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Mohr Salt Preparation and Titration Guide

1. The document describes procedures for preparing and standardizing solutions of ferrous ammonium sulfate (Mohr's salt) and potassium permanganate. 2. Key preparations include making 250mL 0.05M solutions of Mohr's salt and oxalic acid, and determining the molarity of potassium permanganate by titrating against the standard Mohr's salt or oxalic acid solutions. 3. The document provides theoretical background on the redox reactions taking place during titration and calculations for determining the molarity of potassium permanganate from the titration results.

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Suyash Chauhan
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0% found this document useful (0 votes)
594 views26 pages

Mohr Salt Preparation and Titration Guide

1. The document describes procedures for preparing and standardizing solutions of ferrous ammonium sulfate (Mohr's salt) and potassium permanganate. 2. Key preparations include making 250mL 0.05M solutions of Mohr's salt and oxalic acid, and determining the molarity of potassium permanganate by titrating against the standard Mohr's salt or oxalic acid solutions. 3. The document provides theoretical background on the redox reactions taking place during titration and calculations for determining the molarity of potassium permanganate from the titration results.

Uploaded by

Suyash Chauhan
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

1

Experiment No. 1
Preparation Of Ferrous Ammonium Sulphate (Mohr Salt)

Aim : To Preparare Ferrous Ammonium Sulphate (Mohr Salt)


Materials Required:
Beaker, Conical flask(250ml), Funnel, Glass rod, Tripod Stand, Bunsen Burner

Chemical Required :
Ferrous Sulphate, Ammonium Sulphate, Dilute H2SO4, Distilled water

Theory: When a mixture containing equimolar proportions of ferrous sulphate and ammonium sulphate
is crystallised from its solution, a double salt is formed. The formation of double salt may be
shown as follows:
FeSO4 + (NH4)2 SO4 + 6H2O → FeSO4 . (NH4)2 SO4 . 6H2O
Ferrous ammonium sulphate (Mohr’s salt)
Fe2+ and ions undergo hydrolysis, therefore, while preparing aqueous solutions of ferrous sulphate in
water, 2-3 mL dilute sulphuric acid is added to prevent the hydrolysis of these salts.

Procedure :
 Dissolve 3.5 g of ferrous sulphate and 1.7 g of ammonium sulphate (weighed separately), in 5 mL of
distilled water contained in a 50 mL conical flask by heating.
 Add about 5 mL of dilute sulphuric acid to the flask and concentrate the solution by heating till the
crystallization point is reached.
 Allow the mixture to cool to room temperature slowly.
 On cooling, light green crystals of ferrous ammonium sulphate separate out.
 Decant the mother liquor and wash the crystals by shaking with very small amounts of 1:1 cold water
and alcohol mixture to remove sticking mother liquor.
 Separate the crystals by filtration wash with alcohol, dry between the folds of a filter paper and record
the yield.

Result : Yield of potash alum/Mohr’s salt is 3.8 g.

Precaution:
 Cool the solution slowly to get good crystals. Avoid rapid cooling.
 Do not disturb the solution while cooling.
 Avoid prolonged heating while preparing crystals of ferrous ammonium sulphate, as it may oxidise
ferrous ions to ferric ions and change the stoichiometry of the crystals.

Krishnendu Barik, PGT Chemistry


2

Experiment No. 2
Preparation Of 250 ml M/20 Ferrous Ammonium Sulphate (Mohr Salt)
Solution

Aim : To Prepare 250 ml M/20 Ferrous Ammonium Sulphate (Mohr Salt) Solution
Materials Required:
Volumetric flask (250ml), Funnel, Electronic Balance.

Chemical Required :
Mohr salt , Dilute H2SO4, Distilled water

Theory :
Molecular mass of Mohr salt = 392 g/mole
𝑀𝑎𝑠𝑠 𝑜𝑓 𝑆𝑢𝑏𝑠𝑡𝑎𝑛𝑐𝑒
Molarity (M) = 𝑀𝑜𝑙𝑎𝑟 𝑀𝑎𝑠𝑠 𝑜𝑓 𝑠𝑢𝑏𝑠𝑡𝑎𝑛𝑐𝑒 𝑥 𝑉𝑜𝑙𝑢𝑚𝑒
Mass of Substance (W) = Molarity x Molar Mass of Substance x Volume
Mass of Substance (W) = 0.05 x 392 x 0.25 = 4.9 g
4.9 gm of Mohr salt is to be dissolved in distilled water so that net volume of solution is 250 ml.

Procedure :

i. Weigh 4.9 g of ferrous ammonium sulphate and transfer it into a 250 mL measuring flask through a
funnel.
ii. Transfer the solid sticking to the funnel with the help of distilled water into the flask and add dilute
H2SO4 into the flask drop wise to get the clear solution.
iii. Shake the flask till the substance dissolves and make the solution upto the mark.

Result : 250 ml M/20 Mohr salt solution prepared.

Precaution :
Shake the flask continuously while adding distilled water so that the solution becomes homogenous.
Add some dilute H2SO4 to avoid hydrolysis of Mohr salt.
Avoid parallax error while making solution upto the mark.

Krishnendu Barik, PGT Chemistry


3

Experiment No. 3

Titration of KMnO4 with Mohr Salt


Aim : To determine the strength of supplied solution of KMnO4 solution by titrating against
the standard M/20 Mohr salt solution.
Required Apparatus :
Conical flask(250ml), Beaker, Burette(50ml), Pipette(20ml), Test tube, Funnel, Burette stand, Glazed tile
Chemicals Required :
Ferrous Ammonium Sulphate Solution, KMnO4 solution, 2M H2SO4, Distilled water.

Theory:
Ferrous (Fe2+) ions present in the ferrous ammonium sulphate solution are readily oxidised by
permenganate ions in acidic medium according to the chemical reaction :

2KMnO4 + 8H2SO4 + 10FeSO4.(NH4)2SO4.6H2O → K2SO4 + 2MnSO4 + 5Fe2(SO4)3 + 10(NH4)2SO4 +


68H2O

Ionic Reaction :
MnO4- + 5Fe2+ + 8H+ → Mn2+ + 4H2O + 5Fe3+
As the reaction proceeds MnO4- gets reduced to Mn2+ and hence pink color disappears and Fe2+ gets
oxidised to Fe3+.

Indicator : KMnO4 a self indicator.


Change at end point : Colorless to pink.
Procedure
 Rinse and fill the clean burette with potassium permanganate solution. Remove air bubbles if any, from
the burette tip by releasing some solution through it.
 Take 20 mL of 0.05 M ferrous ammonium sulphate solution in a conical flask and add 10ml of 1.0 M
H2SO4 to it.
 Titrate the above solution with potassium permanganate solution till the colour of the solution changes
to permanent pink. Swirl the content of the flask during the titration.
 Repeat the titration, until three concordant readings are obtained.
 Record the readings as shown in observation and calculate the strength of potassium permanganate
solution in mols/litre.

Observations:
Strength of supplied Mohr salt : 0.05 M = M/20

Sl. Volume Of Burette Reading Volume Of Concordant


No. Mohr Salt Initial Reading Final reading KMnO4 Volume
ml
1 20 ml 0 9.5 9.5
2 20 ml 0 9.4 9.4 9.4 ml
3 20 ml 0 9.4 9.4

Krishnendu Barik, PGT Chemistry


4

Calculations :
5 moles of Mohr salt is completely oxidised by 1 mole of KMnO4.
Strength of unknown KMnO4 Solution in molarity is given by
(M1× V1)/ (M2×V2) = n1/n2 Strength of unknown KMnO4 = M1
M1 = (M2 × V2 × n1 )/n2×V1 Volume of unknown KMnO4 = V1 = 9.4 ml
M1 = (M × 20× 1 )/(5×9.4 x20) Strength of Mohr Salt = M2 = M/20
M1 = M/ 47 = 0.021 M Volume of Mohr salt = V2 = 20 ml
No. of moles of KMnO4 = n1=1
No. of moles of Mohr Salt = n2=5

Molarity of Unknown KMnO4 = 0.021 M


Strength of KMnO4 = Molarity of KMnO4 × Molecular mass of KMnO4
= 0.021 x 158 = 3.16 g/L

Results :
Molarity of Unknown KMnO4 =0.021mol/lt
Strength of KMnO4 = 3.16 g/lt.

Precaution :
Always rinse the burette and the pipette with the solutions to be taken in them.
Never rinse the conical flask with experimental solutions.
Remove the air gaps from the burette.
Always use freshly prepared FeSO4 solution.

Krishnendu Barik, PGT Chemistry


5

Experiment No. 4
Preparation Of 250 ml M/20 Oxalic Acid Solution
Aim : To Prepare 250 ml M/20 Oxalic Acid (Mohr Salt) Solution
Materials Required:
Volumetric flask (250ml), Funnel, Electronic Balance.

Chemical Required :
Oxalic Acid , Distilled water

Theory :
Molecular mass of Mohr salt = 126 g/mole
𝑀𝑎𝑠𝑠 𝑜𝑓 𝑆𝑢𝑏𝑠𝑡𝑎𝑛𝑐𝑒
Molarity (M) = 𝑀𝑜𝑙𝑎𝑟 𝑀𝑎𝑠𝑠 𝑜𝑓 𝑠𝑢𝑏𝑠𝑡𝑎𝑛𝑐𝑒 𝑥 𝑉𝑜𝑙𝑢𝑚𝑒
Mass of Substance (W) = Molarity x Molar Mass of Substance x Volume
Mass of Substance (W) = 0.05 x 126 x 0.25 = 1.575g
1.575 gm of Oxalic Acid is to be dissolved in distilled water so that net volume of solution is 250 ml.

Procedure :

Weigh 1.575 g of oxalic acid and transfer it into a 250 mL measuring flask through a funnel.
Transfer the solid sticking to the funnel with the help of distilled water into the flask to get the clear solution.
Shake the flask till the substance dissolves and make the solution upto the mark.

Result : 250 ml M/20 Oxalic Acid solution prepared.

Precaution :
Shake the flask continuously while adding distilled water so that the solution becomes homogenous.
Add some dilute H2SO4 to avoid hydrolysis of Mohr salt.
Avoid parallax error while making solution upto the mark.

Krishnendu Barik, PGT Chemistry


6

Experiment No. 5

Titration of KMnO4 with Oxalic Acid Solution


Aim : To determine the strength of supplied solution of KMnO4 solution by titrating against
the standard M/20 Mohr salt solution.
Required Apparatus :
Conical flask(250ml), Beaker, Burette(50ml), Pipette(20ml), Test tube, Funnel, Burette stand, Glazed tile
Chemicals Required :
Oxalic Acid Solution, KMnO4 solution, 2M H2SO4, Distilled water.
Theory:
Oxalic acid solution are readily oxidised by permenganate ions according to the chemical reaction :
2KMnO4 + 3H2SO4 + 5H2C2O4⎯ → K2SO4 + 2MnSO4 + 8H2O + 10 CO2
Ionic Reaction : 2 MnO4- + 5C2O42– + 16H+ ⎯→2Mn2+ + 10CO2 + 8H2O
As the reaction proceeds MnO4- gets reduced to Mn2+ and hence pink color disappears and C2O42– gets
oxidised to CO2.
Indicator : KMnO4 a self indicator.
Change at end point : Colorless to pink.
Procedure
 Rinse and fill the clean burette with potassium permanganate solution. Remove air bubbles if any, from
the burette tip by releasing some solution through it.
 Take 20 mL of 0.05 M oxalic acid solution in a conical flask and heat it to 60oC.
 Titrate the above solution with potassium permanganate solution till the colour of the solution changes
to permanent pink. Swirl the content of the flask during the titration.
 Repeat the titration, until three concordant readings are obtained.
 Record the readings as shown in observation and calculate the strength of potassium permanganate
solution in mols/litre.
Observations:
Strength of supplied Oxalic Acid : 0.05 M = M/20

Sl. Volume Of Burette Reading Volume Of Concordant


No. Mohr Salt Initial Reading Final reading KMnO4 Volume
ml
1 20 ml 0 18.6 18.6
2 20 ml 0 18.6 18.6 18.6 ml
3 20 ml 0 18.5 18.5

Calculations :
5 moles of Oxalic Acid is completely oxidised by 2 mole of KMnO4.
Strength of unknown KMnO4 Solution in molarity is given by
(M1× V1)/ (M2×V2) = n1/n2 Strength of unknown KMnO4 = M1
M1 = (M2 × V2 × n1 )/n2×V1 Volume of unknown KMnO4 = V1 = 18.6 ml
M1 = (M × 20× 2 )/(5×18.6 x 20) Strength of Oxalic Acid solution = M2 = M/20
M1 = M/ 47.5 = 0.021 M Volume of Oxalic Acid = V2 = 20 ml
No. of moles of KMnO4 = n1=2
No. of moles of Mohr Salt = n2=5
Krishnendu Barik, PGT Chemistry
7

Molarity of Unknown KMnO4 = 0.021 M


Strength of KMnO4 = Molarity of KMnO4 × Molecular mass of KMnO4
= 0.021 x 158 = 3.16 g/L

Results :
Molarity of Unknown KMnO4 =0.021mol/lt
Strength of KMnO4 = 3.16 g/lt.

Precaution :
Always rinse the burette and the pipette with the solutions to be taken in them.
Never rinse the conical flask with experimental solutions.
Remove the air gaps from the burette.
Do not boil the solution.

Krishnendu Barik, PGT Chemistry


8

Experiment No. 6
Detection of Functional Group In given Unknown Organic Sample

Aim : To detect the Functional Group In given Unknown Organic Sample.


Sample NO : 1
PHYSICAL PROPERTIES :
Colour : Colourless
State : Liquid
Odour : Smell of Vinegar.

EXPERIMENT OBSERVATION INFERENCE


1. The sample was dissolved Unsaturation is not present in
in acetone and a KMnO4 Pink colour does not the sample.
solution is added to it disappear.
dropwise.
2. The sample was dissolved Compound may contain
in water and treated with blue Litmus paper changes to red. --OH (Phenolic) or --COOH
litmus paper. group.
3. To the sample solution few --OH (Phenolic) is absent.
drops of neutral FeCl3 was No change in colour.
added.
[Link] pinch of sodium Brisk effervescence evolved --COOH group is present
bicarbonate to the sample and confirmed.
taken in a test tube.
5. To the small amount of the Fruity smell evolved. --COOH group is present
sample taken in a test tube is and confirmed.
ethanol and few drops of
conc.H2SO4 is added and
heated.
[Link] the small amount of the No precipitation. Carbonyl group is absent.
sample 2,4 DNP solution is
added along with few drop is
added and shaken.
[Link] the solution is acidic
test for primary amine is not
performed.

The given organic sample contains --COOH functional group. It is a carboxylic acid.

Krishnendu Barik, PGT Chemistry


9

Experiment No. 7
Detection of Functional Group In given Unknown Organic Sample

Aim : To detect the Functional Group In given Unknown Organic Sample.


Sample NO : 2
PHYSICAL PROPERTIES :
Colour : Pinkish.
State : Liquid.
Odour : Carbolic odour.
EXPERIMENT OBSERVATION INFERENCE
1. The sample was dissolved Unsaturation is not present in
in acetone and alkaline Pink colour changes. the sample.
KMnO4 solution is added to
it dropwise.
2. The sample was dissolved Compound may contain
in water and treated with blue Litmus paper changes to red. --OH (Phenolic) or --COOH
litmus paper. group.
3. To the sample solution few --OH (Phenolic) is present
drops of neutral FeCl3 was Violet colour. and confirmed
added.
[Link] pinch of sodium No brisk effervescence --COOH group is absent.
bicarbonate to the sample evolved
taken in a test tube.
5. To the small amount of the Fruity smell does not --COOH group is absent.
sample taken in a test tube is evolved.
ethanol and few drops of
conc.H2SO4 is added and
heated.
[Link] the small amount of the No precipitation. Carbonyl group is absent.
sample 2,4 DNP solution is
added along with few drop is
added and shaken.
[Link] the solution is acidic
test for primary amine is not
performed.

The given organic sample contains --OH (Phenolic) functional group.

Krishnendu Barik, PGT Chemistry


10

Experiment No. 8
Detection of Functional Group In given Unknown Organic Sample

Aim : To detect the Functional Group In given Unknown Organic Sample.


Sample NO : 3
PHYSICAL PROPERTIES :
Colour : Colourless.
State : Liquid.
Odour : Pleasant Smell.
EXPERIMENT OBSERVATION INFERENCE
1. The sample was dissolved
in acetone and alkaline Pink colour does not Un saturation is not present
KMnO4 solution is added disappear. in the sample.
drop wise to it.
2. The sample was dissolved --OH (Phenolic) or --COOH
in water and treated with blue No change in group is absent.
litmus paper. colour.
3. To the sample solution few --OH (Phenolic) is absent
drops of neutral FeCl3 was No change in colour
added.
[Link] pinch of sodium No Brisk effervescence --COOH group is absent.
bicarbonate to the sample evolved
taken in a test tube.
[Link] the small amount of the Yellow precipitation. Carbonyl group is present
sample 2,4 DNP solution is and confirmed.
added along with few drop is
added and shaken.
[Link] amount of sample is
treated with Tollens' reagent No grey precipitation. --CHO group is absent.
and heated in water bath.
[Link] amount of sample is
treated with Fehlings reagent No red precipitate. --CHO group is absent.
and heated in water bath.
[Link] test with Tollen's
reagent is negative the
compound contains keto
group.

The given organic sample contains ---C=O (keto) as functional group. It is a ketone.

Krishnendu Barik, PGT Chemistry


11

Experiment No. 9
Detection of Functional Group In given Unknown Organic Sample

Aim : To detect the Functional Group In given Unknown Organic Sample.


PHYSICAL PROPERTIES :
Colour : Colourless.
State : Liquid.
Odour :
EXPERIMENT OBSERVATION INFERENCE
1. The sample was dissolved
in acetone and alkaline Pink colour does not Un saturation is not present
KMnO4 solution is added disappear. in the sample.
drop wise to it.
2. The sample was dissolved --OH (Phenolic) or --COOH
in water and treated with blue No change in group is absent.
litmus paper. colour.
3. To the sample solution few --OH (Phenolic) is absent
drops of neutral FeCl3 was No change in colour
added.
[Link] pinch of sodium No Brisk effervescence --COOH group is absent.
bicarbonate to the sample evolved
taken in a test tube.
The sample was dissolved in --NH2 group is absent.
water and treated with red No change in
litmus paper. colour.
[Link] the small amount of the Yellow precipitation. Carbonyl group is present
sample 2,4 DNP solution is and confirmed.
added along with few drop is
added and shaken.
[Link] amount of sample is Grey precipitation. --CHO group is absent.
treated with Tollens' reagent
and heated in water bath.

The given organic sample contains ---CHO as a functional group. It is an aldehyde.

Krishnendu Barik, PGT Chemistry


12

Experiment No. 10
Detection of Functional Group In given Unknown Organic Sample

Aim : To detect the Functional Group In given Unknown Organic Sample.


PHYSICAL PROPERTIES :
Colour : Reddish brown
State : Liquid.
Odour : Unpleasant Smell
EXPERIMENT OBSERVATION INFERENCE
1. The sample was dissolved
in acetone and alkaline Pink colour does not Un saturation is not present
KMnO4 solution is added disappear. in the sample.
drop wise to it.
2. The sample was dissolved --OH (Phenolic) or --COOH
in water and treated with blue No change in group is absent.
litmus paper. colour.
3. To the sample solution few
drops of neutral FeCl3 was Change in colour Since the sample does not
added. respond to litmus test
phenolic -OH is absent.
[Link] pinch of sodium No Brisk effervescence --COOH group is absent.
bicarbonate to the sample evolved
taken in a test tube.
[Link] sample was dissolved --NH2 group may be present.
in water and treated with red Red litmus turns blue.
litmus paper.
[Link] amount of the --NH2 (aromatic) group
sample is dissolved in dilute Orange red dye formed. present and confirmed.
HCl and cooled to ice
followed by addition of
NaNO2 solution. this solution
is then added to a test tube
containing alkaline solution
of 2 naphthol.
[Link] the small amount of the No precipitation. Carbonyl group is absent.
sample 2,4 DNP solution is
added along with few drop is
added and shaken.

The given organic sample contains ---NH2 (Aromatic) as a functional group. It is a primary aromatic
amine.

Krishnendu Barik, PGT Chemistry


13

Experiment No. 11
Analysis of Acid and Basic radical in given inorganic salt.
Aim : To detect Acid and Basic Radical In given Unknown Inorganic Sample.

SAMPLE 1
Experiment Observation Inference
1. PHYSICAL EXAMINATION
Colour of the sample is noted White colour Cu2+,Fe2+,Fe3+,Ni2+, Mn2+,Co2+
are absent
A little amount of the sample is Pungent smell evolved NH4+ may be present
rubbed between thumb and
finger.
[Link] Test Tube Heating : Pungent gas evolved along NH4+ ,Cl- may be present
Heated small amount of the with formation of white
sample in a dry test tube. sublimate
[Link] test was performed. No characteristic colour in Ca2+,Sr2+,Ba2+and Cu2+ may be
the flame absent.
[Link] activity test was No characteristic bead but Pb2+, Cu2+,Zn2+,As3+ may be
performed. white incrustation around absent and NH4+ may be present.
the edge of cavity.
[Link] being white in colour Borax bead test was not performed.
[Link] amount of the sample is Effervescence with S2-, NO2-,may be absent.
treated with dilute H2SO4 and evolution of colourless, CO32- may be present.
and pass the gas through lime odourless gas
water
[Link] amount of the solid Colourless and odourless NO3-, Cl-, Br- may be absent.
sample is treated with gas evolved with CO32- may be present.
concentrated H2SO4. effervescence.
Confirmatory test for acid radicals :
[Link] amount of the solid Effervescence with CO32- is present and
sample is treated with Dilute evolution of colourless, confirmed.
H2SO4 and the evolved gas is odourless gas which turns
passed through lime water. lime water milky.
Preparation of aqueous extract :
Aqueous extract of the sample was prepared and following test for acid radical was
performed.
9. Small amount of the sample is Lime water turns milky and CO32- is present and
treated with dilute H2SO4 and milkiness disappears on confirmed.
and pass the gas through lime passing excess lime water.
water
10. To the aqueous solution of White precipitate was CO32- is present and confirmed
sample MgSO4 solution was formed
added.
[Link] the solution with No precipitate formed. Cl - is absent.
dilute HNO3 and AgNO3
solution was added.

Krishnendu Barik, PGT Chemistry


14

[Link] the solution with No precipitate formed. SO42- is absent.


dilute HCl and BaCl2 solution
was added.
[Link] prepared FeSO4 No brown ring was formed. NO3- was absent.
solution is added to the sample
solution and 2ml of conc.H2SO4
was added carefully along the
wall of the container.
[Link] the solution with No precipitate is produced. PO43- is absent.
conc. HNO3 and a pinch of
ammonium molybdate was
added to it.
Confirmatory test for basic
radicals :
15. Heated the solid sample with Colourless gas with pungent NH4+ (Group 0) may be
NaOH solution in a test tube. smell evolves. present.
Following test was performed
with the evolved gas:
16.A glass rod dipped in HCl White dense fumes NH4+ (Group 0)is present and
was brought near the mouth of produced confirmed.
the test tube.
17.A cotton plug dipped in Plug turns reddish brown NH4+ (Group 0) is present and
Nessler's reagent brought at the confirmed.
mouth of the test tube.
Since NH4+ (Group 0) is present and confirmed analysis for other Group is not done.

The given salt contains :


 Basic Radical : NH4+

Acid Radical : CO32-

Krishnendu Barik, PGT Chemistry


15

Experiment No. 12
Analysis of Acid and Basic radical in given inorganic salt.
Aim : To detect Acid and Basic Radical In given Unknown Inorganic Sample.
SAMPLE 2
Experiment Observation Inference
1. PHYSICAL EXAMINATION
Colour of the sample is noted White colour Cu2+,Fe2+,Fe3+,Ni2+, Mn2+,Co2+
are absent
A little amount of the sample is No pungent smell evolved NH4+, S2- may be absent
rubbed between thumb and
finger.
[Link] Test Tube Heating : Formation of white sublimate NH4+ may be present
Heated small amount of the
sample in a dry test tube.
[Link] test was performed. No characteristic colour in the Ca2+,Sr2+,Ba2+and Cu2+ may be
flame absent.
[Link] activity test was No characteristic bead but white Pb2+, Cu2+,Zn2+,As3+ may be
performed. incrustation around the edge of absent and NH4+ may be
cavity. present.
[Link] being white in colour Borax bead test was not performed.
[Link] amount of the sample is No gas evolves S2-, NO2-, CO32- may be absent.
treated with dilute H2SO4 .
[Link] amount of the solid Pungent smelling gas evolved . Cl- may be present
sample is treated with It gives dense white fumes with
concentrated H2SO4. rod dipped in NH4OH.
8. Heated a pinch of mixture Greenish yellow gas with Cl- may be present
with conc. H2SO4 and MnO2 pungent smell evolves.
Confirmatory test for acid radicals :
Preparation of aqueous extract :
Aqueous extract of the sample was prepared and following test for acid radical was performed.
9. To the aqueous solution of No precipitate was formed CO32- is absent
sample MgSO4 solution was
added.
[Link] the solution with Curdy White precipitate Cl - is present and confirmed.
dilute HNO3 and AgNO3 formed which dissoved in
solution was added. excess NH4OH
[Link] the solution with No precipitate formed. SO42- is absent.
dilute HCl and BaCl2 solution
was added.
[Link] prepared FeSO4 No brown ring was formed. NO3- was absent.
solution is added to the sample
solution and 2ml of conc.H2SO4
was added carefully along the
wall of the container.
Confirmatory test for basic radicals :
13. Heated the solid sample with Colourless gas with pungent NH4+ (Group 0) may be
NaOH solution in a test tube. smell evolves. present.

Krishnendu Barik, PGT Chemistry


16

Following test was performed


with the evolved gas:
14.A glass rod dipped in HCl White dense fumes produced NH4+ (Group 0)is present and
was brought near the mouth of confirmed.
the test tube.
15.A cotton plug dipped in Plug turns reddish brown NH4+ (Group 0) is present
Nessler's reagent brought at the and confirmed.
mouth of the test tube.
Since NH4+ (Group 0) is
present and confirmed analysis
for other Group is not done.

The given salt contains:


Basic Radical : NH4+
Acid Radical : Cl-

Krishnendu Barik, PGT Chemistry


17

Experiment No. 13
Analysis of Acid and Basic radical in given inorganic salt.
Aim : To detect Acid and Basic Radical In given Unknown Inorganic Sample.
Sample 3
Experiment Observation Inference
1. PHYSICAL EXAMINATION:
Colour of the sample is noted White colour Cu2+,Fe2+,Fe3+,Ni2+, Mn2+,Co2+
are absent
A little amount of the sample No characteristic smell. NH4+, S2- may be absent.
is rubbed between thumb and
finger.
[Link] Test Tube Heating : No gas evolves. NH4+ , S2- ,NO2-, NO3-,Cl- may
Heated small amount of the be absent.
sample in a dry test tube. No formation of white
sublimate. NH4+ may be absent.

Cracking sound does not PbNO3 or Ba(NO3)2 may be


occurs. absent.

No change in colour of residue. Cu2+, Zn2+ , Mn2+ Fe3+ may be


absent.
3. Flame test was performed. No characteristic colour in the Ca2+,Sr2+,Ba2+and Cu2+ may be
flame absent.
4. Charcoal activity test was No characteristic bead but white Pb2+, Cu2+,Zn2+,As3+ may be
performed. incrustation around the edge of absent and NH4+ may be
cavity. present.
5. Sample being white in colour Borax bead test was not performed.
6. Small amount of the sample No specific reaction takes place. S2-, NO2-, CO32- may be absent.
is treated with dilute H2SO4 .
7. Small amount of the solid No specific reaction takes place. NO3-,Cl-, Br- , I- ,CO32- may be
sample is treated with absent.
concentrated H2SO4.
Confirmatory test for acid radicals :
Preparation of aqueous extract :
Aqueous extract of the sample was prepared and following test for acid radical was performed.
[Link] the aqueous solution of No precipitate was formed. CO32- may be absent.
sample MgSO4 solution was
added.
[Link] the solution with No precipitate formed. Cl - is absent.
dilute HNO3 and AgNO3 solution
was added.
[Link] the solution with White precipitate formed SO42- is present and
dilute HCl and BaCl2 solution was which is insoluble in HCl & confirmed.
added. HNO3 .
11. Acidified the solution with White precipitate formed SO42- is present and
acetic acid and lead acetate was soluble in excess hot confirmed.
added to it. ammonium acetate solution,

Krishnendu Barik, PGT Chemistry


18

Experiment Observation Inference


[Link] prepared FeSO4 No brown ring was formed. -
NO3 was absent.
solution is added to the sample
solution and 2ml of conc.H2SO4
was added carefully along the
wall of the container.
Confirmatory test for basic radicals :
13. Heated the solid sample with No specific reaction takes NH4+ (Group 0) is absent.
NaOH solution in a test tube. place.
Following test was performed
with the evolved gas:
14. No specific reaction takes NH4+ (Group 0) is absent.
(i)A cotton plug dipped in place.
Nessler's reagent brought at the
mouth of the test tube.
(ii) A glass rod dipped in HCl No specific reaction takes NH4+ (Group 0) is absent.
was brought near the mouth of the place.
test tube.
Preparation of aqueous extract :
Aqueous extract of the sample was prepared and following test for basic radical was performed.
15. Dilute HCl is added to the No precipitate . Gr I radicals , Pb2+ is absent
sample solution.
16. Dilute HCl is added to the No precipitate. Group II radicals , Pb2+,
sample solution and H2S gas is Cu2+,Hg2+,Cd2+,As3+ is
passed. absent.
17. To the Aqueous solution of White precipitate Group III radicals,Al3+ may
the sample taken in a test tube be present.
NH4Cl was added and made Fe3+, Fe2+ is absent.
alkaline with NH4OH.
The solution is filtered and the
filtrate is preserved for Group IV.
With the residue analysis for
Group III is proceeded.
[Link] of Group III :
The white precipitate formed in
test no.18 is dissolved by boiling
with NaOH solution.
With this solution following test
were performed:
(i) Added NH4Cl to one part of White gelatinous precipitate Al3+ is present and confirmed
the solution and boiled formed
(ii) Another portion of the
solution is acidified with dil. HCl Al3+ is present and confirmed
and added few drops of blue Blue precipitate floating in
litmus followed by ammonia. colourless solution.
3+
Since Al is present analysis for other Group is not done.
The given salt contains :
Basic Radical : Al3+ Acid Radical : SO42-
Krishnendu Barik, PGT Chemistry
19

Experiment No. 14
Analysis of Acid and Basic radical in given inorganic salt.
Aim : To detect Acid and Basic Radical In given Unknown Inorganic Sample.
Sample 4
Experiment Observation Inference
1. PHYSICAL
EXAMINATION : White colour Cu2+,Fe2+,Fe3+,Ni2+, Mn2+,Co2+
Colour of the sample is noted are absent
A little amount of the sample is No characteristic smell. NH4+ , S2- may be absent.
rubbed between thumb and
finger.
2. Dry Test Tube Heating : Pungent gas evolved. NH4+ ,Cl- may be present.
Heated small amount of the
sample in a dry test tube. No change of colour of the salt. Cu2+,Fe2+Zn2+,Cd2+,Co2+ are
absent
[Link] test was performed. Apple green colour appeared observed Ba2+ may be absent.
with unaided eye.
[Link] activity test was No characteristic bead. Pb2+, Cu2+,Zn2+,As3+, NH4+
performed. may be absent
[Link] being white in colour Borax bead test was not performed.
[Link] amount of the sample No specific reaction takes place. S2-, NO2-, CO32- may be absent.
is treated with dilute H2SO4 .
[Link] amount of the solid Colourless gas with pungent smell Cl- may be present.
sample is treated with evolved . It gives dense white fumes
concentrated H2SO4. with rod dipped in NH4OH.
8. Heated a pinch of mixture Greenish yellow gas with pungent Cl- may be present
with conc. H2SO4 and MnO2 smell evolves.
Confirmatory test for acid radicals :
Preparation of aqueous extract ::
Aqueous extract of the sample was prepared with distilled water and following test for acid radical was
performed
[Link] the aqueous solution of No precipitate. CO32- is absent.
sample MgSO4 solution was
added.
[Link] the solution with Curdy white precipitate formed Cl - is present and confirmed.
dilute HNO3 and AgNO3 solution which is soluble in excess NH4OH.
was added.
[Link] a pinch of solid sample The solution turned yellow.
with K2Cr2O7 in a test tube. The
evolved reddish gas is passed
through NaOH solution.
The yellow solution is acidified Cl - is present and confirmed.
with acetic acid and few drops of
lead acetate is added. Yellow precipitate formed
12. Acidified the solution with No precipitate formed. SO42- is absent.
dilute HCl and BaCl2 solution was
added.

Krishnendu Barik, PGT Chemistry


20

[Link] prepared FeSO4 No brown ring was formed. NO3- was absent.
solution is added to the sample
solution and 2ml of conc.H2SO4
was added carefully along the
wall of the container.
Confirmatory test for basic radicals :
14. Heated the solid sample with No specific reaction takes place. NH4+ (Group 0) may be
NaOH solution in a test tube. absent.
Following test was performed
with the evolved gas:
15.(i)A cotton plug dipped in No specific reaction takes place. NH4+ (Group 0) may be
Nessler's reagent brought at the absent.
mouth of the test tube. No specific reaction takes place.
(ii) A glass rod dipped in HCl
was brought near the mouth of the NH4+ (Group 0) may be absent.
test tube.
Preparation of aqueous extract : :
Aqueous extract of the sample was prepared and following test for basic radical was performed.
16. Dilute HCl is added to the No precipitate Gr I radicals , Pb2+ is absent
sample solution.
17. Dilute HCl is added to the No precipitate Group II radicals , Pb2+,
sample solution and H2S gas is Cu2+,Hg2+,Cd2+,As3+ is absent
passed.
18. To the Aqueous solution of No precipitate Group III radicals,Fe3+,Al3+ is
the sample taken in a test tube absent.
NH4Cl was added and made
alkaline with NH4OH.
19. To the Aqueous solution of No precipitate Group IV radicals, Co2+,
the sample taken in a test tube Ni2+,Mn2+,Zn2+are absent.
NH4Cl was added and made
alkaline with [Link] H2S
gas is passed.
[Link] NH4Cl to the aqueous White precipitate formed. Group V radicals,
solution of the sample and made Ca2+,Ba2+,Sr2+ may be present.
alkaline with NH4OH and then
(NH4)2CO3 was added.
The solution is filtered and the
filtrate is preserved for Group VI.
With the residue analysis for
Group V is proceeded.

21. Analysis of Group V :


The white precipitate is washed
with hot water and dissolved in
minimum amount of hot dilute
acetic acid.
K2CrO4 is added to the warm
solution. Yellow precipitate formed Ba2+ is present and confirmed.
The yellow solution is filtered and
the residue is washed with hot Ba2+ is present and
confirmed.
Krishnendu Barik, PGT Chemistry
21

water and flame test was Apple green flame obtained through
performed. open eye.

With the filtrate following tests


were performed : Sr2+ is absent.
(i) Ammonium Sulphate was
added to a small portion of the No precipitate.
filtrate.
Ca2+ is absent.
(ii) Ammonium oxalate solution
was added to the one portion of No precipitate
the filtrate.
Since Ba2+ is present analysis for
Group VI radical is not done.

The given salt contains:


Basic Radical : Ba2+
Acid Radical : Cl -

Krishnendu Barik, PGT Chemistry


22

Experiment No. 15
Analysis of Acid and Basic radical in given inorganic salt.
Aim : To detect Acid and Basic Radical In given Unknown Inorganic Sample.
SAMPLE 5
Experiment Observation Inference
1. PHYSICAL EXAMINATION :
Colour of the sample is noted White colour Cu2+,Fe2+,Fe3+,Ni2+, Mn2+,Co2+ are
absent
A little amount of the sample is No characteristic smell. NH4+ , S2- may be absent.
rubbed between thumb and finger.

[Link] Test Tube Heating : Smell of vinegar obtained. CH3COO- group may be present.
Heated small amount of the
sample in a dry test tube.
[Link] test was performed. Bluish white flame. Pb2+ may be present.
[Link] being white in colour Borax bead test was not performed.
[Link] amount of the sample is Vinegar like smell. CH3COO- may be present.
treated with dilute H2SO4 . White ppt. formed.
6. Small amount of the solid No gas evolves. CO32-, Cl-, NO3- may be absent.
sample is treated with Only white ppt. formed.
concentrated H2SO4.
Confirmatory test for acid radicals :
Preparation of aqueous extract :
Aqueous extract of the sample was prepared and following test for acid radical was performed.
[Link] the aqueous solution of No precipitate was formed. CO32- may be absent.
sample MgSO4 solution was
added.
8 .Acidified the solution with No precipitate formed. Cl - is absent.
dilute HNO3 and AgNO3 solution
was added.
9. Acidified the solution with No precipitate formed. SO42- is absent.
dilute HCl and BaCl2 solution was
added.
10.A pinch of sample is rubbed Smell of vinegar, CH3COO- is present and
with oxalic acid and rubbed. confirmed.
[Link] solution mixed with Red colouration.
FeCl3 and mixture divided into
two parts.
(i) Dilute HCl added to one Red colour disappears CH3COO- is present and
portion. confirmed.
(ii) Another part is boiled with Red colour obtained
water.
Confirmatory test for basic radicals :

Experiment Observation Inference

Krishnendu Barik, PGT Chemistry


23

13. Heated the solid sample with No specific reaction takes NH4+ (Group 0) is absent.
NaOH solution in a test tube. place.
Following test was performed
with the evolved gas:
14. No specific reaction takes NH4+ (Group 0) is absent.
(i)A cotton plug dipped in place.
Nessler's reagent brought at the
mouth of the test tube.
(ii) A glass rod dipped in HCl was No specific reaction takes NH4+ (Group 0) is absent.
brought near the mouth of the test place.
tube.
Preparation of aqueous extract :
Aqueous extract of the sample was prepared and following test for basic radical was performed.
15. Dilute HCl is added to the White precipitate . Gr I radicals , Pb2+ may be present.
aqueous extract.
The solution is filtered and the
filtrate is preserved for analysis of
other Group.
With the residue analysis for
Group I is proceeded'
[Link] residue of Group I is
dissolved in hot water and with
the solution following test was
performed : Pb2+ is present and confirmed.
(i) Added K2CrO4 solution to one Yellow precipitate formed.
part of the solution. Pb2+ is present and confirmed
(ii) Added KI solution to another Yellow precipitate obtained.
portion of the solution.
Since Pb2+ is present analysis for other radical is not done.
The given salt contains :
Basic Radical : Pb2+
Acid Radical : CH3COO-

Krishnendu Barik, PGT Chemistry


24

Experiment No. 16
Analysis of Acid and Basic radical in given inorganic salt.
Aim : To detect Acid and Basic Radical In given Unknown Inorganic Sample.
SAMPLE 5
Experiment Observation Inference
1. PHYSICAL EXAMINATION :
Colour of the sample is noted White colour Cu2+,Fe2+,Fe3+,Ni2+, Mn2+,Co2+ are
absent
A little amount of the sample is No characteristic smell. NH4+ , S2- may be absent.
rubbed between thumb and finger.

[Link] Test Tube Heating : Cracking sound is obtained PbNO3 may be present.
Heated small amount of the
sample in a dry test tube.
[Link] test was performed. Bluish white flame. Pb2+ may be present.
[Link] being white in colour Borax bead test was not performed.
5. Small amount of the sample is No specific observation CO32-, S2- may be absent.
treated with dilute H2SO4 .
6. Small amount of the solid No gas evolves. CO32-, Cl-, NO3- may be absent.
sample is treated with Only white ppt. formed.
concentrated H2SO4.
7. Small amount of the solid Brown fume evolves NO3- may be present.
sample is treated with
concentrated H2SO4 in presence
of Cu turning.
Confirmatory test for acid radicals :
Preparation of aqueous extract :
Aqueous extract of the sample was prepared and following test for acid radical was performed.
[Link] the aqueous solution of No precipitate was formed. CO32- may be absent.
sample MgSO4 solution was
added.
8 .Acidified the solution with No precipitate formed. Cl - is absent.
dilute HNO3 and AgNO3 solution
was added.
9. Acidified the solution with No precipitate formed. SO42- is absent.
dilute HCl and BaCl2 solution was
added.
10. Aqueous solution of sample is Brown Ring was formed. NO3- is present and confirmed.
diluted with equal volume of
freshly prepared FeSO4 and a
small amount of concn. H2SO4
was added to it.
Confirmatory test for basic radicals :
Experiment Observation Inference
13. Heated the solid sample with No specific reaction takes +
NH4 (Group 0) is absent.
NaOH solution in a test tube. place.
Following test was performed
with the evolved gas:
Krishnendu Barik, PGT Chemistry
25

14. No specific reaction takes NH4+ (Group 0) is absent.


(i)A cotton plug dipped in place.
Nessler's reagent brought at the
mouth of the test tube.
(ii) A glass rod dipped in HCl was No specific reaction takes NH4+ (Group 0) is absent.
brought near the mouth of the test place.
tube.
Preparation of aqueous extract :
Aqueous extract of the sample was prepared and following test for basic radical was performed.
15. Dilute HCl is added to the White precipitate . Gr I radicals , Pb2+ may be present.
aqueous extract.
The solution is filtered and the
filtrate is preserved for analysis of
other Group.
With the residue analysis for
Group I is proceeded'
[Link] residue of Group I is
dissolved in hot water and with
the solution following test was
performed : Pb2+ is present and confirmed.
(i) Added K2CrO4 solution to one Yellow precipitate formed.
part of the solution. Pb2+ is present and confirmed
(ii) Added KI solution to another Yellow precipitate obtained.
portion of the solution.
Since Pb2+ is present analysis for other radical is not done.
The given salt contains :
Basic Radical : Pb2+
Acid Radical : NO3-.

Krishnendu Barik, PGT Chemistry


26

Krishnendu Barik, PGT Chemistry

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