Volumetric Analysis of KMnO4 Solutions
Volumetric Analysis of KMnO4 Solutions
ANALYSIS
EXPERIMENT NO. 1
Aim: To prepare a standard solution of Mohr salt (M/20) and determine volumetrically the
molarity and strength of the given KMNO4 solution.
Theory:
Procedure:
Burette - Potassium Permanganate
Conical flask – 10 ml of Mohr Salt (M/20) + 10 ml of 2M H2SO4
Indicator – KMnO4 is a self-indicator
End point – Colourless to pale pink colour
Calculations:
From the overall balanced equation, it is clear that 2 moles of KMnO4 react with 10 moles
of Mohr salt
𝑀"#$%! 𝑋 𝑉"#$%! 2 1
= =
𝑀#&'( *+,- 𝑋 𝑉#&'( *+,- 10 5
𝑀"#$%! 𝑋 𝑉"#$%! 1
=
10 𝑋 10 5
20
𝑀"#$%! 𝑋 𝑉"#$%! 1
=
0.05 𝑋 10 5
0.05 𝑋 10
𝑀"#$%! =
5 𝑋 𝑉"#$%!
𝑆𝑡𝑟𝑒𝑛𝑔𝑡ℎ = 𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑋 𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑜𝑓 𝐾𝑀𝑛𝑂.
𝑆𝑡𝑟𝑒𝑛𝑔𝑡ℎ = 𝑀"#$%! 𝑋 158
Result: The concentration of the given KMnO4 is ________M.
The strength of the given KMnO4 solution is ____________g/L.
Experiment No. 2
Aim: To prepare a standard solution of Oxalic acid(M/40) and determine volumetrically the
molarity and strength of the given KMNO4 solution.
Theory:
Ionic Equations:
Procedure:
Burette - Potassium Permanganate
Conical flask – 10 ml of oxalic acid (M/40) + 10 ml of 2M H2SO4
Indicator – KMnO4 is a self-indicator
End point – Colorless to pale pink color
Ignition Test: A small amount of sample is No sooty flame observed Presence of aliphatic
taken in a spatula and ignited by inserting into compound
a Bunsen flame.
Litmus Test: A drop of the sample is placed Blue litmus turned red Presence of carboxylic acid
on a blue litmus paper. functional group
Bicarbonate Test: To a small amount of the Brisk effervescence observed Carboxylic acid functional
sample a pinch of sodium bicarbonate is group is confirmed.
added.
Ester Test: To the sample, 1- 2ml ethanol Sweet smelling ester formed Carboxylic acid functional
and a few drops of concentrated sulphuric group is confirmed.
acid is added. The mixture is then heated in a
water bath.
Ignition Test: A small amount of sample is No sooty flame observed Presence of aliphatic
taken in a spatula and ignited by inserting into compound
a Bunsen flame.
Litmus Test: A drop of the sample is placed Blue litmus remained blue Absence of carboxylic acid
on a blue litmus paper. functional group
Bicarbonate Test: To a small amount of the No brisk effervescence Absence of carboxylic acid
sample a pinch of sodium bicarbonate is observed functional group
added.
2, 4 DNP Test: To the sample a few drops of Orange precipitate observed Presence of carbonyl group
2, 4- DNP reagent is added. The mixture is observed. May be aldehyde o
shaken and heated in water bath. ketone.
Fehling’s Test: To the sample equal Reddish brown precipitate Presence of aldehyde group
quantities of Fehling’s A and Fehling’s B observed. observed.
solution are added. The mixture is then heated
in a water bath.
Tollen’s Test: To the sample 1-2 ml of Formation of silver mirror is Aldehyde group is confirmed
Tollen’s reagent is added. The mixture is then observed.
heated in a water bath.
Ignition Test: A small amount of sample is No sooty flame observed Presence of aliphatic
taken in a spatula and ignited by inserting into compound
a Bunsen flame.
Litmus Test: A drop of the sample is placed Blue litmus remained blue Absence of carboxylic acid
on a blue litmus paper. functional group
Bicarbonate Test: To a small amount of the No brisk effervescence Absence of carboxylic acid
sample a pinch of sodium bicarbonate is observed functional group
added.
2, 4 DNP Test: To the sample a few drops of Orange precipitate observed Presence of carbonyl group
2, 4- DNP reagent is added. The mixture is observed. May be aldehyde o
shaken and heated in water bath. ketone.
Fehling’s Test: To the sample equal No reddish-brown precipitate Absence of aldehyde group
quantities of Fehling’s A and Fehling’s B observed. observed.
solution are added. The mixture is then heated
in a water bath.
Sodium nitroprusside Test: To the sample Wine red colouration is Ketone group is confirmed.
sodium nitroprusside solution is added. Then observed.
1ml of sodium hydroxide is added.
Ignition Test: A small amount of sample is No sooty flame observed Presence of aliphatic
taken in a spatula and ignited by inserting into compound
a Bunsen flame.
Litmus Test: A drop of the sample is placed Blue litmus remained blue Absence of carboxylic acid
on a blue litmus paper. functional group
Bicarbonate Test: To a small amount of the No brisk effervescence Absence of carboxylic acid
sample a pinch of sodium bicarbonate is observed functional group
added.
2, 4 DNP Test: To the sample a few drops of No orange precipitate is Absence of carbonyl group
2, 4- DNP reagent is added. The mixture is observed observed.
shaken and heated in water bath.
Fehling’s Test: To the sample equal No reddish-brown precipitate Absence of aldehyde group
quantities of Fehling’s A and Fehling’s B observed. observed.
solution are added. The mixture is then heated
in a water bath.
Sodium nitroprusside Test: To the sample No wine red colouration is Absence of ketone group is
sodium nitroprusside solution is added. Then observed. observed.
1ml of sodium hydroxide is added.
Ester test: To the sample, 1- 2ml acetic acid Sweet smelling ester formed Alcohol functional group is
and a few drops of concentrated sulphuric confirmed.
acid is added. The mixture is then heated in a
water bath.
Preparation of original salt solution (OS): To a pinch of salt taken in a test tube add
10 mL of distilled water and shaken well.
Experiment Observation Inference
1. Silver nitrate test: Curdy white precipitate Presence of chloride is
To a part of OS, which is soluble in excess confirmed.
add few drops of of ammonium hydroxide
silver nitrate solution is obtained.
solution.
2. Barium chloride No characteristic Absence of sulphate.
test: To a part of observation.
OS add BaCl2
solution.
3. Lead acetate test: No characteristic Absence of sulphate.
To a part of OS, observation.
add lead acetate
solution.
4. Brown ring test: To No characteristic Absence of nitrate.
a part of OS, add observation.
twice the part of
freshly prepared
ferrous sulphate
solution and then
add Conc.
Sulphuric acid
slowly along the
inner sides of the
test tube.
5. To the part of OS, No characteristic Absence of phosphate.
add Conc. HNO3 in observation.
excess and allow it
to boil until all the
vapours get
evolved. Then cool
the content slowly
and add ammonium
molybdate reagent.
6. To the part of OS, No characteristic Absence of phosphate.
add dil. HCl and observation.
heat and cool it.
Then add magnesia
mixture to the
content.
Basic radical Analysis - Group Analysis
1. Zero Group radical: Pungent smelling gas Presence of zero group
To a pinch of salt which gives dense white radical – Ammonium.
taken in a test tube, fumes with a glass rod
few drops NaOH dipped in Conc. HCl when
solution is added shown at the mouth of test
and heated. tube.
Result:
1. The given acid radical is chloride.
2. The given basic radical is Ammonium.
3. So, the given simple salt is Ammonium chloride.
Analysis of simple salt – (Copper sulphate)
Experiment Observation Inference
1. Colour: Colour of Blue colour May be copper salt.
the salt is noted
2. Smell: Smell of the No characteristic smell Absence of ammonium or
salt is noted acetate salt
3. Action of heat: Blue colour salt turns May be copper sulphate
A pinch of salt in white. salt.
the dry test tube is
heated.
4. Flame test:
A pinch of salt is Blue colour flame Presence of copper salt.
taken in a watch
glass and made into
a paste with Conc.
HCl. Introduce the
paste into luminous
part of the flame.
5. Ash test:
To the pinch of salt No characteristic coloured Absence of Aluminium,
taken in a test tube, ash. zinc and magnesium.
few drops of cobalt
nitrate solution is
added. A filter
paper is soaked
into the solution
and burn it until it
turns into ash.
Dry tests:
1. Dil HCl test: To the No brisk effervescence is Absence of carbonate.
pinch of salt taken seen.
in a test tube, few
drops of Dil. HCl is
added.
2. Conc. H2SO4 test: No characteristic Absence of Chloride,
To the pinch of salt observation. Nitrate and acetate.
taken in a test tube,
few drops of Conc.
H2SO4 is added and
heated slightly.
3. MnO2 test: To a No characteristic Absence of chloride.
pinch of a salt in observation.
the test tube add
half a pinch of
MnO2 and then add
few drops of conc.
H2SO4 and heat.
4. Chromyl chloride No yellow orange Absence of chloride.
test: To the pinch vapours.
of salt taken in a
test tube, a pinch of
potassium
dichromate and few
drops of Conc.
H2SO4 is added and
then heated gently.
5. Copper turning No red brown fumes. Absence of nitrate.
test: To the pinch
of salt taken in a
test tube, add
copper turnings and
Conc. H2SO4 and
heated.
6. Ferric chloride test: No red precipitation. Absence of acetate.
To the pinch of salt
taken in a test tube,
add few ml of
neutral ferric
chloride solution
and heated.
7. Ester test: To a No characteristic Absence of acetate.
pinch of salt add observation.
few mL of ethyl
alcohol and few
drops of conc.
H2SO4 and warm
heat it gently.
Preparation of original salt solution (OS): To a pinch of salt taken in a test tube add
20 mL of distilled water and shaken well.
Experiment Observation Inference
1. Silver nitrate test: No characteristic Absence of chloride
To a part of OS, observation.
add few drops of
silver nitrate
solution.
2. Barium chloride White precipitate Presence of sulphate is
test: To a part of insoluble in conc. HCl is confirmed.
obtained.
OS add BaCl2
solution.
3. Lead acetate test: White precipitate soluble Presence of sulphate is
To a part of OS, in ammonium acetate and confirmed.
add lead acetate sodium hydroxide mixture
solution. is obtained.
4. Brown ring test: To No characteristic Absence of nitrate.
a part of OS, add observation.
twice the part of
freshly prepared
ferrous sulphate
solution and then
add Conc.
Sulphuric acid
slowly along the
inner sides of the
test tube.
5. To the part of OS, No characteristic Absence of phosphate.
add Conc. HNO3 in observation.
excess and allow it
to boil until all the
vapours get
evolved. Then cool
the content slowly
and add ammonium
molybdate reagent.
6. To the part of OS, No characteristic Absence of phosphate.
add dil. HCl and observation.
heat and cool it.
Then add magnesia
mixture to the
content.
Result:
1. The given acid radical is Sulphate.
2. The given basic radical is Copper.
3. So, the given simple salt is Copper sulphate.
Analysis of simple salt – (Copper nitrate)
Experiment Observation Inference
1. Colour: Colour of Blue colour. Presence of copper.
the salt is noted
2. Smell: Smell of the No characteristic smell Absence of ammonium or
salt is noted acetate salt
3. Flame test:
A pinch of salt is Blue colour flame. Presence of copper.
taken in a watch
glass and made into
a paste with Conc.
HCl. Introduced
the paste into
luminous part of
the flame.
4. Ash test:
To the pinch of salt No characteristic coloured Absence of Aluminium,
taken in a test tube, ash. zinc and magnesium.
few drops of cobalt
nitrate solution is
added. A filter
paper is soaked
into the solution
and burn it until it
turns into ash.
Dry tests:
1. Dil HCl test: To the No brisk effervescence is Absence of carbonate.
pinch of salt taken seen.
in a test tube, few
drops of Dil. HCl is
added.
2. Conc. H2SO4 test: Brown gas. May be Nitrate.
To the pinch of salt
taken in a test tube,
few drops of Conc.
H2SO4 is added and
heated slightly.
3. Chromyl chloride No yellow orange Absence of chloride.
test: To the pinch vapours.
of salt taken in a
test tube, a pinch of
potassium
dichromate and few
drops of Conc.
H2SO4 is added and
then heated gently.
4. Copper turning Brown fumes. Presence of nitrate.
test: To the pinch
of salt taken in a
test tube, add
copper turnings and
Conc. H2SO4 and
heated.
5. Ferric chloride test: No red precipitation. Absence of acetate.
To the pinch of salt
taken in a test tube,
add few ml of
neutral ferric
chloride solution
and heated.
Wet test:
6. Barium chloride No white precipitate. Absence of sulphate is
test: To a part of confirmed.
salt solution (OS),
BaCl2 solutions is
added.
7. Brown ring test: To A brown ring is formed at Presence of Nitrate is
a part of OS add the junction of two layers. confirmed.
freshly prepared
FeSO4 solutions is
added and
Conc.H2SO4 is
added along the
inner sides of the
test tube slowly.
Result:
1. The given acid radical is Nitrate.
2. The given basic radical is Copper.
3. So, the given simple salt is Copper nitrate.
S.N Experiment Observations Inference
o
Preliminary Tests
4.Action of Heat
4 Take a small amount of the given Gas evolution: Reddish
salt taken in a dry test tube, heat it brown vapours. Reddish brown vapours.
gently; then strongly.
Flame Test :
5 To a small amount of the given No characteristic flame Absence of Cu2+,Br2+,Sr2+,Ca2+
salt taken in a watch glass, add a
drop of Con. HCl and make it into
a paste. Introduce into non-
luminous part of the flame using a
charred match stick.
Ash Test:
6 A pinch of the salt is mixed with Blue Ash Presence of Al3+
Conc.HNO 3 and a few drops Co
(NO 3)2. A filter paper is dipped in
the above mixture and ignited.
Ester Test:
13 Take a small pinch of the salt in a No Characteristic odour Absence of CH3COO-
test-tube. Add few ml Conc.
H2SO4 and heat. Now ethyl alcohol
(1 ml). Shake. Pour the contents of
the tube in a beaker
full of water. Stir.
Action of NaOH:
14 Heated a pinch of salt with No Characteristic gas Absence of NH4+
Conc.solution of NaOH
CONFIRMATORY TEST FOR ANION
Preparation of Sodium Extract:
Take 1 tablespoon full of salt in a boiling tube. Mix about 2 tablespoon full of
solid sodium carbonate and add 15 mL of distilled water to it. Stir and boil the content for about 10 minutes.
Afterwards solution was cooled and filtered using a filter paper.A colorless filtrate was obtained.
-
Confirmatory test for NO3 :
-
1 (Brown Ring test): Add a few ml of A Brown ring is formed at Presence of NO is
3
freshly prepared solution of the junction of the two confirmed.
ferrous sulphate to a few ml of liquids.
water extract / sodium extract and
added Conc.H2SO4 slowly along
the sides of the test tube
To a few ml of original solution (i) Gelatinous white ppt soluble Presence of Al3+ is
1. added NaOH solution. in excess of NaOH confirmed.
To a few ml of original solution added (ii) A red lake was obtained. Presence of Al3+ is
2. few drops of aluminon reagent ( confirmed
triammonium salt of aurintricarboxylic
acid) stirred well and added NaOH in
drops.
Result:
NO3-
Cation: Al3+
Result:
1. The given acid radical is chloride.
2. The given basic radical is ferric.
3. The simple salt is ferric chloride.
Experiment –5
Aim: To analyze the given salt and identify the anion and cation present in it.
Result: The anion present in the given salt is sulphate (SO 42--) and cation is Nickel
(Ni2+.)
(Please note below equations for cations and anion to be written on the blank
page of the journal with pencil.)
Equations:
Ni2+
Ni2+ + 2NH4OH + +
2NH 4+ + 2H O2
Nickel dimethyl
glyoxime
SO 42--
1 SO 42-- + BaCl2 BaSO4 ↓ + 2Cl--
.2 ↓
SO 2-- + Pb(CH COO) PbSO + CH COO--
4 3 2 4 3
Aim -Determination of one cation and one anion in a given salt.
Apparatus – Test tube , test tube holder, test tube stand, Burner, wire gauze , dropper
Observation Table
Experiment Observation Inference
A) Physical White Pb2+, Ba2+, Al3+, Zn2+, Cu2+ may
Examination be present.
1) Colour
2) Smell -Take a pinch of the Odourless NH4 +, S2– and CH3COO– may
Salt in between fingers and be absent.
rub it with a drop of water
3. Dry heating test -
Heated a pinch of the salt in a
dry test tube
observations :
(a) Gas evolved A colourless, odourless gas CO32– may be present.
evolved which turned lime
water milky.
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======
S.No. Experiment Observations Inference
Preliminary Tests
I Physical Examination
iii.Solubility
Action of Heat
Flame Test:
Ash Test:
Take a pinch of salt dissolves in few ml water. This is called Original solution.
Identification of Group Analysis:
+
1 To a few ml of the original solution No characteristic Absence of NH4
added Nessler’s reagent followed precipitate
by excess of NaOH