0% found this document useful (0 votes)
36 views15 pages

Salt Analysis

The document outlines methods for the physical and wet analysis of various salts, detailing tests for color, odor, state, density, deliquescence, dry heating, flame tests, and reactions with dilute and concentrated sulfuric acid. It includes specific observations and inferences for identifying ions such as NH4+, CO32-, SO42-, Cl-, Br-, I-, and others. Additionally, confirmatory tests for each ion are provided to ensure accurate identification of the salt components.

Uploaded by

dangwalakshiitb
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
0% found this document useful (0 votes)
36 views15 pages

Salt Analysis

The document outlines methods for the physical and wet analysis of various salts, detailing tests for color, odor, state, density, deliquescence, dry heating, flame tests, and reactions with dilute and concentrated sulfuric acid. It includes specific observations and inferences for identifying ions such as NH4+, CO32-, SO42-, Cl-, Br-, I-, and others. Additionally, confirmatory tests for each ion are provided to ensure accurate identification of the salt components.

Uploaded by

dangwalakshiitb
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
You are on page 1/ 15

Salt Analysis

I. Physical Examination of Salts


a. Colour of the Salt
Test Observation Inference

Blue Cu2+

Pale green Fe2+

Reddish brown Fe3+

Flesh colour Mn2+


Colour of the Salt

Bluish green Ni2+

Reddish pink Co2+/Co3+

Colourless Absence of Cu2+, Fe2+, Fe3+,


Mn2+, Ni2+, Co2+, Co3+ ions.

b. Odour of the Salt


A small amount of the salt is taken on the watch glass, a drop of water is
added, mixed using glass rod, and inhaled.
Test Observation Inference

Ammonia smell NH4+ ions may be present.


(To get strong smell of NH3,
add 2 drops of NaOH and
then rub.)

Rotten egg smell S2-


Odour of the Salt

Vinegar smell CH3COO-

Odourless Absence of NH4+, S2-,


CH3COO-

c. State
Test Observation Inference

State Crystalline solids Absence of MgCO3, CaCO3


Amorphous solids Presence of MgCO3, CaCO3

d. Density
Test Observation Inference

Heavier Presence of Pb2+, Ba2+, Hg2+,


Cd2+
Density
Lighter Absence of Pb2+, Ba2+, Hg2+,
Cd2+

e. Deliquescency
A pinch of salt is taken and is exposed to air in the watch glass for some time.
A paste of the salt appears if the salt is deliquescent.
Test Observation Inference

Paste of salt appears. ZnCl2, FeCl3, Ca(NO3)2,


Deliquescence is observed. MgCl2
Deliquescency
Not deliquescent. Absence of ZnCl2, FeCl3,
Ca(NO3)2, MgCl2

f. Dry Heating Test


Test Observation Inference

Salt decomposes with the May be CO32-


liberation of colourless and
odourless gas

Salt forms white sublimate May be NH4Cl

Brown white sublimate May be NH4Br

Violet sublimate May be NH4I


Dry Heating Test
Colourless suffocated smell May be SO32-
(burnt smell of sulphur)

Reddish brown fumes with May be NO3


pungent odour

Decripitation observed Pb(NO3)2, Ba(NO3)2, NaCl


(crackling sound)

Salt swells May be PO43-


Salt melts May be MgCl2, (NH4)2SO4

Salt melts with the May be (CH3COO)2Pb


appearance brownish black
at the bottom of the test tube

Loss of water of May be sulphate of Ag, Mg,


crystallisation Cr, Sr

g. Flame Test
One gram of salt is taken and 2-3 drops of conc. HCl are added and a paste is
prepared with the help of a glass rod. This paste is taken with the help of glass
rod and exposed to non-luminous flame of burner.
Test Observation Inference

Golden yellow Na+

Lilac flame K+

Grassy green Ba2+

Brick red Ca2+

Crimson red Sr2+


Flame Test

Dull bluish white Pb2+

Parrot green Cu2+

Green flashes Zn2+

No characteristic coloured Absence of Na+, K+, Ba2+,


flame Ca2+, Sr2+, Pb2+, Cu2+, Zn2+.

II. Wet Tests: Analysis of Acid Radicals Group I Dilute H2SO4 Test
Test Observation Inference

Colourless gas with brisk CO32- may be present.


One gram of salt is taken in effervescence.
a test tube and one drop of Colourless gas with burnt SO32- may be present.
dil. H2SO4 is added. smell of sulphur/suffocating
gas.
Colourless gas with rotten S2- may be present.
egg smell.

Brown gas with pungent NO32- may be present.


odour.

NOTE: If no changes are observed on treatment of the salt with dil. H2SO4, then we need to
carry out the reaction with conc. H2SO4. If no reaction occurs in cold condition, the test tube
is heated. If salt contains Cl-, Br- and I-, they respond to cold conc. H2SO4. If NO3- and
CH3COO- are present, they respond to hot conc. H2SO4 only.

Test Observation Inference

1 g of salt is taken in a test Colourless gas with a strong May be Cl-.


tube and one drop of conc. pungent odour. HCl gas is
H2SO4 is added. released.

Glass rod dipped in NH4OH Dense white fumes are seen.


are exposed to these
vapours.

Cl-. + H2SO4 → HCl + H2SO4


HCl + NH3 → NH4Cl

Pass the brown fumes / Brown fumes with pungent May be Br- or NO3-.
vapours obtained through a odour are observed.
test tube containing FeSO4
solution. FeSO4 does not turn brown May be Br-.
black.

Br- + H2SO4 → HBr + HSO4-

FeSO4 turns brown black. May be NO3-.

NO3- + H2SO4 → HNO3 + HSO4-

If no reaction occurs in cold Violet fumes are instantly May be I-.


conc. H2SO4 then the test evolved.
tube is heated.
I- + H2SO4 → HI + HSO4-

Colourless gas with vinegar May be CH3COO-.


odour is evolved.

CH3COO- + H2SO4 → CH3COOH + HSO4-


Salt decomposes with the May be C2O42-.
formation of CO2 and CO
gas.

C2O42- + H2SO4 → 4CO2 + 2SO2 + H2O

If any of the above changes are observed, confirmatory tests are performed. If no changes are
observed, then tests for SO42- and PO43- are carried out.

Test for SO42- (BaCl2 Test)


1 ml of salt solution is taken A white ppt is formed which May be SO42-.
and 1 ml of BaCl2 solution is is insoluble in excess of dil.
added to this. HCl.

SO42- + BaCl2 → BaSO4 + 2Cl-

Test for PO42-


1 ml of conc. HNO3 is added Yellow ppt is formed. May be PO43-.
to the salt in a test tube. The
contents are boiled and
excess of ammonium
molybdate solution is added.

Confirmatory Tests:
1. CO32- (Lime Water Test)
To 1 g of salt in a test tube, Lime water turns milky. CO32- is confirmed.
dil HCl is added and CO2
gas liberated is passed
through lime water taken in
another test tube.

CO2 + Ca(OH)2 → CaCO3 + H2O

2. Sulphide Ion (S2- )


(a) Lead Acetate Test
To the aqueous solution of Black ppt is obtained. S2- is confirmed.
given salt, 1 ml of lead
acetate is added.

S2- + (CH3COO)2Pb → PbS ↓ + 2CH3COO-

(b) Sodium Nitroprusside test


To the aqueous solution of Violet colouration is seen. S2- is confirmed.
given salt, few drops of
sodium nitroprusside are
added.

S2- +[Fe(CN)5NO]2- → [Fe(CN)5NOS]4-

3. Sulphite Ion (SO32- )


To the aqueous solution of Green colouration is seen. SO32- is confirmed.
given salt, few drops of
potassium dichromate and
dil. H2SO4 are added.

6SO3 + 2Cr2O7-. + 4H+ → 4Cr3+ + 6SO43- + 2H2O

4. Nitrite Ion (NO22- )


To the aqueous solution of Solution turns dark brown or NO2- is confirmed.
given salt, few drops of black.
CH3COOH + FeSO4 is
added.

6SO2 + 2Cr2O7- + 4H+ → 4Cr3+ + 6SO42- + 2H2O

5. Chloride Ion (Cl- )


(a) Silver Nitrate Test
To the aqueous solution of A curdy white ppt is Cl- is confirmed.
given salt 1 ml of silver obtained which is soluble in
nitrate is added. excess NH4OH.

AgNO3 + Cl- → AgCl + NO3-

(b) Chromylchloride Test


1 g of salt + 1 g of K2Cr2O7 Yellow orange vapours are Cl- is confirmed.
and then 1 ml of conc. formed.
H2SO4 is added.

4Cl- + K2Cr2O7 + 3H2SO4 → 2CrO2Cl2 + 2K+ + 3H2O + 3SO42-

Yellow orange vapour is A yellow solution is formed.


passed through NaOH
solution.
CrO2Cl2 + 2NaOH → Na2CrO4 + 2NaCl + H2O

1 ml of dil. CH3COOH is Yellow ppt is formed.


added to the yellow solution
+ 1 ml of lead acetate.

Na2CrO4 + (CH3COO)2Pb → PbCrO4 + CH3COONa

6. Bromide Ion (Br- )


(a) Silver Nitrate Test
1 ml of salt solution + 1 ml Pale yellow ppt which is Br- is confirmed.
of AgNO3 solution partially soluble in excess of
NH4OH.

AgNO3 + Br- → AgBr + NO3-


AgBr + 2NH3 → [Ag(NH3)2]Br

(b) Chlorine Water Test (Orange Globule)


1ml of salt solution + 2 An orange globule is Br- is confirmed.
drops of CCl4 or CS2 + conc. formed.
solution of Cl2 water.
Shake well.

2Br- + Cl2 → Br2 + 2Cl-

7. Iodide Ion (I- )


(a) Silver Nitrate Test
1 ml of salt solution + 1 ml Curdy white or pale yellow I- is confirmed.
of AgNO3 soluton ppt is formed which is
insoluble in excess of
NH4OH.

I- + AgNO3 → AgI + NO3-

(b) Globule Test


1 ml of salt solution + 2ml A violet globule is formed. I- is confirmed.
of CCl4 or CS2 + conc.
solution of Cl2 water.
Shake well.

2I- + Cl2 → I2 + 2Cl-


8. Nitrate Ion (NO3- )
(a) Copper Chips Test
1 ml of salt solution + conc Brown fumes are evolved. NO3- is confirmed.
H2SO4 + heat strongly.

2NO3- + H2SO4 → 2HNO3 + SO42-

Few pieces of copper chips Intense brown fumes are


are added to the above test absorbed.
tube, only under hot
conditions.

4HNO3 + Cu → Cu(NO3)2 + 2NO2 + 2H2O

(b) Brown Ring Test


Add a small quantity of A dark brown ring is NO3- is confirmed.
freshly prepared solution of obtained at the junction of 2
FeSO4 + aqueous solution of layers.
salt + conc. H2SO4 slowly on
the sides.

NO3- + H2SO4 → HNO3 + HSO4-


6FeSO4 + 3H2SO4 + 2HNO3 → 3Fe2(SO4)3 + 4H2O + 2NO
FeSO4 + NO + 5H2O → [Fe(NO)(H2O)5]SO4

9. Carbonate Ion (CH3COO- )


(a) Ester Test
Small quantity of salt + 2 ml Pleasant fruity smell of CH3COO- is confirmed.
of conc. H2SO4 and heat. ester.
Now add 1 ml of ethanol and
shake in a test tube. Pour the
contents of the test tube in a
beaker full of water. Stir.

CH3COOH + C2H5OH → CH3COOC2H5 + H2O

(b) Oxalic Acid Test


1 g of salt is taken in a water Vinegar odour is obtained. CH3COO- is confirmed.
glass and some amount of
oxalic acid is mixed with it
and a mixture is rubbed with
a drop of water.

CH3COO- + (COOH)2 → 2CH3COOH + (COO)2-


10. Oxalate Ion (C2O42- )
(a) CaCl2- Test
1 ml of dil. CH3COOH is A white ppt is formed. C2O42- is confirmed.
added to 1 ml of salt solution
and heated to remove CO2.
Then add 1 ml of CaCl2
solution.

Add 1 ml of dil. HNO3 to the Ppt dissolves.


above ppt and warm.

C2O42- + CaCl2 → CaC2O4 + 2Cl-

(b) Potassium Permanganate Test


4-5 drops of dil. H2SO4 are Pink colour of KMnO4 C2O42- is confirmed.
added to 1 ml of salt solution dissolves and liberation of
and warmed to 60-70°C, CO2 gas takes place.
then 2-3 drops of dil.
KMnO4 are added.

5CH3COO- + 2MnO4- + 16H+ → 2Mn2+ + 10CO2 + 8H2O

11. Sulphate Ion (SO42- )


(a) Lead Acetate Test
1 ml of salt solution is added A white ppt is formed. SO42- is confirmed.
to 1 ml of lead acetate.

SO42- + (CH3COO)2Pb → PbSO4 + 2CH3COO-

Hot ammonium acetate is White ppt dissolves.


added to the above ppt.

PbSO4 + 2CH3COONH4 → (CH3COO)2Pb + (NH4)2SO4


SALTS IN THE SYLLABUS

NH4+, Pb2+, Cu2+, Al3+, Fe3+, Zn2+, Co3+, Ni2+, Mn2+, Ba2+, Sr2+, Ca2+, Mg2+

PROCEDURE

Analysis of ‘0’ Group Radicals (NH4+)


Test Observation Inference

1g of salt is added to 1ml of Ammoniacal/pungent smell Presence of NH4+.


NaOH in a test tube and gas is evolved.
heated on a flame.

NH4+ + NaOH → NH3 + Na+ + H2O

Confirmatory Test
(a) Conc. HCl Test
The glass rod is dipped in Dense white fumes are NH4+ is confirmed.
conc. HCl and exposed to evolved.
the above vapour evolved.

NH3 + HCl → NH4Cl

(b) Nessler’s Reagent Test


To 1 ml of aqueous solution A brown precipitate is NH4+ is confirmed.
of salt 1-2 drops of KOH is formed.
added and then Nessler’s
reagent is added.

NH3 + 2K2[HgI4] + 3KOH → NH2.HgO.HgI + 7KI + 2H2O


Note: Before going to analyse the basic radical the saturated/concentrated solution is
prepared by the following solvents. The resulting solution is said to be original solution
(O.S.).

Original Solution (O.S.)


Cold water: if not soluble → hot water: if not soluble → dil. HCl: if not soluble → conc.
HCl: if not soluble → dil. HNO3: if not soluble → conc. HNO3: if not soluble → aqua regia

Analysis of Ist Group Basic Radicals


Test Observation Inference

To 1 ml of original solution A white precipitate is May be Pb2+ or Ag+.


dil. HCl is added in a test formed.
tube.

Pb2+ + 2HCl → PbCl2 ↓ + 2H+

Confirmatory Test for Pb2+


The precipitate formed in the above step is dissolved in hot water and divided into 2 parts.
(a) Potassium Dichromate Test
Part I + K2CrO4 (1 ml) Yellow precipitate is Pb2+ is confirmed.
solution in a test tube. formed.

PbCl2 + K2CrO4 → PbCrO4 ↓ + 2KCl

(b) Potassium Iodide Test


Part II + KI (1 ml) solution Yellow precipitate is Pb2+ is confirmed.
in a test tube. formed.

PbCl2 + 2KI → PbI2 ↓ + 2KCl

Analysis of IInd Group Basic Radicals


Test Observation Inference

1 ml of O.S. + 1 ml of dil. Black precipitate is formed. Pb2+ or Cu2+ is formed.


HCl + 1 ml of H2S in a test
tube.

Pb2+ + H2S → PbS + 2H+


Cu2+ + H2S → CuS + 2H+

The black precipitate is dissolved in minimum quantity of 50% of HNO3 acid. The resultant
of solution has 2 parts.
Part I + 1 ml of dil. H2SO4 + 1 ml of ethanol
----------------------- White ppt -- Pb2+ is indicated.
Dissolve the ppt in hot ammonium acetate solution and divide solution in two parts. Perform
potassium iodide and potassium chromate test as confirmatory test for lead ion same as that
of first group basic radical analysis.
----------------------- If there is no white precipitate then NH4OH is added in excess to IInd part
so that blue coloured solution is obtained. Divide it into 2 parts.
Presence of Cu is indicated.

Confirmatory Test for Cu2+


(a) Potassium Ferrocyanide Test
To Ist part of above solution A chocolate brown ppt is Cu2+ is confirmed.
potassium ferrocyanide is formed.
added in a test tube.

2Cu2+ + K4[Fe(CN)6] → Cu2[Fe(CN)6] + 4K+

(b) Potassium Iodide Test


To another part of the blue A white colouration in Cu2+ is confirmed.
solution, ½ ml of dil. brown ppt is formed.
CH3COOH and 1 ml of KI is
added.

2Cu2+ + 4KI → Cu2I2 + I2 + 4K+

Analysis for the IIIrd Group Basic Radical


Test Observation Inference

Excess of solid ammonium Reddish brown ppt is Fe3+ may be present.


chloride and excess of formed.
NH4OH is added to 1 ml of
O.S.

Fe3+ + 3NH4OH → Fe(OH)3 + 3NH4+

The ppt obtained in the Gelatinous white precipitate Al3+ may be present.
above step is dissolved in is formed.
dil. HCl and the solution is
divided into 2 parts.

Al3+ + 3NH4OH → Al(OH)3 + 3NH4+


Confirmatory Test for Al3+
Blue Lake Test
The above obtained solution First appears red colour Al3+ is formed.
is mixed with 1-2 drops of followed by blue
blue litmus and 1 ml of colouration.
NH4OH.

NH4OH (little in excess) Blue ppt in solution. Al3+ is confirmed.

Al(OH)3 + 3HCl → AlCl3 + 3H2O → Red soln


AlCl3 + 3NH4OH → Al(OH)3 + 3NH4Cl

Analysis for the IVth Group Basic Radical


Test Observation Inference

To 1 ml of O.S. NH4Cl, Black ppt. Co2+, Ni2+ present.


NH4OH and H2S are added.
Co(OH)2 + H2S → CoS + 2H2O
Ni(OH)2 + H2S → NiS + 2H2O

Buff or flesh ppt. Mn2+ present.

Mn(OH)2 + H2S → MnS + 2H2O

Dull white ppt. Zn2+ present.

Zn(OH)2 + H2S → ZnS + 2H2O

Confirmatory Tests for Zn2+ and Mn2+ (NaOH Test)


The white ppt is dissolved in small amount of dil HCl and H2S is boiled. Mn2+ and Zn2+ are
confirmed.

M.S. + 2HCl → MCl2 + H2S (where M = Zn, Mn, Co, Ni)

Confirmatory Tests for Mn2+


(a) NaOH Test
To one part of the solution A white ppt is formed. Mn2+ is confirmed.
NaOH is added and shaken
well.

MnCl2 + 2NaOH → Mn(OH)2 + 2NaCl


(b) Bromine Water Test
To 1 ml of above formed ppt Black and brown ppt. Mn2+ is confirmed.
bromine water is added.

Br2 + H2O → 2HBr + [O]


Mn(OH)2 + [O] → MnO(OH)2

Confirmatory Tests for Zn2+


(a) NaOH Test
To 1 ml of the dissolved ppt A white ppt is formed. Zn2+ is confirmed.
solution small amount of
NaOH is added.

Excess of NaOH is added to White ppt is dissolved.


same ppt.

ZnCl2 + 2NaOH → Zn(OH)2 + 2NaCl


Zn(OH)2 + 2NaOH → Na2ZnO2 + 2H2O

(b) Potassium Ferrocyanide Test


To the other part of the White or persian blue ppt is Zn2+ is formed.
dissolved ppt solution add 1 formed.
ml of K4[Fe(CN)6] and
shake well.

ZnCl2 + K4[Fe(CN)6] → Zn2[Fe(CN)6] + 4KCl

Analysis for the Vth Group Basic Radicals


Test Observation Inference

In this group while analysing the following order should be strictly followed: Ba2+, Sr2+,
Ca2+.

1 ml of O.S. + NH4Cl + White ppt is formed. Ba2+, Sr2+, Ca2+ is present.


NH4OH + (NH4)2CO3 are
added.

M2+ + (NH4)2CO3 → MCO3 + 2NH4+ (where M = Ba2+, Sr2+, Ca2+)

The white ppt is dissolved in small amount of CH3COOH and the solution is divided into
three parts.
Confirmatory Test for Ba2+: K2CrO4 Test
Part 1 + 1 ml of K2CrO4 Yellow ppt is formed. Ba2+ is formed.

Ba2+ + K2CrO4 → BaCrO4 + 2NH4+

Confirmatory Test for Sr2+: (NH4)2SO4 Test


Part 2 + 1 ml of (NH4)2SO4 White ppt is formed. Sr2+ is confirmed.

Sr2+ + (NH4)2SO4 → SrSO4 + 2NH4+

Confirmatory Test for Ca2+: (NH4)2C2O4 Test


Part 3 + 1 ml of (NH4)2C2O4 White ppt is formed. Ca2+ is confirmed.

Ca2+ + (NH4)2C2O4 → CaC2O4 + 2NH4+

Analysis for the VIth Group Radicals


Test Observation Inference

1 ml of O.S. + NH4Cl + White ppt is formed on Mg2+ is present or


NH4OH + (NH4)2PO4 are scratching the sides of the confirmed.
added. test tube with a glass rod.

3Mg2+ + 2(NH4)3PO4 → Mg(PO4)2 + 6NH4+

You might also like