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General Procedure - Salt Analysis

Chemistry

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0% found this document useful (0 votes)
9 views

General Procedure - Salt Analysis

Chemistry

Uploaded by

lol344466
Copyright
© © All Rights Reserved
Available Formats
Download as DOCX, PDF, TXT or read online on Scribd
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SALT ANALYSIS

GENERAL PROCEDURE

Aim:
To identify the anion and cation present in the given simple salt by performing
suitable tests.

Preliminary tests for anions and cations:

S.No Experiment Observation Inference


I
1. Colour: i) Blue or Bluish green. i) May be Cu2+
ii) Green. ii) May be Ni2+
iii) Pale green. iii) May be Fe2+
iv) Dark brown. iv) May be Fe3+
v) Pink. v) May be Co2+
vi) Pale pink. vi) May be Mn2+
vii) White. vii)May be Pb2+, Ca2+,
Al3+, Zn2+, Ba2+, Sr2+,
Mg2+, NH4+

2. Smell:
Take a pinch of salt between the i) Ammoniacal smell. i) May be NH4+
fingers and rub it with a drop of ii) Vinegar like smell. ii) May be CH3COO-
water.

3. Dry heating test:


Heat a pinch of salt in a dry test i) Salt decrepitates. i) May be Pb(NO3)2 or
tube and observe the change. Ba(NO3)2
ii) Colourless, odourless ii) May be CO32-
gas.
iii) Colourless, pungent iii) May be Cl-
smelling gas.
iv) Brown coloured gas. iv) May be Br- or NO3-
vi) Ammoniacal smell. vi) May be NH4+

4. Flame test:
To a pinch of salt in a watch i) Brick red flame. i) May be Ca2+
glass add few drops of conc. ii) Apple green red flame. ii) May be Ba2+
Hydrochloric acid and make a iii) Crimson red flame. iii) May be Sr2+
paste. Introduce this paste into iv)Blue flame surrounded iv) May be Cu2+
the flame. by a green colour.
5. Caustic soda test:
Take a pinch of salt in a dry test A colourless gas with May be NH4+
tube, add sodium hydroxide ammoniacal smell is
solution and heat gently. Dip a evolved which forms
glass rod in conc. Hydrochloric dense white fumes with
acid and introduce it into the test conc. Hydrochloric acid.
tube.

II Identification of anion
(Acidradical):

1. Dilute Hydrochloric acid test:


To the given salt add dilute Brisk effervescence due to May be CO32-
Hydrochloric acid. the evolution of a
colourless gas which turns
lime water milky.
2. Dilute Sulphuric acid test:
To the given salt add dilute Brisk effervescence due to May be CO32-
Sulphuric acid. the evolution of a
colourless gas which turns
lime water milky.
3. Conc. Sulphuric acid test:
To the given salt add i) Colour, pungent smelling i) May be Cl-
conc.Sulphuric acid. Heat if gas is evolved which gives
required. dense white fumes with a
glass rod dipped in
Ammonium hydroxide.
ii)Reddish brown gas which ii)May be Br-
turns starch paper yellow.
4. Potassium permanganate test:
To the salt add few drops of Pink colour of Potassium May be Cl-, Br- or I-
dil.Sulphuric acid, warm and permanganate gets
then add few drops of Potassium decolourised.
permanganate solution.

5. Manganese dioxide test:


To the salt add a pinch of i)Greenish yellow gas is i)May be Cl-
Manganese dioxide, conc. evolved.
Sulphuric acid and heat. ii)Reddish brown vapour is ii)May be Br-
evolved.
iii)Violetvapour is evolved. iii)May be I-

6. Copper turnings test:


To the salt add few Copper Brown gas is evolved and May be NO3-
turnings, conc. Sulphuric acid the solution turns blue or
and heat. green in colour.

7. Barium chloride test:


To the salt solution add Barium i)White precipitate (i)May beSO42-
chloride solution. insoluble in
dil.Hydrochloric acid.

ii)White precipitate soluble ii)May be CO32- or PO43-


indil.Hydrochloric acid.

III Confirmatory tests for anions:


-

1. Carbonate:
(i) Barium chloride test: i) White precipitate soluble i) Presence of CO32- is
To the salt solution add Barium in dil.Hydrochloric acid. confirmed.
chloride solution.

2. Chloride:
(i) Silver nitrate test:
To the salt solution add Silver White precipitate soluble Presence of Cl- is
nitrate solution. in Ammonium hydroxide confirmed.
is formed.

3. Bromide:
Silver nitrate test: Pale yellow precipitate Presence of Br- is
To the salt solution add Silver sparingly soluble in confirmed.
nitrate solution. Ammonium hydroxide is
formed.

4. Nitrate:
Brown ring test:
To the salt solution add equal A brown ring is formed at Presence of NO3- is
volume of freshly prepared the junction of two confirmed.
Ferrous sulphate solution. Add liquids.
few drops of conc.Sulphuric acid
along the sides of the test tube.

6. Sulphate:
Lead acetate test: White precipitate soluble Presence of SO42- is
To the salt solution add Lead in excess of Ammonium confirmed.
acetate solution. acetate is formed.

IV Cation analysis(Basic radical):


Preparation of Salt solution:
Dissolve the given salt in
distilled water and prepare the
salt solution.

1. Group analysis:
Group 1:
To the salt solution add dilute i) White precipitate soluble i)May be Pb2+
Hydrochloric acid. in hot water is formed.

2. Group 2:
To the salt solution add dilute i)Black precipitate. i)May be Cu2+
Hydrochloric acid and pass
Hydrogen sulphide gas.

3. Group 3:
To the salt solution add i)Gelatinous white i)May be Al3+
Ammonium chloride solution precipitate.
and Ammonium hydroxide ii)Reddish brown ii)May be Fe3+
solution. precipitate.

4. Group 4:
To the salt solution add i)Dirty white precipitate. i)May be Zn2+
Ammonium chloride solution, ii)Buff coloured precipitate. ii)May be Mn2+
Ammonium hydroxide solution iii)Black precipitate. iii)May be Ni2+ or Co2+
and pass Hydrogen sulphide gas.
.

5. Group 5:
To the salt solution add White precipitate is formed. May be Ba2+, Sr2+ or Ca2+
Ammonium chloride solution,
Ammonium hydroxide solution
and Ammonium carbonate
solution.

6. Group 6: May be Mg2+


To the salt solution add White precipitate is formed.
Ammonium chloride solution,
Ammonium hydroxide solution
and Ammonium phosphate
solution.

Since all the above cations are


abent, the given cation must be
Ammonium.(Zero group)

V Confirmatory tests for cations:

1. Lead:
(i) Potassium chromate test: i)Presence of Pb2+ is
To the salt solution add i)Yellow precipitate is confirmed.
Potassium chromate solution. formed.

(ii) Potassium iodide test: ii)Presence of Pb2+ is


To the salt solution add ii)Yellow precipitate is confirmed.
Potassium iodide solution. formed which dissolves in
hot water and on cooling
reappears as golden
spangles.

2. Copper:
(i) Potassium ferrocyanide
test: i)Presence of Cu2+ is
To the salt solution add i)Chocolate brown confirmed.
Potassium ferrocyanide solution. precipitate is formed.

(ii) Ammonium hydroxide test: ii)Presence of Cu2+ is


To the salt solution add ii)Blue precipitate is confirmed
Ammonium hydroxide solution. formed which dissolves in
excess of Ammonium
hydroxide to give a deep
blue precipitate.

3. Aluminium:
(i) Sodium hydroxide test: i)Presence of Al3+ is
To the salt solution add Sodium i)White precipitate soluble confirmed
hydroxide solution. in excess of Sodium
hydroxide solution is
formed.
(ii) Blue litmus test: ii)Presence of Al3+ is
To the salt solution add few ii)Blue lake is formed confirmed.
drops of blue litmus solution which floats on a clear
followed by few drops of solution.
Ammonium hydroxide solution.

4. Ferric: .
(i) Potassium ferrocyanide
test: i)Presence of Fe3+ is
To the salt solution add i)Deep blue colouration is confirmed.
Potassium ferrocyanide solution. obtained.

(ii) Potassium thiocyanide test: ii)Presence of Fe3+ is


To the salt solution add ii)Blood red colour is confirmed.
Potassium thiocyanide solution. obtained.

iii)Presence of Fe3+ is
(iii) Potassium permanganate iii)Pink colour of Potassium confirmed.
test: permanganate solution is
To the salt solution add not decolourised.
Potassium permanganate
solution.

5. Zinc:
(i) Sodium hydroxide test: i)Presence of Zn2+ is
To the salt solution add Sodium i)White precipitate is confirmed.
hydroxide solution. formed.

(ii) Potassium ferrocyanide


test: ii)Presence of Zn2+ is
To the salt solution add ii)White or bluish white confirmed.
Potassium ferrocyanide precipitate is formed.
solution.

6. Manganese:
Lead peroxide test. Presence of Mn2+ is
To the salt solution add Lead Pink coloured solution is confirmed.
peroxide and conc. Nitric acid. formed.
Boil, cool and dilute the
solution.

7. Nickel:
Dimethyl gyloxime
test(DMG): Presence of Ni2+ is
To the salt solution add DMG Rosy red precipitate is confirmed.
and few drops od Ammonium formed.
hydroxide solution.

8. Cobalt:
Potassium thiocyanide test: Presence of Co2+ is
To the salt solution add Blue colouration is confirmed.
Potassium thiocyanide solution. obtained.

9. Barium:
Potassium chromate test: Presence of Ba2+ is
To the salt solution add Pale yellow precipitate is confirmed.
Potassium chromate solution. formed.

10. Strontium:
Ammonium sulphate test: Presence of Sr2+ is
To the salt solution add White precipitate is formed. confirmed.
Ammonium sulphate solution
and warm.

11. Calcium:
Ammonium oxalate test: Presence of Ca2+ is
To the salt solution add White precipitate is formed. confirmed.
Ammonium sulphate solution
and few drops of Ammonium
hydroxide solution.
12. Magnesium:
Magneson regent test: Presence of Mg2+ is
To the salt solution add Blue precipitate is formed. confirmed.
Magneson reagent.

13. Ammonium:
(i) Nessler’s reagent test: i)Presence of NH4+ is
To the salt solution add ew drops i)Reddish brown precipitate confirmed.
of Nessler’s reagent followed by is formed.
drops of Sodium hydroxide
solution.
ii)Presence of NH4+ is
(ii) Sodium hydroxide test: ii)Colourless, pungent confirmed.
To the salt solution add few smelling gas which gives
drops of Sodium hydroxide dense white fumes with a
solution and heat. glass rod dipped in conc.
Hydrochloric acid is
evolved.
Result:
(i) The anion present in the given salt is ---------------------.
(ii) The cation present in the given salt is ---------------------.
(iii) The given salt is ---------------------.

CHEMISTRY INVOLVED IN INORGANIC QUALITATIVE ANALYSIS

ANION ANALYSIS:

Dil. H2SO4 Test:

CO32- + H2SO4  SO42- + H2O + CO2


(Brisk effervescence)
Ca(OH)2 + CO2  CaCO3 + H2O
(Lime water) (Milky appearance)

Conc. H2SO4 Test:

(a)Chloride:

NaCl + H2SO4 NaHSO4 + HCl


(Pungent smelling colourless gas)
HCl + NH4OH  NH4Cl
(Pungent (Dense white fumes)
smelling
Colourless gas)
(b)Bromide:

NaBr + H2SO4 NaHSO4 + HBr


H2SO4 + 2HBr  SO2 + Br2 + 2H2O
(Reddish brown vapour)
(c)Iodide:

NaI + H2SO4 NaHSO4 + HI


H2SO4 + 2HI  SO2 + I2 + 2H2O
(Violet vapours)

KMnO4 Test:
Decolourisation of pink colour of KMnO4
2KMnO4 + 3H2SO4 K2SO4 + 2MnSO4 + 3H2O + 5(O)

(a)Chloride:

NaCl + H2SO4 NaHSO4 +HCl


2HCl + (O)  H2O +Cl2
(b)Bromides:

NaBr + H2SO4 NaHSO4 + HBr


2HBr + (O)  H2O + Br2

(c)Iodides:

NaI + H2SO4  NaHSO4 + HI


2HI + (O)  H2O + I2

MnO2 Test:

(a) 2NaCl + MnO2 + 3H2SO4 2NaHSO4 + MnSO4 + 2H2O + Cl2


(Greenish Yellow gas)
(b) 2NaBr + MnO2 + 3H2SO4 2NaHSO4 + MnSO4 + 2H2O + Br2
(Reddish brown vapour)
(c) 2NaI + MnO2 + 3H2SO4  2NaHSO4 + MnSO4 + 2H2O + I2
( Violetvapour)

Copper turnings test:

NaNO3 + H2SO4  Na2SO4 + 2HNO3


4HNO3 + Cu  Cu(NO3)2 + 2H2O + 2NO2
(Solution (Reddish
turning blue) brown gas)

Barium chloride test:

Na2SO4 + BaCl2 BaSO4 + 2NaCl


(White ppt insoluble in dilHCl)

Confirmatory test for anions:

Carbonate:
Barium chloride test:

Na2CO3 + BaCl2 2 NaCl + BaCO3


(White ppt)
BaCO3 + 2HCl  BaCl2 + CO2 + H2O
(White ppt soluble in dilHCl)

Chloride:

Silver nitrate test:

NaCl + AgNO3 AgCl + NaNO3


(White ppt)
AgCl + NH4OH  [Ag(NH3)4}Cl + 4H2O
(Soluble complex)

Chromyl chloride test:

4NaCl + K2Cr2O7 + 3H2SO4 2Na2SO4 + K2SO4 + 2CrO2Cl2 + 3H2O


(Reddish orange vapours
of chromyl chloride)

CrO2Cl2 +NaOH Na2CrO4 + 2H2O + 2NaCl


(Yellow solution,
Sodium chromate)
Na2CrO4 + (CH3COO)2Pb  PbCrO4 + 2CH3COONa
(Yellow ppt
Lead chromate)

Bromide:

Silver nitrate test:

NaBr + AgNO3 AgBr+ NaNO3


(Pale yellow ppt
sparingly soluble in
ammonium.hydroxide)

Iodide:

Silver nitrate test:

NaI + AgNO3 AgI+ NaNO3


(Yellow ppt
insoluble in
ammonium.hydroxide)

Nitrate:

Brown ring test:

NaNO3 + H2SO4 NaHSO4 + HNO3


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

Sulphate:

Lead acetate test:

Na2SO4 +Pb(CH3COO)2 PbSO4 + 2CH3COONa


White ppt

Cation Analysis- Group analysis:

 Group 1

Pb(NO3)2 + 2HCl PbCl2 + 2HNO3


White ppt

 Group 2

CuCl2 + H2S CuS + 2HCl


Black ppt
 Group 3

AlCl3 + 3NH4OH Al(OH)3 + 3NH4Cl


Gelatinous
whiteppt

FeCl3 + 3NH4OH Fe(OH)3 + 3NH4Cl


Reddish
brownppt

 Group 4

Co(OH)2 + H2S CoS + 2H2O


Black ppt
Ni(OH)2 + H2S NiS + 2H2O
Black ppt

Zn(OH)2 + H2S ZnS + 2H2O


White ppt

Mn(OH)2 + H2S MnS + 2H2O

Buff ppt

Group 5

 BaCl2 + (NH4)2CO3 BaCO3 White ppt+ 2NH4Cl

White ppt
 SrCl2 + (NH4)2CO3 SrCO3 + 2NH4Cl

 CaCl2 + (NH4)2CO3 CaCO3 White ppt + 2NH4Cl

Group 6

 MgCl2 + NH4OH + (NH4)2HPO4 Mg(NH4)PO4 White ppt +2NH4Cl +


H2O

Confirmatory tests – Lead

 Potassium chromate test:


PbCl2+ 2K2CrO4 PbCrO4 Yellow+ppt
2KCl

 Potassium iodide test:


PbCl2+ 2KI PbI2 Yellow+ppt2KCl

Confirmatory tests – Copper

Potassium ferrocyanide test:


 CuSO4 + K4[Fe(CN)6] Cu2[Fe(CN)6] Chocolate + 2K2SO4
brownppt

Ammonium hydroxide test:


Blue
 CuSO4 + 4NH4OH [Cu(NH3)4]SO4 solution
+ 4H2O

[ NOTE: When NH4OH solution is added to Cu2+ ions, a pale blue ppt of Cu(OH)2 is
formed which dissolves in excess NH4OH to form a blue solution. ]
Confirmatory tests- Aluminium:
 Sodium hydroxide test:
Al3+ + NaOHAl(OH)3 + Na+
Al(OH)3 (white ppt)+ NaOH Na[ Al(OH)4] (soluble complex)

 Blue lake test:


AlCl3 + 3NH4OH 3NH4Cl + Al(OH)3 White ppt

[NOTE: White ppt of Al(OH)3 adsorbs the blue colour from litmus and being light
floats
on the solution.]
Confirmatory tests – Ferric:

 Potassium ferrocyanide test:


4FeCl3 + 3K4[Fe(CN)6] 12KCl + Fe4[Fe(CN)6]3
Ferric ferrocyanide (Prussian blue colouration)
 Potassium thiocyanide test:
FeCl3 + 3KCNS 3KCl + Fe(CNS)3
Ferric thiocyanide (Blood red colouration)

Confirmatory tests- Zinc

 Sodium hydroxide test:


ZnCl2 + 2NaOH Zn(OH)2White ppt+ 2NaCl
Zn(OH)2 + 2NaOH Na2ZnO2sodium zincate (soluble) +2H2O

 Potassium ferrocyanide test:


2ZnCl2 + K4[Fe(CN)6] Zn2[Fe(CN)6] white or bluish white ppt + 4KCl

Confirmatory test- Manganese

 Lead peroxide test:


2Mn(NO3)2 + 5PbO2 + 6HNO3 2HMnO 4(pink solution) + 5Pb(NO3)2
+2H2O

Confirmatory test- Nickel

 Dimethyl glyoxime test:

NiCl2 + 2NH4OH + 2 CH3 C NOH

CH33 C
CH NOH
Dimethyl glyoxime
OH O

CH3 CC N N C CH3
Ni + 2NH4Cl + 2H2O
CH3 C N N C CH3

O OH

Bright red complex


(ppt)

Confirmatory test - Cobalt

 Potassium thiocyanide test:

CoCl2 + 4 NH4CNS (NH4)[Co(CNS)4] + 2 NH4Cl


Ammonium cobalthiocyanate
(bluecolouration)

Confirmatory test – Barium

 Potassium chromate test:


BaCl2 + K2CrO4 BaCrO4Yellow ppt+ 2KCl

Confirmatory test – Strontium

 Ammonium sulphate test:


Sr(NO3)2 + (NH4)2CO3 SrCO3 white ppt+ 2NH4NO3
Confirmatory test – Calcium

 Ammonium oxalate test:


CaCl2 + (NH4)2C2O4 CaC2O4 white ppt+ 2NH4Cl

Confirmatory tests– Ammonium

 Sodium hydroxide test:


NH4Cl +NaOHNaCl + H2O + NH3 ( Pungent gas)
NH3 + HCl NH4Cl ( Dense white fumes)

 Nessler’s reagent test:


2K2[HgI4] + NH3 + 3KOH H2N.HgO.HgI Brown ppt +7KI + 2H2O

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