GENERAL PROCEDURE FOR SALT ANALYSIS- final

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GENERAL PROCEDURE FOR SALT ANALYSIS

S. EXPERIMENT OBSERVATION INFERENCE


No
I. PRELIMINARY TESTS
1. PHYSICAL STATE:
a) Colour of the substance Colourless Absence of Cu2+ , Fe2+
ions
b) Appearance Crystalline Absence of CO32- or S2-
ions.
2. SOLUBILITY Soluble Absence of CO32- or S2-
A little of the salt is shaken ions.
with water
3. ACTION OF HEAT: 1) Decripitation occurs with the 1) May be Pb(NO3)2
A small amount of the salt is evolution of reddish brown gas. salt.
heated gently in a dry test tube. 2) Evolution of reddish brown gas -
2) May be NO3 ions.
3) Salt sublimes with the evolution 3) May be NH4+ salt
of pungent smelling gas, giving
dense white fumes with a glass rod
dipped in conc. HCl.
4) The salt turns yellow on hot, 4) May be Zn2+ salt.
white when cold.

5) The salt turns dark brown when 5) May be Pb2+ salt


hot, and yellow when cold.
6) The salt turns to colourless 6) May be CuSO4 salt.
7) No characteristic change. 7) Absence of CO32- ,
NO3-, NH4+, Pb2+ and
Zn2+ ions.
4. FLAME TEST: 1) Brick red flame. 1) Presence of Ca2+ ion.
A small amount of the salt
is made into a paste with conc. 2) Crimson red flame 2) Presence of Sr2+ ion.
HCl in a watch glass and 3) Grassy green flame. 3) Presence of Ba2+ ion.
introduced into the non-
luminous part of the Bunsen 4) Bluish green flame 4) Presence of Cu2+ ion
flame.
5) No characteristic coloured flame. 5) Absence of Ca2+,
Sr2+ , Cu2+ and Ba2+
ions.

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5. ASH TEST: 1) Green coloured ash. 1) Presence of Zn2+ ion.
A filter paper is soaked into a (ZnO.CoO-Cobalt zincate)
paste of the salt with conc.
2) Blue coloured ash. (Co(AlO2)2) 2) Presence of Al3+ ion.
HNO3 and Co(NO3)2 solution
in a watch glass and burnt. 3) Pink coloured ash. (MgO.CoO) 3) Presence of Mg2+ ion.
4) No characteristic coloured ash. 4) Absence of Zn2+,
Al3+ and Mg2+ ions.
II. IDENTIFICATION TESTS FOR ACID RADICALS
EXPERIMENT OBSERVATION INFERENCE
6. ACTION OF Conc.H2SO4 1) Colourless gas with brisk 1) Presence of C2O42-
To a small amount of the salt 2 effervescence evolved. ion.
to 3 ml of Conc. H2SO4 is 2) No characteristic change. 2) Absence of C2O42-
added. ion.
7. ACTION OF Conc.H2SO4 1) Colourless pungent smelling gas -
1) Presence of Cl ion.
To a small amount of the salt 2 evolved.
to 3 ml of Conc. H2SO4 is 2) No characteristic change. -
2) Absence of Cl ion.
added, then heat the contents for
2min.
8. ACTION OF NaOH: 1) Pungent smelling gas forming 1) Presence of NH4+
A small amount of the salt is dense white fumes with a glass rod ion.
dipped in conc. HCl and also turns
heated with 2 to 3 ml of NaOH. red litmus paper blue.
2) No characteristic change 2) Absence of NH4+
ion.
9. COPPER TURNINGS TEST: 1) Reddish brown gas is evolved. -
1) Presence of NO3
A small amount of the salt is ion.
heated with Copper
2) No characteristic change 2) Absence of NO3-
Turnings and a few drops of
ion.
conc.H2SO4.
10. LEAD ACETATE TEST 1) A white precipitate is obtained 1) Presence of SO42- ion.
To a small amount of salt 2 ) No characteristic change 2-
2) Absence of SO4 ion.
solution, 2 ml of lead acetate
solution is added.
11. ESTER TEST 1) Pleasant fruity smelling ester is -
1) Presence of CH3COO
formed.
To a small amount of the salt is ion.
heated with few drops of
Conc.H2SO4 and C2H5OH. 2) No Characteristic change 2) Absence of
-
CH3COO ion.

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III. CONFIRMATORY TEST FOR ACIDIC RADICALS
i) BARIUM CHLORIDE TEST: 1) A white precipitate, insoluble in 1) Presence of SO42-
To a few drops of the original conc. HCl. ion is confirmed.
2+ 2-
solution, add 2 ml of BaCl2 Ba (aq) + SO 4 (aq) BaSO 4 (s)(white)

solution. 2. No Characteristic change. 2) Absence of SO42-


ion.
ii) CHROMYL CHLORIDE 1) Red orange vapours evolved are -
1) Presence of Cl ion
TEST: passed through NaOH to get a yellow
solution, which on adding Lead is confirmed.
To a small amount of the acetate forms a- yellow precipitate.
salt a pinch of K2Cr2O7 is K2Cr2O7+ 4Cl + 3H2SO4
added and heated with few K2SO4+2SO42-+2CrO2Cl2+3H2O
drops of Conc.H2SO4 (chromyl chloride-yellow vapours)

CrO2Cl2+NaOH Na2CrO4 + 2H2O


+ 2NaCl
Na2CrO4+ (CH3COO)2Pb PbCrO4 +
2CH3COONa
2) No Characteristic change -
2) Absence of Cl ion.
iii) BROWN RING TEST: 1) Brown ring is formed at the 1) Presence of NO3-
To a few drops of original junction of the two layers. ion is confirmed.
solution add freshly prepared NO3- + 3Fe2+ + 4H+ → 3Fe3+ +
FeSO4 solution and then add NO + 2H2O
conc. H2SO4 drop by drop along
the sides of the test tube. [Fe(H2O)6]2+ + NO →
[Fe(H2O)5(NO)]2+
2) No Characteristic change 2) Absence of NO3- ion.
iv) Test With KMnO4 1) Colourless, odourless gas evolved 1) Presence of C2O42-
To a few drops of original with brisk effervescence, also Colour ion
solution add dilute KMnO4 is of KMnO4 becomes colourless
added and then conc. H2SO4 is 5(C2O4)2- + 16H++2 MnO4-→
added drop by drop along the 10CO2 + 8 H2O + 2Mn2+
sides of the test tube colourless)

2) No Characteristic change 2) Absence of C2O42-


ion
v) Test with Neutral FeCl3: 1) Reddish brown coloured 1) Presence of
To a few drops of original precipitate. CH3COO- ion
solution add neutral FeCl3 , 3 CH3COO- + FeCl3
then heat the solution for 2 →(CH3COO)3Fe + 3Cl-
min.
(CH3COO)3Fe + H2O→ (CH3COO)
(OH) Fe + 2 CH3COOH
2) No Characteristic change 1) Absence of CH3COO-
ion

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IV. IDENTIFICATION OF THE BASIC RADICALS
PREPARATION OF ORIGINAL SOLUTION:
The original solution is prepared by dissolving the salt in water.
GROUP IDENTIFICATION
1. ZERO GROUP 1) Pungent smelling gas forming 1) Presence of zero
A small amount of the salt is dense white fumes with a glass rod group cation
heated with 2ml of NaOH. dipped in conc. HCl and also turns
red Litmus paper blue.
NH4+ (aq) + OH- (aq)  NH3(g) + H2O(I)
2) No Characteristic change. 2) Absence of zero
group cation.
2. 1ST GROUP: 1) White precipitate is formed. 1) Presence of First
To a few drops of the original Pb2+(aq) + HCl(aq)  PbCl2(white) Group cation. (Pb2+)
solution 2 ml of dilute HCl is 2) No characteristic change. 2) Absence of First
added. Group cation (Pb2+)
3. 2ND GROUP: 1) Black precipitate is formed. 1) Presence of Second
To a few drops of the original Cu2++Na2S CuS (Black Precipitate) + Group cation ( Cu2+).
solution 2 ml of dil.HCl is 2Na+
added and followed by 2ml of
2) No characteristic change.. 2) Absence of Second
Na2S solution.
Group (Cu2+).
4. 3RD GROUP: 1) Gelatinous white precipitate is 1) Presence of Third
To a few drops of the original formed. Group cation (Al3+).
solution 1 ml NH4Cl and 2 ml Al3+ + 3NH4OHAl(OH)3 + 3NH4+
NH4OH solutions are added. (Gelatinous white precipitate)

2) No characteristic change. 2) Absence of Third


Group cation (Al3+).
5. 4TH GROUP: 1) Dirty white precipitate is formed . 1) Presence of Fourth
To a few drops of the original Zn 2+ + H2S(aq)  ZnS(s)(White) + 2H+ Group cation (Zn2+).
solution 1 ml NH4Cl and 2 ml 2) No characteristic change. 2) Absence of Fourth
NH4OH solutions are added
Group cation (Zn2+).
followed by 2ml of Na2S
solution.
6. 5TH GROUP: 1) White precipitate is formed. 1) Presence of Fifth
To a few drops of the original Group cations (Ca2+,
solution 1 ml Sr2+or Ba2+).
NH4Cl, 2 ml NH4OH and 2ml 2) No Characteristic change. 2) Absence of Fifth
(NH4)2CO3 solutions are added. Group cations (Ca2+,
Sr2+or Ba2+).

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7. 6TH GROUP: 1) White precipitate is formed. 1) Presence of Sixth
To a few drops of the original Group cation (Mg2+)
solution 1 ml NH4Cl, 2 ml 2) No Characteristic change 2) Absence of Sixth
NH4OH and 2 ml Di Sodium Group (Mg2+).
Hydrogen Phosphate are added.
V. CONFIRMATORY TESTS FOR BASIC RADICALS
1. ZERO GROUP - Reddish brown precipitate is formed. Presence of NH4+
ion is confirmed
AMMONIUM 1. NH4+ + NaOH  NH4OH + Na+

To a few drops of the 2. NH4OH  NH3 + H2O


original solution 2ml of NaOH 3. NH3 + 2K2HgI4 + 3KOH 
and Nessler’s reagent (K2HgI4) H2N.HgO.HgI (Reddish brown precipitate)
are added. + 2KI + 2H2O
2. FIRST GROUP- LEAD 1) Yellow precipitate is formed. 1) Presence of Pb2+ is
i) To a few drops of the confirmed.
Pb2+ +K2CrO4  PbCrO4 ( Yellow
original solution K2CrO4 is
precipitate) + 2KOH
added.
ii) To a few drops of the 2) Yellow precipitate soluble in hot 2) Presence of Pb2+ is
original solution KI is added. water which reappears as golden
confirmed
yellow spangles on cooling.
Pb2+(aq)+ 2I-(aq) PbI2(S) (Yellow)
3. SECOND GROUP- Blue precipitate is formed.
COPPER
Cu(OH)2(s) + NH3(aq) 
To a few drops of the [Cu(NH3)4] aq)(blue) +2OH-(aq)
2+ Presence of Cu2+ is
original solution NH4OH is A chocolate brown precipitate is confirmed
added. Followed by potassium obtained
ferrocyanide solution is
added.
4. THIRD GROUP - A bright Blue lake is formed Presence of Al3+ is
ALUMINIUM
Al3+ (aq) +3OH- confirmed.
i) To a few drops of the
original solution NH4OH (aq) Al(OH)3(s)(white) (adsorb blue colour)
and Blue litmus solution
are added.
5. FOURTH GROUP- ZINC Bluish white precipitate is formed Presence of Zn2+ is
i) To a few drops of the which is soluble in excess of Sodium confirmed.
original solution hydroxide & insoluble in dilute acid.
K4[Fe(CN)6] is added.. 2Zn2++K4[Fe(CN)6]Zn2[Fe(CN)6]
+
(Bluish White) + 4K

6. FIFTH GROUP White precipitate is formed which is Presence of Ca2+ is


i) CALCIUM: To a few drops insoluble in Acetic acid. confirmed.
of the original solution NH4 Ca2+(aq) + (NH4)2C2O4(aq)CaC2O4(S)
OH and (NH4)2C2O4 are added. +
(white) + 2NH4 (aq)

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ii) BARIUM: To a few drops Yellow precipitate is formed, which is Presence of Ba2+ is
of the original solution soluble in conc.acids. confirmed.
K2CrO4 is added Ba2 (aq) + K2CrO4(aq) 
+

BaCrO4(S)(yellow) + 2K+
iii) STRONTIUM: To a few White precipitate is formed Presence of Sr2+ is
drops of the original solution confirmed.
Sr2+(aq) +(NH4)2SO4(aq)SrSO4(S)
NH4 OH and (NH4)2SO4 +
(white) +2NH4 (aq)
crystals are added.
7. SIXTH GROUP- Blue precipitate is formed Presence of Mg2+ is
MAGNESIUM confirmed
i) To a few drops of the
original solution Magneson
reagent (an alkaline solution of
p- nitrobenzenene azo
resorcinol) is added.
Result:
The given simple salt contains
i) Acid radical as :
ii) Basic radical as :
The given simple salt is confirmed as _________ (formula of the salt).

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