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Comprehensive Guide to Salt Analysis

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0% found this document useful (0 votes)
44 views10 pages

Comprehensive Guide to Salt Analysis

Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd

SALT ANALYSIS

Salt analysis comes under Qualitative analysis in which components of salts are identified.

Radical: An atom or group of atom having distinct charge + or - .

Salt consist of 1. Basic radical or cation positively Charged species.

2. Acidic radical or Anion negatively charged species.

Classification of cations :

Cation group Cations Group reagents Colour of the ppt.


Group 0 NH4+ ------- -------
Group - I Pb+2 Dil. HCl PbCl2
Group - II Pb+2 H2S in presence of dil.
PbS (Brownish-Black)
Cu+2 HCl CuS (Black)
As+3 As2S3 (Yellow)
Group - III Fe+2,Fe+3 Solid NH4Cl + Excess Fe(OH)3 (Brown)
Al+3 NH4OH Al(OH)3 (Dirty white)
Group - IV Zn+2 H2S in presence of ZnS (Dirty-white)
Ni+2 NH4Cl +NH4OH NiS (Black)
Mn+2 Mns (Light- pink)
Co+2 CoS (Black)
Group - V Ba+2 (NH4)2CO3 in presence BaCO3 (white)
Sr+2 of NH4Cl+NH4OH SrCO3 (white)
Ca+2 CaCO3 (white)
Group - VI Mg+2 None ------

Classification of Anion:

1. Dilute H2SO4 group: CO3-2, S-2, SO3-2,NO2-.

2. Conc. H2SO4 group: Cl-, Br-, I-, NO3-, CH3COO-, C2O4-2.

3. Miscellaneous Group: SO4-2, PO4-3.

1|Page
SALT ANALYSIS
Test for Anions: Diluted Group:

1. Carbonate ion CO3-2:

Experiment Observation Inference


B) Indicatory Test Brisk effervescences, May be CO3-2.
O.S + dil. H2SO4 evolution of colorless
odourless gas (CO2)
Above soln.+ lime water It turns milky CO3-2 present.
C) Confirmatory test White ppt.
i) O.S +BaCl2 solution CO3-2 Confirmed.
ii) O.S + AgNO3 Soln.
iii)O.S + few drops of
MgSO4 soln.
2. Sulphite ion SO3-2

Experiment Observation Inference


B) Indicatory Test Evolution of colorless gas May be SO3-2.
O.S + dil. H2SO4 with smell of burning sulphur
(SO2)
Above soln.+ BaCl2 Soln. White ppt. May be SO3-2
C) Confirmatory test White ppt.
Above soln. + dil. HCl
excess to dissolve + wait
till effervescence ceases
+divide it into 2 parts.
1. Add KMnO4 Pink color of KMnO4 SO3-2 Confirmed.
discharged
2. Add Br2 water Reddish brown color of SO3-2 Confirmed.
bromine discharged
3. Sulphide ion S-2:

Experiment Observation Inference


-2
B) Indicatory Test Evolution of colorless gas May be S .
O.S + dil. H2SO4 with smell of rotten egg.
C) Confirmatory test Black ppt. S-2 Confirmed.
1. lead acetate test: O.S +
Acetic acid soln + Lead
acetate + heat till black
ppt .
2. Sodium nitroprusside Transient purple color S-2 Confirmed.
test: O.S+Sod.
Nitroprusside reagent.
3. Cadmium carbonate test: Yellow ppt. S-2 Confirmed.
O.S+ dist. Water+solid
CdCO3
Salt + AgNO3 Black ppt.

2|Page
SALT ANALYSIS

4. Nitrite ion NO2-

Experiment Observation Inference


B) Indicatory Test
O.S + dil. H2SO4 Evolution of pungent light May be NO2-.
brown gas.
C) Confirmatory test
1. Starch-Iodide test: O.S + Starch Iodide paper turns NO2- Confirmed.
Acetic acid soln + Starch Deep blue.
Iodide paper
2. Thiourea test :
O.S+excess of acetic acid
soln.+pinch of solid NO2- Confirmed.
thiourea+few drops of Blood red color
dil. HCl+few drops of
FeCl3 soln.

Concentrated group

1. Chloride ion Cl-:

Experiment Observation Inference


B) Indicatory Test Colorless pungent gas. Forms May be Cl-.
O.S + Conc. H2SO4+glass white fumes with NH4OH.
rod dipped in NH4OH [Link]
the mouth of T.T.
C) Confirmatory test
1. Silver nitrate test: O.S + Curdy white ppt. Cl- Confirmed.
dil. HNO3 +wait+AgNO3
soln.
2. Chromyl chloride Test :
O.S+K2Cr2O7 soln.+conc.
H2SO4+boil+NaOH+ Yellow ppt. Cl- Confirmed.
acetic acid + lead acetate.

3|Page
SALT ANALYSIS

2. Bromide ion Br-:

Experiment Observation Inference


B) Indicatory Test
O.S + Conc. H2SO4 Reddish brown Vapour. May be Br-.
Add MnO2 Intensifies brown color.
C) Confirmatory test
1. Silver nitrate test: O.S + Yellow ppt. Br- Confirmed.
dil. HNO3 +wait+AgNO3
soln.
2. Chlorine water or layer
Test : O.S+1 ml CCl4
+conc HNO3 dropwise Orange color in CCl4 layer Br- Confirmed.
Cl2 water with constant (lower).
shaking.

3. Iodide ion I-:

Experiment Observation Inference


B) Indicatory Test
O.S + Conc. H2SO4 Violet vapour. May be I-.
Add MnO2 Intensifies violet color
C) Confirmatory test
1. Silver nitrate test: O.S + Yellow ppt. I- Confirmed.
dil. HNO3 +wait+AgNO3
soln.
2. Chlorine water or layer
Test : O.S+1 ml CCl4
+conc HNO3 dropwise Violet color in CCl4 layer. I- Confirmed.
Cl2 water with constant (lower).
shaking.

4|Page
SALT ANALYSIS

4. Nitrate ion NO3-

Experiment Observation Inference


B) Indicatory Test
O.S + Conc. H2SO4 Evolution of brown fumes. May be NO3-.
Add Cu chips+Heat More brown fumes

C) Confirmatory test
1. Brown ring test: O.S + Brown ring form at the NO3- Confirmed.
dil. H2SO4 +wait+fresh junction of two liquids.
FeSO4 soln.+conc.H2SO4
along the side of the T.T
2. Diphenylamine Test :
O.S+1 ml diphenylamine Blue ring form at the junction NO3- Confirmed.
reagent along the side of of two liquids.
the T.T

4. Acetate CH3COO-:

Experiment Observation Inference


B) Indicatory Test
O.S + Conc. H2SO4 Strong smell of vinegar May be CH3COO-.

C) Confirmatory test
Neutral Ferric chloride Brick red color. CH3COO- Confirmed.
test: O.S + dil. HCl +
fresh FeCl3 soln.

Sulphate ion SO4-2

Experiment Observation Inference


C) Confirmatory test
Barium chloride test: O.S White ppt. SO4-2 Confirmed.
+ dil. HCl + BaCl2 soln.

5|Page
SALT ANALYSIS
Lead acetate test: O.S White ppt. SO4-2 Confirmed.
acetic acid soln.+Boil+1 ml
lead acetate soln.

Test for Cations:

Group zero: NH4+:

Experiment Observation Inference


B) Indicatory Test
a) Salt+ Conc. NaOH+Heat Strong smell of ammonia. NH4+ may be present.
b) Take a rod dipped in Evolution of white fumes. NH4+ present.
HCl at the mout of T.T.

C) Confirmatory test
1. Salt + dist. water + Red-brown ppt. NH4+ Confirmed.
nessler’s reagent

Group I: Pb+2 ion:

Experiment Observation Inference


B) Indicatory Test
a) Salt + dist. Water + dil. White ppt. Pb+2 may be present.
HCl

C) Confirmatory test
Above soln. + dist. water + White crystalline Pb+2 Confirmed.
boil + cool + divide it
into two parts :
a) add 1ml potassium Bright yellow ppt. Pb+2 Confirmed.
chromate.
b) add 1ml KI Yellow ppt. Pb+2 Confirmed.

Group II: Pb+2,Cu+2,As+3ion:

Experiment Observation Inference


B) Indicatory Test
a) Above group I soln. + Black or yellow ppt Group II present
pass H2S. Black—may be Pb+2, Cu+2.
Yellow—may be As+3.
If Black ppt: add 50%
HNO3+heat. Black ppt dissolve and give
clear transparent soln.

6|Page
SALT ANALYSIS
If soln is colorless. Pb+2 present.
If soln. is blue Cu+2 present.

Test for Pb+2: divide the


soln. into three parts
C) Confirmatory test
a) add 1ml potassium Bright yellow ppt. Pb+2 Confirmed.
chromate.
b) add 1ml KI Yellow ppt. Pb+2 Confirmed.
c) add dil. H2SO4 White ppt. Pb+2 Confirmed.

Test for Cu+2:


C) Confirmatory test
Above blue soln. add Bluish white ppt. Cu+2 Confirmed.
NH4OH in excess
divide the soln in two
parts Chocolate brown ppt. Cu+2 Confirmed.
a) add acetic acid +
potassium Ferro cyanide White ppt. Cu+2 Confirmed.
b) add acetic acid +
potassium iodide.

Group III: Fe+3,Al+3ion:

Experiment Observation Inference


B) Indicatory Test Group III present
a) Above group II Reddish brown ppt. Fe+3 present.
soln.+boil to remove Gelatinous white ppt. Al+3 present.
H2S +cool+ solid NH4Cl
+ NH4OH soln.
+3
If Al is absent then above
soln. divide in 2 parts:
1. Add few drops of
conc.HNO3.(for Fe+2) Reddish brown ppt. Fe+2 Present.
2. Part for group IV if
Fe+2 is absent.

C) Confirmatory test:
If Red ppt: add dil. HCl to
dissolve and divide the soln.
in two parts.
a) add potassium ferrocyanide Purssian blue color. Fe+3 confirmed.
soln.
b) add potassium thiocyanide Blood red color. Fe+3 confirmed.

Experiment Observation Inference


If gelatinous ppt.

7|Page
SALT ANALYSIS
Dissolve in dil. HCl and
divide into 2 parts Blue lake floating in colorless Al+3 confirmed.
a) add blue litmus soln. + soln.
NH4OH soln. slowly
wait for some minutes. Again White gelatinous Al+3 confirmed.
b) add NH4OH in excess

Group IV: Co+2, Ni+2, Mn+2,Zn+2 ion:

Experiment Observation Inference


B) Indicatory Test
a) Above group III soln. + If Dirty white ppt. Zn+2 present.
pass H2S If buff colored ppt. Mn+2 present.
If Black ppt. May be Co+2, or Ni+2.
C) Confirmatory test:
If Dirty White ppt.: add dil.
HCl to dissolve and divide
the soln. in two parts.
a) add NaOH soln. White ppt. Zn+2 confirmed.
b) add potassium Bluish white ppt. Zn+2 confirmed.
ferrocyanide

If Buff colored ppt:


Dissolve in dil. HCl+ boil
to remove H2S + divide the
soln. into two parts White ppt turns to Mn+2 Confirmed.
a) add NH4OH wait for 2-3 black/brown ppt.
mins. Black brown ppt. Mn+2 Confirmed.
b) add Br2 water + NaOH
Group V: Ba+2, Sr+2, Ca+2 ion:

Experiment Observation Inference


B) Indicatory Test
a) Above group IV soln. + White ppt. May be Ba+2,Sr+2,Ca+2.
boil to remove H2S +
cool + solid NH4Cl +
NH4OH soln.+ saturated
soln. of Ammonium
carbonate.

8|Page
SALT ANALYSIS
C) Confirmatory test:
White ppt.: add excess
water(half T.T)+filter+ and
divide the Filterate in three
parts.
a) add acetic acid+ potassium Bright yellow ppt. Ba+2 confirmed.
chromate soln.
b) add acetic acid + White ppt. Sr+2 confirmed.
ammonium sulphate.
c) add acetic acid + White ppt. Ca+2 confirmed.
ammonium oxalate.
Group VI: Mg+2 ion:

Experiment Observation Inference


B) Indicatory Test
a) Salt + dist. Water + solid White crystalline ppt. Mg+2 confirmed.
NH4Cl+NH4OH
soln.+NaH2PO4
b) salt + dist. Water + dil. Blue ppt. Mg+2 confirmed.
HCl + few drops of
magneson reagent.+
NaOH
Systematic analysis of Salt:

Experiment Observation Inference


A) Preliminary Test
1. Physical test:
a. Colour
b. Odour
c. Deliquescence
2. Flame Test: Salt + Dark green May be Cu+2
make Brick red May be Ca+2
a paste on watch glass Grassy-green May be Ba+2
in conc. HCl + Pt Loop Deep-red May be Sr+2
+ Heat on flame
Test for Anions :
B) Indicatory Test:

Result: The given salt contain Anion:

Cation:

Salt :

Application of solubility product principle in qualitative analysis


9|Page
SALT ANALYSIS
The concepts of solubility product and common ion effect play an important role in
qualitative analysis for the separation of basic radicals (cations) into different groups.
Weak acids and weak bases ionise in water slightly and an equilibrium is established in
their solutions. For example, in the ionization of a weak base NH 4OH as:

The ionization constant for the base,

If solid NH4Cl is added to the solution, the concentration of NH4+ ions increases.
According to Le Chatelier's principle, the equilibrium shifts to the left. As a result, the
concentration of OH- is considerably decreased and the weak base NH4OH becomes
even weaker in the presence of its salt.

This is common ion effect and may be defined as the suppression of the degree of
dissociation of a weak acid or a weak base by the addition of a strong electrolyte
containing a common ion.
Qualitative analysis
The common ion effect is generally employed in qualitative analysis.
The cations of group II (Hg2+, Pb2+, Bi3+, Cu2+, As3+, Sb3+, Sn2+) are precipitated as their
sulphides (such as CuS, PbS) by passing H 2S gas in the presence hydrochloric acid
(Common H+ ions).
The cations of group III are precipitated as their hydroxides by NH4OH in the presence
of NH4Cl.
The cations of group V are precipitated as their carbonates by the addition (NH 4)2CO3,
in the presence of HCl.

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