Beruflich Dokumente
Kultur Dokumente
AIM
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
EXPERIMENTAL PROCEDURE
1
2
CALCULATION (1)
Volume of oxalic acid (V1)=
Normality of oxalic acid (N1)=
Volume of KOH consumed (V2)=
Normality of KOH consumed (N2)= V1 N1 / V2
1
2
CALCULATION(2)
ml of KOH Normality of KOH Eq.wt of KOH
Acid value =
Weight of Oil Sample
AIM
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
RESULT
The saponification value of the given oil sample was found to be_____________.
4
TABULAR COLUMN
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 = _________________
5
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:
PROCEDURE
1. Pipette out 20 ml of 0.1 N potassium dichromate solution into a clean conical flask.
2. Add 1 test tube of dilute H2SO4 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
RESULT
The iodine value of the given oil sample was found to be =___________.
7
TABULAR COLUMN
Titration I
Standardisation of Sodium thiosulphate:
Burette solution :Sodium thiosulphate
Pipette solution :Potassium dichromate
Additional solution :1 test tube of dil H2SO4 solution
Indicator : Starch
End point :Disappearance of blue
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 : 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
2 Blank V1 =
CALCULATION:
Iodine value = (V1 V2) x N1 x Equivalent weight of Iodine x 100
W x 1000
where
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 = _____________.
8
4. ESTIMATION OF SILICA CONTENT (ANALYSIS OF CEMENT)
AIM
APPARATUS REQUIRED
Crucible, Desiccator, Beaker, Water bath, No 40 Wattman filter paper, Pipette, Electric
Bunsen Burner, Stirrer
CHEMICALS REQUIRED
PROCEDURE
CALCULATION:
Weight of cement taken (w) = g
% of silica = ( b a ) x100
w
% of silica = ____________
RESULT
AIM
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
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
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
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
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 HNO3 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
RESULT
The percentage of total fatty matter present in the given sample of soap was found to
be_________.
12
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 H2SO4 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 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
RESULT
The total alkali content of the given soap sample was found to be___________.
13
9. ESTIMATION OF RESIDUAL CHLORINE IN WATER
AIM
APPARATUS REQUIRED
CHEMICALS REQUIRED
Potassium iodide, Sulphuric acid, Sodium thio sulphate, Bleaching powder, Starch
Indicator
PROCEDURE
RELATED EQUATIONS
2 KI + Cl2 2 KCl + I2
KI + I2 KI3
I2 + 2 Na2S2O3 2 NaI + Na2S4O6
I2 + Starch Complex having deep blue complex
RESULT
The amount of Residual chlorine in the water sample was found to be _________%.
14
Titration I:
Titration II:
2
15
CALCULATION
= _________ %
16
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:
RESULT
The percentage purity of the given sample of Glycerol was found to be _________%.
Titration I:
1
2
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
18
1
2
1
2
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 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
19
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.
Result:
S.No Proximate Analysis of Percentage
1. Moisture
2 Volatile Matter
3 Ash
4 Fixed Carbon
20
Calculation: