General Procedure For Salt Analysis

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GENERAL PROCEDURE FOR SALT ANALYSIS

PRELIMINARY TESTS

EXPERIMENT OBSERVATION INFERENCE


1.Colour of salts. 1. Blue Cu2+ copper salts.
2. Bluish green Ni2+ nickel salts
3. Pale green Fe2+ ferrous salts
4. Light pink Mn2+ manganese salts
5. Dark brown Fe3+ ferric salts.
6. White Absence of Cu2+, Ni2+, Fe2+,
Mn2+, Fe3+salts
2.Solubility in dilute HCl
To a little amount of salt add Insoluble Pb2+ present
dilute HCl. Soluble Pb2+ absent

3.Action with dilute H2SO4


To a little amount of the salt 1. Colourless and Presence of carbonate- CO32-
add a few drops of dilute odourles (gas CO2
H2SO4 and warm if necessary. with brisk efferences)
which turns lime
water milky.
2. Colourless, pungent Presence of sulphite - SO32-
smell, gas SO2 which
turns acidified
potassium dichromate
K2Cr2O7
3. Colourless gas H2S Presence of sulphide- S2-
with a rotten egg
smell which turns lead
acetate paper black.
4. Reddish brown gas Presence of nitrite- NO2-
NO2 with pungent
smell which turns
ferrous sulphate
paper black.
5. No reaction. Absence of CO32- ,SO32-, S 2-
and NO2-.

4.Ammonium molybdate
test:- Canary yellow ppt. Presence of phosphate-
PO43-
To a little amount of salt add
conc. HNO3 and boil and add
excess of ammonium
molybdate.
5.Barium chloride test:-
To a little amount of salt add White ppt, insoluble in conc. Presence of sulphate SO42-
dilute HCl and BaCl 2 to HCl.
solution.
6.Conc. Sulphuric acid test:-
To a little amount of the 1. Colourless pungent Presence of chloride- Cl-
given salt in the test tube smelling gas HCl which
add a few drops of conc. gives dense white
H2SO4 and heat. 2. fumes with a glass rod
dipped in NH4OH.
3. Colourless vapours Presence of CH3COO-
CH3COOH with
vinegar smell.
4. Reddish brown gas Presence of nitrate NO3-
NO2 which turns
FeSO4 paper black.
5. Reddish brown Br2 gas Presence of Br-.
which turns moist
starch paper yellow.
6. Violet paper turning Presence of I-.
starch paper blue [I2].
7. No reaction. Absence of Cl-, CH3COO-,
NO3-, Br-, I-.
7.Flame test:-
To a little amount of the salt 1. Bluish green coloured Presence of Cu2+ salts.
taken in a watch glass add a flame.
few drops of conc. HCl and 2. Brick red coloured Presence of Ca2+ salts.
make a paste. Introduce this flame.
paste into the flame with a 3. Crimson red coloured Presence of Sr2+ salts.
glass rod. flame.
4. Apple green coloured Presence of Ba2+ salts.
flame.
5. No characteristic Absence of Cu2+, Ca2+, Sr2+,
colour flame Ba2+ salts.
GROUP SEPARATION

The original solution is prepared with water

EXPERIMENT OBSERVATION INFERENCE


1.To a little amount of salt 1. White Presence of Pb2+ [group 1].
add dil.HCl precipitate(ppt). Absence of Pb2+
2. No white ppt.

2.To the above solution pass 1. Black ppt. Presence of Cu2+


H2S gas [yellow ammonium 2. Yellow ppt. Presence of Cd 2+[ group 1]
sulphide solution] 3. No characteristic Absence of Cu2+ and Cu2+
coloured ppt. [group 2]
3.Boil to expel H2S gas and 1. Gelatinous white ppt. Presence of Al3+
add NH4Cl + NH4OH 2. Dirty green ppt. Presence of Fe2+
solutions. 3. Reddish brown ppt. Presence of Fe3+
4. No characteristic Absence of Al3+, Fe2+, Fe3+ [
coloured ppt. group 3]
4.To the above solution pass 1. Dirty white ppt. Presence of Zn2+
H2S gas. 2. Black ppt. Presence of Ni2+
3. Buff coloured ppt. Presence of Mn2+
4. No characteristic Absence of Zn2+, Ni2+, Mn2+.
coloured ppt. [group 4]

5.Boil to expel H2S gas and 1. White ppt. May be Ca 2+or Ba2+or Sr2+
add NH4Cl ,NH4OH and 2. No white ppt. salts.
(NH4)2CO3 solutions. Absence of Ca2+,Ba2+
,Sr2+salts. [Group 5]
6.To the salt solution add 1. White ppt. Presence of Mg 2+
NH4Cl, NH4OH and Na2HPO4 2. No white ppt. Absence of Mg2+ [group 6].
solutions
7.To a part of the solution 1. Reddish brown ppt. Presence of NH4+
add Nessler’s reagent 2. No reddish ppt. Absence of NH4+
followed by sodium [group7/ZERO group].
hydroxide solutions.

CONFIRMATORY TEST FOR ACID RADICALS


1.SILVER NITRATE TEST:-

EXPERIMENT OBSRVATION INFERENCE


SS + dilute HNO3 and AgNO3 Curdy white ppt. completely Presence of Cl- confirmed.
solution. soluble in NH4OH.
Pale yellow ppt. sparingly Presence of Br- confirmed.
soluble in NH4OH.
Yellow ppt. insoluble in Presence of I- confirmed.
NH4OH.

2,MANGANESE DIOXIDE TEST:-

EXPERIMENT OBSREVATION INFERENCE


salt + MnO2 and Greenish yellow gas Presence of chloride
concentrated H2SO4 and heat. confirmed.
Reddish brown gas. Presence of bromide
confirmed.
Violet vapours. Presence of iodide
confirmed.

3.CONFIRMATORY TEST FOR NO3 - (NITRATE)

EXPERIMENT OBSEVATION INFERENCE


Brown ring test:-
SS +small quantity of freshly Brown ring is formed at the Presence of NO3- confirmed.
prepared FeSO4 solution + junction of the two liquids.
dilute H2SO4. Then add conc.
H2SO4 drop wise along the
sides of the test tube.

Copper turnings test:-


To a little amount of salt add Reddish brown gas. Presence of (nitrate) NO3-.
Cu turnings and concentrated
H2SO4 and heat.
CONFIRMATORY TEST FOR CH3COO-

EXPERIMENT OBSERVATION INFERENCE


FeCl3 test:-
SS+ neutral FeCl3 solution Reddish colouration changes Presence of CH3COO -
and heat to boil. to brown ppt. on boiling. confirmed.
Ester test:-
Treat a pinch of the given salt Fruity smell. Presence of CH3COO-
with conc. H2SO4 and add confirmed.
alcohol. Heat the mixture
and smell the vapours.

CONFIRMATORY TEST FOR SO42-

EXPERIMENT OBSERVATIO INFERENC


N E
lead acetate test:-
SS+ lead acetate solution. White ppt. Presence
soluble in of SO42-
excess of confirme
hot d.
ammonium
acetate
solution.
Barium chloride test:-
To a little amount of the salt White ppt. Presence
add dilute HCl and BaCl2 insoluble in of SO42-
solution. conc. HCL. confirme
d.

CONFIRMATORY TEST FOR S2-

EXPERIMENT OBSERVATION INFERENCE


Lead acetate test:-
SS + dil. CH3COOH+ lead black ppt. Presence of S2- confirmed.
acetate solution.

CONFIRMATORY TEST FOR NO2-

EXPERIMENT OBSERVATION INFERENCE

KMnO4 test:-
SS+ few drops of acidified Pink colour of KMnO4 is Presence of NO2- confirmed.
KMnO4 solution. discharged.
CONFIRMATORY TEST FOR SO32-

EXPERIMENT OBSERVATION INFERENCE


KMnO4 test:-
SS+ a few drops of acidified Pink colour of KMnO4 is Presence of SO32- confirmed.
KMnO4 solution. discharged.

CONFIRMATORY TEST FOR CO32-

Reaction with dilute HCl:-


To one portion of the Brisk effervescence with
solution add dilute HCl. evolution of CO2, which turns Presence of soluble
lime water milky. Co32- confirmed.

To a second solution add White ppt.


MgSO4 solution.
CONFIRMATORY TEST FOR BASIC RADICALS

Original solution (O.S.) is prepared in water.

EXPERIMENT OBSERVATION INFERENCE


1. For Cu2+
1. To a little of the O.S. Chocolate brown ppt. Presence of Cu2 confirmed.
add
K4[Fe(CN)6] solution.

2. For Cd2+
To a few drops of the O.S.add White ppt. Presence of Cd2+ confirmed.
K4[Fe(CN)6].
3. For Pb2+
1. To a few drops the Yellow ppt. Presence of Pb2+ confirmed.
O.S. add K2CrO4
solution.
2. To a few drops of the Bright yellow ppt. which Presence of Pb2+ confirmd.
O.S. add KI solution. dissolves in water on heating
and reappears as golden
yellow sprangles.

EXPEIMENT OBSERVATION INVERSTION


4. For Al3+
1. To a few of the O.S White precipitate soluble an Presence of Al3+confirmed.
add NaOH first in excess is of NaOH.
drops then in excess.
2. Ash test Blue tined ash.
To a small amount of Presence of ( magnesium)
the salt taken in a Mg2+
watch glass add cobalt
nitrate and
concentrated HNO3
and make into a
paste. Introduce a
filter paper dipped in
this paste into the
flame.
5. For Fe2+ FERROUS
To a few drops of the add Deep blue colouration. Presence of Fe2tconfirmed.
potassium ferricyanide .
K3[Fe(CN)6]solution.

6. For Fe3+ FERRIC


To a few drops of the O.S add Blood red colour. Presence of Fe3+ confirmed.
potassium thiocyanate -KCNS
solution.
7. For Zn2+
1. To a few drops of Bluish white ppt. Presence of Zn2+ confirmed.
the O.S. add
potassium
ferrocyanide
solution.
2. Ash test:-
To a small amount Bluish tinted ash. Presence of Zn2+ confirmed.
of the salt taken in
watch glass add
cobalt nitrate and
conc. HNO3 and
make a paste.
Introduce a filter
paper dipped in
this paste into the
flame.
2+
8. For Mn
To a few drops of O.S. add White ppt. turning brown. Presence of Mn2+ confirmed.
NaOH and Br2 water.
9. For Ni2
1. To a few drops of the Rosy red ppt. Presence of Ni2+ confirmed.
O.S. add a few drops
of dimethyl glyoxime
(DMG) and NH4OH.

10. For Ba2+:-


1. To a few drops of the Yellow ppt. Presence of Ba2+ confirmed.
O.S. add K2CrO4
solution.
2. Flame test:-
To a little amount of Apple green coloured flame.
the salt taken in the
watch glass add a few
drops of con. HCl and
make a paste.
Introduce this paste in
the flame using a glass
rod.
11. For Ca2+:-
1. To a few drops of the White ppt. Presence of Ca2+ confirmed.
O.S. add ammonium
oxalate solution.
2. Flame test:-
To a little amount of Brick red coloured flame.
the salt taken in the
watch glass add a few
drops of con. HCl and
make a paste.
Introduce this paste in
the flame with a glass
rod.
12. For Sr2+:-
1. To a few drops the White ppt. Presence of Sr2+ confirmed.
O.S. add ammonium
sulphate solution.
2. Flame test:-
To a little amount of Crimson red coloured flame.
the salt taken in watch
glass add con. HCl and
make a paste.
Introduce this paste in
the flame with glass
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