10:

Solutions Na2CO3 + H2SO4 Na2SO3 + H2SO4

Color of Gas Colorless Colorless

Odor of Gas Vinegar-like Mabaho

Formula of Gas CO2 H2SO3

Test for Gas Observations Loss of precipitates Paper with K2Cr2O7 turns from orange to light green

Na2S + H2SO4

Colorless

Rubber-like

H2S

Faint orange to white Pb(CH3COO)2

Na2S2O3 + H2SO4 NaNO2 + H2SO4

Colorless Colorless

Gunpowder-like Water-like

S2O3 NO2

Green-ish Loss of precipitates

DAY 11:

Solution ( Na2SO4 ( Na2SO3 ( Na2CO3 ( Na3PO4 ( Na2CrO4 ( NaF ( Na2Cr2O7 ( NaNO2 ( Na2S ( Na2S2O3 ( ) ) ) ) ) ) ) ) ) )

+BaCl2 ) -

+3M HCl (

+ KMnO4 )

+

++

+

+-

Purple

+

+-

Purple

+ (yellow)

+-

Red

+ (white)

++

+ (orange)

+-

Dark Red

-

-

+

++

+

++

Confirmatory Tests for Cations +: Add 5 drops 3M HCl to 10 drops unknown => Centrifuge and decant => Treat the ppt with separate 2mL portions of hot water Ag (twice), shaking the test tube while the test tube is heated in the water bath. Decant the first 2mL portion of hot water and treat the precipitate with the second 2mL portion of hot water. => Centrifuge and decant => Add 1mL 6M NH +. Add 6M HNO3 until acidic. White ppt confirms Ag 3 to the precipitate and stir, =>

Fe3+, Ni2+: Add 5 drops 3M NaOH to 10 drops unknown => Centrifuge and decant. => Add the water to the precipitate and discard the washing. Add enough water to give a total volume of about 1 mL. Stir. => Divide the solution into two equal portions. => (1)Add 3 drops of 1M KSCN. A deep red color confirms the presence of Fe3+. => (2) Add 6M NH 3 dropwise until the solution is basic to litmus. Add 5 drops of dimethyglyoxime [(CH3)2C2(NOH)2] solution and stir. Formation of a bright red precipitate confirms the presence of 2+. Ni Zn2+: (1)Add 5 drops 3M NaOH to 10 drops unknown. Centrifuge and decant. To the hydroxide of zinc, acid 6M NH

3 drop by drop with

stirring until it dissolves. Then add 2 drops of thioacetamide solution. Stir and heat in water bath for 3 minutes. Formation of a white 2+. (2)To a fresh sample of unknown solution, precipitate, which dissolves, when the solution is acidified, confirms the presence of Zn add 10 drops of thioacetamide solution, stir and heat in the water bath for 3 minutes. Formation of white precipitate, which dissolves when the solution is acidified with 6M HCl, confirms the presence of Zn2+.

Cu2+: Add concentrated NH 2+. presence of Cu

3 dropwise to the unknown solution until the solution is distinctly basic. A deep blue solution confirms the

Ca2+: To the unknown solution, add 6 drops of H

2O and concentrated CH3COOH dropwise. Then add 6 drops of 1M (NH4)2C2O4 and 2+. stir and heat in the water bath. The presence of a white precipitate confirms the presence of Ca Mg2+: To the unknown solution, add 6M NH

3 until basic. Then add a small amount of dibasic ammonium phosphate (NH4)2HPO4 until 2+ precipitate as a white MgNH 2+. Mg 4HPO4 6H2O. If the precipitate dissolves in 6M CH3COOH, then the unknown contains Mg Al3+: Add 2 drops of aluminon reagent (C

22H23O9N23) to the unknown solution. Add 3-5 drops of 6M NH3 o make the solution just 3+. If color basic. Mix this and let it stand. A flocculent precipitate colored a characteristic of red by the dye proves the presence of Al and precipitate are indefinite, make the solution acid with 3M HCl, then basic with NH + concentration so that the 3, to build up the NH4 solution becomes less basic.

Confirmatory Tests for Anions CO 2-, SO 2-, PO 2-: Add 5 drops of BaCl 3 3 4 2 to 10 drops unknown => Centrifuge and decant => Add 1mL of 3M acetic acid dropwise to the solid. Stir. Add 2 more drops of 3M CH3COOH. Stir, if bubbles are observed, continue to add 3M CH3COOH until no bubbles are 2- Test for CO noted. This destroys the CO3 2 gas. => Divide the solution into 2 portions => (1) Add: 5 drops of 6M HCl, 5 drops of 0.5M 2-. => (2) Add: 5 Ba(CH3COO)2 or Ca(CH3COO)2, 5 drops of 3% H2O2. Formation of a white precipitate confirms presence of SO3 drops of concentrated HNO 3, 5 drops of ammonium molybdate solution. Heat in water bath for 1 minute. Formation of yellow 3-. precipitate confirms the presence of PO4 SO 2-, CrO 2-: Add 5 drops of BaCl 4 4 2 to 10 drops unknown => Centrifuge and decant => Wash precipitate with 1mL water. Discard washings. Add 10 drops of 3M HCl and stir. If soluble proceed to (2). If not, proceed to (1) => (1) Add BaSO4. Add 10 drops of H2O and 2-. => (2) If soluble, BaCrO 5 drops concentrated HCl and stir. White precipitate confirms SO4 4. Add 6M NH3. Yellow precipitate 2-. confirms CrO4 Cl-, Br-, I-, CNS-: Add 5 drops AgNO 3 to 10 drops unknown => Centrifuge and decant => AgCl (White/Dirty White), AgBr (Cream/Light Yellow), AgI (Yellow), AgCNS(White) => Add 2-6 drops 6M NH3. If soluble, add 3M HNO3. Stir until the solution is acidic -. If insoluble proceed to next step => Divide (Check with litmus paper). Formation of white precipitate confirms the presence of Cl precipitate into two. => (1) Place a very small amount of solid on a watch glass. Add 2 drops of 3M HCl and 1 drop of FeCl 3. A red-. => (2) Add 1mL of H blood solution confirms the presence of CNS 2O to the bulk of the residue. Acidify with 6M CH3COOH. Add 1 microspatula of Zn dust and stir thoroughly for 3 mins. Centrifuge. => Disregard residue. Divide solution into two portions. => Test with litmus paper if solution is acidic. If not, acidify with a few drops of 6M CH3COOH. Add 10 drops of oil and a few crystals of NaNO2. - is present. If no, proceed to next step. => Dilute with H2O to a volume of 2mL and shake vigorously. Did solution turn violet? If yes, I Yellowish color in oil layer confirms the presence of Br-.

NO -: (1) Place 1 drop of unknown in spot plate. Add 2 drops of concentrated H 3 2SO4 and 1 drop of napthylamine. Wait several -. (2) Place 5-10 drops of unknown solution in a small teest tube. minutes. Development of purple color confirms the presence of NO3 Without shaking the test tube, add 5 drops of freshly prepared solution of FeSO 4 and 2-3 drops concentrated H2SO4. Observe the -. (3) Place a small crystal of FeSO formation of brown ring at the junction of the solution. This indicates the presence of NO3 4 in a depression of a spot plate. Add 1 drop of unknown and 1 drop of concentrated H2SO4. Formation of a brown ring around the crystal -. indicates the presence of NO3 NO -: (1) Add 1 micro spatula of urea to 1mL 3M HCl. Place 10 drops of this solution to 10 drops of unknown. Evolution of gas confirms 2 the presence of NO -. (2) Add a freshly prepared solution of FeSO 2 4 to 5 drops unknown. Then, add 2 drops of concentrated H2SO4. -. The rapid evolution of a brown gas confirms the presence of NO2 CH -: Warm 50mg of the unknown with 2 drops ethanol and 2 drops of sulfuric acid. The fruity odor of the product is apparent if 3COO

the mixture is allowed to cool and then diluted with water on a watch glass.

CrO 2-, Cr 2-: acidify 10 drops unknown solution with concentrated sulfuric acid. Cool. Get 2 drops of this solution and mix to a 4 2O7 solution of 1 drop 20% H 2- if the 2O2 and 5 drops ether. Shake. Blue color in the upper ethereal layer confirms the presence of CrO4 original solution is yellow, and Cr 2if the original unknown solution is orange. 2O7 C 2-, F-: acidify 10 drops of unknown solution with 3M CH 2O4 3COOH. Boil. Add 10 drops of CaCl2 solution. If precipitate forms, -. centrifuge. Wash the precipitate with hot water. Add 5 drops of 1M H2SO4 and heat. White residue confirms the presence of F Centrifuge and decant. Add 1 drop of dilute KMnO 2-. 4 to the liquid. Decolorization of KMnO4 confirms the presence of C2O4 S2-, SO 2-, PO 3-: Add 5 drops of AgNO 2-(dark brown precipitate), SO 2-(white precipitate), PO 33 4 3 to 10 drops of unknown. => S 3 4 (yellow precipitate).