VOLUMETRIC ANALYSIS A (MOHR’S SALT)
Aim: To prepare a 250 ml M/50 solution of Mohr’s salt and with the help
of this solution determine the strength and molarity of the given KMnO4
solution.
Materials required: Burette, weighing tube, beaker, pipette, weighing box,
measuring flask, conical flask, funnel, test tube and weighing balance.
Chemicals required: dil. H2SO4, Mohr’s salt, distilled water, given KMnO4
solution and distilled water.
Theory:
The process of addition of known solution (concentration) to a measured
volume of a substance to be estimated until the reaction between them is
complete is called titration. The titration between Mohr’s salt and KMnO4 is
a redox titration where KMnO4 (acidic medium) acts as oxidizing agent. In
presence of H2SO4 (dil), KMnO4 dissolves ferrous salt to ferric salt and itself
becomes colourless. In this reaction the pink colour of KMnO4 disappears
due to its reduction to Mn2+ state.
The chemical reaction and the molecular chemical equation:
Reduction half reaction –
2KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5[O]
Oxidation half reaction –
[2FeSO4(NH4)2SO4.6H2O + H2SO4 + [O] → Fe2(SO4)3 + 2(NH4)2SO4 + 13H2O] x
5
Overall reaction –
2KMnO4 + 10FeSO4(NH4)2SO4.6H2O+ 8H2SO4 → K2SO4+ 2MnSO4+
5Fe2(SO4)3+ 10(NH4)2SO4+ 68H2O
Solution in burette : KMnO4 (oxidizing agent)
Solution in pipette: Std. solution of M/50 Mohr’s salt acting as reducing
agent.
Indicator: KMnO4 (self indicator)
End point: Colourless to light pink
Observation:
S.No Volume of ferrous Burette Reading Volume(V) Concordent
ammonium sulfate of reading
(Mohr’s salt) used KMnO4 used
(x) (y) V = (y-x)ml
1. 25 ml
2. 25 ml
3. 25 ml
Calculations:
(a) Calculation of the amount of Mohr’s salt used for 250 ml of M/50
solution:
M= WB x 1000/ MB x V(ml)
WB = weight of Mohr’s salt used
MB = molar mass of Mohr’s salt
V = volume of solution
1/50 = WB x 1000/ 392 x 250
WB = 250 x 392 / 50 x 1000
WB = 1.96 gram
(b) Calculation of the molarity of given solution:
M1V1/ x1 = M2 V2/ x2
Where,
• M1, M2 are molarity of Mohr’s salt and KMnO4 solution respectively.
• V1, V2 are volumes of Mohr’s salt and KMnO4 respectively.
M2 = 25 x 2/10 x 50 x V
= _______ mol/litre
(c) Strength of given KMnO4 solution
Strength = M2 x molar mass of KMnO4
= 0.010 x 158
= ______g/l
Results and Discussion:
1. Molarity of given KMnO4 solution is _______moles/liter
2. The strength of given potassium permanganate solution is _____/L
Precautions:
1. Potassium permanganate is dark, so always read the upper meniscus.
2. Rinse the pipette and burette before use.
3. Use dilute sulfuric acid for acidifying the potassium permanganate.
4. Clean all the apparatus with distilled water before starting the
experiment and then rinse with the solution to be taken in them.
5. Take accurate readings once it reaches the endpoint and doesn’t go
with average readings.
6. Do not use a rubber cork burette as it can be attacked by KMnO4.
VOLUMETRIC ANALYSIS B (OXALIC ACID)
Aim: To prepare a standard solution of 250 ml M/50 oxalic acid and with
the help of this solution determine the strength and molarity of the given
KMnO4 solution.
Materials required: Burette, weighing tube, beaker, pipette, weighing box,
measuring flask, conical flask, funnel, test tube and weighing balance.
Chemicals required: dil. H2SO4, oxalic acid, distilled water, given KMnO4
solution and distilled water.
Theory:
In this redox titration MnO4 – ion is the oxidizing agent and C2042- is the
reducing agent. The titration is carried out in acidic medium in which hepta
valant MnO4– ion is reduced to divalent Mn2+ ion which is colourless. Hence
KMnO4. acts as a self-indicator. As long as the reducing agent is present in
the solution it remains colourless. Once all the reducing agent is exhausted
an extra drop of KMnO4 makes the solution light pink. This is the end point.
The chemical reaction is slow at room temperature hence before titration
oxalic acid needs to be heated at 50 to 60◦C.
The chemical reaction and the molecular chemical equation:
Reduction half reaction –
2KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5[O]
Oxidation half reaction –
[H2C2O4 + [O] → 2CO2 + H2O] x 5
Overall reaction –
2KMnO4 +5 H2C2O4 → K2SO4+ 2MnSO4+ 8H2O+10 CO2
Solution in burette : KMnO4 (oxidizing agent)
Solution in pipette: Std. solution of M/50 Mohr’s salt acting as reducing
agent.
Indicator: KMnO4 (self indicator)
End point: Colourless to light pink
OBSERVATION :
Weight of weighing tube = 5.7 grams
Weight of weighing tube + salt = 6.33 grams
Observation:
S.No Volume of ferrous Burette Reading Volume(V) Concordent
ammonium sulfate of reading
(Mohr’s salt) used KMnO4 used
(x) (y) V = (y-x)ml
1. 25 ml
2. 25 ml
3. 25 ml
Calculations:
(a) Calculation of the amount of Oxalic acid used for 250 ml of M/50
solution:
M= WB x 1000/ MB x V(ml)
WB = weight of oxalic acid used
MB = molar mass of oxalic acid
V = volume of solution
1/50 = WB x 1000/ 392 x 250
WB = 250 x 126/ 50 x 1000
WB = 0.63 g
(b) Calculation of the molarity of given solution:
M1V1/ x1 = M2 V2/ x2
Where,
• M1, M2 are molarity of oxalic acid and KMnO4 solution respectively.
• V1, V2 are volumes of oxalic acid and KMnO4 respectively.
• x1 and x2 are stoichiometric coefficient of oxalic acid and KMnO4 in
balance equation respectively.
M2 = 25 x 2/5 x 50 x V
= ______mol/litre
(c) Strength of given KMnO4 solution
Strength = M2 x molar mass of KMnO4
= _______ x 158
= ______ g/l
Results and Discussion:
1. Molarity of given KMnO4 solution is ______moles/liter
2. The strength of given potassium permanganate solution is ______g/L
Precautions:
1. Potassium permanganate is dark, so always read the upper meniscus.
2. Rinse the pipette and burette before use.
3. Use dilute sulfuric acid for acidifying the potassium permanganate.
4. Clean all the apparatus with distilled water before starting the
experiment and then rinse with the solution to be taken in them.
5. Take accurate readings once it reaches the endpoint and doesn’t go
with average readings.
6. Do not use a rubber cork burette as it can be attacked by KMnO4.
SALT ANALYSIS
(Salt A- AMMONIUM BROMIDE)
Aim: To identify one anion and one cation in the given salt sample.
Materials required: Test-tube, test tube holder, test tube stand, dropper,
glass rod and spatula.
Chemicals required: Nessler’s reagent, neutral ferric chloride solution,
ammonium molybdate solution, calcium chloride solution, NaOH and dil.
HCl.
Colour of salt: White
Physical state of salt: Solid
Odour of salt: Odourless
Cation Analysis
Zero group radical- NH4+
Group reagent- NaOH solution
Observation:
S.No. Experiment Observation Inference
1. Test for Anion
Salt + dil. H2SO4 No change C032-,S032-,N02-
,S2-,CH3C00-
absent.
Salt + conc. H2SO4 Reddish brown Br- maybe
fumes
Salt + AgNO3 soln A pale yellow ppt Br- confirmed
partially soluble in
NH4OH
2. Test for cation
Salt + NaOH soln Smell of ammonia NH4+ maybe
detected
A rod dipped in dil. HCl White fumes of NH4+ maybe
is brought near the NH4Cl evolved
mouth of test tube.
Salt soln+ NaOH+ Brown ppt NH4+ confirmed
Nessler’s reagent
Result : Salt contains NH4+ cation and Br- anion.
(Salt B – LEAD ACETATE)
Aim: To identify one anion and one cation in the given salt sample.
Materials required: Test-tube, test tube holder, test tube stand, dropper,
filter paper and spatula.
Chemicals required: dilute H2SO4 , dil. HCl, KI, K2Cr2O4 and FeCl3 soln
Colour of salt: White
Physical state of salt: Solid
Odour of salt: Vinegar like
Cation Analysis
Group 1 radical- Pb2+
Group reagent- dil. HCl
Group ppt: Occurs in form of chloride.
Observation:
S.No. Experiment Observation Inference
1. Test for Anion
i Salt + dil. H2SO4 Vinegar like smell CH3C00-
evolved due to maybe
formation of
CH3COOH
ii Salt + FeCl3 soln Blood red color of CH3C00-
ferric acetate confirmed
Fe(CH3COO)3
obtained.
2. Test for cation
i Salt + NaOH soln No change observed NH4+ absent
ii Salt solution + dil. HCl White ppt formed Pb2+ may be
iii The white ppt is dissolved
in hot water and divided
into two parts
iv To the first part KI A yellow pity of PbI2 Pb2+confirmed
solution is added lead iodide is formed
v To the second part K2Cr04 Orange yellow ppt of Pb2+confirmed
solution is added PbCrO4 is formed
Result : Salt contains Pb2+ cation and CH3C00- anion
(Salt C- CALCIUM CHLORIDE)
Aim: To identify one anion and one cation in the given salt sample.
Materials required: Test-tube, test tube holder, test tube stand, dropper,
filter paper and spatula.
Chemicals required: dil. H2SO4, conc. H2SO4, NH4OH, AgNO3, FeSO4,
diphenylamine, NaOH, dil. HCl, NH4Cl, (NH4)2C2O4, (NH4)2CO3, K2CrO4,
CH3COOH, (NH4)2SO4 and distilled water.
Colour of salt: White
Physical state of salt: Solid
Odour of salt: Odourless
Cation Analysis
Group V radical- Ba2+, Ca2+, Sr2+
Group reagent- (NH4)2CO3 in presence of NH4OH and NH4Cl.
Group ppt- Occur in form of carbonates
Observation:
S.No. Experiment Observation Inference
1. Test for Anion
i Salt + dil. H2SO4 No change C032, S032-,
N02, S2-,
CH3C00-
absent.
ii Salt + conc. H2SO4 Pungent Cl- maybe
smelling gas
was evolved
ii Salt + AgNO3 soln White ppt of Cl- confirmed
AgCl obtained
2. Test for cation
i Salt + NaOH soln No smell of NH4+absent
NH3 evolved
ii Salt soln +dil. HCl No ppt formed Pb2+ absent
iii Salt soln +dil. HCl+H2S No ppt formed Cu2+, As3+
absent
iv Salt soln + dil. HCl+ No ppt formed Fe3+, Al3+
NH4OH+NH4Cl absent
v Salt soln + dil. HCl+ No ppt formed Ni2+, Co2+
NH4OH+NH4Cl+H2S absent
vi Salt soln + dil. HCl+ White ppt was Group V (Ba2+,
NH4OH+NH4Cl+(NH4)2CO3 obtained Ca2+, Sr2+)
present
vii Collect a small amount of ppt
and add CH3COOH, divide it into
three parts
viii Two first part add K2CrO4 No yellow ppt Ba2 + absent
formed
ix Two second part add (NH4)2SO4 No white ppt Sr2 + absent
formed
x Two third part add NH4C204 white ppt was Ca2+ confirmed
obtained
Result : Salt contains Ca2+ cation and Cl-anion
(Salt D-ALUMINIUM SULPHATE)
Aim: To identify one anion and one cation in the given salt sample.
Materials required: Test-tube, test tube holder, test tube stand, dropper,
filter paper and spatula.
Chemicals required: HCl dil., H2SO4 conc., H2SO4 dil.,BaCl2 soln, AgNO3
soln, NH4OH, H2S gas, NH4Cl, litmus soln (blue and red), K4 [Fe(CN)6]
Colour of salt: White
Physical state of salt: Solid
Odour of salt: Odourless
Cation Analysis
3rd group radical- Fe2+ and Al3+
Group reagent- Dilute HCl in presence of NH4OH and NH4Cl
Group ppt- Occur in form of hydroxides
Observation:
S.No. Experiment Observation Inference
1. Test for Anion
i Salt + dil. H2SO4 No change C032-,S032-
,N02-,S2-
,CH3C00-
absent.
ii Salt + conc. H2SO4 No change Cl-, Br- I-, NO3-
absent
iii Salt + BaCl2 soln A white ppt of SO4 2-
BaSO4 is observed confirmed
2. Test for cation
i Salt + NaOH soln No smell of NH4+ absent
ammonia evolved
ii Salt soln +dil. HCl No white ppt Pb2+absent
observed
iii Salt soln +dil. HCl+ H2S gas No change Cu2+, As3+
absent
iv Salt soln + dil. HCl+ White gelatinous Al3+ maybe
NH4OH+NH4Cl ppt is formed
Al(OH)3
v The white ppt is dissolved in Blue ppt is Al3+ confirmed
dil. HCl and few drops of blue suspended in
litmus soln is added to it. colourless
Then NH4OH soln is added in medium(lake)
excess.
Result : Salt contains Al3+ cation and SO4 2-anion
(Salt E-ZINC SULPHATE)
Aim: To identify one anion and one cation in the given salt sample.
Materials required: Test-tube, test tube holder, test tube stand, dropper
and spatula.
Chemicals required: HCl dil., BaCl2 soln, AgNO3 soln, NH4OH, H2S gas,
NH4Cl, litmus soln (blue and red) and K4 [Fe(CN)6]
Colour of salt: White
Physical state of salt: Solid
Odour of salt: Odourless
Cation Analysis
Zero group radical- NH4+
Group reagent- NaOH solution
Observation:
S.No. Experiment Observation Inference
1. Test for Anion
i Salt + dil. H2SO4 No change C032-,S032-
,N02-,S2-
,CH3C00-
absent.
ii Salt + conc. H2SO4 No change Cl-, Br- I-, NO3-
absent
iii Salt + BaCl2 soln A white ppt of SO4 2-
BaSO4 is formed confirmed
which is insoluble
in any mineral acid
2. Test for cation
i Salt + NaOH soln No smell of NH4+ absent
ammonia detected
ii Salt soln +dil. HCl No white ppt Pb2+absent
observed
iii Salt soln + dil. HCl+ No ppt formed Fe3+, Al3+
NH4OH(excess)+NH4Cl absent
iv Salt soln +dil. HCl+ H2S gas No change Cu2+, As3+
absent
v Salt soln + dil. HCl+ Dirty white ppt is Zn2+ maybe
NH4OH+NH4Cl+ H2S gas formed
vi The ppt is dissolved in dil. Bluish white ppt is Zn2+
HCl and K4 [Fe(CN)6] soln is formed confirmed
added to it.
Result : Salt contains Zn2+ cation and SO4 2- anion
SALT + NA2S ---- WHITE PPT
SALT + K4[FE(CN)6] ---- GREENISH PPT
(FUNCTIONAL GROUP A- PHENOLIC GROUP)
Aim: To detect the presence of functional group in each of the given organic
compound.
Materials required: Test-tube, test tube holder, test tube stand, burner,
dropper and spatula.
Chemicals required: CAN (NH4)2[CO(NO3)6], sodium metal, conc. H2SO4,
ethanoic acid, FeCl3 soln, distilled water and blue litmus soln.
Physical state of salt: Liquid
Colour of organic compound: Colourless
Odour of organic compound : Characteristic smell
Observation:
S.No. Experiment Observation Inference
i OC +CAN soln No red color complex Alcoholic group
observed absent
ii Litmus test
OC(2ml) + blue litmus The litmus solution Phenolic group
solution (1ml) turns red may be
iii Ferric chloride test
OC(1ml) + FeCl3 Appearance of violet Phenolic group
solution (1ml) color confirmed
iv Cerric ammonium
nitrate test
OC + CAN solution Brown ppt is formed Phenolic group
confirmed
Result : The given organic compound contains Phenolic functional group.
(FUNCTIONAL GROUP B- KETONE GROUP)
Aim: To detect the presence of functional group in each of the given organic
compound.
Materials required: Test-tube, test tube holder, test tube stand, dropper
and spatula.
Chemicals required: CAN (NH4)2[CO(NO3)6], sodium metal, conc. H2SO4,
FeCl3 soln, distilled water, blue litmus soln, 2,4-DNP soln, sodium
nitroprusside, NaHCO3, NaOH, KI and Iodine soln.
Physical state of salt: Liquid
Colour of organic compound: Colourless
Odour of organic compound : Characteristic smell
Observation:
S.No. Experiment Observation Inference
i OC +CAN soln No red colour Alcoholic
complex observed group absent
ii OC + FeCl3 solution No violet colour Phenolic
appears group absent
iii OC + NaHCO3 No red colour appears Carboxylic
group absent
iv 2,4-DNP Test
(Carbonyl group test)
OC + 2,4-DNP soln An orange-yellow ppt Carbonyl
was formed group present
v Sodium nitroprusside Test
OC(2 ml)+ Sodium Deep wine red colour Ketone group
nitroprusside soln (2ml)+ is observed confirmed
few drops of NaOH
vi Iodoform Test
OC (2 ml) + KI soln (2ml)+ Pale yellow coloured Ketone group
Iodine soln+ NaOH compound i.e., is confirmed
observed
Result : The given organic compound contains Ketonic functional group.
(FUNCTIONAL GROUP C-AMINE GROUP)
Aim: To detect the presence of functional group in each of the given organic
compound.
Materials required: Test-tube, test tube holder, test tube stand, dropper
and spatula.
Chemicals required: CAN (NH4)2[CO(NO3)6], sodium metal, conc. H2SO4,
conc. HCl, CHCl3, FeCl3 soln, distilled water, red litmus soln, 2,4-DNP soln,
sodium nitroprusside, NaHCO3, NaOH, alcoholic KOH, NaNO3 and β-
naphthol.
Physical state of salt: Liquid
Colour of organic compound: Colourless
Odour of organic compound : Characteristic smell
Observation:
S.No. Experiment Observation Inference
i OC +CAN soln No red colour Alcoholic
complex observed group absent
ii OC + FeCl3 solution No violet colour Phenolic
appears group absent
iii OC + NaHCO3 No red colour Carboxylic
appears group absent
iv OC + 2,4-DNP soln No orange-yellow Carbonyl
ppt was formed group absent
v OC + red litmus soln Soln turns blue Amine group
maybe
vi OC( 2 ml)+ conc. HCl(1ml)+ A very unpleasant Amine group
2,4-DNP + few drops of CHCl3 smell evolved confirmed
+alc. KOH (2ml)
vii Azo-dye test
OC( 2 ml)+ conc. HCl+ cold Orange red colour Amine group
soln of NaNO3 + β- naphthol+ is formed confirmed
few drops of NaOH.
Result : The given organic compound contains Amine functional group.
(FUNCTIONAL GROUP D-CARBOXYLIC ACID)
Aim: To detect the presence of functional group in each of the given organic
compound.
Materials required: Test-tube, test tube holder, test tube stand, water bath,
burner, dropper and spatula.
Chemicals required: CAN (NH4)2[CO(NO3)6], ethanol, conc. H2SO4, FeCl3
solution, blue litmus soln and NaHCO3.
Physical state of salt: Liquid
Colour of organic compound: Colourless
Odour of organic compound : Vinegar like smell
Observation:
S.No. Experiment Observation Inference
i OC +CAN soln No red colour Alcoholic
complex observed group absent
ii OC + FeCl3 solution No violet colour Phenolic
appears group absent
iii Litmus Test Blue litmus soln Carboxylic
OC + blue litmus soln turns red group maybe
iv Sodium Bicarbonate test Strong Carboxylic
OC + NaHCO3 effervescence is group
evolved confirmed
v Ester Test Pleasant fruity Carboxylic
OC (1ml) + conc. H2SO4 (1-3 smell evolved group
drops) + methyl alcohol (3ml). confirmed
Heat the content in water bath.
Result : The given organic compound contains Carboxylic functional group.
