1.

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

1) Take 20 ml of 0.1 N oxalic acid solution in a 250 ml conical flask.
2) Add 1 or 2 drops of phenolphthalein indicator to this solution.
3) Titrate this solution against KOH taken in a burette.
4) The appearance of pink color indicates the end point.
5) From the volume of the KOH solution in burette, find the normality of KOH.

EXPERIMENTAL PROCEDURE

1) Weigh 5 gm of oil and transfer it into 250 ml conical flask.
2) Add 50 ml of neutralized alcohol solution to the oil solution.
3) Heat this mixture for 10 minutes by using the heater.
4) Take the solution after 10 minutes and add 1 or 2 drops of phenolphthalein indicator.
5) Titrate this against the KOH solution from the burette.
6) The appearance of pink color indicates the end point.
















ESTIMATION OF ACID VALUE (ANALYSIS OF OIL)
TABULAR COLUMN
Titration I: Standardisation of Potassium hydroxide
Burette solution : KOH
Pipette solution : Oxalic acid
Indicator : Phenolphthalein
End point : Appearance of pink colour

BURETTE READING
(ml)
S.NO VOLUME OF
OXALIC ACID
(ml) INITIAL FINAL
VOLUME OF
KOH
CONSUMED (ml)
Concordant
Value (ml)

1


2



CALCULATION (1)
Volume of oxalic acid (V
1
)=
Normality of oxalic acid (N
1
)=
Volume of KOH consumed (V
2
)=
Normality of KOH consumed (N
2
)= V
1
N
1
/ V
2


Normality of KOH (N
2
) = _______________.

Titration II: Estimation of acid value
Burette solution : KOH
Pipette solution : Oil + 50 ml of neutralized alcohol
Indicator : Phenolphthalein
End point : Appearance of pink colour

BURETTE READING (ml) S.NO WEIGHT OF
OIL
(gm)
INITIAL FINAL
VOLUME OF KOH
(ml)
Concordant
Value (ml)

1


2



CALCULATION(2)
Acid value =
Sample Oil of Weight
KOH of wt Eq KOH of Normality KOH of ml .

Equivalent weight of KOH = 56.11
Acid Value = __________.
RESULT
The acid value of the given oil sample was found to be___________.




2. 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

1) Weigh 1 gm of oil and transfer into the round bottomed flask.
2) Add 20 ml of 0.5 N alcoholic KOH solution to the round bottomed flask.
3) Follow the above procedure without taking oil for blank titration.
4) Reflux both round bottomed flasks for 1 hour.
5) After reflux, allow both the round bottomed flasks to cool.
6) Titrate both the samples using 0.5 N HCl with phenolphthalein indicator.
7) The disappearance of pink indicates the end point.

RESULT

The saponification value of the given oil sample was found to be_____________.










TABULAR COLUMN

Titration : Estimation of saponification value
Burette solution : HCl
Flask solution : Alcoholic KOH (with and without oil)
Indicator : Phenolphthalein
End point : Disappearance of pink colour

BURETTE READING
(ml)
S.NO VOLUME OF
OIL
SOLUTION
(gl)
VOLUME OF
ALCOHOLIC
KOH SOLUTION (ml) INITIAL FINAL
TITER
VALUE
((ml)

1


2


Blank
( Without Oil)




CALCULATION

Saponification Value

= (Titre value of blank in ml Titre value of sample in ml) x N
KOH
x Equivalent wt of KOH
Weight of the sample
Saponification value = _________________























3. 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 an 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

Wijs 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 ( Na
2
S
2
O
3
5H
2
O) 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

1. Pipette out 20 ml of 0.1 N potassium dichromate solution into a clean conical flask.
2. Add 1 test tube of dilute H
2
SO
4
and 10 ml of 15% KI solution to the conical flask.
3. Titrate against thiosulphate from the burette until it turned into pale yellow.
4. Add 1 ml of starch indicator and titrate against thiosulphate solution.
5. End point is disappearance of blue color.


EXPERIMENTAL PROCEDURE

1. Weigh 0.5 gm of oil and transfer into Iodine flask.
2. Add 10 ml of chloroform and warm slightly and cool for 10 minutes
3. Add 25 ml of Wijs solution in the same flask and shake vigorously.
4. Then allow the flask to stand for half an hour in dark place.
5. 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.
6. Add 1 ml of starch indicator and again titrate against the sodium thiosulphte solution from
the burette.
7. Disappearance of blue color indicates end point.
8. Repeat the above procedure without taking sample(ie Oil) and note the corresponding
reading for blank titration.



RESULT

The iodine value of the given oil sample was found to be =___________.


















TABULAR COLUMN
Titration I
Standardisation of Sodium thiosulphate:
Burette solution :Sodium thiosulphate
Pipette solution :Potassium dichromate
Additional solution :1 test tube of dil H
2
SO
4
solution
Indicator : Starch
End point :Disappearance of blue

BURETTE READING
(ml)
VOLUME OF SODIUM
THIOSULPHATE SOLUTION
(ml)
S.NO VOLUME OF
K
2
Cr
2
O
7
SOLUTION
(ml)
INITIAL FINAL
1


2



CALCULATION
Volume of K
2
Cr
2
O
7
( V
1
) =
Normality of K
2
Cr
2
O
7
(N
1
) =
Volume of sodium thiosulphate solution (V
2
) =
Normality of sodium thiosulphate solution ( N
2
) = (V
1
x N
2
)

/ V
2
Titration II
Estimation of Iodine value:
Burette solution : Std. Sodium thiosulphate solution
Pipette solution : 20 ml of oil
Additional solution : 25 ml of Wijs solution + 20 ml of KI ( 15%)+50 ml of water
Indicator : Starch
End point : Disappearance of blue color

BURETTE READING
(ml)
VOLUME OF SODIUM
THIOSULPHATE SOLUTION
(ml)
S.NO VOLUME OF
SOLUTION (ml)
INITIAL FINAL
1

Oil solution V
2
=
2

Blank V
1
=
CALCULATION:
Iodine value = (V
1
V
2
) x N
1
x Equivalent weight of Iodine x 100
W x 1000
where
V
1
= Volume of thiosulphate required by blank,ml N
1
= Normality of thiosulphate
V
2
= Volume of thiosulphate required by sample,ml W= Weight of the sample
Iodine value = _____________.



4. 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 Wattman filter paper, Pipette, Electric
Bunsen Burner, Stirrer

CHEMICALS REQUIRED

Given sample of Portland cement, 1:1 HCl.

PROCEDURE

1) Weigh 2 gm of cement accurately and transfer into china dish
2) Add 2 ml of water to prevent lumping
3) Add 10 ml of 1:1 HCl to this and allow to digest for 10 minutes
4) Add 50 ml of water and transfer the contents from china dish into beaker
5) Add 50 ml of 1:1 HCl into beaker to make it to acidic medium
6) Then filter through No:40 Wattman filter paper
7) Incinerate in the pre weighed crucible
8) Cool it in a desiccator.
9) Weigh the crucible with its content.
10)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 =______________.









5) ESTIMATION OF MIXED OXIDE CONTENT (ANALYSIS OF CEMENT)

AIM

To estimate the mixed oxide content in the given cement sample

APPARATUS REQUIRED

Crucible, Desiccator, Beaker, Water bath, No 40 Wattman filter paper, Pipette, Electric
Bunsen Burner, Stirrer

CHEMICALS REQUIRED

Given sample of Portland cement, 1:1 HCl, 15% NaOH solution, NH
4
Cl, NH
3
, Ammonium
oxalate etc.


PROCEDURE

1) Weigh 2 gm cement and transfer into a china dish
2) Add 2 ml of water to prevent lumping
3) Add 10 ml of 1:1 HCl to this and allow to digest for 10 minutes.
4) Add 50 ml of water and transfer the contents from china dish to a beaker
5) Add 50 ml of 1:1 HCl to this beaker to make the acidic medium
6) Filter the solution through No 40 Wattman filter paper
7) Collect the filtrate in a beaker and make up to 250 ml
8) Pipette out 100 ml of the above solution into a beaker and boil it
9) Add 2 gm of NH
4
Cl to avoid the precipitation of Ca and Mg compounds
10) Add 20 ml of NH
3
to the boiling solution to make the solution alkaline
11) Boil the solution for about 5 minutes until a pale brown jelly precipitate formed
12) Cool the solution and filter the solution into No 40 Wattman filter paper.
13) Then incinerate the in a preweighed crucible and cool it in desiccator.
14) 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 (Fe
2
O
3
+ Al
2
O
3
) = ( b a ) x250 x100
w x 100
% of Mixed oxide content = ____________

RESULT

The amount of mixed oxide content was found to be=_____________.





6) ESTIMATION OF CALCIUM OXIDE CONTENT
AIM
To estimate the calcium oxide content in the given cement sample

APPARATUS REQUIRED
Crucible, Desiccator, Beaker, Water bath, No 40 Wattman filter paper, Pipette, Electric
Bunsen Burner, Stirrer.

CHEMICALS REQUIRED

Given sample of Portland cement, 1:1 HCl, 15% NaOH solution, NH
4
Cl, NH
3
, Ammonium
oxalate etc.

PROCEDURE

1) Weigh 2 gm cement and transfer into china dish.
2) Add 2 ml of water to prevent lumping.
3) Add 10 ml of 1:1 HCl to this and allow to digest for 10 minutes.
4) Add 50 ml of water to transfer the contents from china dish to a beaker.
5) Add 50 ml of 1:1 HCl to this beaker to make the acidic medium
6) Filter the solution through No 40 Wattman filter paper
7) Collect the filtrate in a beaker and make it up to 250 ml
8) Pipette out 100 ml of above solution into a beaker and boil it
9) Add 2 gm of NH
4
Cl to avoid the precipitation of Ca and Mg compounds
10) Add 20 ml of NH
3
to the boiling solution to make the solution alkaline
11) Boil the solution for about 5 minutes until a pale brown jelly precipitate formed
12) Cool the solution and filter the solution into No 40 Wattman filter paper.
13) Heat the collected filtrate
14) Dissolve 1 gm of ammonium oxalate in 10 ml of boiling water and add to the boiling
filtrate
15) White precipitate of oxalate is formed during the above procedure.
16) Then filter through No 40 Wattman filter paper.
17) Incinerate the preweighed crucible and cool it in a desiccator.
18) Find the amount of calcium oxide content from the difference in weight.

ESTIMATION OF CALCIUM OXIDE CONTENT
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 =_______________.




7) 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 HNO
3


PROCEDURE
1) Weigh 5 gm of soap accurately and transfer into 250 ml beaker
2) Add 100 ml hot water to completely dissolve the soap.
3) Add 40 ml of 0.5 N HNO
3
until contents were slightly acidic
4) Heat the mixture over water bath until the fatty acids were floating as a layer above the
solution
5) Then cool it suddenly in ice water in order to solidify the fatty acids and separate them.
6) Add 50 ml of chloroform to the remaining solution and transfer it to a separating
funnel.
7) Shake the solution and allow the solution to separate into 2 layers. Drain the bottom
layer.
8) Add 50 ml of chloroform to the remaining solution in the separating funnel
9) Separate the fatty acid dissolved chloroform again as in the previous case and transfer it
to the collected fatty matter.
10) Weigh the fatty matter in a pre weighed china dish.
11) Allow the contents to evaporate and weigh the residue.
12) From the difference in weight, calculate the % of fatty matter in the given soap sample.

CALCULATION

Weight of the china dish (x) = _____________

Weight of china dish + Soap after drying (y)=______________

% of fatty mater = (y x) * 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_________.





8) 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
1) Weigh about 5 gm of soap.
2) Add 100 ml distilled water.
3) Gently heat until complete dissolution.
4) Transfer quantitatively to a separating funnel.
5) Add few drops of methyl orange indicator
6) Add 10 ml of H
2
SO
4
until solution becomes pink.
7) Allow to cool at room temperature.
8) Add 100 ml diethyl ether.
9) Shake vigorously for one minute.
10) Allow to stand still two phases are completely separated.
11) Take the bottom of the aqueous solution layer into a second separating funnel.
12) Carry out the second extraction of the acid solution by shaking with diethyl ether.
13) Take the aqueous acid solution into a conical flask. Wash twice with 50 ml of 1N
Sodium chloride solution by shaking for a minute.
14) Filtrate the resulting conical flask solution with Sodium hydroxide.
The total alkali content, expressed as a percentage (m/M), is given by the formula:

[ ]
m
T V T V
m
m
2 2 1 1
4
%

=

Calculation:
Volume of H
2
SO
4
solution (V1) = ml
Volume of NaOH solution (V2) = ml
Normality of H
2
SO
4
(T1) = N
Normality of NaOH (T2) = N
Mass of Soap (M) = g

RESULT
The total alkali content of the given soap sample was found to be___________.




9. ESTIMATION OF RESIDUAL CHLORINE IN WATER

AIM

To estimate the amount of residual chlorine in water

APPARATUS REQUIRED

Burette, Pipette, Conical flask, Pestle and mortar.

CHEMICALS REQUIRED

Potassium iodide, Sulphuric acid, Sodium thio sulphate, Bleaching powder, Starch
Indicator

PROCEDURE

1) Weigh about 0.5 gm of bleaching powder and transfer into mortar
2) Add small amount of water to the bleaching powder and grind them well with the help
of pestle
3) Allow the solution to settle in a few minutes, transfer the liquid portion into a 250 ml
standard flask.
4) Repeat the above procedure until all the contents of bleaching powder are completely
transferred into 250 ml flask.
5) Add additional water to make it exactly 250 ml.
6) Pipette out 10 ml of the Bleaching powder solution (made up solution) into a conical
flask
7) Add 10 ml of 15% KI and 10 ml of 1 N H
2
SO
4
to this solution and then shake well.
8) Titrate against 0.1 N sodium thiosulphate solution until yellow color appeared
9) Add 1 or 2 drops of starch indicator that turns the solution blue.
10) Then titrate against sodium thiosulphate solution until the blue color disappears.

RELATED EQUATIONS

2 KI + Cl
2
2 KCl + I
2

KI + I
2
KI
3

I
2
+ 2 Na
2
S
2
O
3
2 NaI + Na
2
S
4
O
6

I
2
+ Starch Complex having deep blue complex


RESULT

The amount of Residual chlorine in the water sample was found to be _________%.








Titration I:

Standardization of Sodium thio sulphate solution

Burette solution : Sodium thio sulphate solution
Pipette solution : Standard K
2
Cr
2
O
7
solution
Additional solution : 10 ml of H
2
SO
4
+ 10 ml of 15% KI
Indicator : Starch
End point : Blue to green

BURETTE READING
(ml)
S.NO VOLUME OF K
2
Cr
2
O
7

SOLUTION
(V
1
) ml INITIAL FINAL
VOLUME OF SODIUM
THIO SULPHATE SOLUTION
(ml)


1



2


Volume of K
2
Cr
2
O
7
(V
1
) =
Normality of K
2
Cr
2
O
7
(N
1
) =
Volume of Na
2
S
2
O
3
(V
2
) =
Normality of Na
2
S
2
O
3
(N
2
) = (V
1
xN
1
) / V
2


Titration II:

Estimation of Available Chlorine:
Burette solution: Standard Sodium Thio sulphate solution
Pipette solution : 10 ml of Bleaching powder solution + 10 ml of H
2
SO
4
+ 10 ml of 15%KI
Indicator : Starch
End point : Blue to colorless

BURETTE READING (ml) S.NO VOLUME OF BLEACHING
POWDER SOLUTION
(V
3
) ml
INITIAL FINAL
VOLUME OF SODIUM
THIO SULPHATE
SOLUTION (V
4
)ml


1



2












CALCULATION

1 equivalent of Cl
2
= 1 Equivalent of I
2

1000 ml of 1 N Na
2
S
2
O
3
.5H
2
O solution is equivalent to 35.46 g of Cl
2

1000 ml of 0.1 N Na
2
S
2
O
3
.5H
2
O solution is equivalent to 3.546 g of Cl
2

1 ml of 0.1 N Na
2
S
2
O
3
.5H
2
O is equivalent to 3.546 x 10
-3
g of Cl
2

Volume of Na
2
S
2
O
3
solution consumed V
4
= ________ ml

V
4
ml of N
2
normality solution of Na
2
S
2
O
3
.5H
2
O
is equivalent to (X
1
) = (V
4
x N
2
x 3.546 x 10
-3
) / (1 x 0.1)
= _________ g.

10 ml of Bleaching powder solution contains X
1
g of Cl
2.



250 ml of Bleaching powder solution contains = (X
1
x 250) / 10 = X
2
g of Cl
2
.
Weight of bleaching powder taken = w g
% of chlorine = X
2
x 100 / w

= _________ %































10. 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:
K2Cr2 O7 + 4 H2SO4 K2SO4 + Cr2 (SO4)3 + 3 (O) + 4 H2O
C3 H8 O3 + 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.

CHEMICALS REQUIRED
Glycerol (standard and sample), 10% KI solution, starch, dil. H2SO4 , Sodium thiosulphate and
Potassium dichromate solutions.

PROCEDURE
I. Standardization of Sodium thiosulphate:

1) Titrate 20 ml of std. Potassium dichromate solution + 20 ml of dil. H2SO4 + 10 ml of
10% KI solution against Sodium thiosulphate solution.
2) 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.
3) Repeat the above procedure for concordant values.
II. Estimation of Glycerol:
1) 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.
2) Heat the contents of iodine flask on a water bath for 60 min and cool.
3) Add 1 test tube of dil. H2SO4 and 10 ml of 10 % KI solution to the above solution.
4) Titrate the liberated iodine against std. Sodium thiosulphate solution using starch
indicator. End point is the colour change from blue to green.
5) Repeat this procedure with pure standard Glycerol.




RESULT
The percentage purity of the given sample of Glycerol was found to be _________%.

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

Burette Reading (ml) S.NO Volume Of
K
2
Cr
2
O
7

Solution
(V1) ml
Initial Final
Volume Of Sodium
Thio Sulphate
Solution
(ml)
Concordant
Value (ml)

1


2



Volume of K
2
Cr
2
O
7
(V1) =
Normality of K
2
Cr
2
O
7
(N1) =
Volume of Na
2
S
2
O
3
(V2) =
Normality of Na
2
S
2
O
3
(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:

Burette Reading (ml) S.NO Volume Of
Glycerol
Solution
(V
3
) ml
Initial Final
Volume Of Sodium
Thio Sulphate
Solution (V4)ml
Concordant
Value (ml)

1


2



B. Estimation of Standard Glycerol:

Burette Reading (ml) S.NO Volume Of
Glycerol
Solution
(V
3
) ml
Initial Final
Volume Of Sodium
Thio Sulphate
Solution (V
5
)ml
Concordant
Value (ml)

1


2






sample
V
N
N V
Glycerol sample with O Cr K unreacted of Volume =

=
1
2 4
7 2 2

std
V
N
N V
Glycerol dared s with O Cr K unreacted of Volume =

=
1
2 5
7 2 2
tan
Volume of reacted
7 2 2
O Cr K =
7 2 2
O Cr K volume taken initially volume of unreacted
7 2 2
O Cr K
= 60 - volume of unreacted
7 2 2
O Cr K
Glycerol of mg 10 152 . 0 1
7 2 2
= O Cr K N of ml
( )
mg w solution sample the in Glycerol of Amount
N ml V
sample
sample
= = =

10
152 . 0
60
1

( )
mg w solution dard s the in Glycerol of Amount
N ml V
std
std
= = =

tan 10
152 . 0
60
1



100 =
std
sample
w
w

ml V dichromate unreacted to ing correspond te thiosulpha of Volume
4
=
100
tan
=
Glycerol dard s of weight
Glycerol sample of weight
Glycerol of purity Percentage





11. PROXIMATE ANALYSIS 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 -110
0
C. 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.
100

=
taken coal of Weight
Weight of Loss
Moisture %
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 C
0
50 925 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.
100

=
taken coal of Weight
matter volatile of removal to due weight in Loss
Matter Volatile %
iii) Ash: The residual coal was then heated in a muffle furnace at 50
0
C 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.
100

=
taken coal of Weight
taken ash of Weight
Ash %
( ) Matter Volatile Ash Mositure of Carbon Fixed % % % 100 + + =
Result:
S.No Proximate Analysis of Percentage
1. Moisture
2 Volatile Matter
3 Ash
4 Fixed Carbon










Calculation:

Weight of coal taken = g
Weight of crucible = g
Wt. of coal + crucible = g
After heating to 105
0
C (Oven) = g
100

=
taken coal of Weight
Weight of Loss
Moisture % ) i
After heating Muffle Furnace 925
0
C
100

=
taken coal of Weight
matter volatile of removal to due weight in Loss
Matter Volatile % ) ii
Heating half an hour in muffle furnace 50
0
C
100

=
taken coal of Weight
taken ash of Weight
Ash % ) iii

( ) Matter Volatile % Ash % Mositure of % Carbon Fixed of % + + =100






























12. FLASH AND FIRE POINT

Aim:
To determine flash and fire point for the given sample.

Apparatus Required:
Pensky Martens closed flash tester, thermometer and sample.

Procedure:
i) All parts of the cup were cleaned and dried before starting the test.
ii) The cup was filled with sample to be tested to the level indicated by filling mark.
iii) The lid was placed on the cup and thermometer was inserted.
iv) The material to be tested and tester was brought to a temperature of C
0
5 15 , lower than
the estimated flash point.
v) The heat was supplied at such a rate that the temperature in thermometer increased.
vi) The stirrer was turned at low flow rates such that the stirrer was directed in the downward
direction.
vii) 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.
viii) The temperature was increased till fuel burned for 5 second. The fire point temperature
was noted.
Result:
The flash and fire point for the given sample was found to be ____
0
C and
________
0
C

respectively.

Tabular Column:

Sample Flash Point (
0
C) Fire Point (
0
C)










DEPARTMENT OF CHEMICAL ENGINEERING
LAB MANUAL
CH 2257 - CHEMICAL ANALYSIS LAB
INDEX

S.NO NAME OF THE EXPERIMENT PAGE NO REMARKS
1 Estimation of Acid value ( Analysis of Oil) 1
2 Estimation of Saponification value(Analysis of Oil) 3
3 Estimation of Iodine value (Analysis of Oil) 5
4 Estimation of Silica content (Analysis of Cement) 8
5 Estimation of Mixed oxide content(Analysis of Cement) 9
6 Estimation of Calcium oxide content(Analysis of Cement) 10
7 Estimation of Total fatty matter content 11
8 Estimation of Total alkali content 12
9 Estimation of Residual chlorine in water 13
10 Estimation of Purity of Glycerol 16
11 Estimate the Proximate analysis of the given sample of coal 19
12 Determine the Flash and Fire point for the given samples 21





Prepared by Reviewed by Approved by





CH2257 CHEMICAL ANALYSIS LAB 0 0 3 2


OBJECTIVE



To learn basic principles involved in estimation and characterization of industrially important
materials.

I. Soap Analysis
a. Estimation of total fatty acid.
b. Estimation of percentage alkali content.

II. Oil Analysis
a. Estimation of free acid
b. Determination of Saponification value
c. Determination of iodine value

III. Cement Analysis
a. Estimation of Silica content
b. Estimation of mixed oxide content
c. Estimation calcium oxide content
d. Estimation of calcium oxide by rapid method

IV. Coal Analysis
a. Estimation of Sulphur present in coal
b. Ultimate analysis of coal
c. Proximate analysis of coal

V. Analysis of Bleaching Power
a. Estimation of Available Chlorine

VI. Analysis of Glycerol
a. Estimation of purity of glycerol

VII. Analysis of fuels
a. Flash point
b. Fire point
c. Cloud point
d. Pour point
e. Aniline point

TOTAL : 45 PERIODS
REFERENCES
1. Technical Analysis Manual, Chemistry Division, Chemical Engineering Department, A.C.
Tech. Anna University (2007).
2. Hand book of Chemical Analysis by Griffin.
















SSN COLLEGE OF ENGINEERING

SSN NAGAR, KALAVAKKAM 603 110.





DEPARTMENT OF CHEMICAL ENGINEERING







CHEMICAL ANALYSIS
LAB MANUAL