Exp.

No: Date:
DETERMINATION OF IODINE VALUE OF AN OIL
Aim: To determine the iodine value of the given sample of oil.
Apparatus required:
Burette, Pipette, Stoppered flask, Conical flask, Measuring jar, Funnel and Standard measuring
flask.
Chemicals or Reagents required:
Oil, 0.1N Potassium dichromate (K2Cr2O7), 0.1N Soium thio sulphate (Na2S2O3.5H2O), 10%
Potassium iodide (KI), Wij’s solution,6N Sulphuric acid (H2SO4) and Carbon tetra chloride (CCl4).
Principle:
Iodine value or iodine index of oil is defined as the mass of Iodine in gram that is consumed by
100gms of oil. This value measures the unsaturation present in the oil, this un-saturation is in the forms
of double bonds which react with iodine compounds. Higher the iodine number, the more unsaturated
fatty acid bonds are present in a fat.In a typical procedure, a known weight of oil sample mixed with a
known excess of Wij's solution (solution of Iodine monochlorate in glacial acetic acid). The unreacted
ICl (Iodine monochlorate) is titrated back with a standard solution of thio using starch as indicator.
Procedure:
I. Standardization of Thio:
 Prepare a standard solution of 0.1N K2Cr2O7
 Take 20ml of this solution add to it, 20ml of 6N H2SO4 and 20 ml of 10%KI in a conical flask.
 Add few drops of thio until the solution becomes yellow in colour and then add starch
indicator. The solution becomes steel blue in colour.
 Titrate this solution against thio, until steel blue colour disappears and tabulate the reading.
II. Determination of Iodine Value:
 Weigh out accurately about 1gm of the oil into a 250ml glass stoppered flask.
 Dissolve it in 25ml of carbon tetrachloride and then accurately add 20ml Wij's solution with
the help of a pipette. Stopper the flask and shake for about 20 minutes.
 Add 20ml of 10% KI solution with shaking for about 10 minutes.
 Titrate it with (excess of iodine) 0.1N thio solution using starch as indicator, until the
disappearance of blue colour (end point is colourless) and tabulate the readings.
 Perform a blank experiment simultaneously by repeating the entire procedure with out using
oil. Note the thio solution required for the blank experiment also.

Observation and Calculation:

Titration-I: Standardization of Thio
Burette solution : Thio Solution
Pipette solution : Standard K2Cr2O7
Indicator : Starch
End point : Appearance of steel blue colour

Volume of Burette reading (ml) Volume of thio

S.No. Concordant value
K2Cr2O7 (ml) Initial Final (ml) (ml)

1. 20 0

2. 20 0

 Volume of dichromate taken (V1) =

 Normality of dichromate (N1) =
 Volume of thio run down (V2) =
V1 x N1 = V2 x N2
N2 = V1 x N1 / V2
 Normality of thio (N2) =

Titration-II: Determination of Iodine Value

Burette solution : Thio Solution
Pipette solution : Oil Sample
Indicator : Starch
End point : Disappearance of blue colour

Volume of ICl Burette reading (ml)

S.No Analysis Volume of Thio
(ml) Initial Final (ml)

1. Blank 20 0

2. Oil sample 20 0

 Weight of oil taken (W) = 1 gm

 Volume of thio consumed for 20 ml of Wij's solution, (V3) =
 Volume of thio consumed for oil + 20 ml of Wij's solution, (V4) =
Therefore,
 Volume of thio consumed by oil = V3 – V4 =
 Strength of iodine in oil (g/lit) = N2 * Equivalent wt. of Iodine (127)
=
=
 Strength of iodine in (V3 – V4) ml of oil =
[Strength of iodine in oil (g/lit) * (V3 – V4)] / 1000

Iodine value of the given sample of oil

= Strength of iodine in (V3 – V4) ml of oil * 100
Wt. of oil taken

RESULT:

INFERENCE:

Exp.No: Date:
 DETERMINATION OF SAPONIFICATION VALUE OF AN OIL
Aim: To determine the saponification value of a given sample of oil.

Apparatus required:
Burette, Pipette, Round bottom flask, Reflux condenser, Standard measuring flask, Conical flask
and Measuring jar.
Chemicals or Reagents required:
Oil, 0.5N Alcoholic potassium hydroxide (KOH), 0.5 N Hydrochloric acid (HCl), 0.5N Sodium
Carbonate (Na2CO3) and Alcohol.
Principle:
Saponification is a hydrolysis of an ester with alkali to give alcohol and salt of the
acid.Saponification is the number of mg of alkali required to saponify fatty materials present in 1gm of
oil. A known weight of the oil is mixed with a known excess of std. alcoholic alkali solution and
reflux.The unreacted alkali is titrated with std. acid using phenolphthalein as indicator.
Procedure:
I. Standardization of HCl:
 Prepare 0.5N std. Na2CO3 solution
 Take 20ml of this solution in a conical flask and add few drops of methyl orange indicator.
 Titrate it against std.HCl, until the appearance of pale pink colour. Tabulate the reading.
II. Standardization of KOH:
 Take 20ml of 0.5N alcoholic KOH and add few drops of phenolphthalein indicator.
 Titrate it against std. HCl, until the disappearance of pale pink colour. Tabulate the reading.
III. Determination of Saponification value:
 Transfer about 2gms of accurately weighed oil sample to a round bottom flask and add 20ml of
0.5N alcoholic KOH and 20ml of alcohol through a pipette.
 Fit the round bottom flask with reflux condenser and reflux the condensate on a water bath for a
minimum period of one hour.
 Cool the condenser, disconnect it and rinse it with small amount of distilled water and collect the
washings in a conical flask.
 Add 5 drops of phenolphthalein indicator and titrate the contents of the two flasks with Std.
solution of 0.5N HCl until the pink colour has just disappears.
 Perform a blank experiment simultaneously by repeating the entire procedure without using oil.

Observation & Calculation:

Titration-I: Standardization of HCl
Burette solution : Hydrochloric Acid
Pipette solution : Standard Na2CO3
Indicator : Methyl Orange
End point : Appearance of pale pink colour

S.No Volume of Burette reading (ml) Volume of HCl Concordant value

Na2CO3 (ml) Initial Final (ml) (ml)

1. 20 0

2. 20 0

Normality of HCl (N2) =

Titration-II: Standardization of KOH
Burette solution : Hydrochloric Acid
Pipette solution : Alcoholic KOH solution
Indicator : Phenolphthalein
End point : Disappearance of pink
 colour

S.No Volume of KOH Burette reading (ml) Volume of HCl Concordant value
(ml) Initial Final (ml) (ml)

1. 20 0

2. 20 0

 Volume of KOH
taken (V3) =
 Normality of std. HCl (N4 = N2) =
 Volume of std. HCl run
down (V4) =
V3 x N3 = V4 x N4
V4 x N4 /
N3 = V3

Normality of KOH (N3) =

Titration-III: Determination of Saponification of Oil
Burette solution : Hydrochloric Acid
Pipette solution : Oil Sample
Indicator : Phenolphthalein
End point : Disappearance of pink colour

Volume of KOH Burette reading (ml) Volume of HCl

S.No Analysis
(ml) Initial Final (ml)

1. Blank 20 0

2. Oil sample 20 0

 Weight of oil taken (W) = 2 gm

 Volume of HCl consumed for 20 ml of alcoholic KOH, (V5) =

 Volume of HCl consumed for oil + 20 ml of alcoholic KOH,(V6) =

Therefore,
Volume of HCl consumed by oil = (V5 – V6)=
Volume of KOH consumed by oil, (V7) = [(V5 – V6) * N4] / N3

=
=

Strength of KOH in oil (g/lit or mg/ml) = N3 * Equivalent wt. of KOH (56)

=
Amount of KOH in V7 ml of oil (mg) = Strength of KOH in oil (mg/ml) * V7
=
=
Saponification value of the given sample of oil
 = Amount of KOH in V7ml ofoil W

RESULT:

INFERENCE:

Exp.No: Date:
DETERMINATION OF ACID VALUE OF AN OIL
Aim: To determine the acid value of the given sample of an oil.
Apparatus required:
Burette, Pipette, Conical flask, Beaker and Measuring jar.
Chemicals or Reagents required:
Oil, 0.1N KOH, Neutral Ethyl alcohol, Oxalic acid, Phenolphthalein indicator.
Principle
The acid value (also known as neutralization number) of an oil is defined as the milligrams of potassium hydroxide
(KOH) required to neutralize the free acid present in 1gm of an oil.
For the determination of acidity of an oil, a known weight of oil is dissolved in a suitable organic
solvent and is titrated with a standard solution of KOH using phenolphthalein as indicator. The reaction is
RCOOH (free acid in oil) + KOH → RCOOK + H2O
Procedure:
I. Standardization of KOH:
 Prepare a standard 0.1N Oxalic acid solution.
 Take 20ml of this solution and add few drops of phenolphthalein indicator.
 Titrate it against KOH, until the appearance of pale pink colour. Tabulate the reading.
II. Determination of Acid value:
 Weigh accurately 10gms of the given sample of oil in a dry 250ml conical flask.
 Add 50ml of a mixture of equal volume of 95% alcohol and water.
 Agitate the whole mixture and then heat it to the boiling point for 10 minutes and cool it.
 Add a drop of phenolphthalein indicator and titrate it against the standard solution of potassium
hydroxide, till the pink colour persists for 10 seconds.
 Perform a blank titration by following exactly all the above described steps without taking oil.
 The difference in the volume of potassium hydroxide required in these two titrations will represent
the equivalent of acid present in the oil.

Observation and Calculation:

Titration-I: Standardization of KOH
Burette solution : Standard KOH solution
Pipette solution : Oxalic Acid Solution
Indicator : Phenolphthalein
End point : Appearance of pale pink colour
Volume of Concordant value
S.No. Oxalic acid Burette reading (ml) Volume of KOH
(ml)
(ml) Initial Final

1. 20 0

2. 20 0

 Volume of std. Oxalic acid taken (V1) =

 Normality of std. Oxalic acid (N1) =
 Volume of KOH run down (V2) =
V1 x N1 = V2 x N2
N2 = V1 x N1 / V2

Normality of KOH (N2) =

Titration-II: Determination of Acid value of Oil

Quantity of the oil taken (W) =
Volume of KOH solution (a) =
Normality of KOH solution =
Volume of KOH solution required for blank (b) =
 Therefore,
Volume of KOH equivalent to acid content of oil = (a – b)
=

Now,1ml of KOH solution = 5 mg of KOH

Therefore (a – b) ml of KOH solution = (a – b) X 5mg of KOH
Therefore,

Acid value of oil solution = (a – b) X 5 mg of KOH

W g of oil

=
=

RESULT:

INFERENCE:

Exp. No: Date:

DETERMINATION OF FATTY MATTER CONTENT IN SOAP
Aim: To determine the total fatty matter present in the given sample of soap.
Apparatus required:
 Beaker, Hot water bath, Standard flask, Measuring jar, Watch glass, Glass rod and Oven.
Chemicals or Reagents required:
Soap and Nitric acid (dilute).
Principle:
Soap is defined as the sodium (alkali) salt of higher fatty acid (present in oil). It is the product that results
from the reaction between a fatty acid and an alkali (strong base).
Soap is produced by Saponification or basic hydrolysis reaction of a fat or oil. The reaction is Fat (in
oil) + NaOH → Sodium salt of fatty acid (Soap) + Glycerol
Here, the fatty acid portion (in oil) is turned into salt because of the presence of NaOH. Although the
reaction is shown as a single step, it is actually a two step reaction. The second step is that the ester bonds are
broken and the glycerol turns into alcohol. In cleansing soaps, the fatty acids (come form oils and fats are metallic
salts of high molecular weight) are linear chain mono-carboxylic acids. They are water soluble. In acid medium
soaps are converted into its fatty acid, they are insoluble in water at cold conditions. These insoluble fatty acids may
be separated and gives the total fatty matter of soap.
Procedure:
 Weigh about 20gms of the soap sample and dissolve it in 150ml of hot water.
 Transfer the solution while hot into a 250ml standard flask and make up to the mark.
 Pipette out 100ml of the made up original solution into a 250ml beaker.
 Add dilute nitric acid until the contents become slightly acidic.
 Heat the solution on the water bath until all the fatty acids are collected in a clear layer on top and the
solution below is perfectly clear.
 Weigh accurately about 5g of paraffin wax and add to the contents of the beaker.
 Continue the heating on the water bath, till the wax completely melts and gets mixed with the fatty acids as
the top layer and the solution remains perfectly clear.
 Cool in ice water or let it stand overnight.
 Remove carefully, the wax layer containing fatty acids and wash it with distilled water.
 Dry carefully between the faces of the filter papers and transfer to a previously weighed watch glass.
 Weigh accurately the wax layer and subtract from it, the amount of wax previously taken.
 Report as a percentage.

Observation and Calculation:

Weight of soap transferred =

Weight of wax taken =
Weight of total fatty matter + wax =
Weight of total fatty matter alone =
100ml solution contains =
250ml solution contains =

Percentage of total fatty matter = Amount of Fatty matter in 250ml X 100

Weight of Soap

RESULT:

Exp.No: Date:
ESTIMATION OF ALKALI CONTENT IN SOAP
Aim: To estimate the amount of alkali content in soap.
Apparatus required:
 Conical flask, Beaker, Standard measuring flask, Pipette, Burette and Measuring jar.
Chemicals required:
Soap, 0.5N Hydrochloric acid (HCl), 0.5N Sodium hydroxide (NaOH), 0.5N Sodium carbonate (Na 2CO3)
and Phenolphthalein.
Principle:
Soap is defined as the sodium (alkali) salt of higher fatty acid (present in oil). It is the product that results
from the reaction between a fatty acid and an alkali (strong base).
Soap is produced by Saponification or basic hydrolysis reaction of a fat or oil. The reaction is
Fat (in oil) + NaOH → Sodium salt of fatty acid (Soap) + Glycerol
Here, the fatty acid portion (in oil) is turned into salt because of the presence of NaOH. Although the
reaction is shown as a single step, it is actually a two step reaction. The second step is that the ester bonds are
broken and the glycerol turns into alcohol.
In cleansing soaps, the fatty acids (come form oils and fats are metallic salts of high molecular weight) are
linear chain mono-carboxylic acids. They are water soluble. In acid medium soaps are converted into its fatty acid,
they are insoluble in water at cold conditions. These insoluble fatty acids may be separated and gives the total fatty
matter of soap.
Procedure:
I. Standardization of HCl:
 Prepare 0.5N std. Na2CO3 solution.
 Take 20ml of this solution in a conical flask and add few drops of methyl orange indicator.
 Titrate it against std.HCl, until the appearance of pale pink colour. Tabulate the reading.
II. Standardization of NaOH:
 Prepare 0.5N std.NaOH solution.
 Take 20ml of this solution in a conical flask and add few drops of phenolphthalein indicator
 Titrate it against std.HCl, until the disappearance of pale pink colour. Tabulate the reading.
III. Estimation of Alkali content:
 Dissolve 5gm of soap in 100ml of hot water, in a 250ml beaker.
 To this add 40ml of 0.5N HCl.
 Heat the solution on a water bath and collect the fatty acids layer and separate it.
 Cool the solution and filter it using distilled water.
 Combine the washings & filtrate and titrate the excess acid with NaOH solution (0.5N).
 The amount of HCl consumed is calculated in terms of Na 2O and expressed in terms of percentage.

Observations and Calculations:

Titration-I: Standardization of HCl
Burette solution : Hydrochloric Acid solution
Pipette solution : Std. Na2CO3Solution
Indicator : Methyl Orange
End point : Appearance of pale pink colour

Volume of Burette reading (ml) Volume of HCl Concordant value

S.No.
Na2CO3 (ml) Initial Final (ml) (ml)

1. 20 0

2. 20 0

 Volume of Na2CO3 taken (V1) =

 Normality of Na2CO3 (N1) =
 Volume of HCl run down (V2) =
 V1 x N1 = V2 x N2
N2 = V1 x N1 / V2

Normality of HCl (N2) =

III. Estimation of Alkali content in Soap:

 Initial weight of soap taken, W1 =
The titration between the presence of excess acid (in washings and filtrate) and the NaOH gives,
 Volume of NaOH consumed by HCl, V5 =
 Volume of HCl reacted with NaOH, V6 = V5 N3 / N4
=
=
Volume of HCl consumed by alkali in soap, V7(ml) = 40 – V6

=
No. of grams of NaOH consumed, W2 (gm)
= [V7 * N3 * Equiv. wt. of NaOH (40)] / 1000

=
Based on the reaction,
2 NaOH → Na2O + H2O
(Mol. wt) 80 62 18

Amount of Na2O present in soap, W3 (gm) = (62 / 80) * W2

=
=

Percentage (%) of Na2O present in the soap

= Amount of Na2O present in soap, W3 X 100 Initial
weight of soap taken, W1

RESULT:

Exp. No: Date:

DETERMINATION OF AVAILABLE CHLORINE IN BLEACHING
POWDER
Aim: To determine the percentage of available chlorine (Cl 2) in a given sample of bleaching powder.
Apparatus required:
Conical flask, Beaker, Standard measuring flask, Pipette, Burette and Measuring jar.
Chemicals required:
Bleaching powder, 0.1N Thio (Na2S2O3.5H2O), 6N Sulphuric acid (H2SO4), 10% Potassium Iodide (KI),
0.1N Potassium dichromate (K2Cr2O7),acetic acid and Starch.
Principle:
Bleaching powder consists essentially of a mixture of calcium hypo chlorite (CaO 2Cl2) and the basic
chloride (CaCl2.Ca(OH)2.H2O). Bleaching powder is made by passing chlorine gas over dry slaked lime at
temperature ranging between 40 to 55 oC. At higher temperatures beyond this limit, a considerable amount to
chlorine is formed. Hence a careful control of the temperature is necessary. Chemically, bleaching powder is
Calcium chloro hypochlorite which when treated with water forms Calcium chloride and Calcium hypochlorite
according to the equation.

2 CaClOCl CaCl2 + Ca (OCl) 2
The chlorine of the hypochlorite is the bleaching agent and is called the available chlorine of the bleaching
powder. The available chlorine is estimated by the Bunsen and Wagner method. Bleaching powder solution or
suspension is treated with an excess of a solution of KI in strongly acid medium liberates CI 2, and is titrated with a
solution of standardized sodium thio sulphate.
Procedure:
I. Standardization of Thio:
 Prepare a standard solution of 0.1N K2Cr2O7 solution.
 Take 20ml of this solution add to it, 20ml of 6N H2SO4 and 20 ml of 10%KI in a conical flask.
 Add few drops of thio till the solution becomes yellow in colour and then add starch indicator till
the solution becomes steel blue in colour.
 Titrate this solution against thio, until steel blue colour disappears and tabulate the reading.
II. Determination of Cl2 content in bleaching powder:
 Weigh out accurately about 5 gm of the bleaching powder in to a clean mortar. Add a little water,
rub the mixture to a paste and grind the residue with little more water.
 Pour off the milky liquid into 500ml std. measuring flask. Repeat the operation until the whole of
the sample as been transferred to the flask and make up the volume with distilled water.
 After well shaken, pipette out 50ml of the turbid solution into a clean conical flask.
 Add 10ml of 10% KI and 10ml of acetic acid and titrate it against 0.1N thio solution, as before,
using starch as indicator & tabulate the readings.

Observation and Calculation:

Titration-I: Standardization of Thio
Burette solution : Thio Solution
Pipette solution : Standard K2Cr2O7
Indicator : Starch
End point : Disappearance of blue colour
Volume of thio
Volume of K2Cr2O7 Burette reading (ml) (ml) Concordant value
S.No. (ml) (ml)
Initial Final

1. 20 0

2. 20 0

 Volume of dichromate taken (V1) =

 Normality of dichromate (N1) =
 Volume of thio run down (V2) =
V1 x N1 = V2 x N2
N2 = V1 x N1 / V2

Normality of thio (N2) =

 Titration-II: Determination of Cl2 content in bleaching powder

Burette solution : Sodium thio sulphate solution

Pipette solution : Bleaching powder solution

Indicator : Starch indicator

End point : Disappearance of blue colour

Volume of Burette reading (ml)

S.No. Bleaching Volume of Thio Concordant value
powder solution (ml) (ml)
(ml) Initial Final

1. 50 0

2. 50 0

 Volume of Thio run down (V3) =

 Normality of std. Thio (N3 = N2) =
 Volume of Bleaching powder solution taken (V4) =
V3 x N3 = V4 x N4
N4 = V3 x N3 / V4

Normality of Bleaching powder solution (N4) =

Initial weight of bleaching powder taken, W1 =

Strength of available Chlorine (gm/lit) = N 4 X Equivalent weight of Cl2

=
Amount of available chlorine present in 500ml of the solution =

Percentage of available chlorine in bleaching powder

= Amount of available Chlorine in bleaching powder, W2 * 100 Initial
weight of bleaching powder taken, W1

RESULT:

Exp. No: Date:

ESTIMATION OF SILICON DIOXIDE CONTENT IN CEMENT
Aim: To estimate the percentage of silicon-dioxide content in cement.
Apparatus required:
Beaker, Measuring jar, Glass rod, Crucible and Pipette.
Chemicals required:
Cement sample and Conc. Hydrochloric acid (HCl).
Theory:
A cement is a binder, which sets and hardens independently and can bind other materials. The methods of
production of cement are;
 Cement rock beneficiation
 Portland cement production
Process description: Cement or calcium rock is ground and fed to hydro-separators where the overflow goes directly
to the final thickener, being thickened for satisfactory composition. Then it is floated to remove silica-mica and talc.
Floatation is based on the ability of collecting agent to wet certain materials entrained in an air froth, which rises to
the surface and overflows. The flotation cell and the thickener are cascaded units. In later units, flotation liquor is
recycled and beneficiated, then it is fed directly to the cement kilns. In the kiln, it is superheated and dried to form
cement granule or powder.
Cement contains about 17-25% of silica. Silica reacts with lime to form calcium silicate (C 3S & C2S) which
determines strength to the cement.
Procedure:
 Weigh 2 gm of cement accurately and transfer it to a beaker.
 Add 5ml of conc. HCl and 20ml of distilled water to it.
 Heat the mixture for about half an hour till the effervescence ceases.
 Cool the contents of the flask and filter through a Whatmann filter paper.
 Transfer the filter paper along with the residue to the crucible. Dry in a muffle furnace at 200°C.
 Note down the dried residue weight.

Observations & Calculations:

Weight of cement sample taken W1 (gm) =

Weight of empty crucible W2 (gm) =

Weight of gravimetric filter paper W3 (gm) =

Weight of the filter paper + residue after incineration W4 (gm) =
Weight of silicon dioxide residue W5 (gm) = W4 – (W2 + W3)

Percentage of silicon dioxide = Weight of silicon dioxide residue, W5 * 100

Weight of cement sample taken, W1

RESULT:

Exp.No: Date:
ESTIMATION OF MIXED OXIDE CONTENT IN CEMENT
Aim: To estimate the percentage of mixed oxide content in cement.
Apparatus required:
Std. measuring flask, Conical flask, Crucible, Beaker and Measuring jar.
Chemicals required:
Cement, Ammoniumchloride (NH4Cl), Bromine water, 1:1NH3 solution and Methyl orange.
Theory:
A cement is a binder, which sets and hardens independently and can bind other materials. The methods of
production of cement are;
 Cement rock beneficiation
 Portland cement production
Process description: Cement or calcium rock is ground and fed to hydro-separators where the overflow goes directly
to the final thickener, being thickened for satisfactory composition. Then it is floated to remove silica-mica and talc.
Floatation is based on the ability of collecting agent to wet certain materials entrained in an air froth, which rises to
the surface and overflows. The flotation cell and the thickener are cascaded units. In later units, flotation liquor is
recycled and beneficiated, then it is fed directly to the cement kilns. In the kiln, it is superheated and dried to form
cement granule or powder.
The presence of iron oxide in cement imparts strength and colour.
Procedure:
 Collect the filtrate from silicon dioxide experiment and dilute to 100ml in a standard measuring flask.
 Transfer it to a 250ml conical flask and add 5gm of NH 4Cl, 5ml of bromine water and 2 drops of methyl
orange indicator.
 Boil the mixture for 15 to 20 minutes, cool and add 1:1 NH3 until the solution turned yellow.
 Filter the solution through a Whatmann filter paper and wash with 2% NH 4Cl.
 Dissolve the precipitate in 1:1 HCl and filter it again through a Whatmann filter paper and wash with 2%
NH4NO3 solution.
 Transfer the filter paper along with residue to a crucible and dry at 200°C in a muffle furnace.
 Note down the dried residue weight.

Observations & Calculations:

Weight of cement sample taken W1 (gm) =

Weight of empty crucible W2 (gm) =

Weight of gravimetric filter paper W3 (gm) =

Weight of the filter paper + residue after incineration W4 (gm) =

Weight of mixed dioxide residue W5 (gm) = W4 – (W2 + W3)

Percentage of mixed oxide = Weight of mixed oxide residue, W5 * 100

Weight of cement sample taken, W1

RESULT :
Exp.No: Date:
ESTIMATION OF CALCIUM OXIDE CONTENT IN CEMENT
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, NH4Cl, NH3, 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 NH4Cl to avoid the precipitation of Ca and Mg compounds
10) Add 20 ml of NH3 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.
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 =_______________

Exp. No: Date:

 ESTIMATION OF PURITY OF GLYCEROL
Aim: To determine the purity of the given sample of glycerol by dichromatic method.
Apparatus required:
Conical flask, Beaker, Standard measuring flask, Pipette, Burette, Measuring jar and Tri-pod
stand.
Chemicals required:
Glycerol, 0.5N Ferrous Ammonium Sulphate (FAS) (Mohr’s Salt) [Fe(SO4)2(NH4)2.6H20], 6N Sulphuric acid
(H2SO4), 0.5N Potassium dichromate (K2Cr2O7) and Potassium ferri-cyanide K3[Fe(CN)6].
Theory:
Glycerol is a colorless, odorless syrupy liquid. It contains one secondary and two primary alcoholic groups
as, it is of form

CH2OH
|
CHOH
|
CH2OH
The three hydro-phylic hydroxyl groups are responsible for its solubility in water. It is a normal
ingredient of soap and is used for the manufacture of many compounds.
It has a molar mass of 92.0938 g/mol, density of 1.261 g/cc and viscosity of 1.5 Pa-s. It has a
melting point of 18oC and boiling point of 290oC. The dichromate method is based on the fact that
potassium dichromate in the presence of sulphuric acid completely oxidizes glycerol to CO 2 and H2O. The
amount of potassium dichromate left behind is estimated by titration with ferrous ammonium sulphate.
From the amount of dichromate reacted the purity of glycerol is calculated.
Procedure:
I. Standardization of Ferrous Ammonium Sulphate
 Prepare a standard solution of 0.5 N K2Cr2O7
 Take 20ml of this solution and add to it 20 ml of 6N H2SO4 in a conical flask.
 Titrate it against FAS using potassium ferric-cyanide, as external indicator.
 The end point is appearance of dark blue colour.
 Repeat it for concordant value and tabulate it.
II. Estimation of Purity of Glycerol
 Weigh about 5g of glycerol and transfer it into a 100ml standard measuring flask and make the
solution up to the level.
 20ml of glycerol solution, 20ml of 6N H 2SO4 and 40ml of 0.5N K2Cr2O7 is taken in a beaker or
conical flask and heat the content over a water bath for 30 to 45 minutes.
 Cool the contents and titrate it against FAS using potassium ferri-cyanide as external indicator. End
point is the change of colour to dark blue.
 The amount of dichromate reacted with glycerol is calculated and from this the purity of glycerol
can be estimated.

Observation and Calculation:

Titration-I: Standardization of FAS

Burette solution : FAS Solution
Pipette solution : Standard K2Cr2O7
Indicator : Potassium ferric-cyanide

End point : Appearance of dark blue colour

Volume of
Burette reading (ml) Volume of FAS Concordant value
 (ml) (ml)
(ml) Initial Final

1. 20 0

2. 20 0

 Volume of dichromate taken (V1) =

 Normality of dichromate (N1) =
 Volume of FAS run down(V2) =
V1 x N1 = V2 x N2
N2 = V1 x N1 / V2

Titration-II: Estimation of Purity of Glycerol

Burette solution : FAS Solution
Pipette solution : Glycérol
Indicator : Potassium ferric-cyanide
End point : Appearance of dark blue colour

Volume of Burette reading (ml) Volume of FAS Concordant value

S.No Glycerol Solution
(ml) (ml)
(ml) Initial Final

1. 20 0

2. 20 0

 Initial weight of Glycerol taken, W1 = 5gm By

principle,
 Volume of FAS consumed by titration, V3 (ml) = Volume of K2Cr2O7 unreacted
=
 Volume of K2Cr2O7 reacted, V4 (ml) = K2Cr2O7 taken initially – V3
=
=
Amount of K2Cr2O7, W2 (gm) = (Normality * Equiv. wt. of K2Cr2O7) * V4 =
[(0.5/1000) * 49] * V4
=
We know that,
1gm of K2Cr2O7 = 0.1341gm of Glycerol.
‘W2’ gm of K2Cr2O7 is equivalent to (0.1341* W2) gm of Glycerol [W3]

Percentage (%) purity of Glycerol,

= (Amount of Glycerol estimated) * (Volume of glycerol prepared) * 100
(Initial weight of Glycerol) (Volume of glycerol taken)

= [W3 / W1] * [100 / 20] * 100

RESULT:
Expt. No: Date:

DETERMINATION OF MOLECULAR WEIGHT OF POLYMERBY VISCOMETRY

Aim: To determine the molecular weight of the given polymer.

Apparatus Required:
Beaker, Pipette, Viscometer, stop watch.
Chemicals Required:
Polymer, Benzene or Toluene.
Principle:
The size of the polymer molecule depends on the number of repeat units it contains and that this number
represents the degree of polymerization (DP).It provides another way of expressing the molecular weight of polymer
as follows.
M= DP X M0 or DP= M/M0

where M is the molecular weight of the polymer, DP its degree of polymerization and M 0 the molecular weight of
the monomer or repeating unit. So the degree of polymerization can be calculated from the molecular weight of the
polymer.

Viscosity is an useful technique for determining the molecular weight of polymer. The viscosity of a high
polymer soluction is related to the molecular weight of the polymer by Mark-Kuhn-Houwink (MKH) equation,

[η] = K.Ma

where, [η] is the intrinsic viscosity and M is the average molecular weight of polymer. K and a are constants for a
given solvent-polymer system at a particular temperature. The constant lies between 0.6 to 0.8 and K x 10 4 lies
between 0.5 to 5.0.

If η and ηo are the absolute viscosities of a solution and pure solvent, respectively and t and t o are their
corresponding flow time, then, t/t0 = η/ηo. The term η/ηo is known as the relative viscosity. This term and other
terms related to viscosity measurements are given as follows:

Relative viscosity ηr = η/ηo = t/t0,

Specific viscosity, ηsp = (η- ηo )/ ηo = (t-to)/to;

Reduced viscosity, ηred = (ηsp / C);

Intrinsic viscosity, [η] = (ηsp / C)ηo.

where C is the concentration in g/dl of the polymer in the solvent.

Intrinsic viscosity can be obtained by plotting (η sp /C) against concentration and extrapolating the curve to
C=0; the intercept on the ordinate axis is the intrinsic viscosity.

Procedure:
I.Preparation of polymer solution:
 Weigh accurately 500 mg of the dried, powdered polymer to a 100 ml standard flask.
 Dissolve it in solvent (benzene or toluene) and fill the flask up to the mark.
 Concentration of the solution is 0.5%.
 Make solutions of 0.1%, 0.2%, 0.3% and 0.4% by appropriate dilution.

II.Measurement of flow time with Ostwald Viscometer:

 Pipette out 10 ml of the solvent in to the wide arm of the dry viscometer.
 Using a rubber ball, force air in to the wide arm so as to raise the level of the liquid into the capillary arm
above the higher mark.
  Then release the pressure and with a timer, measure the time in which the liquid meniscus moves from the
upper mark to the lower mark.
 Repeat to get three values and use the average as the flow time to.
 Similarly, determine the flow times for polymer solutions of different concentrations using same volume,
properly cleaning and drying the viscometer whenever the solution is to be changed.
 Note the temperature at which the experiments are to be carried out.
Observations & Calculations

Temperature of the lab = ------------------ oC

Value of K for the solvent =

Value of ‘a’ for the solvent =

Volume of the liquid used = --------------- ml

Flow time of the solvent = --------------- s.

Polymer Solution Flow time (s)

ηr ηsp ηred
concentration
1 2 3 Mean = t/to = ηr-1 = ηsp/C
C%

[η] = KMa

log[η] = log K +( a x log M)

log M = (log[η]- log K)/a

M = antilog {(log[η]- log K)/a}

DP = M/M0

RESULT

Expt.No: Date:

ESTIMATION OF THE STRENGTH OF HYDROCHLIRIC ACID BY pH METRY

Aim: To estimate the strength of given hydrochloric acid given using pH meter.
Apparatus required:
Burette, pipette, beaker, pH meter, electrodes, standard measuring flask.

Chemicals/Reagents:
Hydrochloric acid, Sodium Hydroxide, Sodium carbonate, Oxalic acid.

Principle:
Methyl red, also called C.I. Acid Red 2, is an indicator dye that turns red in acidic solutions. It is an azo dye,
and is a dark red crystalline powder. Methyl red is a pH indicator; it is red in pH under 4.4, yellow in pH over 6.2,
and orange in between, with a pKa of 5.1. Murexide and methyl red are investigated as promising enhancers of
sonochemical destruction of chlorinated hydrocarbon pollutants. Methyl red is classed by the IARC in group 3 -
unclassified as to carcinogenic potential in humans.
In practice, a pH value is defined by the equation below:
pH=-log10 [H+]
This equation means that the pH value is a common logarithm expressing the reciprocal of the hydrogen ion
concentration. The pH value of a neutral solution is obtained as 7 from the following calculation:
[H+]=10-7
When the hydrogen ion concentration decreases (e.g., [H +] =10-10), the pH value is 10 showing that the
solution is alkaline. When it increases (e.g., [H+]=10-3), the pH value is 3 showing that the solution is acid.
A large number of animals and plants inhabit lakes, rivers, and oceans. The pH values of those water areas
differ depending on the kinds of animals and plants that can live there. In general, the pH values which allows
animals and plants to live are in the neutral range. Animals and plants can no longer live if the pH values of their
habitat become acidic or alkaline. The cause of such pH changes are mainly wastewater from factories and
households.
The measuring methods for pH values include using an indicator reagent, the metal electrode methods
(hydrogen electrode method, quinhydrone electrode method, and antimony electrode method), and the glass
electrode method. The glass electrode method is considered to be the standard measuring method. In practice,
however, pH values are obtained from hydrogen ion activity (thermodynamic activity) rather than hydrogen ion
concentrations.
Sorenson introduced the pH scale of hydrogen ion concentration. Ionic product of water is 10 -14.Therefore it
is neutral. If the hydrogen ion concentration is more the 10 -7 the solution is acidic whereas it is alkaline if the
hydrogen ion concentration is less than 10 -7 .

The most convenient and reliable method of measuring pH of a solution is to use an electrolytic instrument
called pH meter which measures the EMF of the concentration formed from a reference electrode. The test solution
and glass electrode are sensitive to hydrogen ions. In the pH meter, the values are directly displaced as pH values.

Procedure:

I. By Volumetric Analysis:

 Prepare exactly 0.1N sodium carbonate, in a 100 ml standard volumetric flask.

 Pipette out 20 ml of the unknown hydrochloric acid in a 250 ml conical flask.
 Add 5 drops of methyl red indicator, and titrate against sodium carbonate solution taken in the burette.
 Change of color is noted from red to yellow.

II. By pH metry:

 Standardize the pH meter using pH 4 buffer solution.

 Wash the electrode with distilled water.
 Pipette out 20ml of the given hydrochloric acid solution into to a clean beaker.
 Immerse the electrode in to the drug solution.
 Note the pH value by the addition of each 1ml of 0.1N NaOH solution from the burette.
  After well stirring, continue the addition up to a pH of 13.
 After the jump, repeat the experiment by adding 0.01 ml nearing the end point.
 Draw a graph by plotting pH Vs the volume of std NaOH solution.
 Determine the equivalence point from the graph.
 Calculate the strength of hydrochloric acid.
 The molecular weight of hydrochloric acid 36.5.

Observation and Calculation:

Titration-I: By Volumetric Analysis

Burette solution : Hydrochloric acid

Pipette solution : Std.Na2CO3 solution

Indicator : Methyl Red

End point : Colour change from red to yellow

Burette reading (ml) Volume of

S.No Volume of Sodium Concordant
Hydrochloric
. carbonate (ml) Initial Final value (ml)
acid (ml)

1. 20

2. 20

Volume of Sodium carbonate solution (V1) =

Normality of Sodium carbonate solution (N1) =

Volume of HCl solution taken (V2) =

V1 x N1 = V2 x N2

N2 = V1 x N1 / V2

Normality of Hydrochloric acid (N2) =

Weight per litre = Equivalent mass x Normality

Amount of the substance in 100 ml of the solution =

Titration- II: Standardisation of NaOH

Burette solution : Std. Hydrochloric acid

Pipette solution : Sodium hydroxide solution

 Indicator : Phenolphthalein

End point : Disappearance of pink colour

Volume of NaOH Burette reading (ml) Volume of HCl Concordant value

S.No.
solution (ml) Initial Final (ml) (ml)

1. 20

2. 20

Volume of HCl solution (V3) =

Normality of HCl solution (N3) =

Volume of NaOH solution taken (V4) =

V3 x N3 = V4 x N4

N4 = V3 x N3 / V4

Normality of Sodium Hydroxide solution (N4) =

Titration-III: By pH metry
Volume of pH pH/V Volume of pH pH/V
NaOH NaOH

(ml) (ml)

Model
Graph:
Equivalence point (from Graph) =

Normality of drug solution = V5 x N4 / N2

Weight per litre = Equivalent mass x Normality

Amount of the substance in 100 ml of the solution =

RESULT: