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Salt Analysis

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25 views27 pages

Salt Analysis

Uploaded by

rishikareer394
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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QUALITATIVE ANALYSIS OF INORGANIC SALTS -PROCEDURE

Preliminary tests
Experiment Observation Inference
Color Colorless/White Fe2+,
Fe3+,Mn2+,Co2+,Cu2+may be
absent

Pale pink Mn2+ may be present

2) Physical state Crystalline solid NH4+, Cl-, Br-, NO3- Al3+,Ba2+


may be absent

CO32- may be present


Amorphous solid

Solubility in water Soluble NH4+, Cl-,Br-, NO3- may be


present

CO32- may be present


Insoluble

4) Smell
NH4+, may be present
Take a pinch of the salt Ammoniacal smell
between the fingers and rub
it with a drop of water.
CH3COO- may be present
Vinegar like smell
Smell like rotten egg S2- may be present

Flame Test: Brick red color Presence of Ca2+

Take a small amount of salt Crimson red color Presence of Sr2+


on a watch glass and make a
paste with con. HCl.Take a
small quantity of the salt on Grassy green color Presence of Presence of Ba2+
a platinum loop and heat the
mixture strongly in the flame

Green flashes Presence of Zn2+ orMn2+

Dull bluish white Presence of Presence of Pb2+

No characteristic colour to Absence of Ba2+, Pb2+, Zn2+


the flame orMn2+, Ca2+ ,Sr2+

Dry heating test

Heat a pinch of the salt in a


dry test tube

i) Gas evolved Colorless odorless gas Presence of CO32-


turning lime water milky

Pungent smelling gas which


gives white fumes with
Ammonium Presence of Cl-
hydroxide./Greenish yellow
gas
Characteristic vinegar smell Presence of CH3COO-
is obtained

Characteristic smell of
ammonia gas is obtained
which gives white fumes
when glass rod dipped in Dil
+
HCl is brought near the Presence of NH4
mouth of the test tube.

Reddish brown gas which


Presence of NO3-
turns ferrous sulphate
solution black

Reddish brown gas which Presence of Br-


turns starch paper orange
yellow.

ii)Sublimate formed White sublimate Presence of NH4+

+
ii) Residue Yellow when hot , white Presence of Zn2
when cold

Brown when hot , yellow


Presence of Pb2+
when cold

White salt becomes black on


heating Presence of CH3COO-
White residue glows on Presence of Ba2+,Sr2+,Ca2+,
heating Mg2+,Al3+

Detection of acid radicals:


I) Analysis of group I acid radical:

Salt + Dil H2SO4 Brisk effervescence with the Group I acid radical is
liberation of colorless
odorless gas is present (CO32-)

No Brisk effervescence
Group I acid radical is

is absent

Confirmatory Test

1) Salt + Dil HCl, pass the Lime water turns milky Presence of CO32- is
gas through lime water. confirmed

CaCO3 + 2HCl CaCl2 + CO2 + H2O

Ca(OH)2(aq)+ CO2(g)→ CaCO3(s)+ H2O(l)

II) Analysis of group II acid radical:

Salt in a dry test tube + Conc. A colorless pungent smelling Group II acid radical Cl-
H2SO4 gas which gives a dense may be present
white fumes with glass rod
dipped in ammonium
hydroxide is exposed to the
mouth of the test tube
Reddish brown vapors with Group II acid radical Br-
pungent smell may be present

Colourless vapors , vinegar Group II acid radical


-
smell turns blue litmus red CH3COO may be present

No characteristic observation CH3COO-,Cl- ,Br- are


absent

If no reaction in cold, add a Reddish brown fumes are Group II acid radical NO3-
piece of Cu or paper ball to evolved may be present.
the test tube containing salt
and heat.

Confirmatory Test for Br-

1) Silver nitrate test: Pale yellow ppt is formed Presence of Br- is confirmed.
which is sparingly soluble
in ammonium hydroxide.
Salt solution + dil HNO3 ,
boil for some time , cool
and add silver nitrate
solution.

2) Chlorine water test


Carbon di sulphide layer
Salt solution + dil HCl acquires orange Presence of Br- is confirmed.
and1-2 ml of carbon di- colouration.
sulphide and then chlorine
water. Shake vigorously
and allow to stand.
3) MnO2 Test: Heat a Yellowish brown vapors
small quantity of the salt are evolved.
with MnO2 and conc.
H2SO4 Presence of Br- is confirmed.

Silver nitrate test:

KBr + AgNO3 KNO3 + AgBr

( pale yellow ppt)

Chlorine water test

2KBr + Cl2 2KCl + Br2

MnO2 Test:

2KBr + MnO2 + 3H2SO4 2KHSO4 + MnSO4 + 2H2O + Br2

Confirmatory Test for NO3-

Brown ring Test A brown ring is formed at the Presence of NO3- is


junction of layers of acid and confirmed
Salt solution + equal volume the solution
of freshly prepared ferrous
sulphate solution. Add a
drop of Conc H2SO4 slowly
along the sides of the test
tube.

Copper chip test : Salt +


Conc . H2SO4 + copper chip
and heat strongly Brown fumes are evolved

Presence of NO3- is
confirmed
2KNO3 + H2SO4 K2SO4 + HNO3

FeSO4 + 3H2SO4 + 4HNO3 Fe2(SO4)3 + 4 H2O + 2NO

FeSO4 + NO + 5H2O [Fe( H2O)5(NO)]SO4

Copper chip test

2KNO3 + H2SO4 K2SO4 +2 HNO3

4 HNO3 + Cu Cu(NO3)2 + 2NO2 + 2H2O

Confirmatory Test for Cl-

1) Chromyl chloride Test:

Salt + solid potassium


dichromate in a test tube +
Conc. H2SO4 . Orange red vapors are
evolved

Pass the vapours through Presence of Cl- is confirmed.


NaOH solution taken in Solution turns yellow.
another test tube.

To the above yellow


solution, add acetic acid and
lead acetate solution. Yellow ppt is obtained.

2) Silver nitrate test:

Salt solution + dil HNO3 , White precipitate is formed


Presence of Cl- is confirmed.
boil for some time , cool and which is soluble in NH4OH
add silver nitrate solution.
MnO2 Test: Heat a small Greenish yellow gas with Presence of Cl- is confirmed.
quantity of the salt with pungent irritating smell is
MnO2 and conc. H2SO4 evolved.

Chromyl chloride Test:

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


(chromyl chloride)

CrO2Cl2 + 4 NaOH Na2CrO4 + NaCl + 2H2O

Sodium chromate

Na2CrO4 + CH3COO)2Pb PbCrO4 + 2 CH3COONa

Leadchromate

Silver nitrate test

NaCl + AgNO3 AgCl + NaNO3

AgCl + 2NH4OH [AgNH3)2]Cl + 2H2O

Soluble complex

MnO2 Test:

2NaCl + MnO2 + 3H2SO4 2NaHSO4 + MnSO4 + 2H2O + Cl2


Confirmatory Test for CH3COO-

Oxalic acid Test Vinegar smell Presence of CH3COO-


confirmed
Take a small quantity of the
salt on a watch glass, mix it
with solid oxalic acid and
form a paste with water,
smell

Ester test:

Salt + iml of Conc. Presence of CH3COO-


H2SO4and warm. Add confirmed
C2H5OH . Add contents in to
Pleasant fruity smell
a beaker full of water

Oxalic acid test

COOH

+ 2CH3COONa COONa + 2 CH3COOH

COOH COONa

Ester TeST

2CH3COONa + H2SO4 Na2SO4 + Na2SO4 + 2 CH3COOH

CH3COOH + C2H5OH CH3COOC2H5 + H2O

fruity smell

III) Analysis of group III acid radical:

Test for SO42-


Barium chloride Test:

1) Salt solution + Barium White precipitate insoluble in Presence of Group III acid
chloride Dil HCl radical SO42- is confirmed

2) Lead acetate Test

Salt solution + Lead acetate White precipitate is obtained Presence of Group III acid
soluble in excess of hot radica SO42- is confirmed
ammonium acetate.

Barium chloride Test

Na2SO4 + BaCl2 BaSO4 + 2 NaCl

White

Lead acetate Test

Na2SO4 + Pb(CH3COO)2 PbSO4 + 2CH3COONa

White ppt

Detection of Basic radical:


Preparation of original solution(O S)

About one spatula of the salt is dissolved in the minimum amount of the solvent in a boiling
tube in the following order.

i) Water ii) Dil. HCl iii) Dil. HNO3

Water (Cold) Soluble Original solution

Insoluble Not original solution

Dil. HCl Soluble Original solution

Identification of basic radicals


Salt + NaOH, boil Pungent smelling ammonia Group 0 is present (NH4+ )
gas is evolved.

No Characteristic smell is
observed Group 0 is absent

O.S + 1 to 2 ml of Dil. HCl White precipitate is formed Group I is present (Pb2+)

No white precipitate is Group I is absent


formed

Pass H2S gas through the Black precipitate is formed Group II is present (Cu2+,
above solution Pb2+)

Group II is absent

No black precipitate is
formed

O.S + Solid Ammonium Group III is present (Al3+,


chloride + Ammonium Reddish/ White gelatinous Fe3+)
hydroxide in excess till the precipitate is formed
solution become basic.

Group III is absent


No precipitate
Pass H2S gas through the Black precipitate / buff Group IV is present
above solution colored / white precipitate is
formed Black (Ni2+, CO2+)

Buff (Mn2+)

White (Zn2+)

No precipitate
Group IV is absent

White precipitate is formed


O.S + Solid NH4Cl +
NH4OH + (NH4)2CO3 Group V is present (Ba2+,
Solution Sr2+, Ca2+)

No precipitate
Group V is absent

O.S + Solid Ammonium


Chloride + Ammonium White precipitate Group VI (Mg2+) is present
Hydroxide + Ammonium
Hydrogen Phosphate

Confirmatory test for Group 0

Nessler’s reagent test Reddish brown precipitate Presence of NH4+ is


is formed confirmed.
O.S + Nessler’s reagent +
NaOH

2[K2HgI4] + NH3 + 3KOH H2N.HgO.HgI 7KI + 2H2O

Confirmatory test for Group I

Boil the white precipitate


with 5-10 ml of water and
divide it into 3 parts.
Part 1 – cool under tap White crystalline Presence of Pb2+ confirmed
precipitate

Part 2 + KI solution Presence of Pb2+ confirmed


Yellow precipitate

Part 3 + Potassium Presence of Pb2+ confirmed


chromate Yellow precipitate

1) On cooling precipitate settles down as PbCl2 is less soluble in cold water


2) PbCl2 +2 KI PbI2 + 2KCl
3) PbCl2 + K2CrO4 PbCrO4 + 2KCl
Yellow ppt

Confirmatory test for II

If the precipitate is black,


dissolve it in 50% HNO3
and divide it into 2 parts.

Part 1+ Dil. H2SO4 +


Alcohol White precipitate Pb2+ is present

Dissolve white precipitate


in hot ammonium acetate
solution and divide it into 2
parts.

Part 1 + KI solution
Yellow precipitate is
formed which dissolves in 2+
boiling water crystalizes on Pb confirmed
cooling
Part 2 + K2CrO4 solution Yellow precipitate soluble
in NaOH
Pb2+ confirmed

Confirmatory test for Al3+

1.Lake test :

Presence of

Dissolve white precipitate Blue precipitate floating in Al3+ confirmed


in Dil.HCl, add 2 drops of colourless solution
blue litmus solution. To this
add, NH4OH solution
dropwise

2.NaOH Test: Gelatinous precipitate is


formed. Presence of
O.S + NaOH drop wise
Al3+ confirmed

Add excess of NaOH to the Gelatinous precipitate


precipitate dissolves.

Add solid NH4Cl The precipitate reappears

Lake test

Al(OH)3 + 3HCl AlCl3 + 3H2O …… soluble

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

Blue colour absorbs on


this.
Confirmatory test for of Group IV Basic radical (Zn2+)

O.S + Dil. NaOH dropwise White precipitate soluble in


and add excess of NaOH excess of excess of dil
NaOH is formed. Zn2+ is confirmed

White or bluish white


O.S + Potassium Ferro precipitate is formed
Cyanide Zn2+ is confirmed

1) NaOH TEST

ZnCl2 + 2NaOH Zn(OH)2 + 2NaCl


White ppt
2) Zn(OH)2 + 2NaOH Na2ZnO2 + 2H2O
Soluble
2 ZnCl2 + K4[Fe(CN)6] Zn2[Fe(CN)6] + 4KCl

Confirmatory test for Mn2+

1) Dissolve buff coloured White precipitate turns Mn2+ confirmed


precipitate in dil HCl , boil black or brown.
off H2S.To the above
solution add NaOH . Then
add Br2 water.

2) To the black precipitate


add Conc HNO3 and lead
peroxide.Boil ,cool and Pink coloured solution is
obtained. Mn2+ confirmed
allow to settle.
Confirmatory test for Group V

Dissolve the precipitate in hot


dil acetic acid. Divide it in to
three parts.

Part I + potassium chromate Presence of


solution Yellow precipitate. Ba2+ confirmed

Part II+Ammonium sulphate White precipitate. Presence of


solution.
Sr2+ confirmed

Part III + Ammonium oxalate


solution + Ammonium White precipitate.
hydroxide and scratch the
Presence of
sides of the test tube.
Ca2+ confirmed
Flame Test:

Take a small amount of salt on


a watch glass and make a
paste with con. HCl.Take a
small quantity of the salt on a
platinum loop and heat the
Brick red color Presence of
mixture strongly in the flame
Ca2+ confirmed
Presence of

Crimson red color Sr2+ confirmed

Grassy green color Presence of

Ba2+ confirmed

BARIUM

BaCO3 + 2CH3COOH CH3COO)2Ba + CO2 + H2O

CH3COO)2Ba + K2CrO4 2CH3COOK + BaCrO4

STRONTIUM yellow ppt

SrCO3 + 2 CH3COOH (CH3COO)2Sr + CO2 + H2O

(CH3COO)2Sr + (NH4)2SO4 CH3COONH4 + SrSO4

CALCIUM White ppt

CaCO3 + 2CH3COOH (CH3COO)2Ca + CO2 + H2O

(CH3COO)2Ca + (NH4)2C2O4 CH3COONH4 + CaC2O4

Confirmatory teat for Group VI

O.S + Solid Ammonium White precipitate is formed Mg2+ confirmed.


Chloride + Ammonium
Hydroxide + Ammonium
Hydrogen Phosphate

MgCl2 + NH4OH + (NH4)2HPO4 Mg(NH4)PO4 + 2NH4Cl


+ H2 O

white
O.S + Dil NaOH White precipitate insoluble Mg2+ confirmed.
in excessNaOH is formed

MgCl2 + NaOH → Mg(OH)2 + 2 NaCl

RESULT: Acid radical present is ________ Acid radical present is ___________

The given salt is _______________________

Expt No _________________ Date: ___________

FUNCTIONAL GROUP ANALYSIS

Experiment Observation Inference

Test for unsaturation

Bromine Test
Dissolve the compound in Orange red colour of Compound is unsaturated
water and add bromine water bromine water is discharged
and shake

Orange red colour of


bromine water is not Compound is unsaturated
discharged
Alkaline KMnO4
Test(Bayer’s Test) Pink colour of KMnO4 is Compound is unsaturated
Dissolve the compound in discharged
water and add 1-2 drops of
alkaline KMnO4 solution and
shake Pink colour of KMnO4 is
discharged Compound is unsaturated

Test for Alcoholic group

Ceric Ammonium Alcoholic group(----OH) is


nitrate test: Organic present
compound + ceric ammonium Pink or red colour is formed
nitrate reagent and shake well
Alcoholic group(----OH) is
No Pink or red colour is absent
formed

Test for Phenolic group

Neutral FeCl3 Test:

1mL of neutral FeCl3 +


2-3 drops of organic Phenolic( Ar_---OH)
compound Violet colouration group is present

Phenolic( Ar_---OH)
group is absent
No Violet colouration

Test for carbonyl group


Yellow or orange crystals
Shake the organic
are formed Carbonyl group is present(
compound with 2-3 mi of ---CHO or >CO)
2,4 dinitro phenyl
hydrazine. No Yellow or orange
crystals are formed No Carbonyl group is
present(---CHO or >CO)
Test for Aldehydic Pink or magenta colour is
group formed.
Aldehydic(-CHO) group is
present
Shiff’s reagent test: Add 1
ml of Shiff’s reagent to No Pink or magenta colour
the organic compound is formed.
Ketonic (>CO) group is
present

Test for Carboxylic acid


Brisk effervescence is Carboxylic (--COOH)
group
observed group is present
Sodium hydrogen
carbonate test: Add a
No Brisk effervescence is Carboxylic (--COOH)
pinch of NaHCO3 to 1ml
observed group is absent
of organic compound.

Test for Amino group Amino group (--NH2)is


present
Compound is soluble

Solubility test: Shake a


Amino group (--NH2)is
small amount of the given Compound is insoluble
absent
compound in a clean test
tube and add 2-3 ml of dil
HCl.
Colour changes to blue Amino group (--NH2)is
present
Litmus test: Place a drop
Amino group (--NH2)is
of given organic Colour does not change absent
compound on a moist red
litmus paper.

CONFORMATORY
TESTS

Alcoholic group:
Fruity smell is observed.
1) Ester Test :To 1 ml of
organic compound + Presence of ----OH group
Glacial acetic acid + 2-3 is confirmed.
drops os conc. H2SO4 .
Warm the mixture on a
Presence of ----OH group
water bath for 5 min and
is confirmed.
pour it in to cold water
taken in a beaker and
smell it

2) Sodium metal Test :


Brisk effervescence due to
Compound + anhydrous Presence of Phenolic(
evolution of hydrogen gas
CaSO4 + sodium metal Ar__OH) group confirmed

Phenolic group:

Liebermann’s Test :
Add few ml of phenol in a
test tube containing A deep blue colour or deep
sodium nitrite crystals. green colour is developed.
Heat irt for a minute and The colour turns red on
allow it to cool. Then add adding water . Presence of ----OH group
is confirmed.
about 1 ml of conc.
Blue or green colour
H2SO4 appears on adding excess of
NaOH

Pink colour is formed.


Phthalein Dye test:
Take Organic compound
and Phthalic anhydride in
a clean test tube and add
1-2 drops conc. H2SO4 .
Heat the test tube . Cool
and pour the mixture in to
a beaker containing
NaOH solution.

Carboxylic group Presence of ----COOH


group is confirmed.
Ester Test: Organic
compound + ethyl alcohol
and 1-2 drops of conc.
H2SO4 . Warm the mixture
on a water bath for 5 min
and pour it in to cold Fruity smell
water taken in a beaker Presence of -----CHO
and smell it group is confirmed.

Aldehydic group
Shining silver mirror is
Tollens reagent test : formed
Presence of -----CHO
Warm a test tube group is confirmed.
containing organic
compound and Tollens’s
reagent on a water bath. Red Precipitate is formed.

Fehling’s solution Test:


Take 1 ml each of
Fehling’s solution A and
B in a test tube and add
few drops of the given
organic compound. Warm
Presence of >CO group is
the test tube in a water
confirmed.
bath .

Ketonic Group Violet colour is appeared.

m- Dinitro benene test:

Organic compound + m- Presence of >CO group is


Dinitro benene . Add confirmed
about 1 ml of dil NaOH
solution and shake the test
tube

Sodium nitro prusside


test : Organic compound Red colour is appeared. Presence of ---NH2 group
+ Sodium nitro prusside is confirmed
and shake the test tube .
Add about 1 ml of dil
NaOH solution drop wise

3) Sodium bisulphite
Test

Tale 2 ml of saturated
sodium bisulphite
Crystalline white Presence of >CO
solution and 1 ml of the
precipitate is formed group is confirmed.
given organic compound.
Shake the test tube well
and leave it for 15 – 20
min.

Test for amino group Presence of ---NH2 group


is confirmed
Carbyl amine test:

0.2 g of solid KOH +


ethanol in a test tube.
Warm until KOH Un pleasant odour
dissolves. To this add few
drops of chloroform and
organic compond and
warm gently on a water
bath.

Azo dye test:

Take three test tubes


A,B,C

In test tube A dissolve the


organic compound in 2ml
of dil HCl. In Test tube B
prepare aqueous solution
Red or orange dye is
of NaNO2. In test tube C
formed
dissolve beta naphthol in
dil. NaOH. Cool all the
three test tubes in ice
bath. Now add NaNO2
solution to test tube A and
the resulting solution to
test tube C.
EQUATIONS OF CONFIRMATORY TESTS
1) –OH GROUP

2) –COOH GROUP

3)—ArOH GROUP
3) >C=O GROUP

5)-NH2 GROUP
6)-CHO GROUP

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