Mohr Salt Preparation and Titration Guide
Mohr Salt Preparation and Titration Guide
Experiment No. 1
Preparation Of Ferrous Ammonium Sulphate (Mohr Salt)
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.
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.
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.
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.
Experiment No. 3
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 :
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+.
Observations:
Strength of supplied Mohr salt : 0.05 M = M/20
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
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.
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.
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.
Experiment No. 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
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.
Experiment No. 6
Detection of Functional Group In given Unknown Organic Sample
The given organic sample contains --COOH functional group. It is a carboxylic acid.
Experiment No. 7
Detection of Functional Group In given Unknown Organic Sample
Experiment No. 8
Detection of Functional Group In given Unknown Organic Sample
The given organic sample contains ---C=O (keto) as functional group. It is a ketone.
Experiment No. 9
Detection of Functional Group In given Unknown Organic Sample
Experiment No. 10
Detection of Functional Group In given Unknown Organic Sample
The given organic sample contains ---NH2 (Aromatic) as a functional group. It is a primary aromatic
amine.
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.
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.
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.
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.
[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.
water and flame test was Apple green flame obtained through
performed. open eye.
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 :
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-
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