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Aim: To estimate the amount of Ferrous iron in the whole of the given solution using a standard
solution of Potassium Dichromate.
Principle: Ferrous Iron is oxidized to Ferric iron by Potassium Dichromate in acid solution. The
completion of oxidation reaction is marked by the appearance of Blue violet color of
Diphenylamine, which is used as an internal indicator.
Chemical reactions:
K2Cr2O7 + 4H2SO4 K2SO4 + Cr2(SO4)3 + 4H2 + 3(O)
2FeSO4 + H2SO4 + (O) Fe2(SO4)3 + H2O
K2Cr2O7 = 3(O) = 6Fe
Procedure:
1) Preparation of standard potassium dichromate:
i) Weigh out accurately the given pure crystalline sample of potassium dichromate and
transfer into 100 ml standard (volumetric) flask provided with a funnel.
2) Estimation of Iron:
i) Make up given solution up to the mark with distilled water and shake the flask for
uniform concentration.
ii) Rinse the pipette with the ferrous solution and pipette out 20ml into a clean conical
flask add 20ml of the acid mixture (sulphuric acid and phosphoric acid), and
four to five drop of diphenylamine indicator.
iii) Fill the burette with the prepared potassium dichromate solution after rinsing it,
with the same.
iv) Titrate the solution in the conical flask against the standard potassium dichromate
from the burette till the color changes to blue violet.
Result: Amount of Ferrous iron present in the whole of the given solution (100 ml) =
_______ gm
_______________________________________________________________________
Preparation of Standard (K2Cr2O7) solution:
N= (W1-W2) X 10 / 49 =
Bur Volume of
Volume of the standard
ette consume (V1)
S.No solution(V2)
Readi
ng
Initial Final
1 20 ml
2 20 ml
3 20 ml
V2 = 20 ml
Calculation:
N1 = Normality of K2Cr2O7 solution =
N2 = Normality of Ferrous iron solution = ?
V1 = Volume of K2Cr2O7 solution =
V2 = Volume of Ferrous iron solution = 20 ml
N1 V1= N2 V2
N2 = N 1 V1 / V2
Amount of Ferrous iron present in the whole of the given solution (100 ml) = N2 X 55.85/10
=
Result: Amount of Ferrous iron present in the whole of the given solution (100 ml) =
_______ gm.
Experiment-2
ESTIMATION OF FERRIC IRON
(Redox Titrations)
Aim: To estimate the amount of Ferric iron in the whole of the given solution using a
standard solution of Potassium Dichromate.
Chemicals Required: K2Cr2O7, SnCl2, HgCl2, HCl, Ferric ion solution, H2SO4, Ortho
phosphoric acid, Diphenylamine & distilled water.
Principle: Ferric Iron is reduced to ferrous iron by stannous chloride in the present of
Hydrochloric acid at a temperature of 70-900C.
The ferrous iron formed is titrated with standard Potassium dichromate solution
in the presence of Sulphuric acid and Phosphoric acid using diphenylamine as
indicator.
Chemical reactions:
Procedure:
1) Preparation of standard potassium dichromate:
i) Weigh out accurately the given pure crystalline sample of potassium
dichromate and transfer into 100 ml standard (volumetric) flask provided
with a funnel.
ii) Dissolve the dichromate in a small quantity of distilled water, and make up
to the mark.
iii) The contents in the flask are shaken well for uniform concentration.
iv) Calculate the normality of potassium dichromate.
Result:
Amount of Ferric iron present in the whole of the given solution (100 ml) = ______ gm.
______________________________________________________________________
_____
Preparation of Standard solution:
W1 = Weight of bottle + substance = ____________ gms
W2 = Weight of bottle = ____________ gms
Weight of substance = (W1-W2 ) = ____________ gms.
Normality of the solution (K2Cr2O7) = (W1-W2) X 10/Equivalent Weight=
= (W1-W2) X 10/49=
Bur Volume of
Volume of the standard
ette consume (V1)
S.No solution(V2)
Readi
ng
Initial Final
1 20 ml
2 20 ml
3 20 ml
V2 = 20 ml
Experiment-3
ESTIMATION OF COPPER
(IODOMETRY)
Aim: To estimate the amount of Copper present in the given solution using a standard
solution of Potassium Dichromate and Hypo as the link solution.
Chemicals Required: K2Cr2O7, Hypo (Na2S2O3), KI, Conc.HCl, dil. Acetic acid, NaHCO3,
H2SO4, CuSO4, Ammonia solution, Starch & distilled water.
Principle:
Any cupric salt in neutral medium when treated with Potassium Iodide forms
a white precipitate of cuprous iodide and iodine is set free quantitatively.
The liberated Iodine is treated against Hypo using starch as the indicator.
Chemical reactions:
CuSO4 + 2KI CuI2 + K2 SO4
2CuI2 Cu2I2 + I2
I2 + 2Na2S2O3 +O2 Na2S2O6 + 2NaI
2CuSO4 = I2 = Na2S2O3
Procedure:
3. Estimation of copper:
i. Make up the given solution of copper to 100 ml with distilled water and
shake well for uniform concentration.
ii. Pipette out 20 ml of this solution into a clean conical flask.
iii. Add few drops of ammonia when bluish white precipitate is obtained.
iv. Redissolve the precipitate in dilute acetic acid. Now add 10 ml of 5% KI,
when iodine is liberated giving a brown colour.
v. Titrate this solution against standard hypo solution till light yellow colour is
obtained.
vi. Now add 2 ml of starch solution and continue the titration till blue colour
changes to creamy white, which is the end point.
vii. Repeat the titration for concurrent values and calculate the amount of
copper.
______________________________________________________________________
_____
Preparation of Standard solution:
W1 = Weight of bottle + substance = ____________ gms
W2 = Weight of bottle = ____________ gms
Weight of substance = (W1-W2 ) = ____________ gms.
Normality of the solution = (W1-W2) X 10/Equivalent Weight =
= (W1-W2) X 10/49=
Bur Volume of
Volume of the standard
ette consume (V2)
S.No K2Cr2O7 solution (V1)
Readi
ng
Initial Final
1 20 ml
2 20 ml
3 20 ml
V1 = V2 =
Bur Volume of
Volume of the Copper
ette consume (V4)
S.No solution (V3)
Readi
ng
Initial Final
1 20 ml
2 20 ml
3 20 ml
V3 = 20ml V4 =
Amount of Copper present in the whole of the given solution (100 ml) = N3 X 63.54/10
Result: Amount of Copper present in the whole of the given solution (100 ml) = ______ gm.
Experiment-4
ESTIMATION OF CALCIUM HARDNESS OF WATER
(COMPLEXOMETRY)
Aim: To estimate the Calcium hardness of the given solution using a standard solution of
EDTA.
Principle:
Hard water which contains calcium and magnesium ions forms a wine red
colored complex with the indicator, Eriochrome Black-T.
Ethylene diamine tetra acetic acid (EDTA) forms a colourless stable complex
with free metal ion like Ca, Mg.
i.e., Metal + Indicator Metal indicator complex (wine red colour)
When EDTA is added from the burette, it extracts the metal ions from the metal
ion-indicator complex thereby releasing the free indicator. (The stability of
metal ion-indicator complex is less than that of the metal ion- EDTA complex,
and hence EDTA extracts metal ion form the ionindicator complex.)
Procedure:
1. Preparation of standard solution of EDTA:
i. Weigh out accurately about 0.3722 gms of EDTA sample into
a 100ml standard flask and dissolve in a minimum quantity of
distilled water.
ii. Make up the solution upto the mark with distilled water and shake
the flask well for uniform concentration.
Result: The calcium hardness of the given water sample = _________ ppm.
______________________________________________________________________
_____
Preparation of Standard solution:
W1 = Weight of bottle + substance = ____________ gms
W2 = Weight of bottle = ____________ gms
Weight of substance = (W1-W2) = ____________ gms.
Molarity of the solution = (W1-W2) X 10 / 372.24 =
Bur Volume of
Volume of the Copper
ette consume (V1)
S.No solution (V2)
Readi
ng
Initial Final
1 20 ml
2 20 ml
3 20 ml
V2 = 20ml V1 =
Calculations:
M1 = Molarity of EDTA =
V1 = volume of EDTA solution =
M2 = Molarity of calium solution = ?
V2 = Volume of Calcium solution = 20 ml
M1V1 = M2V2
M2 = Molarity of calium solution = M1V1/V2
Calcium hardness of the given sample water = M2 X 100 X 1000
Calcium hardness of the given sample water = M2 X V1 X100 X 1000/V2
Result: The calcium hardness of the given water sample _________ ppm.
Experiment-5
ESTIMATION OF COPPER BY EDTA
(COMPLEXOMETRY)
Aim: To estimate the Copper in the given solution by preparing a standard solution of
EDTA.
Principle:
Fast sulphone Black-F indicator is specific in its reaction with copper in
ammonia solution, it forms red complex with copper.
In the titration of copper in ammonical solution the colour changes at the end
point from pale blue to bright green depend upon the concentration of Cu++ ions.
Procedure:
Bur Volume of
Volume of the standard
ette consume (V1)
S.No solution (V2)
Readi
ng
Initial Final
1 20 ml
2 20 ml
3 20 ml
V2 = 20ml V1 =
Calculation:
M1 = Molarity of EDTA =
V1 = volume of EDTA solution =
M2 = Molarity of copper solution = ?
V2 = Volume of Copper solution = 20 ml
M1V1 = M2V2
M2 = Molarity of copper solution = M1V1/V2
Experiment-6
ESTIMATION OF FERROCYANIDE
(PRECIPITATION TITRATIONS)
Aim: To estimate the amount of Potassium Ferrocyanide in the given solution by preparing a
standard solution of Zinc.
Principle:
Zinc ions in neutral or acid medium reacts with Potassium Ferrocyanide solution
form sparingly soluble potassium zinc Ferro cyanide.
Biphenyl benzidine is used as indicator. At the end point the colour of the solution changes
from Blue violet to pale green.
Procedure:
1. Preparation of Standard Zinc solution:
i. Weigh out the given zinc oxide into a 100 ml standard flask,
dissolve it in 10 ml of diluted sulphuric acid and make upto the
mark with distilled water and shake the flask well for uniform
concentration.
2. Standardisation of Potassium Ferrocyanide:
i. Make up the given potassium Ferro-cynidesolution with
distilled water and shake the flask well for uniform
concentration.
ii. Rinse the pipette zinc oxide solution and pipette out 20 ml of
zinc solution into 250 ml conical flask; add 20 ml of distilled
water, 20 ml of 7N H2SO4, and 8 grams of ammonium sulphate
and 3-4 drops of diphenyl benzidine indicator.
iii. Titrate the solution slowly, with vigorous shaking against
potassium ferro-cynide until the colour changes from blue
violet to green.
iv. Repeat the titration to get concurrent values.
Bur Volume of
Volume of the standard
ette consume (V2)
S.No solution (V1)
Readi
ng
Initial Final
1 20 ml 0 ml
2 20 ml
3 20 ml
V1 = 20ml V2 =
M1 = Molarity of Zinc oxide solution =
V1 = volume of Zinc oxide solution = 20 ml
M2 = Molarity of Potassium ferrocyanide solution = ?
V2 = Volume of Potassium ferrocyanide solution =
n1, n2 indicates number of molecules involved in the reaction
n1= 3, n2= 2
Calculation:
M2 = M1V1 n2/V2 n1 =
M2 =
Experiment-7
DETERMINATION OF PERCENTAGE PURITY OF PYROLUSITE
(ANALYSIS OF MINERALS AND ORES)
Aim: To estimate the amount of MnO2 present in the given sample and hence percentage
purity of Pyrolusite.
Principle:
The MnO2 present in the pyrolusite sample is reduced by a known excess of
standard sodium oxalate in acid medium.
The unreacted sodium oxalate is titrated against a standard KMnO4, until pale pink
coloured end point is obtained.
Procedure:
i. Weigh out accurately the given powdered pyrolusite sample into
a clean dry conical flask and pipette out 40 ml of standard sodium
oxalate solution and add 50 ml of 4N (H2SO4) sulphuric acid, put a
small funnel into the mouth of the conical flask.
ii. Heat with small flame till particles are MnO2 disappear in the conical
flask.
iii. Rinse the funnel with distilled water into the conical flask, titrate the
hot solution, containing the unreacted sodium oxalate with standard
KMnO4 solution till there is a pale pink colour.
Calculations:
Titer value = V =
Blank =
1 ml of 1N KMnO4 = 1N Na2C2O2 = 0.04346 g of MnO2
Percentage of MnO2 =
Note: Blank from the instructor i.e., 20 ml of oxalate equivalent to permanganate of certain
normality.
Experiment-8
PERCENTAGE PURITY OF LIME-STONE
(ANALYSIS OF MINERALS AND ORES)
Aim: To determine percentage purity of the sample of Lime stone (estimation of Calcium).
Principle:
The given Lime stone sample is weighed out into a beaker and dissolved in HCl.
Procedure:
i. Weigh out accurately the given Lime stone sample into a 400
ml beaker, add 10 ml of distilled water, then add 10 ml of dilute
Hydrochloric acid along the sides of the beaker and completely
dissolve the lime-stone sample.
ii. Add 4 to 5 drops of methyl red indicator, heat the solution to boiling
add about 25 ml of 10% solution of ammonium oxalate solution with
constant stirring.
iii. To the hot solution add 1:1 Ammonium hydroxide drop wise with
stirring until the solution is neutral (Red to Yellow).
iv. Allow the solution to stand for 30 minutes on water bath.
v. Test for complete precipitation and decant clear supernatant liquid
through a Whatman No. 40 filter paper and quantitatively transfer the
precipitate to the filter paper.
vi. Wash the precipitate on filter paper repeatedly until the washings are
free from oxalate/chlorides.
vii. Transfer the precipitate present on the filter paper into a 400 ml
beaker, add 25 to 30 ml dilute suphuric acid, warm the solution and
titrate with standard permanganate solution to a pale pink colour end-
point.
Bur Volume of
Volume of the standard
ette consume (V)
S.No solution
Readi
ng
Initial Final
1 20 ml 0 ml
2 20 ml
3 20 ml
V=
Calculations:
Titer value = V =
Amount of calcium present in the sample = Titer value (V) X Normality KMnO4 X 0.2004 =
Result:
Amount of calcium present in the sample =
Percentage purity of the given sample of Limestone = %
Experiment-9
ESTIMATION OF MANGANESE IN STEEL
(Colorimetric Estimation)
Aim: To estimate the percentage of Manganese present in a sample of mild steel
calorimetrically.
Principle:
The given steel sample is dissolved in nitric acid. Manganese (II) is oxidized
to permanganic acid by heating with lead peroxide and conc. Nitric acid.
The intensity of the permanganic acid is measured in the colorimeter and the
amount of manganese is estimated.
Procedure:
1. Dissolution of the steel sample:
i. Weight out about 0.5 grams (500 mg) of the given steel sample
into a clean 250 ml conical flask and add about 30 ml of 1:3
nitric acid heat to boiling, till the sample goes into solution.
ii. Boil gently for about 10 to 15 minutes, to oxidize any carbon
present, cool and transfer into a clean 100 ml standard flask.
iii. Wash the conical flask twice with about 10 ml portions of
distilled water and transfer into the standard flask.
iv. Make up the solution upto the mark with distilled water and
shake well for uniform concentration.
2. Development of Colour:
i. Transfer 20 ml of the prepared solution into a clean conical
flask add about 10ml of syrupy phosphoric acid and about 20
ml of 1:3 nitric acid and heat the solution to boiling.
ii. Add two spatulas of lead peroxide and continue the boiling for
about 5 minutes.
iii. Take out the flask from the stand and allow it to cool and settle.
iv. Decant the supernatant liquid into a 100 ml standard flask,
wash the precipitate twice with little distilled water and collect
the supernatant liquid and the washings into the standard flask
and make up the solution with distilled water and shake well
uniform concentration.
v. Transfer about 10 ml of the solution into a clean centrifuge
tube and centrifuge the solution to separate out any lead
peroxide particles.
vi. Measure the optical density in the colorimeter and calculate the
amount of Manganese from the standard calibration curve.
Experiment-10
ESTIMATION OF FERRIC IRON IN CEMENT
(Colorometric Estimation)
Aim: To estimate the amount of Iron (Ferric) present in a sample of cement by
calorimetrically using ammonium thiocyanate as a reagent.
Principle:
Ammonium thio-cyanate yields a blood red colour with ferric iron and the
colour produced is stable in nitric acid medium. Its optical density is measured
in a photo colorimeter and the concentration of ferric iron is found from a
standard calibration curve.
Procedure:
i. Weight out accurately about 0.1 gram of the cement sample into
a clean 250 ml beaker add about 5 ml of water to moisten the
sample.
ii. Place a glass rod and cover the beaker with a watch glass add
about 5 ml conc.
iii. Hydrochloric acid (HCl) dropwise and heat the solution till the
sample dissolved.
iv. Keep the beaker on a small flame and evaporate the solution to
almost dryness to expel the excess acid.
2. Development of Colour:
Concentration in Milligrams O. D
0.5 0.11
0.10 0.22
0.15 0.32
0.20 0.40
0.25 0.50
0.30 0.62
0.35 0.70
0.40 0.80
X = corresponding amount of from the calibration curve =
Calculation:
Percentage of Fe3+ present in the given cement sample = X x 10 x 100 / (W1 W2) mg