Technical Analysis Lab Manual 2016-2017

CH6411 – Technical Analysis Lab 2016-17
CH6411 - TECHNICAL ANALYSIS LAB
INDEX
Exp. Date Name of the Experiments Page Faculty
No No Initial
1 1
Estimation of Total Fatty Matter Content
2 3
Estimation of Total Alkali Content
3 5
Estimation of Acid Value ( Analysis of Oil)
4 8
Estimation of Saponification Value(Analysis of Oil)
5 10
Estimation of Iodine Value (Analysis of Oil)
6 14
Estimation of Silica Content (Analysis of Cement)
7 15
Estimation of Mixed Oxide Content(Analysis of Cement)
8 Estimation of Calcium Oxide Content(Analysis of 17
Cement)
9 Estimate the Proximate Analysis of the Given Sample of 19
Coal
10 21
Estimation of Available Chlorine (Bleaching Powder)
11 25
Estimation of Purity of Glycerol by Dichromate Method
Estimation of Flash and Fire Point of the Given Sample
12 29
(Pensky Martens Closed Cup Method)
13 Cleveland Open Cup Apparatus for Flash and Fire Point 30
Determine the Viscosity of the Given oil (Saybolt

14 33
Viscometer)
Determine the Viscosity of the Given oil (Redwood
15 37
Viscometer)
Determine the Calorific Value of the given sample (Bomb
16 41
Calorimeter)
Beyond the Syllabus
17 Estimation of COD of the Given Sample of Wastewater 48
18 Estimation of Glucose (Bertrand’s Method) 51
Department of Chemical Engineering, SSN College of Engineering, Chennai 1

Expt. No :
Date :
1) Estimation of Total Fatty Matter Content
Aim:
To analyze the sample of the given soap and to determine the total fatty matter content
Apparatus Required:
Grinding bowl, Beaker, Stirrer, Glass plate, Conical flask, Pipette, Burette, Standard flask,
Separating funnel, Water bath, Electric Bunsen Burner, Funnel, Desiccator, China dish.
Chemicals Required:
Given sample of soap, Water, Chloroform, Sodium carbonate, 0.5 N HNO3
Procedure:
• Weigh 5 gm of soap accurately and transfer into 250 ml beaker
• Add 100 ml hot water to completely dissolve the soap.
• Add 40 ml of 0.5 N HNO3 until contents were slightly acidic.
• Heat the mixture over water bath until the fatty acids were floating as a layer above the
• solution.
• Transfer about 5 gm of paraffin wax (to be exactly weighed) to the contents and continue
heating over water bath until the fatty acids and molten paraffin wax mix thoroughly and
rise to the top as separate layer.
• Then cool the mixture suddenly ice water in order to solidify the tip layer containing fatty
acids and paraffin wax.
• Separate the solid cake through filtration. Remove excess water by pressing the cake
between the folds of filter paper.
• Dry the cake in a pre weighed china dish in a hot air oven, cool it in a desiccators and
weigh.
• From the difference in weight, calculate the % of fatty matter in the given soap sample.

Calculation:
Weight of the soap sample (w1) = _____________ (g)

Weight of paraffin wax (w2) = _____________ (g)
Weight of china dish (x) = ______________ (g)
Weight of china dish + Cake after drying (y) = ______________ (g)
Weight of dry solid cake = Weight of fatty acids + Paraffin wax
= w3 = (y-x) g
Weigh to fatty acids present in the given sample of soap = (w3- w2)g
% of fatty mater = (w3– w2) * 100

Weight of soap sample
% of fatty matter = ___________.
Result:
The percentage of total fatty matter present in the given sample of soap was found to
be_________.

Expt. No :
Date :
2) Estimation of Total Alkali Content
Aim:
To analyze the given soap sample and to determine the total alkali content
Apparatus Required:
Beaker, Stirrer, Glass plate, conical flask, Pipette, Burette, Standard flask, separating funnel.
Chemicals Required:
Given sample of soap, Diethyl Ether, Sodium Chloride, 100 g/l aqueous solution, Sulphuric acid,
1N aqueous solution, Sodium Hydroxide, 1N aqueous solution, Methyl orange indicator.
Procedure:
• Weigh about 5 gm of soap.

• Add 100 ml distilled water.
• Gently heat until complete dissolution.
• Transfer quantitatively to a separating funnel.
• Add few drops of methyl orange indicator
• Add 10 ml of H2SO4 until solution becomes pink.
• Allow to cool at room temperature.
• Add 100 ml diethyl ether.
• Shake vigorously for one minute.
• Allow to stand still two phases are completely separated.
• Take the bottom of the aqueous solution layer into a second separating funnel.
• Carry out the second extraction of the acid solution by shaking with diethyl ether.
• Take the aqueous acid solution into a conical flask. Wash twice with 50 ml of 1N Sodium
chloride solution by shaking for a minute.
• Titrate the resulting conical flask solution with Sodium hydroxide.
• The total alkali content, expressed as a percentage (m/M), is given by the formula:
 m  4[V1T1 − V2T2 ]
% =
m m

Calculation:
Volume of H2SO4 solution (V1) = ____ml

Volume of NaOH solution (V2) = _____ml
Normality of H2SO4 (T1) = _____N
Normality of NaOH (T2) = _____N
Mass of Soap (M) = ____g
% Alkali content = (Mass of alkali / Mass of soap ) x 100
= (W/M) x 100
= [(V1 T1 - V2 T2) x 4] /M
Result:
The total alkali content of the given soap sample was found to be___________.

Expt. No :
Date :
3) Estimation of Acid Value (Analysis of Oil)
Aim:
To calculate the number of milligrams of potassium hydroxide required to neutralize the free fatty
acid in 5 gm of oil.
Theory:
Acid value indicates the proportion of free fatty acid present in an oil or fat and may be defined as
the number of milligrams of caustic potash required to neutralize the acid in 1 gm of the sample.
The normal acid value for most samples lies within 0.5. If any titrable acid other than a fatty acid
is present in the sample, it will be an error. A high acid value indicates a stale oil or fat stored
under improper conditions.
Procedure:
Standardization of KOH:
• Take 20 ml of 0.1 N oxalic acid solution in a 250 ml conical flask.

• Add 1 or 2 drops of phenolphthalein indicator to this solution.
• Titrate this solution against KOH taken in a burette.
• The appearance of pink color indicates the end point.
• From the volume of the KOH solution in burette, find the normality of KOH.
Experimental Procedure:
• Weigh 5 gm of oil and transfer it into 250 ml conical flask.

• Add 50 ml of neutralized alcohol solution to the oil solution.
• Heat this mixture for 10 minutes by using the heater.
• Take the solution after 10 minutes and add 1 or 2 drops of phenolphthalein indicator.
• Titrate this against the KOH solution from the burette.
• The appearance of pink color indicates the end point.

Tabular Column:
Titration I: Standardization of Potassium hydroxide

Burette solution : KOH
Pipette solution : Oxalic acid
Indicator : Phenolphthalein
End point : Appearance of pink colour
Volume of Oxalic Burette Reading (ml) Volume of KOH Concordant

S.No
Acid (ml) Initial Final Consumed (ml) Value (ml)
1
2
Calculation:
Volume of oxalic acid (V1) =
Normality of oxalic acid (N1) =
Volume of KOH consumed (V2) =
Normality of KOH consumed (N2) = V1 N1 / V2
Normality of KOH (N2) = _______________.

Titration II: Estimation of acid value

Burette solution : KOH
Pipette solution : Oil + 50 ml of neutralized alcohol
End point : Appearance of pink colour
Weight of Oil Burette Reading (ml) Volume of KOH Concordant

S.No
(gm) Initial Final (ml) Value (ml)
1
2
ml of KOH × Normality of KOH × Eq.wt of KOH

Acid value =
Weight of Oil Sample
Equivalent weight of KOH = 56.11
Acid Value = __________.
Result:
The acid value of the given oil sample was found to be___________.

Expt. No :
Date :
4) Estimation of Saponification Value (Analysis of Oil)
Aim:
To calculate the number of milligrams of potassium hydroxide required to completely saponify 1

gm of Oil.
Theory:
Saponification value indicates the average molecular weight of a fat or oil. The saponification
value may be defined as the number of milligrams of caustic potash required to neutralize the fatty
acids obtained by complete hydrolysis of one gram of oil or fat. Thus saponification value gives us
information whether an oil or fat contains high proportion of lower or higher fatty acids. For eg.,
butter has a large proportion of lower fatty acids than lard and tallow, and has high saponification
value. Coconut oil also has a comparatively higher saponification value.
Applications of saponification value:
Saponification value gives us an idea about the molecular weight of fat or oil.
Oil x Saponification Value = Amount of Lye needed to make soap.
Procedure:
• Weigh 1 gm of oil and transfer into the 250 ml round bottomed flask.
• Add 20 ml of 0.5 N alcoholic KOH solution to the round bottomed flask.
• Follow the above procedure without taking oil for blank titration.
• Reflux both round bottomed flasks for 1 hour.
• After reflux, allow both the round bottomed flasks to cool.
• Titrate both the samples using 0.5 N HCl with phenolphthalein indicator.
• The disappearance of pink indicates the end point.

Tabular Column:
Titration : Estimation of saponification value
Burette solution : HCl

Flask solution : 20 ml of Alcoholic KOH (with and without oil)
End point : disappearance of pink colour
S.NO Weight of Oil Volume of Alcoholic Burette Reading (ml) Volume of

Taken KOH solution Initial Final HCl
(g) (ml) ((ml)
2 Blank
(Without Oil)
Calculation:
Saponification Value
= (Titre value of blank in ml – Titre value of sample in ml) x NKOH x Equivalent wt of KOH
Weight of the sample
Saponification value = _________________
Result:
The Saponification value of the given oil sample was found to be_____________.

Expt. No :
Date :
5) Estimation of Iodine Value (Analysis of Oil)
Aim:
To determine the amount of unsaturation present in the given oil. (To determine the iodine value
of oil)
Principle:
The Iodine number is defined as the number of grams of iodine which will add to 100 grams of fat
or oil. Iodine value shows the degree of unsaturation of the constituent fatty acids in an oil or fat
and is thus a relative measure of the unsaturated bonds present in the oil or fat. Iodine value is
expressed in grams of iodine absorbed by 100 gms of oil or fat. Unsaturated compounds absorb
iodine (in suitable form) and form saturated compounds. The amount of iodine absorbed in
percentage is the measure of unsaturation in the oil. No oil has zero iodine value and oils are
classified as drying, semi drying and non drying on the basis of iodine value. Oleic acid containing
1 double bond absorbs 90% of iodine, linoleic acid (2 double bonds) absorbs 181% iodine and
linolenic acid (3 double bonds) absorbs 274% iodine. Non drying oils have 1 double bond and
absorbs iodine below 90%. Semi drying oils contain some proportion of double bonds and have
iodine value below 140.Iodine value for coconut oil is 8, for olive 88, for human fat 105, for
linseed about 200.
Chemicals Required:
Wij’s Solution:
Dissolve separately 7.5 gm of AR Iodine tetrachloride and 8.5 gm of resublimed iodine in glacial
acetic acid by warming on a water bath. Mix the two solutions and dilute to 1 litre with glacial
acetic acid in cold.
Potassium iodide solution ( 15%)
Dissolve 15 gm of AR potassium iodide in 100 ml of water.

Sodium thiosulphate solution (0.1 N)
Dissolve 25 gm of AR sodium thiosulphate crystals ( Na2S2O3 5H2O) in a 1 litre of distilled water.
Starch indicator solution : 1 ml of starch in 100 ml boiling water.
Procedure:
Standardization of Sodium Thiosulphate Solution
• Pipette out 20 ml of 0.1 N potassium dichromate solution into a clean conical flask.
• Add 1 test tube of dilute H2SO4 and 10 ml of 15% KI solution to the conical flask.
• Titrate against thiosulphate from the burette until it turned into pale yellow.
• Add 1 ml of starch indicator and titrate against thiosulphate solution.
• End point is disappearance of blue color.
Experimental Procedure:
• Weigh 0.5 gm of oil and transfer into 250ml Iodine flask.

• Add 10 ml of chloroform and warm slightly and cool for 10 minutes
• Add 25 ml of Wij’s solution in the same flask and shake vigorously.
• Then allow the flask to stand for half an hour in dark place.
• Add 10 ml of KI solution and after that titrate the solution against 0.1 N Sodium
thiosulphate solution until the appearance of yellow color.
• Add 1 ml of starch indicator and again titrate against the sodium thiosulphate solution from
the burette.
• Disappearance of blue color indicates end point.
• Repeat the above procedure without taking sample(ie Oil) and note the corresponding
reading for blank titration.

Tabular Column:
Titration I
Standardisation of Sodium thiosulphate:
Burette solution : Sodium thiosulphate
Pipette solution : Potassium dichromate
Additional solution : 10 ml of dil H2SO4 solution + 10 ml KI solution
Indicator : Starch
End point : Disappearance of blue colour
Volume of Burette Reading Volume of Sodium Concordant Value

S.No K2Cr2O7 (ml) Thiosulphate Solution (ml)
Solution (ml) Initial Final (ml)
1
Calculation:
Volume of K2Cr2O7 ( V1) =

Normality of K2Cr2O7 (N1) =
Volume of sodium thiosulphate solution (V2) =
Normality of sodium thiosulphate solution ( N2) = (V1 x N2) / V2

Titration II
Estimation of Iodine value:
Burette solution : Std. Sodium thiosulphate solution
Pipette solution : 0.5 g of Oil + 10 ml of Chloroform
Additional solution : 25 ml of Wij’s solution + 20 ml of KI (15%)+50 ml of water
Indicator : Starch
End point : Disappearance of blue color
Burette Reading
Weight of Oil Volume of Sodium Thiosulphate
S.No (ml)
taken (g) Solution (ml)
Initial Final
1
Oil solution V2 =
2
Blank V1 =
Calculation:
Iodine value = (V1 – V2) x N1 x Equivalent weight of Iodine x 100

W x 1000
Where, Equivalent weight of Iodine 129.6
V1 = Volume of thiosulphate required by blank, ml
N1 = Normality of thiosulphate
V2 = Volume of thiosulphate required by sample, ml
W= Weight of the sample
Iodine value = _____________.
Result:
The iodine value of the given oil sample was found to be =___________.

Expt. No :
Date :
6) Estimation of Silica Content (Analysis of Cement)

Aim:
To estimate the silica content in the given cement sample
Apparatus Required:
Crucible, Desiccator, Beaker, Water bath, No 40 Whatman filter paper, Pipette, Electric Bunsen
Burner, Stirrer
Chemicals Required:
Given sample of Portland cement, 1:1 HCl.
Procedure:
• Weigh 2 gm of cement accurately and transfer into china dish

• Add 2 ml of water to prevent lumping
• Add 10 ml of 1:1 HCl to this and allow to digest for 10 minutes
• Add 50 ml of water and transfer the contents from china dish into beaker
• Add 50 ml of 1:1 HCl into beaker to make it to acidic medium
• Then filter through No:40 Whatman filter paper
• Incinerate in the pre weighed crucible
• Cool it in a desiccator.
• Weigh the crucible with its content.
• Find out amount of silica.
Calculation:
Weight of cement taken (w) = g
Weight of empty crucible (a) = g
Weight of silica + crucible (b) = g
% of silica = ( b – a ) x100
w
% of silica = ____________
Result:
The amount of silica content was found to be =______________.

Expt. No :
Date :
7) Estimation of Mixed Oxide Content (Analysis of Cement)
Aim:
To estimate the mixed oxide content in the given cement sample
Apparatus Required:
Desiccator, Beaker, Water bath, No 40 Whatman filter paper, Pipette, Electric Bunsen Burner,
Stirrer
Chemicals Required:
Given sample of Portland cement, 1:1 HCl, 15% NaOH solution, NH4Cl, NH3, Ammonium
oxalate etc.
Procedure:
• Weigh 2 g cement and transfer into a china dish

• Add 2 ml of water to prevent lumping
• Add 10 ml of 1:1 HCl to this and allow to digest for 10 minutes.
• Add 50 ml of water and transfer the contents from china dish to a beaker
• Add 50 ml of 1:1 HCl to this beaker to make the acidic medium
• Filter the solution through No 40 Whatman filter paper
• Collect the filtrate in a beaker and make up to 250 ml
• Pipette out 100 ml of the above solution into a beaker and boil it
• Add 2 gm of NH4Cl to avoid the precipitation of Ca and Mg compounds
• Add 20 ml of NH3 to the boiling solution to make the solution alkaline
• Boil the solution for about 5 minutes until a pale brown jelly precipitate formed
• Cool the solution and filter the solution into No 40 Whatman filter paper.
• Then incinerate the in a pre weighed crucible and cool it in desiccator.
• Obtain the amount of mixed oxide content by difference in weight.

Calculation:
Weight of cement taken (w) = g

Weight of empty crucible (a) = g
Weight of mixed oxide content + crucible (b) = g
% of mixed oxide content (Fe2O3 + Al2O3) = ( b – a ) x250 x100

w x 100
% of Mixed oxide content = ____________
Result:
The amount of mixed oxide content was found to be =_____________.

Expt. No :
Date :
8) Estimation of Calcium Oxide Content (Analysis of Cement)
Aim:
To estimate the calcium oxide content in the given cement sample
Apparatus Required:
Crucible, Desiccator, Beaker, Water bath, No 40 Whatman filter paper, Pipette, Electric Bunsen
Burner, Stirrer.
Chemicals Required:
Given sample of Portland cement, 1:1 HCl, 15% NaOH solution, NH4Cl, NH3, Ammonium
oxalate etc.
Procedure:
• Weigh 2 gm cement and transfer into china dish.
• Add 2 ml of water to prevent lumping.
• Add 10 ml of 1:1 HCl to this and allow to digest for 10 minutes.
• Add 50 ml of water to transfer the contents from china dish to a beaker.
• Add 50 ml of 1:1 HCl to this beaker to make the acidic medium
• Filter the solution through No 40 Whatman filter paper
• Collect the filtrate in a beaker and make it up to 250 ml
• Pipette out 100 ml of above solution into a beaker and boil it
• Add 2 gm of NH4Cl to avoid the precipitation of Ca and Mg compounds
• Add 20 ml of NH3 to the boiling solution to make the solution alkaline
• Boil the solution for about 5 minutes until a pale brown jelly precipitate formed
• Cool the solution and filter the solution into No 40 Whatman filter paper.
• Heat the collected filtrate
• Dissolve 1 gm of ammonium oxalate in 10 ml of boiling water and add to the boiling
filtrate
• White precipitate of oxalate is formed during the above procedure.
• Then filter through No 40 Whatman filter paper.
• Incinerate the pre weighed crucible and cool it in a desiccator.
• Find the amount of calcium oxide content from the difference in weight.

Calculation:
Weight of cement taken (w) = (g)

Weight of the empty crucible (a) = (g)
Weight of crucible + calcium oxide (b) = (g)
% of calcium oxide content = ( b – a ) x 250 x 100

w x 100
Result:
The amount of calcium oxide content was found to be =_______________.

Expt. No :
Date :
9) Estimate the Proximate Analysis of the Given Sample of Coal

Aim:
To assess the quality of coal by proximate analysis.
Apparatus and Equipment Required:
Hot air oven, Muffle Furnace, Crucible, Desiccator and sample of coal.
Procedure:
i) Moisture: About 1 gram of finely powdered air dried coal sample was weighed in a
crucible was placed inside an electric hot air oven maintained at 105 -1100C. The crucible was
allowed to remain in the oven for 1 hour and taken out with a pair of tones cooled in a
desiccator and weighed. Loss in weight was reported as moisture.
 Loss of Weight 
% Moisture =   × 100
 Weight of coal taken 
ii) Volatile Matter: The dried sample of coal left in the crucible was covered with a
lid and placed in an electric furnace maintained at 925 ± 50 0 C the crucible was
taken out of the oven after 7 minutes of heating. The crucible was cooled first in air
and then in a desiccator and weighed. Loss in weight was reported as volatile
matter on percentage basis.
 Loss in weight due to removal of volatile matter 

% Volatile Matter =   × 100
iii) Ash: The residual coal was then heated in a muffle furnace at 500C for half an hour.
The crucible was taken out and cooled first in air and desiccator and then weighed.
Heating, cooling and weighing was repeated till constant weight was obtained. The
residue was reported as ash on percentage basis.
 Weight of ash taken 

% Ash =   × 100
Fixed Carbon = 100 − (% of Mositure + % Ash + % Volatile Matter )

Calculation:
Weight of coal taken = g

Weight of crucible = g
Wt. of coal + crucible = g
After heating to 105 oC (Oven) = g
 Loss of Weight 
i ) % Moisture =   × 100
After heating Muffle Furnace 925 oC
 Loss in weight due to removal of volatile matter 

ii ) % Volatile Matter =   × 100
Heating half an hour in muffle furnace 750 oC
 Weight of ash taken 

iii ) % Ash =   × 100
% of Fixed Carbon = 100 − (% of Mositure + % Ash + % Volatile Matter )
Result:
S.No Proximate Analysis of Percentage

1. Moisture
2 Volatile Matter
3 Ash
4 Fixed Carbon

Expt. No :
Date :
10) Estimation of Available Chlorine (Bleaching Powder)

Aim:
To determine the percentage of available chlorine present in the given sample of bleaching powder
Principle:
Available Chlorine
"Available chlorine" is an expression of the equivalent weights of oxidizing agents, with chlorine
gas as a basis, similar to the expression of alkalinity in terms of calcium carbonate equivalents.
The term originated from the need to compare other chlorine-containing compounds to gaseous
chlorine. Available chlorine is based on the half-cell reaction in which chlorine gas is reduced to
chloride ions with the consumption of two electrons. In this reaction, the equivalent weight of
chlorine is the molecular weight of chlorine, 71 g/mole, divided by 2, or 35.5 g/mole.
Cl2 + 2 e → 2 Cl-
Chlorine Chloride ion
The available chlorine of other chlorine-containing compounds is calculated from similar half-cell
reactions, the formula weight of the compound, and the equivalent weight of chlorine.
Theory:
Bleaching powder is added to water as a disinfecting agent and also as a bleaching agent. The
main constituent of bleaching powder is Calcium hypochlorite, Ca(OCl)2 which supplies chlorine
(Cl2) with dilute acids.
Ca(OCl)2 + 4 HCl → CaCl2 + 2 H2O + 2 Cl2
The available chlorine is defined as the percentage of chlorine made available by bleaching
powder when treated with dilute acids.
In chemically pure water, molecular chlorine reacts with water and rapidly hydrolyzes to
hypochlorous acid (HOCl) and hydrochloric acid (HCl):
Cl2 + H2O → HOCl + HCl
Chlorine Water Hypochlorous acid Hydrochloric acid

Hypochlorous acid is a weak acid and dissociates to form a hydrogen ion and a hypochlorite ion.
HOCl = H+ + OCl -
Hypochlorous acid Hydrogen ion Hypochlorite ion
The available chlorine present in the given sample of bleaching powder is iodometrically
determined by treating its solution with an excess of potassium iodide solution in the acidic
medium.
ClO- + 2 H + + 2I- → I2 + H2O + Cl-
The liberated iodine (I2) is treated with sodium thiosulphate (Na2S2O3) solution using freshly
prepared starch solution as indicator to be added near the end point.
( Starch + I2 → Blue colored Starch iodide complex)
I2 + 2Na2S2O3 → Na2S4O6 + 2 NaI
Apparatus:
Weighing balance, Burette, Conical flask, Measuring flask, Funnel, Glass rods, Beakers.
Reagents:
Bleaching powder, Standard Sodium thiosulphate solution (N/10), 10 % Potassium iodide (KI)
solution, dilute Acetic acid, freshly prepared starch indicator.
Procedure:
Preparation of bleaching powder solution:
• Weigh accurately 3 g bleaching powder in a weighing bottle.

• Transfer it to a clean beaker and grind it to a thin paste with water.
• Allow the mixture to settle and pour the milky supernatant liquid into a 250 ml standard
flask.
• Grind the residue with little more water and repeat the procedure until the whole of the
sample is quantitatively transferred into the standard flask.
• Make up the solution to 250 ml and shake the flask well for uniform concentration.

Estimation of Available chlorine:
• Take 10 ml of this solution (in a state of very fine suspension) into a conical flask and add
10 ml of 10% KI solution and 10 ml of dilute acetic acid to the above solution.
• Titrate this solution (containing liberated iodine) against std. sodium thiosulphate solution
taken in a burette.
• When the dark brown colour changes to pale yellow, add 2 ml of freshly prepared starch
indicator which turns the solution colour into blue.
• Continue the titration till the disappearance of blue colour of the solution.
• Note down the volume of the titrant.
• Repeat the titration for concordant values.
Observations and Calculations:
Titration of Bleaching powder solution against std. Sodium thiosulphate solution
Burette solution: Std. Sodium thiosulphate solution

Pipette solution: 10 ml of bleaching powder solution
Reagents added to
sample solution: 10 ml of 10% KI solution + 10 ml dil. acetic acid
Indicator: Freshly prepared starch solution
End point: Disappearance of blue colour
S.No Volume of given Burette Reading in ml Volume of Concordant

Bleaching Initial Final Na2S2O3 Value, ml
solution, ml in ml
1
2
3

Concordant volume of Na2S2O3 solution (V1) = ml

Normality of Na2S2O3 solution (N1) = N
Volume of bleaching powder solution (V2) = 10 ml
Normality of bleaching powder solution (N2) =
= V1N1 /V2
= --------- N
Amount of available chlorine (m) = N2 x Equivalent weight of Cl2
= N2 x 35.45 g /l
= g/l
Amount of available chlorine present in

100 ml of the solution = m x 250 /1000
= g
Percentage of available chlorine present

in the given sample of bleaching powder = (m x 0.25 / w )100
Result:
The percentage of available chlorine present in the given sample of bleaching powder is
_____________.

Expt. No :
Date :
11. Estimation of Purity of Glycerol by Dichromate Method

Aim:
To estimate the percentage purity of the given sample of Glycerol by Dichromate method.
Theory:
Glycerol can be quantitatively oxidized by the known excess of acidified K2Cr2O7 into
Carbon dioxide and water:
K2Cr2O7 + 4 H2SO4 → K2SO4 + Cr2 (SO4)3 + 3(O) + 4 H2O
C3H8O3 + 10 (O) → 3 CO2 + 4 H2O
The amount of dichromate consumed by glycerol can be determined by refluxing glycerol
with a known excess of Potassium dichromate solution and then titrating the unreacted
dichromate against std. Sodium thio sulphate solution using starch indicator.
Apparatus Required:
Burette, Pipette, Conical flask, Iodine flask and water bath.
Chemical Required:
Glycerol (standard and sample), 10% KI solution, starch, dil. H2SO4 , Sodium thiosulphate and
Potassium dichromate solutions.
Procedure:
I. Standardization of Sodium thiosulphate:
• Titrate 20 ml of std. Potassium dichromate solution + 20 ml of dil. H2SO4 + 10 ml of

• 10% KI solution against Sodium thiosulphate solution.
• When the solution turns pale yellow, add 1 ml of freshly prepared starch solution and
• continue the titration. End point is change of colour from blue to green.
• Repeat the above procedure for concordant values.

II. Estimation of Glycerol:
• Pipette out 10 ml of the given sample of glycerol solution into a clean iodine flask.
• Add 60 ml of 0.1 N K2Cr2 O7 and 1 test tube of dil. H2SO4.
• Heat the contents of iodine flask on a water bath for 60 min and cool.
• Add 1 test tube of dil. H2SO4 and 10 ml of 10 % KI solution to the above solution.
• Titrate the liberated iodine against std. Sodium thiosulphate solution using starch
• indicator. End point is the colour change from blue to green.
• Repeat this procedure with pure standard Glycerol.
Observations & Calculations:
Titration I:
Standardization of Sodium thiosulphate solution
Burette solution : Sodium thio sulphate solution

Pipette solution : Standard K2Cr2O7 solution
Additional solution : 10 ml of H2SO4 + 10 ml of 10% KI
Indicator : Starch
End point : Blue to green
S.NO Volume Of Burette Reading (ml) Volume Of Sodium Concordant

K2Cr2O7 Initial Final Thio Sulphate Value (ml)
Solution Solution
(V1) ml (ml)
1
2
Volume of K2Cr2O7 (V1) =

Normality of K2Cr2O7 (N1) =
Volume of Na2S2O3 (V2) =
Normality of Na2S2O3 (N2) = (V1xN1) / V2

Titration II:
Estimation of Glycerol:
Burette solution : Standard Sodium Thiosulphate solution
Solution in Iodine flask : 10 ml of Glycerol sample + 60 ml of K2Cr2O7 + 1 test tube of
H2SO4 +10 ml of 10%KI
Indicator : Starch
End point : Blue to Green
A. Estimation of Sample Glycerol:
Volume Of Burette Reading (ml)

Volume Of Sodium
Glycerol Concordant
S.NO Thio Sulphate
Solution Initial Final Value (ml)
Solution (V4)ml
(V3) ml
1
2
B. Estimation of Standard Glycerol:
Volume Of Burette Reading (ml)

Volume Of Sodium
Glycerol Concordant
S.NO Thio Sulphate
Solution Initial Final Value (ml)
Solution (V5)ml
(V3) ml
1
2
Volume of thiosulphate corresponding to unreacted dichromate = V4 ml
V4 × N 2
Volume of unreacted K 2 Cr2 O7 with sample Glycerol = = Vsample
N1
V5 × N 2
Volume of unreacted K 2 Cr2 O7 with s tan dared Glycerol = = Vstd
N1

Volume of reacted K 2Cr2O7 = K 2Cr2O7 volume taken initially – volume of unreacted K 2Cr2O7
= 60 - volume of unreacted K 2Cr2O7
1 ml of 0.152 N K 2 Cr2 O7 = 10 mg of Glycerol
(60 − V ) ml × N
× 10 = Amount of Glycerol in the sample solution = wsample =
sample 1
mg
0.152
(60 − Vstd ) ml × N1
× 10 = Amount of Glycerol in the s tan dard solution = wstd = mg
0.152
weight of sample Glycerol

Percentage purity of Glycerol = × 100
weight of s tan dard Glycerol
wsample
= × 100
wstd
Result:
The percentage purity of the given sample of Glycerol was found to be _________%.

Expt. No :
Date :
12) Estimation of Flash and Fire Point of the Given Sample (Pensky Martens
Closed Cup Method)
Aim:
To determine flash and fire point for the given sample.
Apparatus Required:
Pensky Martens closed flash tester, thermometer and sample.
Procedure:
• All parts of the cup were cleaned and dried before starting the test.
• The cup was filled with sample to be tested to the level indicated by filling mark.
• The lid was placed on the cup and thermometer was inserted.
• The material to be tested and tester was brought to a temperature of 15 ± 5 0 C , lower than
the estimated flash point.

• The heat was supplied at such a rate that the temperature in thermometer increased.
• The stirrer was turned at low flow rates such that the stirrer was directed in the downward
direction.
• The observed flash point was recorded such that the temperature on thermometer at the
time of test flame application caused a distinct flash in the interior of the cup.
• The temperature was increased till fuel burned for 5 second. The fire point temperature
was noted.
Tabular Column:
Sample Flash Point (0C) Fire Point (0C)
Result:
The flash and fire point for the given sample was found to be ____oC and ________ oC respectively.

Expt. No :
Date :
13) Cleveland Open Cup Apparatus for Flash and Fire Point
Aim:
To determine the flash and fire point temperatures of the given sample of lubricating oil using
Cleveland open cup apparatus.
Apparatus required:
Cleveland open cup apparatus, thermometer, splinter sticks, sample of oil.
Theory:
The flash point of the lubricating oil is defined as the lowest temperature at which it forms vapours
and produces combustible mixture with air. It indicates maximum temperature at which liquid fuel
can be stored without any fire hazard.
A higher flash point temperature is always desirable for any lubricating oil. An oil with a lower
value of flash point burns easily and leaves carbon deposits on the moving parts of the engine.
The minimum flash point of oils used in IC engines ranges between 200 to 250 0C.
The Cleveland open cup apparatus can not be used for oils having an open cup flash below 1750 F.
The fire point is the minimum temperature at which liquid fuel produces sufficient vapors to form
a flammable mixture with air that continuously supports combustion, establishing flame instead of
just flashing.
When the oil is tested using a Cleveland open cup apparatus, it indicates a temperature slightly
above the afore mentioned temperatures. This apparatus shall be used only when specified, in
other cases Pensky Martens method (IP-35) shall be used.
The flash and fire point temperatures depend on the volatility of the oil.

Procedure
• Clean and dry all the brass parts and the passage for gas.
• Clean the cup and fill it with the given sample of oil up to the filling mark. The top of the
meniscus should exactly match the filling mark.
• Insert the thermometer in the holder. Make sure that it does not touch the metallic cup.
• Heat the oil by means of an electric heater at a rate of 10 0 C per minute.
• When the oil gives out vapour, introduce the test flame above the oil, without touching the
surface of the oil. Pass the test flame in a straight line parallel to the oil surface across the
centre of the cup. Repeat this for every 2 oC rise in the thermometer and watch for flash
with a flickering sound.
• Note the temperature at which the first flash appears at any point just above the surface of
the oil. This is the flash point.
• After determining the flash point, continue heating the oil at the rate of 10 oC per minute.
• Apply the test flame at specified intervals as before until the oil ignites and continues to
burn for at least 5 seconds. Note this temperature as the fire point.
• Repeat the test for reproducibility of the results. The results flash point should not differ
from the mean by more than 2 oC and fire point results more than 5 oC.
Cleveland Flash and Fire Point

Tabulations:
S.No Temperature, oC
Trial 1 Trial 2 Trial 3
Flash point
Fire point
Result:
The flash and fire points of the given sample of oil were determined by using Cleveland open cup
method.
The flash point is __________ oC.
The fire point is __________ oC.

Expt. No :
Date :
14) Determine the Viscosity of the Given oil (Saybolt Viscometer)
Aim:
To determine the viscosity of the given oil using Saybolt Viscometer at given temperature.
Theory:
Saybolt viscometer is used for the determination of the viscosity of petroleum products and
lubricants in SUV units. SUV unit is Saybolt viscosity unit which is a measure of kinematic
viscosity. It is also denoted as SUS (Saybolt Universal Seconds). Saybolt Universal Viscometer
can be used only for liquids having times of flow within the range of 32 seconds and 1000
seconds.
In Saybolt viscometer, the given liquid is heated to the required temperature in a constant
temperature bath. When thermal equilibrium is attained, the temperature of the liquid to be tested
remains constant for more than 3 minutes. At this stage, 60 ml of liquid is withdrawn through an
aperture of standard dimension and time required for this is noted. This time is multiplied by the
temperature constant of the instrument to provide the viscosity in centiStokes.
The inner diameter of the oil tube is 2.975 cm and of the outflow tube is 0.1765 cm..
Saybolt Universal viscosity—the efflux time in seconds of 60 ml of sample flowing through a

calibrated Universal orifice under specified conditions.
The following formulae may be used to convert Saybolt Universal Seconds (SUS) units to
centistokes (cSt units).
For SUS values between 32 and 100:

195
cST = 0.226 × SUS −
SUS
For SUS values greater than 100:

135
cST = 0.220 × SUS −
SUS
Procedure:
• Clean the oil tube well with a suitable solvent such as benzene.
• Rinse the cleaned oil tube with the oil to be tested so that the surface is
• completely wetted with the oil. Drain out the oil.
• Insert the cork stopper into the lower end of the air chamber at the bottom of the oil tube.
Fix it properly so as to prevent air passage through it.
• Pour the test sample into the oil tube up to the mark. Keep it well stirred with the oil tube
thermometer.
• Adjust the bath temperature until the temperature of the material remains constant at the
desired value.
• After the temperature of the oil tube remained constant within 0.02 0
C of the desired
temperature for one minute, place the receiving flask in position so that the stream of the
liquid from outlet tube would drain straight into the flask.
• Snap the cork from its position and at the same instant start the timer.
• Stop the timer when the bottom of the meniscus of the liquid reaches the mark on the neck
of the receiving flask. Note the time required.
• Repeat the procedure twice for the same temperature setting.
• Repeat the experiment for two different temperatures.
• Report the results to the nearest 0.1 seconds for viscosity values below 200
• seconds and to the nearest whole second for values 200 seconds or above.
Graph:
A plot of viscosity (y axis) vs temperature (x axis)was obtained.

Saybolt Viscometer
Tabulations and Calculations:
S.No Temperature,0 C Time ,secs Kinematic

Viscosity,cSt
Trial 1 Trial 2 Trial 3 Mean
1
2
3
Formula:
For SUS values between 32 and 100

195
cST = 0.226 × SUS −
SUS
For SUS values greater than 100:

135
cST = 0.220 × SUS −
SUS

Model calculations:
o
Temperature = C
Time taken for flow of 60 ml of the given sample :
Trial 1 = a = sec
Trial 2 = b = sec
Trial 3 = c = sec
Mean = (a + b + c ) / 3 = sec = SUS
Kinematic viscosity = cSt
Result:
The kinematic viscosity of the given oil sample was found at three different temperatures.

Expt. No :
Date :
15) Determine the Viscosity of the Given oil (Redwood Viscometer)
Aim:
To determine the viscosity of the given oil using Redwood Viscometer at a specific temperature.
Theory:
The Redwood viscometer is used for determining the viscosity of an oil expressed as time of flow
in seconds through as specified hole made in an S.S.Rade piece. This is another efflux type
viscometer that works on the same principle of Saybolt viscometer. Redwood seconds is defined
for collection of 50ml of liquid to flow out of orifice.
The Red Wood Apparatus measures viscosity in empirical units and not in absolute units such
as centistokes. The value of viscosity of the liquid may be obtained by comparison with value of
time for the liquid of known viscosity.
It is possible to convert Redwood Viscometer readings to absolute units, for which the
specifications IP 70/62 issued by the Institute of Petroleum London, may be consulted. The
method is primarily applicable for viscosity determination of oils which flow in a Newtonian
manner, that is if it possesses a linear relationship between shearing stress and rate of shear under
the test condition.
The flow time measurements of petroleum products should be made at the following
temperatures:
21.1 oC (70 oF), 37.8 oC (100 oF), 50.0 oC, 60.0 oC, 93.3 oC, 121 oC, 149.0 oC & 204 oC.
For waxy fuel oils the minimum temperature is 49 oC.
For flux oils the temperature of test to be 93.3 oC
The apparatus will correctly indicate the viscosity flow time if it stands between 30 seconds to
2000 seconds. If the flow time measured with this apparatus for any oil exceeds 2000 seconds the
test should be repeated with Redwood Viscometer No.2 which will give the correct value of
viscosity for such highly viscous oils.

Formula:
Kinematic viscosity , cSt = υ = µ /ρ = At- B/t
where t is the viscometer second. A and B are instrument specific constants. For Redwood
viscometer, A= 0.26 and B = 188, t is Redwood seconds. µ and ρ are the absolute viscosity and
density of the sample
Procedure:
• Set up the viscometer, using the spirit level to ensure that it is level.
• Clean the oil-cup with a suitable solvent e.g. carbon tetrachloride and then dry it
thoroughly using soft tissue paper, or some similar material which will not leave any fluff.
Place it in the apparatus.
• Fill the bath with water for determination at 93.3 0 C and below; for higher temperatures,
use an oil having a suitably low viscosity at the test temperature.
• For determinations above 93.3 0 C, fill the bath to a level not less than 10 mm below the
rim of oil cup at the test temperature.
• Place the ball valve on the jet to close it and pour the prepared sample into the oil cup up to
the tip of indicator. Care should be taken to ensure the sample does not contain any
suspended impurities. A filter or metal gauge not coarser than BS 100 mesh can be used to
eliminate the impurities if any.
• Place a clean thermometer and a stirrer in the cup and cover it with a lid.
• Heat the viscometer bath a few degrees above the desired temperature.
• Adjust the temperature of the bath until the sample in the cup is maintained at the test
temperature by constantly stirring the contents of the bath and the oil cup.
• When the temperature of the sample has become steady at the desired value, stop stirring
the sample. Remove the thermometer from the sample.
• Place the clean, dry, standard 50 ml flask centrally below the jet.
• Lift the ball valve and simultaneously start the timer.
• Stop the timer at the instant the lower meniscus of the oil sample reaches the 50 ml
graduation mark of the flask. Note the time required for flow of 50 ml of sample.
• Note the final reading of the oil cup thermometer.
• Reject any determination if the temperature of the oil cup varies during the run by more

than
0.1 oC for temperature of 60 oC or below
0.3 oC at 93.3 oC
0.5 oC at 121 oC
• Report the time in seconds to the nearest 0.5 for value below 200 seconds, and to the
nearest second for values above 200 seconds.
• Repeat the experiment twice for the same temperature setting.
Redwood Viscometer

Tabulations:
S.No Temperature, oC Time taken, sec Viscosity, t

Trial 1 Trial 2 Mean Redwood seconds
Absolute viscosity, cSt = 0.26 t - 188 /t
Result:
The viscosity of the given oil sample using Redwood viscometer No. ___ at
______ oC is _______ Redwood seconds. Corresponding viscosity is ___cSt.

Expt. No :
Date :
16) Determine the Calorific Value of the given sample (Bomb Calorimeter)
Aim:
To determine the calorific value of the given sample by its combustion in a bomb calorimeter.
Theory:
Calorimetry is the process of measuring the heat of chemical reactions or physical changes as well
as heat capacity. Differential scanning calorimeters, isothermal microcalorimeters, titration
calorimeters and accelerated rate calorimeters are among the most common types. A simple
calorimeter just consists of a thermometer attached to a metal container full of water suspended
above a combustion chamber.
A bomb calorimeter is an apparatus used for measuring heats of combustion. Heats of
combustion as determined in an oxygen bomb calorimeter are measured by a substitution
procedure in which the heat obtained from the sample is compared with the heat obtained from
combustion of a similar amount of benzoic acid ( or other standardizing material whose calorific
value is known). These measurements are obtained by burning a representative sample in a high
pressure oxygen atmosphere within a metal pressure vessel or 'bomb'. The energy released by the
combustion is absorbed within the calorimeter and the resulting temperature change within the
absorbing medium is noted ( initial and final temperature).
The heat of combustion of the sample is then calculated by multiplying the temperature
rise in the calorimeter by a previously determined energy equivalent or heat capacity determined
previously with a standardizing material. Corrections must be made for heat transfer occurring in
the calorimeter if any or any side reactions taking place.
Four essential parts are required in any bomb calorimeter: (i) a bomb or vessel in which the
combustible charges can be burned, (ii) a bucket or container for holding the bomb in a measured
quantity of water together with a stirring mechanism, (iii) an insulating jacket to protect the bucket
from transient thermal stresses during the combustion process and (iv) a thermometer or other
sensor for measuring the temperature changes within the bucket.
Principle of Operation:
The sample is weighed and placed in the bomb. The bomb is sealed with oxygen and the sample is
ignited electrically. The complete oxidation of the compound releases heat and this is measured

through the temperature change of the water bath surrounding the bomb. The heat of combustion
at constant volume can be calculated from the resulting rise in temperature.
Procedure:
Experimental set up:
• Level the calorimeter vessel by adjusting the triangular support.
• Remove the inlet cover on the top of the jacket. Fill water up to 5-6 cm from the top of the
jacket and close the cover.
• Fix the bomb support (stand) in the calorimeter vessel and place the vessel in the jacket.
• Assemble oxygen charging system.
• Place the bomb lid on the stand provided on the pressure gauge. Attach ignition wire across
both electrodes. The wire should be tight across the electrodes.
• Make a pellet of the sample, weigh it and place it in the crucible.
• The weight of the sample should be less than 1.10 g for sample of calorific value less than
10000 cal /g. For samples of higher calorific value, 1/2 or 1/3 of 1.1g can be used.
• Place the crucible in the crucible holder ring.
• Tie a knot of thread in the centre of the ignition wire and make sure that the other end of
thread touches the pellet.
• Place approximately 1-2 ml of distilled water from a pipette in the bomb.
• Close the bomb. Connect the oxygen filling assembly making sure that there is no sign of
leakage.
• Slowly rotate the oxygen valve in the direction pointing 'on'. Observe the gauge and allow
the pressure to rise until it is 26 Kg / cm2 and close the valve.
• Cover the water jacket and the vessel using the combined lid. Fix stirrer in the space
provided and dip its propeller in the water jacket. Dip thermometer/ sensor in the water.
• Now the set up is ready for ignition. Make the electrical connections Turn on the stirrer.
Note the initial temperature of water.
• After 2 -3 minutes, switch the sensor reader (temperature indicator) to 'Temp. rise' mode.
Adjust the display to '0.00' by rotating the knob reading 'Temp. adj'. Simultaneously press
the 'fire' button to ignite the sample.
• The temperature will start to rise and gradually become constant. From this point, the
temperature will eventually start to decrease. The peak temperature must be recorded as the

final rise in temperature.
• Turn off the stirrer and firing unit. Remove the stirrer and sensor from the water.
• Now remove the combined lid and disconnect the lead from the bomb. Using the hook, lift
the bomb from the vessel and place it on the table.
• Release the pressure from the bomb using the gas releasing pin and dismantle the bomb.
Clean the bomb interior including crucible and electrodes with water and dry using a soft
cloth or compressed air.
Determination of the calorific value of the given sample:
(A) Determining Water Equivalent

The water equivalent of the system is determined by igniting a pellet of pure, dry benzoic acid of
known calorific value weighing not less than 0.8 and not more than 1.1 g. Record the corrected
temperature rise, T, calculate the calorific values of the thread and wire (CVT, CVW), and evaluate
the water equivalent using the following equation:
(HxM ) + CVT + CVW

W=
T
where
W = Water equivalent in calories / 0C
H = Known calorific value of Benzoic acid in calories/ gram
= 6319 calories/ gram
M = Mass of sample (Benzoic acid) in grams
CVT = Calorific value of thread
= 2.1 / cm ( when using a thread of 10 cm, CVT =2.1 x 10 = 21 calories
CVW = Calorific value of ignition wire
= 2.33 / cm ( when using a wire of 4 cm, CVT =2.33 x 4 = 9.32 calories
T = Final rise in temperature, 0 C

(B) Determining the calorific value of the given sample
Now that the Water Equivalent is known, above combustion procedure is repeated with the
known weight of given sample in the place of benzoic acid.
The calorific value of the sample is calculated by the following equation:
(TxW ) − (CVT + CVW )

CVS =
M
where
CVS = calorific value of the given sample , calories/gram
T = Net corrected temperature rise during combustion of the sample
M = Mass of the sample taken for combustion
Safety Precautions:
(i) Oxygen filled in the bomb should not exceed a gauge pressure of 26 Kg / cm2.
(ii) There should be no leakage of oxygen from the bomb.
(iii) Do not allow the bomb to shake once it is pressurized with oxygen.
(iv) Do not fire if the bomb had been dropped or tilted.
(v) Water level in the calorimeter vessel should be 1-2 cm above the upper surface of
the closure ring of the bomb.
(vi) Stirrer should not be stopped during the experiment.
Instructions:
It is suggested to perform the experiment for water equivalent three to five times and to take the
mean value as W.
While performing the experiment to determine the Water equivalent (W) using benzoic acid, the
same quantity of distilled water must be used for all experiments.
For precise results, the mass values of the benzoic acid and the sample should be corrected to the
third decimal place (0.001g) in the formula.

Tabulations and Calculations:
(A) Determination of water equivalent

S.No Mass of Initial Time, Temp Max Water
Benzoic temperature, sec Rise, oC Temp Equivalnt,
o
Acid, M g C Rise, T oC W, cal/oC
1
Mean W
Temperature rise, oC , T =
Mass of sample (Benzoic acid) in grams = M =
Known calorific value of Benzoic acid in calories/ gram = H
= 6319 calories/ gram
Length of the thread used, cm = LT =
Calorific value of thread, calories = CVT = 2.1 / cm x LT =
Length of the wire used, cm = LW =
Calorific value of ignition wire, calories = CVW = 2.33 / cm x LW =
(HxM ) + CVT + CVW

Water equivalent, W = =
T

Tabulations and Calculations (cont'd)
(B) Determination of Calorific value of the given sample
S.No Mass of Initial Time, Temp Max Temp Calorific

the sample temperature, sec Rise, Rise, Value, CVS
o o
(M) g C C T oC Cal/gram
1
Mean CVS
Net corrected temperature rise during combustion of the sample, oC = T =

Water equivalent, cal/ oC =W=
Length of the thread used, cm = LT =
Calorific value of thread, calories = CVT = 2.1 / cm x LT =
Length of the wire used, cm = LW =
Calorific value of ignition wire, calories = CVW = 2.33 / cm x LW =
Mass of the sample (M) = g
(TxW ) − (CVT + CVW )

CVS = =
M

Bomb Calorimeter
Result:
The calorific value of the given sample was determined using Bomb Calorimeter.
(i) The water equivalent using benzoic acid was found to be Calories/oC
(ii) The calorific value of the given sample was found to be Calories/g.

Expt. No :
Date :
17. Estimation of COD of the Given Sample of Wastewater
Aim:
To estimate the amount of chemical oxygen demand for the given water sample.
Principle:
The organic matter present in the sample gets oxidized completely by dichromate in the presence
of Sulphuric acid to give CO2 and H2O. The excess dichromate remaining after reaction is titrated
with ferrous ammonium sulphate. The dichromate consumed gives oxygen required to oxidation
of organic matter.
Apparatus Required:
Reflux apparatus, heating mantle, Burette
Reagents:
Potassium dichromate, Sulphuric acid, silver sulphate, ferrous ammonium sulphate, ferroin,
mercuric sulphate
Theory:
Chemical oxygen demand (COD) test is commonly used to indirectly measure the amount of
organic compounds in water. Most applications of COD determine the amount of organic
pollutants found in surface water (e.g. lakes and rivers), making COD a useful measure of water
quality. It is expressed in milligrams per liter (mg/L),
The basis for the COD test is that nearly all organic compounds can be fully oxidized to
carbon dioxide with a strong oxidizing agent under acidic conditions. The amount of oxygen
required to oxidize an organic compound to carbon dioxide, ammonia, and water is given by:
This expression does not include the oxygen demand caused by the oxidation of ammonia into
nitrate. The process of ammonia being converted into nitrate is referred to as nitrification. The
following is the correct equation for the oxidation of ammonia into nitrate.
The second equation should be applied after the first one to include oxidation due to
nitrification if the oxygen demand from nitrification must be known. Dichromate does not oxidize

ammonia into nitrate, so this nitrification can be safely ignored in the standard chemical oxygen
demand test.
Potassium dichromate is a strong oxidizing agent under acidic conditions. (Acidity is
usually achieved by the addition of sulfuric acid.) The reaction of potassium dichromate with
organic compounds is given by:
where d = 2n/3 + a/6 - b/3 - c/2. Most commonly, a 0.25 N solution of potassium dichromate is
used for COD determination, although for samples with COD below 50 mg/L, a lower
concentration of potassium dichromate is preferred.
In the process of oxidizing the organic substances found in the water sample, potassium
dichromate is reduced (since in all redox reactions, one reagent is oxidized and the other is
reduced), forming Cr3+. The amount of Cr3+ is determined after oxidization is complete, and is
used as an indirect measure of the organic contents of the water sample.
Because COD measures the oxygen demand of organic compounds in a sample of water, it
is important that no outside organic material be accidentally added to the sample to be measured.
To control for this, a so-called blank sample is required in the determination of COD (and BOD -
biochemical oxygen demand - for that matter). A blank sample is created by adding all reagents
(e.g. acid and oxidizing agent) to a volume of distilled water. COD is measured for both the water
and blank samples, and the two are compared. The oxygen demand in the blank sample is
subtracted from the COD for the original sample to ensure a true measurement of organic matter.
Procedure:
Place 0.2 gm of silver sulphate in the reflux flask. 20ml of unknown water sample, 10ml of 0.1N
potassium dichromate solution are taken in the flask together with glass beads. Add slowly 30ml
of 8 N sulphuric acid and mix thoroughly. Connect the flask to the condenser, mix the contents
before heating. Improper mixing results in bumping and sample may be blown out. Reflux for a
minimum period of 2 hrs, cool and wash the condenser with distilled water. After cooling to room
temperature, titrate excess dichromate with 0.1N ferrous ammonium sulphate using ferroin
indicator sharp color change from blue green to wine red indicates the end point. Reflux blank in
the same manner using distilled water instead of sample.

Tabulation
S. No Sample details Vol. of Initial Final burette Vol. of FAS

sample burette reading
taken reading
01 Unknown water 20
sample
02 Blank 20
Calculations
Quantity of ferrous ammonium sulphate added for blank = A ml =
Quantity of ferrous ammonium sulphate added for sample = B ml =
( A − B ) × N FAS × 8 × 1000
COD =
Quantity of water sample taken
RESULT:
The amount of COD in the given water sample = ________________

Expt. No :
Date :
19. Estimation of Glucose (Bertrand’s Method)
Aim:
To estimate the glucose in the given sample
Principle:
Glucose is a reducing sugar. When glucose is boiled with an excess of alkaline copper hydroxide,
it is oxidized to gluconic acid and Cu(OH)2 gets reduced to cuprous oxide.
CH2OH − (CHOH)4 − CHO+ 2Cu(OH)2 boiling
→CH2OH − (CHOH)4 − COOH+ Cu2 O ↓ +H2O
The precipitated red-coloured Cu2O is dissolved in a warm acidic solution of ferric alum. Cu2O
reduced ferric sulphate (in ferric alum) to ferrous sulphate. The reduced FeSo4 is titrated against
standard KMnO4.
Cu 2 o + Fe2 (SO4 )3 + H 2 SO4 → 2CuSO4 + 2 FeSO4 + H 2 O

10 FeSO4 + 8 H 2 SO4 + 2 KMnO4 → K 2 SO4 + 2 MnSO4 + 5 Fe2 (SO4 )3 + 8 H 2 O.
2Cu ≡ 2 FeSO 4 ≡ 2litres of 1N KMnO4
1 atom of Copper (63.6 g ) ≡ 1 litre of 1N KMnO4
1000 ml of 1N KMnO4 ≡ 63.6 g of Copper.
1 ml. of N 10 KMnO4 ≡ 0.00636 g of Copper
≡ 6.36 mg . of Copper.
From the amount of copper, the equivalent amount of sugar is calculated from the given
conversion table.
Chemical Required
Oxalic acid, Cupric Sulphate (Fehling A), Fehling B solution, Ferric alum, Con. H2SO4 and
Glucose.

Procedure
Titration – I Standardization of Potassium Permanganate solution.
20 ml. of standard oxalic acid solution is pipetted out into a clear 250 ml conical flask. About 20
ml. of dil.H2SO4 is added. The solution is heated to about 600C. (bearable warmth). The hot
solution is then titrated against KMnO4 solution taken in the burette. The end point is the
appearance of pale permanent pink colour. The titration is repeated to get concordant values. The
strength of KMnO4 is calculated.
2−
2 MnO4− + 16 H + + 5C 2 O4 → 2 Mn 2+ + 10CO2 + 8 H 2 O.
Titration II : Estimation of Glucose

The given glucose solution in the bottle is quantitatively transferred and made up to 100 ml. in a
standard falsk. 20 ml. is pipetted out into a clean 259 ml. conical flask. About 20 ml. of CuSO4
(Fehling solution – A) is added, followed by the addition of 20 ml. of tartrate solution (Fehling
solution – B). The solution is then heated to boiling, and maintained at this temperature for 2 to 3
minutes. The red cuprous oxide precipitate formed is allowed to settle. The clear supernatant
liquid is carefully decanted. The precipitate is washed with water to remove the excess of CuSO4.
To the precipitate, acidified ferric alum is added slowly with shaking, till the red precipitate
completely dissolves. About 20 ml. of dil. H2SO4 is added and the solution is titrated against
KMnO4 taken in the burette. The end point is the appearance of pale permanent pink colour.

Calculation
Titration – I : Standardization of KMnO4 Solution
Burette Solution : KMnO4 Solution

Pipette Solution : 20 ml. of oxalic acid
Additional solution: 20 ml of dil. H2SO4 solution
End Point : Pale permanent pink Colour
S.No Volume of Volume of Concordant End
Oxalic acid Burette Reading KMnO4 Sol. Value point
Solution (ml) (ml)
Initial (ml) Final(ml)
Calculation:
Volume of Oxalic acid V1 = 20 ml
Normality of Oxalic acid N1 =
Volume of KMnO4 Solution V2 =
Strength of KMnO4 Solution N2 =
V1 N1 = V2 N 2
N 2 = V1 N 1
V2
Strength of KMnO4 Solution N2 =

Titration – II Estimation of Glucose

Burette Solution : KMnO4 Solution
Pipette Solution : 20 ml. Glucose Solution
Additional solution: 20 ml. of Fehling soln A & B & 20 ml of dil. H2SO4 solution
End Point : Pale permanent pink Colour
S.No Volume of Volume of Concordant End

Glucose Burette Reading KMnO4 Sol. Value point
Solution (ml) (ml)
Initial (ml) Final(ml)
Calculation:
Volume of Glucose solution taken = 20 ml
Volume of KMnO4 required to react with the reduced FeSO4 = A ml.
1 ml. of N/10 KMnO4 - 6.36 mg. of Copper
A ml. of standard KMnO4 = 6.36 x A x str. of KMnO4 / 0.1
= B mg. of copper.
From the conversion table, the glucose equivalent is noted, corresponding to copper equivalent
B mg. of Cu = Z mg. of Sugar
20 ml. of glucose solution contains Z mg. of sugar.
Amount of glucose present in 100 ml. of the made up solution

= 100/20 Z = 5Z mg.
Result
The amount Glucose present in the whole of the given solution =

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CH6411 – Technical Analysis Lab 2016-17

CH6411 - TECHNICAL ANALYSIS LAB

Determine the Viscosity of the Given oil (Saybolt

18 Estimation of Glucose (Bertrand’s Method) 51

Department of Chemical Engineering, SSN College of Engineering, Chennai 1

1) Estimation of Total Fatty Matter Content

Given sample of soap, Water, Chloroform, Sodium carbonate, 0.5 N HNO3

Department of Chemical Engineering, SSN College of Engineering, Chennai 2

Weight of the soap sample (w1) = _____________ (g)

% of fatty mater = (w3– w2) * 100

% of fatty matter = ___________.

Department of Chemical Engineering, SSN College of Engineering, Chennai 3

2) Estimation of Total Alkali Content

• Weigh about 5 gm of soap.

Department of Chemical Engineering, SSN College of Engineering, Chennai 4

Volume of H2SO4 solution (V1) = ____ml

Department of Chemical Engineering, SSN College of Engineering, Chennai 5

3) Estimation of Acid Value (Analysis of Oil)

• Take 20 ml of 0.1 N oxalic acid solution in a 250 ml conical flask.

• Weigh 5 gm of oil and transfer it into 250 ml conical flask.

Department of Chemical Engineering, SSN College of Engineering, Chennai 6

Titration I: Standardization of Potassium hydroxide

Volume of Oxalic Burette Reading (ml) Volume of KOH Concordant

Normality of KOH (N2) = _______________.

Department of Chemical Engineering, SSN College of Engineering, Chennai 7

Titration II: Estimation of acid value

Weight of Oil Burette Reading (ml) Volume of KOH Concordant

ml of KOH × Normality of KOH × Eq.wt of KOH

Equivalent weight of KOH = 56.11

Acid Value = __________.

Department of Chemical Engineering, SSN College of Engineering, Chennai 8

4) Estimation of Saponification Value (Analysis of Oil)

To calculate the number of milligrams of potassium hydroxide required to completely saponify 1

Department of Chemical Engineering, SSN College of Engineering, Chennai 9

Titration : Estimation of saponification value

Burette solution : HCl

S.NO Weight of Oil Volume of Alcoholic Burette Reading (ml) Volume of

Saponification value = _________________

Department of Chemical Engineering, SSN College of Engineering, Chennai 10

5) Estimation of Iodine Value (Analysis of Oil)

Potassium iodide solution ( 15%)

Dissolve 15 gm of AR potassium iodide in 100 ml of water.

Department of Chemical Engineering, SSN College of Engineering, Chennai 11

Sodium thiosulphate solution (0.1 N)

Dissolve 25 gm of AR sodium thiosulphate crystals ( Na2S2O3 5H2O) in a 1 litre of distilled water.

Starch indicator solution : 1 ml of starch in 100 ml boiling water.

Standardization of Sodium Thiosulphate Solution

• Weigh 0.5 gm of oil and transfer into 250ml Iodine flask.

Department of Chemical Engineering, SSN College of Engineering, Chennai 12

Volume of Burette Reading Volume of Sodium Concordant Value

Volume of K2Cr2O7 ( V1) =

Department of Chemical Engineering, SSN College of Engineering, Chennai 13

Iodine value = (V1 – V2) x N1 x Equivalent weight of Iodine x 100

Iodine value = _____________.

Department of Chemical Engineering, SSN College of Engineering, Chennai 14

6) Estimation of Silica Content (Analysis of Cement)

• Weigh 2 gm of cement accurately and transfer into china dish

Department of Chemical Engineering, SSN College of Engineering, Chennai 15

7) Estimation of Mixed Oxide Content (Analysis of Cement)

• Weigh 2 g cement and transfer into a china dish

Department of Chemical Engineering, SSN College of Engineering, Chennai 16

Weight of cement taken (w) = g

% of mixed oxide content (Fe2O3 + Al2O3) = ( b – a ) x250 x100

% of Mixed oxide content = ____________