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SALTANALYSISLABMANUAL 9owo8xhodwx68kh7
SALTANALYSISLABMANUAL 9owo8xhodwx68kh7
To a small amount of e. Slight brown fumes II group acid radical NO3- may
the salt taken in a test turning FeSO4 black are be present.
tube add conc.H2SO4 evolved on heating.
and heat slightly.
MNO3+H2SO4 → MHSO4+HNO3
6FeSO4+3H2SO4+2HNO3 → 3Fe2(SO4)3+2NO+4H2O
FeSO4+NO → FeSO4.NO
f. No characteristic reaction Absence of Cl-, Br-, I-, NO3-, C2O42-
(II Group acid radicals)
Note on Sodium Carbonate Extract :
a. When to prepare :
a) If the salt in insoluble or partly soluble in water,
b) If the salt is colourised ,
c) If the salt contains Ba2+, Pb2+.
If not, prepare water extract by dissolving a small amount of the salt in H2O
b. Why to prepare :
To convert the salt to a colourless sodium salt solution of the given anion
c. How to prepare:
To 1 part of the salt add 3 parts of Na2CO3 and 1 test tube of water. Boil well for two minutes , cool
and filter. The filtrate is called the SODIUM CARBONATE EXTRACT .
Sodium Nitroprusside
test:
c.
To a portion of S.E. or Purple colour is obtained. Presence of S2- is
W.E (to which some confirmed
NaOH has been added),
add 2 drops of sodium
nitroprusside solution. Na2S+Na2[Fe(CN)5NO] → Na4[Fe(CN)5NOS]
(violet)
8. Confirmatory tests
for SO32- :
To the W.E. or S.E. White precipitate is formed. Presence of SO32-
(acidified with
CH3COOH & CO2 is
boiled off), add BaCl2
solution and filter
(i) To one portion of the The precipitate dissolves with evolution of SO2. Presence of SO32-
ppt add dil.HCl
Na2SO3+BaCl2 → 2NaCl+BaSO4 (white)
BaSO3+2HCl → BaCl2+H2O+SO2
(ii) To the W.E. or S.E. The pink colour gets discharged. Presence of SO32- is
add a few drops of confirmed
acidified KMnO4 2KMnO4+3H2SO4 → K2SO4+2MnSO4+3H2O+5[O]
SO32- + [O] → SO42-
9.
a. Confirmatory tests A blue-black solution is obtained Confirms the presence
for NO2- : of NO2-
To a portion of W.E. or
S.E. acidified with dil
H2SO4 add a few drops 2KI+4H2SO4+2MNO2 → 2KHSO4+2NO+2H2O+I2+ 2 MHSO4
of KI followed by a few Starch + I2 → blue-black colouration
drops of starch solution.
a. To a small amount of
the substance taken in a
test tube, add conc-
H2SO4 and warm. Then
add C2H5OH and shake
well. Pour the contents
of the test tube into a
beaker of water. Stir the
solution.
12. Confirmatory tests Deep red-brown vapours turning starch paper Presence of Br – is
for Br-: (moist) yellow and starch iodide paper (moist) confirmed
a. To a pinch of the blue are evolved.
substance taken in a test
tube add a few grains of 2MBr+3H2SO4 → 2MHSO4+2H2O+SO2+Br2(brown)
MnO2 and 2-5cc of conc-
H2SO4 and warm.
To the W.E or S.E in An orange-brown organic layer is formed. Confirms the
b. a test tube add fresh presence of Br–.
chlorine water and
then a few drops of 2Br -+Cl2 → 2Cl - + Br2(orange brown)
CCl4. Shake well.
To prepare chlorine water, take either a single crystal of KMnO 4 or a few grains of MnO2 and add conc-HCl.
Close the mouth of the test tube for 5 seconds. The resulting liquid can be used as chlorine water. (The
chlorine water prepared from MnO2 is very strong. Therefore it must be used sparingly)
To the W.E or S.E (acidified with CaCl2 + Na2C2O4 → CaC2O4(white ppt) + 2 NaCl
acetic acid) add calcium chloride
solution
16. GROUP III. A white precipitate insoluble III group acid radical
Tests for SO42-: even in conc-HCl, is obtained. SO42- may be present.
MSO4+(CH3COO)2Pb → (CH3COO)2M+PbSO4↓(white)
PbSO4+2(CH3COO)NH4 → (NH4)2SO4+(CH3COO)2Pb
17. Confirmatory tests for PO43-: Canary yellow precipitate is formed. Confirms the presence of
a. Ammonium molybdate test: PO43-
To the W.E or S.E.(acidified) or 2M3PO4+3(NH4)2MoO4 → 2(NH4)3PO4+3M2MoO4
the solid substance add conc M2MoO4+2HNO3 → 2MNO3+H2MoO4
HNO3 and boil well. Then add H2MoO4 → H2O+MoO3
excess of ammonium molybdate (NH4)3PO4+12MoO3+6H2O → (NH4)3PO4.12MoO36.H2O
solution.
b. To the W.E. or S.E. (acidified with A white precipitate is formed.
Confirms the presence of
dil-HCl), boil off CO2and then add PO43-
magnesia mixture. M2HPO4+MgCl2+NH4OH → MgNH4PO4(white)+2MCl+H2O
Preparation of Magnesia mixture: Add solid NH4Cl to Mg2+ solution. Add NH4OH till a strong smell of
Ammonia is got.
BASIC RADICAL ANALYSIS
Preparation of original salt solution: (OS)
To the solid salt , add ¼ test tube of water and shake well. If it is insoluble in cold water, heat the water and
the salt mixture. If it is insoluble even in hot water dissolve the salt in minimum quantity of dil-HCl. Boil
well. The resulting solution is called the OS.
REAGENT
GROUP PRECIPITATE COLOUR
I
Dil-HCl PbCl2 White
CuS Black
II Dil-HCl+H2S
CdS Yellow
Fe(OH)2 Green
III NH4Cl+NH4OH Fe(OH)3 Yellowish–brown
Al(OH)3 Gelatinous white
CoS Black
NiS Black
IV NH4Cl+NH4OH+H2S
MnS Buff(flesh)
ZnS White(dirty)
BaCO3
V NH4Cl+NH4OH+(NH4)2CO3 SrCO3 White
CaCO3
a. Green precipitate
Presence of Fe2+
b. Gelatinous white
Presence of Al3+
precipitate
Presence of Fe3+
To the OS, add solid NH4Cl till c. Brown precipitate
it dissolves. Then add excess Absence of Group III ions .
III d. No precipitate
of NH4OH till a pungent smell
of NH3 is got.
A𝑙 3+ +3OH- → Al(OH)3(White)
F𝑒 2++2OH- → Fe(OH)2(Green)
F𝑒 3++3OH- → Fe(OH)3(Brown)
a. Black precipitate Presence of Co2+ or Ni2+
ANALYSIS OF GROUP I
To the second part of the (or OS ) (i) Chocolate brown Presence of Cu2+ is
b. nadd K4[Fe(CN)6] precipitate is formed. confirmed.
Cu +K4[Fe(CN)6 → Cu2[Fe(CN)6] + 4 K+
2+
(chocolate brown)
(ii) White or blue –white Presence of Cd2+ is
precipitate is formed. confirmed
2Cd2++K4[Fe(CN)6] → Cd2[Fe(CN)6]+4K+
Blue-white
[Note: It is a common practice to oxidize Fe2+ to Fe3+ in the III group. If the III group precipitate is
green in color, add few drops of conc. Nitric acid and heat (to convert ferrous ions to ferric ions).
Cool and add excess ammonium hydroxide solution to get the precipitate to ferric hydroxide.
Dissolve the precipitate in dilute HCl and do the confirmatory tests for ferric ions].
[Reasons for adding Ammonium chloride in the III group: Ammonium chloride suppresses the
ionization of ammonium hydroxide (Common ion effect). In the absence of ammonium chloride,
cations of subsequent groups such as Zn2+ and Mn2+ may also be precipitated along with the
hydroxides of Fe3+ and Al3+. Ammonium chloride reduces the concentration of OH- by common
ion effect and buffer action and thus prevent the metals of subsequent groups from being
precipitated as hydroxides, which have higher solubility product values than those of the
hydroxides of group III cations.]
ANALYSIS OF GROUP IV
To the second part or OS add White precipitate is formed. Confirms the presence
b.
(NH4)2SO4 solution. of Sr2+
Sr2++(NH4)2SO4 → SrSO4 (white) +2NH4+
White crystalline precipitate Confirms the presence
To the third part or OS add
c. is formed. of Ca2+
(NH4)2C2O4
Ca +(NH4)2C2O4 → CaC2O4(white crystalline)+ 2NH4+
2+
ANALYSIS OF GROUP-VI