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Volumetric Analysis of KMnO4 Solutions

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0% found this document useful (0 votes)
39 views43 pages

Volumetric Analysis of KMnO4 Solutions

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

VOLUMETRIC

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

To prepare a standard solution of Mohr salt (M/20)


𝑊! 𝑋 1000
𝑀=
𝑀! 𝑋 𝑉
1 𝑊! 𝑋 1000
=
20 392 𝑋 250
0.05 𝑋 392 𝑋 250
𝑊! = = 4.9𝑔
1000
4.9 g of Mohr salt is needed to make (M/20) Mohr salt solution in 250ml.
Observation table:
S.No. Burette reading Volume of KMnO4(ml)
Initial Reading Final reading

Concordant reading = ________ml

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

To prepare a standard solution of Oxalic acid(M/40)


𝑾𝑩 𝑿𝟏𝟎𝟎𝟎
𝑴=
𝑴𝑩 𝑿 𝑽
𝟏 𝑾𝑩 𝑿𝟏𝟎𝟎𝟎
=
𝟒𝟎 𝟏𝟐𝟔𝑿𝟐𝟓𝟎
𝟎. 𝟎𝟐𝟓 𝑿 𝟔𝟑 𝟏. 𝟓𝟕𝟓
𝑾𝑩 = = = 𝟎. 𝟕𝟖𝟕𝟓𝒈
𝟐 𝟐
0.7875 g of Oxalic acid is needed to make (M/40) Oxalic acid solution in 250ml.
Observation table:
S.No. Burette reading Volume of KMnO4(ml)
Initial Reading Final reading

Concordant reading = ________ml


Calculations:
From the overall balanced equation, it is clear that 2 moles of KMnO4 react with 5 moles of
Oxalic acid
𝑀"#$%! 𝑋 𝑉"#$%! 2
=
𝑀%0+,12 +213 𝑋 𝑉%0+,12 +213 5
𝑀"#$%! 𝑋 𝑉"#$%! 2
=
10 𝑋 10 5
40
2 𝑋 10
𝑀"#$%! =
40 𝑋 𝑉"#$%!
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.
IDENTIFICATION
OF
BIOMOLECULES
Experiment No. 3
Aim: To distinguish between reducing carbohydrate and nonreducing carbohydrate
Experiment Sample A Sample B
Fehlings Test: Reddish brown ppt appears No reddish brown ppt is
Few drops of the sample is (Reducing carbohydrate) formed (Non-reducing
treated with 1-2 ml of carbohydrate)
Fehling’s solution A and 1-2
ml of Fehling’s solution B.
The mixture is kept in boiling
water bath.
The test is conducted with
both samples.

Tollens test: Silver mirror formation is No silver mirror formation is


Few drops of the sample is observed observed
treated with 1-2 ml of Tollens (Reducing carbohydrate) (Non-Reducing carbohydrate)
reagent. The mixture is kept
in boiling water bath.
The test is conducted with
both samples.

Iodine test: No-blue black colouration is Blue-Black colouration is


Few drops of the sample is observed observed (Presence of Starch)
treated with 1-2 ml of iodine (Absence of Starch)
solution.
The test is conducted with
both samples.

Result: Sample A is Reducing Carbohydrate and sample B is Non reducing Carbohydrate


Experiment No. 4
Aim: To distinguish between reducing Proteins and Fats
Experiment Sample A Sample B
Biuret test: Violet colouration No Violet colourationis
Few drops of the sample is (Presence of Protein) observed (Absence of Protein)
treated with few drops of
copper sulphate solution and
sodium hydroxide solution.
The test is conducted with
both samples.

Xanthoproteic test : Yellow colouration appears No yellow colouration is


Few drops of the sample is (Presence of Protein) observed (Absence of Protein)
treated with 1-2ml of
concentrated nitric acid and
heated in a water bath.
The test is conducted with
both samples.

Translucent spot test: No translucent spot formation Translucent spot formation is


Few drops of the sample is is seen. observed (Presence of oil/fat).
placed in a filter paper (Absence of fat) As sample is liquid it is oil.
The test is conducted with
both samples.

Result: Sample A is Protein and sample B is an oil


FUNCTIONAL
GROUP
ANALYSIS
EXPERIMENT NO. 5
Aim: To identify the functional group in the given organic compound.

Experiment Observation Inference

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.

Result: The given sample is an aliphatic carboxylic acid.


EXPERIMENT NO. 6
Aim: To identify the functional group in the given organic compound.

Experiment Observation Inference

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.

Result: The given sample is an aliphatic aldehyde.


EXPERIMENT NO. 7
Aim: To identify the functional group in the given organic compound.

Experiment Observation Inference

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.

Result: The given sample is an aliphatic ketone.


EXPERIMENT NO. 8
Aim: To identify the functional group in the given organic compound.

Experiment Observation Inference

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.

Result: The given sample is an aliphatic alcohol.


QUALITATIVE
ANALYSIS
Analysis of simple salt – (Ammonium chloride)
Experiment Observation Inference
1. Colour: Colour of Colourless. Absence of copper,
the salt is noted Manganese, Nickel and
Ferric.
2. Smell: Smell of the Ammoniacal smell. May be presence of
salt is noted ammonium salt.
3. Action of heat: Ammoniacal smell May be ammonium salts.
A pinch of salt in
the dry test tube is
heated.
4. Flame test:
A pinch of salt is No characteristic colour in Absence copper, barium,
taken in a watch the flame. strontium and calcium.
glass and made into
a paste with Conc.
HCl. Introduced
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 No brisk effervescence is Absence of carbonate is
the pinch of salt seen confirmed.
taken in a test tube,
few drops of Dil.
HCl is added.
2. Conc. H2SO4 test: Colourless gas which Presence of Chloride.
To the pinch of salt gives dense white fumes
taken in a test tube, with a glass rod dipped in
few drops of Conc. ammonium hydroxide is
H2SO4 is added and formed.
heated slightly.
3. MnO2 test: To a Greenish yellow gas Presence of chloride.
pinch of a salt in which turns starch iodide
the test tube add paper blue is formed.
half a pinch of
MnO2 and then add
few drops of conc.
H2SO4 and heat.
4. Chromyl chloride
test: To the pinch
of salt taken in a
test tube, a pinch of
potassium Yellow orange vapours.
dichromate and few
drops of Conc. Presence of chloride is
H2SO4 is added and confirmed.
then heated gently.
The vapours are
allowed to pass
through a solution
containing NaOH, Yellow precipitate is
dil. Acetic acid and formed.
lead acetate
solution.
5. Copper turning No red brown fumes. Absence of nitrate.
test: To th 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
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.

Confirmatory test: For Ammonium radical:


Experiment Observation Inference
To the OS, Nesslers’s Orange brown precipitate Presence of ammonium
reagent and NaOH of Milon’base is obtained. radical is confirmed.
solution is added.

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.

Basic radical Analysis - Group Analysis


1. Zero Group radical: No characteristic Absence of zero group
To a pinch of salt observation. radical – Ammonium.
taken in a test tube,
few drops NaOH
solution is added
and heated.
2. To a part of OS, No White precipitate. Absence of I group radical
add dil. HCl. – Lead.
3. To a part of OS, Black precipitate of Cu2S Presence of II group
add dil. HCl and is obtained. radical – Copper.
YAS solution.

Confirmatory test: For Copper radical:


Experiment Observation Inference
To a part of OS add Chocolate brown Presence of Copper
potassium ferro cyanide precipitate is obtained. radical is confirmed.
solution.

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.

Basic radical Analysis - Group Analysis


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.
1. Zero Group radical: No pungent smell. Absence of zero group
To a pinch of salt radical – Ammonium.
taken in a test tube,
few drops NaOH
solution is added
and heated.
2. To a part of OS, No White precipitate. Absence of I group radical
add dil. HCl. – Lead.
3. To a part of OS, Black precipitate is Presence of II group
add dil. HCl and obtained. radical – Copper.
YAS solution.

Confirmatory test: For Copper radical:


Experiment Observation Inference
To a part of OS, add Chocolate brown Presence of Copper
potassium ferrocyanide precipitate is obtained. radical is confirmed.
solution.

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

I Physical Examination Absence of Cu2+,Ni2+,Fe2+,Fe3+,Co2+,Mn2+


1.Colour Colourless
- - -
2 2.Apperance Crystalline May be Cl-,Br-,No3 ,I ,CH3COO ,
except( NH4)2Co3
- -
3 3.Solubility May be Cl-,Br-,No3 ,I ,CH3COO
-
Take a pinch of salt in a test tube, Soluble ,except ( NH4)2Co3.
add few ml of water.

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.

Identification of Anions (Acid Radicals)


Action of dilute H2SO4:
7 To a small portion of the given No Characteristic gas is Absence of S2-, CO3 2-
salt taken in a test tube add 1 or evolved.
2ml of dilute H2SO4
Concentrated H2SO4 Test: -
8 A pinch of the solid salt heated with Reddish brown vapour Presence of NO3
Conc.H2SO4
Maganese dioxide test:(MnO2) Heat
9 a pinch of the salt with a small No Characteristic gas Absence of Cl-, Br -, I-
quantity of MnO2 and Conc. H2SO4.
Copper Turning Test:
-
10 Heat a pinch of salt with Conc. Reddish brown gases of Presence of NO 3
H2SO4 and a few copper turning nitrogen dioxide are evolved

Chromyl Chloride Test: Heated a


11 pinch of the salt with solid K 2Cr2O 7 No Characteristic gas Absence of Cl-
along with Conc. H2SO4

Ammonium molybdate test: Take a


3-
12 pinch of salt add Conc.HNO3 and No Characteristic ppt Absence of PO4 .
boil. Add ammonium molybdate
solution in excess and again boil

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

Analysis of cations: [ Preparation of Original Solution]


Take a pinch of salt dissolves in few ml water.This is called Original solution.
Note: If the salt is insoluble and is a carbonate in the above statement H2O to be prepared by dil.HCl.
Identification of Group Analysis:
To a few ml of the original solution No characteristic ppt Absence of Group I
1 added dil.HCl

To a few ml of the original solution


2 added dil.HCl and passed H2S gas. No black ppt. Absence of group II

3 To a few ml of original solution added Gelatinous white ppt Presence of group


NH4Cl(aq) and NH4OH(aq) III(Al3+)

CONFIRMATORY TEST FOR GROUP III : (Al3+)

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:

The given simple salt contains Anion:

NO3-

Cation: Al3+

The simple salt is : Al(NO3)3……….


S.NO EXPERIMENT OBSERVATION INFERENCE
Preliminary test
1 Colour
Colour of the salt is noted. Brown May be ferric salt.
Appearance
2
Appearance of the salt is Crystalline May be sulphate, nitrate
noted. or chloride salts.
3 Solubility
A little of the salt is shaken Soluble May be sulphate, nitrate
well with distilled water. or chloride salts.
4 Action of Heat
A small amount of the salt is No characteristic change Absence of carbonate,
taken in a dry test tube, heated nitrate, ammonium, zinc
gently at first and then and copper.
strongly.
5 Flame Test
A small amount of the salt is No characteristic coloured Absence of copper,
made into a paste with conc. flame calcium and barium.
HCl in a watch glass and
introduced into the non-
luminous part of the bunsen
flame using a glass rod.
6 Ash Test
The filter paper is soaked in a No characteristic coloured ash Absence of zinc,
mixture of salt and cobalt aluminium, phosphate and
nitrate solution, introduced magnesium
into the bunsen flame and
ignited.
Identification of Acid Radicals
7 Action of dilute hydrochloric acid
A small amount of salt is No characteristic change Absence of carbonate.
added to 2/3 volume of dilute
hydrochloric acid taken in a
test tube.
8 Action of concentrated sulphuric acid
To a small amount of the salt, Colourless gas giving dense Presence of chloride.
2 ml of conc. sulphuric acid is white fumes with a glass rod
added and heated dipped in ammonium
hydroxide and also turning
moist blue litmus paper red
evolves.
9 Manganese dioxide test
A small amount of the salt is Greenish yellow gas with Presence of chloride
heated with a pinch of MnO2 irritating smell turning the
and 1 ml of conc. H2SO4 starch iodide paper and blue
evolves.
11 Copper turnings test
A small amount of the salt is No reddish brown gas evolves Absence of Nitrate
heated with copper turnings
and conc. sulphuric acid and
viewed the test tube vertically
down.
12 Action of Sodium Hydroxide
A small amount of the salt is No pungent smelling gas Absence of ammonium
heated with sodium hydroxide salt.
solution.
13 Chromyl Chloride test
To a small amount of the salt Red orange vapours, evolved is Chloride is confirmed
a pinch of potassium passed through water in test
dichromate is added and tube, yellow solution is
heated with a few drops of obtained. On adding lead
conc. sulphuric acid. acetate solution, yellow
precipitate is formed.
Preparation of sodium carbonate extract
14 The salt is dissolved in water. This is called water extract.
i. Silver Nitrate Test
To a few drops of the extract, A curdy white precipitate
dil. Nitric acid is added until completely soluble in excess of Presence of Chloride
the effervescence ceases and 2 ammonium hydroxide is
ml of silver Nitrate solution is obtained.
added.
ii. Lead acetate test
To a few drops of the extract, No precipitation is obtained Absence of Sulphate.
dilute acetic acid is added
until the effervescence ceases
and 2 ml of the lead acetate
solution is added.
iii. Barium Chloride Test
To a few drops of the extact No white precipitate is Absence of Sulphate.
dil. hydrochloric acid is added obtained
until the effervescence ceases
and 2 ml Barium Chloride is
added.

iv. Brown ring test


To a few drops of the extract, No brown ring is formed Absence of Nitrate
dil. H2SO4 is added until the
effervescence ceases. The
solution is treated with freshly
prepared ferrous sulphate
solution and then conc.
sulphuric acid is added in
drops along the sides of the
test tube.
Identification of basic radical
Preparation of Original Solution
The original solution is prepared by dissolving a gram of the salt in 15 ml of
distilled water.
Group separation
1 A small amount of the salt is No pungent smelling gas Absence of ammonium
heated with sodium hydroxide (Group 0)
solution.
2 To a few drops of original No white precipitate Absence of lead.
solution. dil. HCl is added. (GroupI)
3 To a few drops of original No characteristic precipitate Absence of arsenic and
solution, 2ml of HCl is added copper (Group II)
then H2S gas is passed.
4 To a few drops of original Brown precipitate is obtained, Presence of Ferric ion
solution, 1ml of ammonium soluble in dil. HCl (Group III)
chloride and 2 ml of
ammonium hydroxide are
added.
Confirmatory tests for basic radical
Ferric Iron (Group III)
i. To a few drops of the original Blue coloration is obtained Ferric iron is confirmed
solution, 2 ml of potassium
ferrocyanide is added.
ii. To a few drops of original Blood red coloration is Ferric iron is confirmed
solution, 2ml of ammonium obtained.
thiocyanate solution is added

Confirmatory tests for acid radical


Chromyl Chloride test
To a small amount of the salt Red orange vapours, evolved is Chloride is confirmed
a pinch of potassium passed through water in test
dichromate is added and tube, yellow solution is
heated with a few drops of obtained. On adding lead
conc. sulphuric acid. acetate solution, yellow
precipitate is formed.

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.

S.NO EXPERIMENT OBSERVATION INFERENCE


Preliminary Test
1. COLOUR green May be nickel.
The Colour of given
salt is noted.
2. APPEARANCE Crystalline Absence of carbonate
The appearance of the
given salt is noted
3. SOLUBILITY IN
WATER
A little of the given salt Soluble Absence ofCarbonate
is dissolved in distilled
water in a test tube
4. ODOUR No characteristic Absence of ammonium
smell. and acetate salts.
ANION ANALYSIS
5. ACTION OF
DIL.SULPHURIC ACID
To a little of the substance No characteristic Absence of Carbonate,
taken in a test tube a few reaction sulphite, nitrite and
drops of dil. Sulphuric sulphide.
acid
is added .
6. ACTION OF No characteristic Absence of chloride,
CONC.SULPHURIC reaction bromide, nitrate, acetate
ACID
To a little of the substance
taken in a test tube a few
drops of conc. Sulphuric
acid
is added and warmed.
7. To the salt solution add dil White ppt Presence of sulphate is
HCl and barium chloride insoluble in conc confirmed.
solution.. HCl and Conc SO42-
HNO3.
8. To the salt solution add White ppt Presence of
acetic acid and lead acetate insoluble in dil sulphate is confirmed
solution HCl and soluble SO42-
in ammonium
acetate.
CATION ANALYSIS
Original solution s
prepared by dissolving the
salt in water
9. ZEROGROUP
(AMMONIUM) No characteristic Absence of group zero
To a little of the salt reaction (ammonium).
sodium hydroxide solution NH4+
is added
and heated
10 I GROUP (LEAD)
To a little of the original No characteristic Absence of I group
solution dil. HCI is added. reaction Pb2+
11 II GROUP (COPPER)
To a little of the original No characteristic Absence of II group
solution dil. HCI and reaction Cu2+
Hydrogen sulphide are
added.
12 III GROUP
(ALUMINIUM, IRON)
To a little of the original No characteristic Absence of III group
solution ammonium reaction Al3+, Fe3+
chloride and ammonium
hydroxide are added.
13 IV GROUP (ZINC,
MANGANESE,
NICKEL, COBALT)
To a little of the original Black ppt. is Presence of IV group
solution ammonium obtained. Zn2+,Mn2+,Co2+,Ni2+
chloride, ammonium
hydroxide and
hydrogen sulphide solution
are added
14 To the original solution Greenish ppt is Presence of nickel is
add NaOH obtained. confirmed. Ni2+
15 To the original solution Red ppt Presence of nickel is
add ammonium hydroxide confirmed. Ni2+
and dimethyl glyoxime

Result: The anion present in the given salt is sulphate (SO 42--) and cation is Nickel
(Ni2+.)

The salt is nickel sulphate(NiSO4).

(Please note below equations for cations and anion to be written on the blank
page of the journal with pencil.)

Equations:
Ni2+

1 Ni2+ + H2S NiS ↓ + 2H+


.
2 Ni2+ + 2NaOH Ni(OH)2 ↓ + 2Na+
.
(green)
3
.

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.

(b) Sublimation No sublimate formed. Ammonium halides, iodide


may be absent.

No crackling sound observed. Lead nitrate, barium nitrate,


(c) Decrepitation sodium chloride, potassium
chloride and potassium
iodide may be absent.
Yellow when hot and white
(d) Colour of the residue Zn2+ may be present.
when cold.

B) Identification of Acidic Radicals


Experiment Observation Inference
2-
KMnO4 Test – Pink colour of KMnO4 was not Cl-, Br,- I-, Fe2+ C2O4
To pinch of salt + dil. H2SO4+ discharged are absent
warm + drop of KMnO4 Soln.
2-
Salt + dil. H2SO4+ warm + Colourless, odourless gas Co3 may be present
Drop of KMnO4 Sol. evolved with brisk effervescence,
turned lime water milky.
C) Confirmatory test for Acidic Radicals

Experiment Observation Inference


2-
1. Salt + dil HCl Brisk effervescence with CO3 is Confirmed
evolution of colourless, odourless
gas
which turned lime water milky.
2-
2. Salt +MgSO4 solution White precipitate CO3 is Confirmed

D) Identification of Basic Radicals


Experiment Observation Inference
O.S. + NaOH No Ammonical Smell Zero group absent
O.S. + dil. HCl No precipitate Group I absent
(Pb2+ absent)
O.S. + dil. HCl + H2S gas No precipitate Group II absent
(Hg2+, Cu2+, As3+
absent).
O.S. +solid NH4Cl +few drops No precipitate Group III absent.
of conc.HNO3 +Boil and cool + (Fe3+, Al3+
excess of NH4OH solution. absent).
O.S. +solid NH4Cl +few drops Dirty white precipitate Group IV present.
of conc. HNO3 +Boil and cool (Zn2+ present)
+ excess of NH4OH
solutio.+H2S
gas

E) Confirmatory test for Basic Radicals


Dissolved the above dull white ppt. in dil HCl. Boiled off H2S. Divide the solution into two
parts.
Experiment Observation Inference
2+
a. To one part +NaOH White ppt. soluble in excess Zn confirmed.
solution dropwise of NaOH.
b.To another part +potassium Bluish white ppt. Zn2+ confirmed.
ferrocyanide solution.

Result – The given salt contains

Acidic Radical – CO32-


Basic Radical – Zn2+
Formula of the salt- ZnCO3
Name of the salt- Zinc Carbonate
Precautions-
1) Use minimum quantity of reagent while preparing
2) For dilution always pour acid into water

=====================================================================
======
S.No. Experiment Observations Inference

Preliminary Tests

I Physical Examination

i.Colour Colourless Absence of


Cu2+,Ni2+,Fe2+,Fe3+,Co2+,
Mn2+
- -
2 ii.Appearance Crystalline May be Cl-, Br-, NO 3 , I ,
CH 3COO except (NH4)2CO3

iii.Solubility

3 Take a pinch of salt in a test tube, Soluble May be


add few ml of water. Cl-,Br-,No3-,I-,CH 3COO -,
except (NH4)2CO3.

Action of Heat

4 Take a small amount of the given No characteristic Absence of


salt taken in a dry test tube, heat changes Zn2+,Co2+,Mn2+,Cu2,Pb2+
it gently; then strongly.

Flame Test:

5 To a small amount of the given Crimson Red Presence of Sr2+


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 No characteristic ash Absence of Al3+, Zn2+,


with Conc.HNO 3 and a few Mg2+,
drops Co(NO 3)2. A filter paper is
dipped in the above mixture
and ignited.

Identification of Anions (Acid Radicals)

Action of dilute H2SO4:


2-
7 To a small portion of the given No Characteristic gas is Absence of S2-, CO 3
salt taken in a test tube add 1 or evolved
2ml of dilute H 2SO4

Concentrated H2SO4 Test: Colourless pungent Presence of Cl-


smelling gas which
8 A pinch of the solid salt heated turns moist blue
with Conc.H2SO4 litmus red and dense
white fumes with a
glass rod dipped in
NH4OH

Manganese dioxide test: (MnO2)

9 Heat a pinch of the salt with a Evolution of greenish Presence of Cl-


small quantity of MnO2 and yellow gas having a
Conc. H2SO4. pungent irritating smell.

Copper Turning Test:


-
10 Heat a pinch of salt with Conc. No Characteristic gas Absence of NO3
H2SO4 and a few copper turning

Chromyl Chloride Test: Reddish orange vapours


evolved were passed
11 Heated a pinch of the salt with through water, Yellow Presence of Cl-
solid K 2Cr2O 7 along with Conc. solution is obtained.
H 2SO 4 Yellow solution turns to
precipitate on adding
Lead acetate

Ammonium molybdate test: No Characteristic


12 Take a pinch of salt add precipitate Absence of PO43-.
Conc.HNO3 and boil. Add
ammonium molybdate
solution in excess and again
boil

Ester Test: No Characteristic


odour
13 Take a small pinch of the salt Absence of CH3COO-
in a 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: No Characteristic gas


+
14 Heated a pinch of salt with Absence of NH 4
Conc. NaOH

CONFIRMATORY TEST FOR ANION

Preparation of Water Extract:

A pinch of salt dissolved in water. This is called water extract.

Confirmatory test for


Cl-: (AgNO3 Test)
1 To a few ml of the water A Curdy white Presence of Cl- is confirmed.
extract added AgNO3 precipitate which is
solution. soluble in excess of
NH4OH

2. Chromyl Chloride Test: Reddish orange


vapours evolved were
Heated a pinch of the salt with passed through water, Presence of Cl- is confirmed
solid K 2Cr2O 7 along with Yellow solution
Conc. H 2SO 4 is obtained. Yellow
solution turns to
precipitate on
adding Lead acetate

Analysis of cations: [Preparation of Original Solution]

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

To a few ml of the original solution No white Absence of Group I


added dil.HCl precipitate
2

To a few ml of the original No black Absence of group II


solution added dil.HCl and passed precipitate.
3 H2S gas.

To a few ml of original solution added No characteristic Absence of group III


NH4Cl(aq) and NH4OH(aq) precipitate
4

5 To a few ml of original solution No characteristic Absence of group IV


added NH4Cl(aq) and NH4OH(aq) precipitate
and passed H2S gas.

6 To a few ml of original solution A white precipitate Presence of group V


added NH4Cl(aq), NH4OH(aq) and (Ba2+/Ca2+/Sr2+)
(NH4)2CO3 solution.

CONFIRMATORY TEST FOR GROUP V : (Sr2+)

1 To a few ml of original solution A White ppt Presence of Sr2+ is


added Ammonium sulphate confirmed
solution and
warm.
2 Flame Test :
To a small amount of the given Crimson red flame Presence of Sr2+ is
salt taken in a watch glass, add a confirmed
drop of Con. HCl and make it
into a paste. Introduce into non-
luminous part of the flame using
a charred match
stick
Result:

The given simple salt contains Anion:


Cl-
Cation: Sr+
The simple salt is SrCl2……….

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