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SYSTEMATIC SEMI-MICRO QUALITATIVE ANALYSIS OF A SIMPLE INORGANIC SALT

EXPERIMENT OBSERVATION INFERENCE


Physical Examination-
1. Colour Colourless/white Cu+, Ni+2, Fe+2, Cr+3, Mn+2, Co+2
Absent
2. Smell a) Ammonia smell NH4+ present
b) Rotten eggs smell S-2 present
c) Vinegar smell CH3COO- present
3. Solubility
a) Salt + Water (hot/cold) soluble Given salt is soluble salt
b) Salt + dil. HCl (hot/cold)
Preliminary Test
4. Dry heating test - pinch of Colourless gas evolved with -
salt in dry test tube. Heat it a) Rotten eggs smell S-2 present
on flame. b) Suffocating smell SO3-2 present
c) pungent smell, white fumes Cl- present
when glass rod dipped in Ammonia,
brought near mouth of test tube
d) Vinegar like CH3COO- present
e) Ammonia smell, gas turns Nessler’s NH4+ present
reagent brown

Coloured gases-
a) Reddish brown fumes NO2- or NO3- present
b) Greenish yellow fumes that turn
starch Iodide paper blue Cl- present
c) Reddish brown fumes that turns Starch
paper orange Br- present
d) Dark violet fumes NH4+ present

Sublimate formed a) White NH4+ present


b) Black I- + present

Decrepitation Crackling sound Cl- , CH3COO- , NO2-


present

5. Flame Test - paste of salt prepared in a) Dark green flame Cu2+ present
conc. HCl & glass rod dipped in the paste b) Pink violet flame K+ present
is burnt in blue flame of burner. c) Brick red flame Ca2+ present
d) Grassy green flame Ba2+ present
e) Crimson red flame Sr2+ present

6. dil. H2SO4 test –


Pinch of salt + few drops dil.H 2SO4 a) colourless & odourless gas that turns CO32- present
lime water milky
b) colourless gas with rotten eggs smell, S2- present
turns moist lead acetate paper black
c) Colourless gas, smell of burning SO32- present
Sulphur
d) Reddish brown gas, that turns FeSO4 NO2- present
soln. black
e) No gas evolved Absence of CO32- , S2- ,
SO32-, NO2-

7. Conc. H2SO4 test – a) colourless gas that forms dense white Cl- present
Pinch of salt + Few drops of conc. H2SO4 fumes when glass rod dipped in NH 4OH
soln. is brought near test tube mouth
b) Reddish brown fumes of pungent Br- present
smell that turns starch paper yellow
c) Deep violet vapours that turn starch I- present
paper blue
d) Reddish brown gas that turns fresh NO3- present
FeSO4 soln. black

Confirmatory Test for the Identification of Anions (Acid radicals)


*Preparation of Aqueous solution or Water extract(W.E) of salt – prepared by
dissolving salt in water (water soluble salts)
C.T for Carbonate- CO32-
a) Dil. HCl test - W.E + few drops dil.HCl Colourless, odourless gas with brisk CO3 2- present
effervescence that turns lime water milky
b) MgSO4 test -W.E+few drops MgSO4 soln. White precipitate CO32- confirmed

C.T for Sulphite SO32-


a) Barium chloride test – W.E + few drops White precipitate soluble in dil.HCl SO32- confirmed
BaCl2 soln.
b) Potassium dichromate test – W.E + few Green colour solution SO32- confirmed
drops K2Cr2O7 soln. + few drops dil.H2SO4

C.T for Nitrite NO2-


a) Ferrous sulphate test – W.E + few drops Dark brown/ black colour NO2- confirmed
dil.CH3COOH + few drops FeSO4 soln.
b) Diphenylamine test – W.E + few drops A deep blue colour is obtained NO2- confirmed
Diphenylamine

C.T for Chloride Cl-


a) Silver nitrate test – W.E + dil.HNO 3 + few curdy white precipitate insoluble in Cl- confirmed
drops AgNO3 solution. NH4OH
b) Chromyl chloride test - Salt + solid K Reddish brown vapours
2Cr2O7 + conc.H2SO4. Warm.
Pass vapours through NaOH solution taken Solution turns yellow Cl- confirmed
in another test tube.
Yellow solution + CH3COOH solution. Yellow precipitate

C.T for Bromide Br-


a) Silver nitrate test (AgNO3) - W.E + few Yellow precipitate partially soluble in Br- confirmed
drops dil.HNO3, boil, cool + few drops NH4OH
AgNO3 solution.

C.T for Iodide I-


a) Silver nitrate test (AgNO3) – W.E + Yellow precipitate insoluble in NH4OH I- confirmed
dil.HNO3 + few drops AgNO3 solution.

C.T for Nitrate NO3-


a) Copper turning test – Pinch of salt + Dark brown fumes NO3- confirmed
conc.H2SO4 + Cu turnings. Heat
b) Brown ring test – W.E + Fresh FeSO4 Dark brown ring at the junction of two NO3- confirmed
solution + conc.H2SO4 dropwise along the layers
sides of test tube.

C.T for Acetate CH3COO-


a) Ester test – Pinch of salt + conc. H2SO4. Pleasant fruity smell of Ester CH3COO- present
Heat + Ethanol. Pour the contents in a
beaker with excess water.
b) FeCl3 test - W.E + FeCl3 solution Deep red colour CH3COO- confirmed
divide into two parts-
(i) One part + dil. HCL Red colour disappears
(ii) second part + H2O. Boil Reddish brown ppt

C.T for Sulphate SO42-

a) BaCl2 test – W.E + dil. HCl + BaCl2 White ppt insoluble in dil.HCl SO42- confirmed
solution
b) Lead acetate test – W.E + Acetic acid. white ppt soluble in excess of hot SO42- confirmed
Boil, cool + Lead acetate. Ammonium acetate solution

C.T for Phosphate PO43-


a) W.E + dil HCl. Boil off CO2. Cool + solid White precipitate PO43- confirmed
NH4Cl. Boil, cool + MgSO4 solution + excess
NH4OH solution. Scratch the sides of test
tube.

IDENTIFICATION OF BASIC RADICALS OR CATIONS


Analysis of Zero group – NH4+
a) Sodium hydroxide test – few mg of salt + Evolution of dense white fumes NH4+ present
few drops NaOH solution. Warm gently & a
glass rod dipped in conc. HCl is brought
near mouth of test tube
b) Nessler’s reagent test – few mg of salt + Brown precipitate NH4+ confirmed
NaOH soln. + Nessler’s reagent

Analysis of I group – Pb2+


a) W.E + dil.HCl White precipitate Pb2+ present

C.T for Pb2+ -


a) Potassium Iodide test – W.E + KI solution Yellow precipitate Pb2+ confirmed
b) Potassium chromate – W.E + K2Cr2O7 soln. Yellow ppt

Analysis of II group – Pb2+, Cu2+, AS3+


a) W.E + dil.HCl + solid Na2S black precipitate II group present

b) NH4OH test – W.E + dil.HCl + dil.HNO3 - Blue precipitate


black ppt. To the ppt add NH4OH dropwise Cu2+ present
C.T for Cu2+ - Reddish brown ppt Cu2+ confirmed
Potassium ferrocyanide test – W.E + Acetic
acid + K4FeCN6

Analysis of III group – Fe3+, Al3+


a) W.E + solid NH4Cl. Boil, cool + NH4OH white precipitate III group present
excess

b) W.E + dil. HCl + NaOH dropwise White ppt Al3+ present


C.T for Al3+ - Al3+ confirmed
Lake test – white ppt + dil.HCl + few drops Blue ppt suspended in colourless medium
blue litmus soln. + excess NH4OH soln.

Analysis of IV group – Mn2+, Zn2+


a) W.E + solid NH4Cl. Boil, cool + NH4OH Flesh coloured or white precipitate IV group present
excess + solid Na2S.

b) W.E + NaOH excess White ppt gradually turns brown insoluble Mn2+ present
in NaOH

C.T for Mn2+ - Mn2+ confirmed


Permanganic test – W.E + PbO2 + conc.HNO3. Top part of the soln. is pink coloured
Boil, cool
c) NaOH test- W.E + NaOH drop by drop, White ppt dissolves in excess of NaOH Zn2+ present
excess.
Divide the soln. into two parts-
(i) first part + solid Na2S White ppt Zn2+ present
(ii) second part + acetic acid + K4Fe(CN)6 Bluish white ppt Zn2+ confirmed
soln.

Analysis of V group – Ba2+, Sr2+, Ca2+


a) W.E + solid NH4Cl + NH4OH + NH4CO3 white precipitate V group present
Warm

b) W.E + K2CrO4 soln. Yellow ppt Ba2+ present


c) W.E + Ammonium sulphate, warm White ppt Sr2+ present
d) W.E + Ammonium oxalate White ppt Ca2+ present

e) Flame test – salt + conc. HCl, make paste. a) grassy green flame Ba2+ confirmed
A little paste in glass rod & burnt in non-
luminous flame b) Crimson red flame Sr2+ confirmed

c) brick red flame Ca2+ confirmed

Analysis of VI group – Mg2+


a) Disodium hydrogen phosphate test-
W.E + NH4Cl + NH4OH + disodium
hydrogen phosphate. Scratch inside of test White crystalline precipitate V group present
tube with glass rod

b) W.E + excess of NaOH soln. White ppt insoluble Mg2+ present & confirmed.

RESULT-

The given Inorganic salt contains-


Acid Radical - ……………..
Basic Radical - ………………

REPORT :
The given sample of Inorganic salt is ……………

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