Beruflich Dokumente
Kultur Dokumente
EXPERIMENTAL PROCEDURE
1)
2)
3)
4)
5)
6)
S.NO VOLUME OF
OXALIC ACID
(ml)
VOLUME OF
KOH
CONSUMED (ml)
Concordant
Value (ml)
1
2
CALCULATION (1)
Volume of oxalic acid
(V1)=
(N1)=
(V2)=
(N2)= V1 N1 / V2
WEIGHT OF
OIL
(gm)
VOLUME OF KOH
(ml)
1
2
CALCULATION(2)
Acid value =
Concordant
Value (ml)
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
S.NO
VOLUME OF
OIL
SOLUTION
(gl)
VOLUME OF
ALCOHOLIC
KOH SOLUTION (ml)
BURETTE READING
(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 NKOH x Equivalent wt of KOH
Weight of the sample
Saponification value = _________________
PROCEDURE
STANDARDIZATION OF SODIUM THIOSULPHATE SOLUTION
1.
2.
3.
4.
5.
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
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 H2SO4 solution
Indicator
: Starch
End point
:Disappearance of blue
S.NO
VOLUME OF
K2Cr2O7 SOLUTION
(ml)
BURETTE READING
(ml)
INITIAL
VOLUME OF SODIUM
THIOSULPHATE SOLUTION
(ml)
FINAL
1
2
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
S.NO
VOLUME OF
SOLUTION (ml)
BURETTE READING
(ml)
INITIAL
VOLUME OF SODIUM
THIOSULPHATE SOLUTION
(ml)
FINAL
Oil solution
V2 =
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 = _____________.
(w) =
g
g
% of silica = ( b a ) x100
w
% of silica = ____________
RESULT
The amount of silica content was found to be =______________.
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 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) 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 (Fe2O3 + Al2O3) = ( b a ) x250 x100
w x 100
% of Mixed oxide content = ____________
RESULT
The amount of mixed oxide content was found to be=_____________.
10
)g)
(g)
(g)
11
(x) = _____________
= (y x) * 100
Weight of soap sample
12
ml
ml
N
N
g
RESULT
The total alkali content of the given soap sample was found to be___________.
13
RESULT
The amount of Residual chlorine in the water sample was found to be _________%.
14
Titration I:
Standardization of Sodium thio sulphate solution
Burette solution
Pipette solution
Additional solution
Indicator
End point
BURETTE READING
(ml)
FINAL
INITIAL
VOLUME OF SODIUM
THIO SULPHATE SOLUTION
(ml)
2
Volume of K2Cr2O7
Normality of K2Cr2O7
Volume of Na2S2O3
Normality of Na2S2O3
(V1) =
(N1) =
(V2) =
(N2) = (V1xN1) / V2
Titration II:
Estimation of Available Chlorine:
Burette solution: Standard Sodium Thio sulphate solution
Pipette solution : 10 ml of Bleaching powder solution + 10 ml of H2SO4 + 10 ml of 15%KI
: Starch
Indicator
End point
: Blue to colorless
S.NO VOLUME OF BLEACHING BURETTE READING (ml) VOLUME OF SODIUM
POWDER SOLUTION
THIO SULPHATE
INITIAL
FINAL
(V3) ml
SOLUTION (V4)ml
15
CALCULATION
1 equivalent of Cl2 = 1 Equivalent of I2
1000 ml of 1 N Na2S2O3.5H2O solution is equivalent to 35.46 g of Cl2
1000 ml of 0.1 N Na2S2O3.5H2O solution is equivalent to 3.546 g of Cl2
1 ml of 0.1 N Na2S2O3.5H2O is equivalent to 3.546 x 10-3 g of Cl2
Volume of Na2S2O3 solution consumed V4 = ________ ml
V4 ml of N2 normality solution of Na2S2O3.5H2O
is equivalent to
(X1)
= (V4 x N2 x 3.546 x 10-3) / (1 x 0.1)
= _________ g.
10 ml of Bleaching powder solution contains X1 g of Cl2.
16
Add 60
17
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
Pipette solution
Additional solution
: 10 ml of H2SO4 + 10 ml of 10% KI
Indicator
: Starch
End point
: Blue to green
S.NO
Volume Of
K2Cr2O7
Solution
(V1) ml
Volume Of Sodium
Thio Sulphate
Solution
(ml)
Concordant
Value (ml)
1
2
Indicator
: Starch
End point
: Blue to Green
tube of
18
Volume Of
Glycerol
Solution
(V3) ml
Volume Of Sodium
Thio Sulphate
Solution (V4)ml
Concordant
Value (ml)
Volume Of Sodium
Thio Sulphate
Solution (V5)ml
Concordant
Value (ml)
1
2
Volume Of
Glycerol
Solution
(V3) ml
1
2
V4 N 2
= Vsample
N1
V5 N 2
= 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
sample
) ml N
0.152
(60 Vstd ) ml N1
0.152
mg
mg
wsample
wstd
100
19
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.
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.
Proximate Analysis of
Moisture
Volatile Matter
Ash
Fixed Carbon
Percentage
20
Calculation:
Weight of coal taken
Weight of crucible
Wt. of coal + crucible
After heating to 1050C
= g
= g
= g
(Oven)
Loss of Weight
100
i ) % Moisture =
Weight of coal taken
After heating Muffle Furnace 9250C
Loss in weight due to removal of volatile matter
100
ii ) % Volatile Matter =
Weight of coal taken