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Unknown Solution for the

Separation of Group 1-5 Cations

Add 6M HCl (3-5 drops)

White Precipitate possible

(AgCl, HgCl, PbCl2)

Centrifuge and decant

Supernatant Liquid
White Precipitate
6M HCl (1 drop) (Undergo complete precipitation)
Washing (Cold Water) Centrifuge and decant
Centrifuge and decant
Unknown Solution containing
Group 3 to 5 Cations Unknown Solution containing
White Precipitate Supernatant Liquid (discard)
White Precipitate Supernatant Liquid Group 4 to 5 Cations
(If no more precipitate forms, the
Hot Water (1 mL) 1mL of 5M NH4Cl
unknown solution is ready for analysis
Mix then heat in boiling water bath 15M NH4OH (until basic). Add NH4Cl (30 drops)
of Group II Cations)
Centrifuge and decant add 5 drops in excess Add 6M NH4OO (until alkaline)
10 drops of 1M thioacetamide Hot bath
Mix Add 1mL of 2M (NH4)2CO3 (for complete precipitation)
White Precipitate Supernatant Liquid Heat in water bath (7-10mins) Centrifuge
0.2M K2CrO4 Centrifuge Decant
(2 drops) 3 mL Unknown Solution containing
Washing (Hot Water) Decant
Group 2 to 5 Cations
Centrifuge and decant Yellow Precipitate
Supernatant Liquid
(Presence of Pb+ ion) Place in an evaporating dish Precipitate
A-1 Residue (If no more precipitate forms, the Unknown Solution containing
Litmus paper test Supernatant Liquid unknown solution is ready for the Group 5 Cations
White Precipitate Supernatant Liquid (discard) Add 1mL hot water Analysis of Group V Cations)
Add 10 drops of 6M HNO3 TEST FOR COMPLETE PRECIPITATION: Centrifuge and Decant
6M NH4OH (10 drops) Warm the tube
Centrifuge and decant 6M HNO3 6M HCl (until acidic)
Acidic Alkaline Agitate the suspension Add 5 drops thioacetamide
(10 drops) IF THE: Pour into an evaporating dish
White Precipitate Heat test tube for 5-10 mins Supernatant Liquid Making of Known Solution
Filtrate A White Precipitate 6M NaOH soln. (drop by drop until basic)
(Presence of Ag+ ion) 3% H2O2 soln. (2 drops) If precipitate forms (Add to A-1 residue)
Divide the Filtrate 4 drops excess
Grey Precipitate or Supernatant Liquid Evaporate to a volume of 10 drops Centrifuge Place a moist red litmus paper on the side of the watch glass 0.1 M NaNO3 soln (8 drops)
Add 1mL of 6M acetic acid
Blackening of Residue 6M NH4OH Precipitate Precipitate (did not Decant Cover evaporating dish with watch glass 0.1 M KNO3 soln. (8 drops)
KI solution Stir to dissolve 12M HCl (drop by drop until acidic)
(Presence of Hg+ ion) (dissolved) dissolve) (Repeat until complete precipitation) Heat Water (1 mL)
(2 drops) Heat 5 drops excess
Pale Yellow Precipitate Neutral Solution Add more 6M acetic acid(until complete dissolution) 12M HCl (5 drops)
Filtrate B
(Presence of Ag+ ion) Wash Dilute with water up to 2mL Red litmus paper turns blue
6M HCl (6-10 drops) Add 10 drops of 6M HNO3 Add 5 drops of 1M K2CrO4 (one drop at a time) Acidified Unknown Solution Known Solution
(Presence of NH4+ ion)
Warm the tube Precipitate Supernatant Liquid Stir for 1 min
Acidic Solution Add a drop of 3% H2O2 (If no more precipitate forms, the Centrifuge
A-B-1
add more if necessary unknown solution is ready for
Solution
Transfer to centrifuge tube analysis of Group IV Cations)
Add 0.5 mL water to transfer remaining solids to centrifuge tube FLAME TEST FLAME TEST
Add 6M NaOH (until basic) Yellow Precipitate in solution Supernatant Liquid
1M C2H5NS (thioacetamide) 20 drops
Add 8 drops excess (presence of Barium ion) (possible presence of
Dilute to 4 mL Yellow Flame
Add 5 drops 3% H2O2 Sr, Ca, Mg, CrO4 ions)
Cap test tube w/ deflated balloon (Presence of Na+ ion)
Boil (until bubble of O2 are no longer evolved)
Hot Bath (10 mins)
Centrifuge Add Concentrated NH4OH (until strongly basic)
FLAME TEST:
Filter Centrifuge
Dark Colored Precipitate
Stir FLAME TEST:
Hot bath FLAME TEST:
Green/ Yellow-green flame
Cold Bath (with two thickness (with two thickness
B-1 Filtrate A-2 Precipitate (Presence of Ba+2 ion) Add (NH4)2CO3
Agitate (1 min.) cobalt glass) cobalt glass)
Centrifuge Lavender Flame
Centrifuge and decant Decant (Presence of K+ ion)
Add drops of 6M HNO3 (until acidic) Dilute to 2mL with water
Add 6M NH4OH (until basic) Add 6M NH4OH (until alkaline)
Add 5 more drops excess 5 drops excess
Precipitate Supernatant Liquid Heat in water bath for 5mins Supernatant Liquid (discard) Yellow Precipitate
Centrifuge
Add water (1-2 mL) pH paper Decant Precipitate formed
5M NH4NO3 (2 drops) Add 1M NH4OH
Agitate (1-2 drops) Centrifuge Washing
Add 1 mL water Decant
>0.3 M [H+] soln. Precipitate B-2 Solution
Centrifuge and decant White Precipitate
(discard)
(possible presence of
Precipitate Supernatant Liquid SrCO3, CaCO3, MgCO3)
<0.3 M [H+] soln.
Precipitate Supernatant Liquid (discard)
Colorless solution Yellow Solution Wash with 1mL Add 1mL of 6M acetic acid
1M thioacetamide (5 drops) Decant
Add water (1-2 mL) Centrifuge
Cap w/ balloon
Centrifuge and decant Dissolve residue by adding 5 drops 6M HCl
Hot Bath (10 mins.) Heat to boiling
Dilute to 2mL
Centrifuge and decant Add 10 drops of 0.5M BaCl2 sol’n
Add 5 drops 1M KSCN solution
Precipitate (discard) Supernatant Liquid
Supernatant Liquid (discard) Formation of BaCrO4 (yellow) and
BaSO4 (white) or a mixture of Add 5 drops of 1M (NH4)2SO4
Deep red solution Submerge in boiling water bath
Precipitate Supernatant Liquid both may PRECIPITATE
(Presence of Fe+3 ion) Cool
Centrifuge
Centrifuge and decant Centrifuge
Add 1 drop of 1M (NH4)2SO4
Decant
Cu-As Precipitate
(Undergo complete precipitation)
Carmine red flame FLAME TEST: White precipitate (possible
0.5M KOH (2 mL) (Presence of Sr+2 ion) presence of SrSO4)
Hot Bath (2 mins.) Precipitate Precipitate B-3 Solution
Supernatant Liquid
Centrifuge and decant (If no more precipitate forms, the Wash with 2mL water Add 6M HCl (until acidic) Centrifuge
unknown solution is ready for the Centrifuge Decant
analysis of group III Cations) Add 3 drops of 0.2M K4[Fe(CN)6]
Decant Agitate
Precipitate Supernatant Liquid Centrifuge
(As - Solution) Supernatant Liquid White precipitate
0.5M KOH (2 mL) Residue Liquid used in (possible presence of Mg+2 and Ca+2)
washing (discard) Very Light Green Precipitate
Centrifuge and decant Add concentrated HCl (10-15 drops) (Presence of Zn+2 ion)
Hot Bath (until precipitate dissolves) Add 10 drops of 3% H202 Add 5 drops of 1M (NH4)2 C2O4
Centrifuge and decant Agitate Boiling water bath
Add one drop 6M HNO3
Precipitate (Cu) Supernatant Liquid White precipitate/ Cloud soln.
(presence of Calcium ion)
5M NH4NO3 (2 drops) Precipitate (discard) Supernatant Liquid Blue color that fades quickly
Washing (Presence of Cr+3 ion) Centrifuge
Centrifuge and decant Evaporate (until approx. 4 drops) Decant
Add 2mL water
Divide into two
Precipitate Supernatant Liquid (discard) Supernatant Liquid Precipitate FLAME TEST: Orange-red or Brick-red flame
(possible presence of Mg ion) (possible presence of CaC2O4) (Presence of Ca+2 ion)
6M HNO3 (1 mL) Solution A Solution B
Boiling Water Bath (2 mins.) Add a pinch of NH4Cl
Centrifuge and decant Agitate
Litmus paper Ammonium molybdate
Add a small amount of Nh4OH
6M NH4OH (until basic)
Add (NH4)PO4
6M CH3COOH (until acidic)
Stir
Precipitate (discard) Supernatant Liquid Pour into test tube w/ sodium thiosulfate
Hot Bath
White precipitate/ Cloudiness
15M NH4OH (until basic) (Presence of Mg+2 ion)
Centrifuge and decant Formation of an orange-red
Blue Solution
antimony oxysulfide ring
(Presence of Sn+2, Sn+4 ion)
(Presence of Sb3+ ion)
White Precipitate Deep Blue Colored Solution
(Presence of Bi+3 ion) (Presence of Cu+2 ion)

6M acetic acid (until acidic)

2M K4[Fe(CN)6] (3 drops)

Red Brown Precipitate

(Presence of Cu+2 ion)