Haldia Institute of Technology Engineering Chemistry Laboratory (CH 191 &CH 291)
Haldia Institute of Technology Engineering Chemistry Laboratory (CH 191 &CH 291)
Experiment No: 1
Name: Conductometric titration for determination of the strength of a given HCl
solution by titration against a standard NaOH solution.
Theory:
The monobasic acid HCl being a strong electrolyte undergoes complete ionization and
produces a large number of cations and anions in solution. Moreover ionic conductance of H +
ions being highest (I0 H+ = 350). Thus the initial conductance of a solution will be very high.
When this acid is gradually titrated against a base NaOH, being added from burette, the
following reaction will occur.
The salt, a strong electrolyte remains in the solution in completely ionized form, while water
being a very weak electrolyte ( 10
9
and in presence of H+ ions its ionization is still smaller)
remains partially ionized.
Thereby H+ ions are gradually replaced by equivalent amount of Na + ions which have relatively
much lower ionic conductance than that of H+ ions. Thus the conductance of resulting solution
will decrease steeply.
This trend will continue until all the H+ ions are replaced by Na+ ions i.e. equivalent point is
reached. At equivalent point only NaCl is present.
Beyond equivalent point when further amount of alkali is added Na + and OH- of excess alkali
remain in the solution unutilized. Consequently the conductance of the solution increases due to
the presence of newly added Na+ and OH- ions (Io OH- = 200).
The point of intersection of curve representing the variation of conductance with the volume of
alkali added, corresponding to the minimum conductance and consequently equivalence point.
The volume of alkali added corresponding to the equivalent point represents the volume of alkali
required for neutralization of acid.
Instruments and apparatus:
Conductivity meter
Conductivity cell
Beaker
Burette
Pipette
Volumetric flask
Conical flask
Funnel
Materials:
N
Standard oxalic acid 10
N
2 NaOH solution
N
HCl solution
10
Phenolphthalein indicator
Procedure:
N
1. Prepare 100 ml of standard oxalic acid order 10 .
N
2. Prepare 250 ml of an approximately 2 NaOH solution and standardize it against oxalic acid
solution using phenolphthalein as indicator.
N
3. Prepare 250 ml of an approximately 10 HCl solution.
5. Pipette out 25 ml of HCl solution into the conductivity cell and add water if necessary, so that both the
electrodes are completely immersed within the solution. Join the cell with the conductive bridge and
measure the conductivity very carefully.
7. Measure the conductance of the solution after addition of 10 drops of NaOH and mildly shaking the
beaker. Repeat the process until you have at least six points beyond the end points.
8. Draw a curve by plotting the conductance against the drops of alkali added, find the end point and
calculate the strength of the HCl solution.
Results:
w
W1 W2 W1-W2 = w 1.575 1.575 (N/10)
2 10
3 20
4 30
5 40
6 50
7 60
8 70
9 80
10 90
11 100
12 110
13 120
14 130
15 140
16 150
Calculations:
x
Therefore, 20 drops = 1 ml then x drops = 20 ml
V1S1 = V2S 2
V2S2
S1
Then, V1
Precautions:
Theory:
All pH meters have provision for standardizing the glass electrode in a buffer solution of known
pH.This is necessary because different electrodes have different asymmetry potentials. Once the
adjustment has been made so that the meter Registers correctly known the pH of the buffer solution, the
instrument gives the pH other solution without any calculation.
Measurements of pH are also employed to monitor the course of acid-base titrations. The pH values of the
solution at different stages of acid-base neutralization are determined and are plotted against volume of
1
pHlog
acid/alkali added. On adding abase to an acid, the pH rises slowly in the initial stages H (pH
range is used for only dilute solution, not for concentrated solution) and then it changes rapidly at the end
point. Then it flattens out. The end point of the titration can be detected where the pH changes most
rapidly. However the shape of the inflexion point (i.e. where the pH changes abruptly) and symmetry of
the curve on its two sides depends upon the ionisability of the acid and the base used and on the basicity
of the acid and the acidity of the base.
Apparatus:
Beaker
Burette
Pipette
Materials:
Procedure:
1. Wash the electrodes with distilled water and standardize the pH meter by using buffer solution of pH
=4 and pH=9, now the selector switch is put to a pH range of 7-14.
N
2. Prepare 100 ml of standard oxalic acid order 10 .
3. Prepare 250 ml of an approximately NaOH solution and standardize it against oxalic acid solution
using phenolphthalein as indicator.
N
4. Prepare 250 ml of an approximately 10 HCl solution.
5. Clean the electrodes by distilled water and wipe them with tissue paper.
7. Add NaOH solution from the burette dropwise. Note the corresponding value from the meter. Near the
end point add very small amount of NaOH as possible because change in pH will be very much
appreciable because when the acid is neutralized, further addition of such a small amount raises the pH to
about 9 or 10.
8. Put back the selector to zero position after pH measurement and before removing the electrodes from
solution
9. Plot a graph between pH and drops of NaOH added. From this graph, determine the volume of NaOH
required for the complete neutralization of HCl.
Experimental Data:
w
W1 W2 W1-W2 = w 1.575
1.575 (N/10)
25
Calculation:
Let the number of drops of alkali required to neutralized 25 ml of HCl solution = x
x
Therefore, 20 drops = 1 ml then , x drops = 20 ml
V1S1 = V2S 2
V2S2
S1
Then, V1
Precautions:
Electrodes must be immersed properly in the solution and sufficient time to be allowed
for the electrodes to assume the temperature of the solution.
For pH-metric titration, solution should be stirred mechanically from time to time’
Experiment No.: 03
Name: Determination of dissolved oxygen present in a given water sample
Theory:
Dissolved oxygen (DO) determination measures the amount of dissolved (or free) oxygen
present in water or wastewater. Aerobic bacteria and aquatic life such as fish need dissolved
oxygen to survive. If the amount of free or DO present in the wastewater process is too low, the
aerobic bacteria that normally treat the sewage will die. DO is determined by the titrimetric
method developed by Winkler.
1. Dissolved molecular oxygen in water is not capable of reacting with KI, therefore an oxygen carrier such as
manganese hydroxide is used. Mn(OH)2 is produced by the action of KOH on MnSO4.
2. Mn(OH)2 so obtained reacts with dissolved molecular oxygen to form a brown precipitate of basic
manganic oxide, MnO(OH)2.
3. MnO(OH)2 then reacts with concentrated sulphuric acid to liberate nascent oxygen.
4. Nascent oxygen results in oxidation of KI to I2.
5. This liberated iodine is then titrated against standard sodium thiosulphate solution using starch as an
indicator.
6. Thiosulphate reduces iodine to iodide ions and itself gets oxidized to tetrathionate ion. (Refer the reactions
below).
Iron and nitrite interfere with this procedure. The interference of nitrite can be eliminated by
adding sodium azide. If ferric ion is present, H 3PO4 is used instead of H2SO4
2NaOH + MnSO4 → Mn(OH)2 + K2SO4
2Mn(OH)2 + O2 → 2MnO(OH)2
MnO(OH)2 + H2SO4 → MnSO4 + 2H2O + [O]
2KI + H2SO4 + [O] → K2SO4 + H2O + I2
I2 + I ־ → I3 ־
Apparatus Required:
Burette
Pipette
Conical flask
Beaker
Measuring cylinder
Volumetric flask
Wash bottle
Glass stoppered bottle
Chemicals required:
Sodium thiosulfate
Potassium dichromate
Potassium iodide
Sulfuric acid
Manganese (II) sulfate
Sodium azide
Sodium hydroxide
Ortho phosphoric acid
Starch
Procedure
Weigh out approximately 0.0620 gm of sodium thiosulphate in a clean 250 ml volumetric flask and
dissolve in small amount of distilled water. Then make up to the volume of the flask with distilled water.
Weigh out exact 0.2942 gm of A.R potassium dichromate and transfer it in a 100 ml volumetric flask and
add 50 ml distilled water to it. Dissolve the solid completely in distilled water and then fill the mark with
distilled water.
W
0. 2949 M
=( ) ×( 100 )
Pour 11 ml of concentrated sulfuric acid in a50 ml of distilled water in a100 ml volumetric flask and then
dilute the solution to 100 ml with distilled water and mix properly.
Take 0.1 gm of starch and make a paste with little amount of water. Then pour the paste with
constant stirring to 100 ml of water and boil for 1 minute. Allow the solution to cool at room temperature.
Pipette out 25 ml of standard potassium dichromate solution in a conical flask. Add 25 ml of 4(N) H 2SO4
and 10 ml of 20% KI solution to it. Cover the conical flask with a watch glass and keep it in dark for 3
minutes. Then dilute the solution with 200 ml of distilled water. Titrate the solution with the sodium
thiosulfate solution running from burette. When the colour of the solution becomes pale yellow, add 2 ml
of the starch solution. The solution will turn blue. Continue the titration until the color changes from blue
to colorless.
N1V1 =N2V2
Dissolve 50 gm of manganese (II) sulphate solution in small amount of distilled water and mix well.
Then make up the volume to 100 ml.
Weigh 2.5 gm of NaOH and dissolve in 50 ml of distilled water. Then dissolve 0.675 gm of KI and 0.5 gm
of sodium azide to the solution and mix well.
Take 300 ml water sample in a glass stoppered bottle. The bottle always well stoppered to prevent any
sample exposure to air. Now, add 1 ml of 50% manganese (II) sulphate (MnSO 4) to water sample.
Similarly, add 1 ml of alkaline iodide azide solution. Shake well to mix uniformly. A brown precipitate
will be formed. If precipitate not form then add 2 ml of 2 (N) NaOH solution to the water sample and
allowed to settle down for 15 minutes. Then add 2 ml of concentrated phosphoric acid to dissolve the
precipitation. After the complete dissolution of brown precipitate, iodine is released in the solution. Now
pipette out 100 ml of the solution in a conical flask and titrate the liberated iodine with sodium thiosulfate
solution running from the burette. When the colour of the solution becomes pale yellow, add 2 ml of the
starch solution. The solution will turn blue. Continue the titration until the color changes from blue to
colorless.
Calculation:
V × y × 8 ×1000
1000 mL water sample = mg dissolved oxygen.
V1
Precautions:
Any sample contact with air should be avoided as per as possible. Exposure of air will lead to higher
results.
Exclude air bubbles carefully while replacing the stopper.
Use freshly prepared starch solution for the titration.
Add starch solution while approaching the end point. If the starch solution is added in highly concentrated
iodine solution, some iodine is absorbed since starch gives water insoluble complex with iodine.
Experiment No.: 04
Name: To determine chloride ion in a given water sample by Argentometric method (using
chromate indicator solution
Theory:
Chlorides are present in water usually as NaCl, MgCl 2 and CaCl2. Although chlorides are not harmful as
such, their concentrations over 250 pomp impart a peculiar taste to the water thus rendering the water
unacceptable for drinking purposes.
By argentometric method, chloride ions in a water sample (neutral or slightly alkaline) can be determined
by titrating it against standard silver nitrate (AgNO 3) solution using potassium chromate (K 2CrO4) as an
indicator. The pH should be in between 7-8. At higher pH, silver ions are precipitated as silver hydroxide.
At lower pH, potassium chromate indicator is converted to potassium dichromate (K 2Cr2O7).
Argentometric method is based on the precipitation titration in which silver nitrate solution is released
from the burette to the water sample which contains chloride ions and indicator. The silver ions (from
silver nitrate solution) react with chloride ions (from water sample) and chromate ions (from indicator) to
form white precipitate of silver chloride and red precipitate of silver chromate.
Red colour formed because of formation of silver chromate disappears initially as the solution contains
high concentration of chloride ions.
When the concentration of chloride ions has decreased, the red colour starts disappearing slowly and
slowly on shaking and a stage is reached when all the chloride ions have formed silver chloride. One extra
drop of silver nitrate at this point reacts with potassium chromate and reddish coloured silver chromate is
formed.
2AgNO3 + K2CrO4 → Ag2CrO4 + 2KNO3
Apparatus Required:
Burette
Pipette
Conical flask
Beaker
Measuring cylinder
Volumetric flask
Wash bottle
Chemicals Required:
Silver nitrate
Sodium chloride
Potassium chromate
Procedure:
5gm of potassium chromate is dissolved in about 5ml of distilled water. Few drops of silver nitrate are
added until a definite red precipitate forms. It I allowed to stand for 12 hours, filtered and diluted to 100
ml with distilled water.
2. Preparation of 1000 ml
(50M ) standard sodium chloride (NaCl) solution
Weigh out about 1.17 gm of NaCl and transfer in a1000 ml volumetric flask and add small amount of
distilled water to it. Dissolve completely the solid in distilled water and fill the mark with distilled water
and mix thoroughly.
Table 1: Preparation of
(50M ) standard sodium chloride (NaCl) solution
Weigh about 3.4 gm of silver nitrate and dissolve in 50 ml of distilled water and then dilute to 1000 ml in
a dark bottle.
Table 2: Standardization of silver nitrate solution against standard sodium chloride solution
M1V1 = M2V2
Pipette out 25 ml of the water sample in a conical flask. Add 5 drops of potassium chromate indicator to
it and titrate the solution with silver nitrate solution running from the burette. A red color of silver
chromate appears and again redissolves. Continue the titration until a pinkish or reddish tinge persists in
the yellow solution with constant swirling of the liquid in the conical flask throughout the titration
procedure.
Table 3. Determination of the amount of chloride ion in the given water sample
Suppose y ml of the silver nitrate solution is required for the titration of the given water sample.
= 35.5 gm of Cl
35 .5
¿
1 ml 1(M) silver nitrate solution 1000 gm of Cl
35 .5× y×S2
y ml of S2 (M) silver nitrate solution = 1000 gm of Cl
= (35.5×y×S2) mg of Cl
Therefore,
35 .5× y×S2×1000
1000 ml sample water contains 25 mg of Cl
= A mg/L
Therefore, the concentration of the chloride in the given water sample is A mg/L
Precautions:
Each apparatus should be washed with distilled water which is free of chlorine.
Carefully handle silver nitrate and avoid any skin contact since silver nitrate is corrosive and leave black
spots.
Add same amount of potassium chromate indicator each time.
Perform the titration with constant swirling of the liquid in the conical flask.
Experiment No. –
Name: Determination of percentage composition of sugar solution from
viscosity
Theory:
When a fluid passes through one another, due to internal friction, it experiences a resistance to its
flow which is known as viscosity. The coefficient of viscosity is a measure of the resistance and defined
as the tangential force per unit area required to maintain unit difference of velocity between two layers
unit distance apart. Its unit in CGS system is dyne.sec/cm 2.
When a homogeneous fluid of volume ‘v’ flows through a capillary tube of length ‘l’, radius ‘r’, in time
‘t’, under a driving force ‘p’, the co-efficient of viscosity is given according to Poisseuille’s formula by
Pr4 t
8lv
1 = and 2 =
1
t
11
,o
r
1t
1
2
t
22
1 2
1t
2
where x is the unknown concentration of supplied sugar solution.
Apparatus:
Viscometer (Ostwald)
Stop watch
Pipettes
Beakers
Materials:
Distilled water
Procedure:
The weight of dry specific gravity bottle, filled with water and with supplied solution was
taken. At first 5%, 10%, 15% and unknown sugar solution were prepared by proper dilution. The
density of the solution was determined. The viscometer was cleaned thoroughly a clamped
vertically. Then a fixed amount of sugar solution was taken in it by sucking up and allowed to
fall freely between the two marks and time was noted and repeated for three times. For 5%, 10%,
15% and unknown solution the same was repeated.
Experimental Data:
W1 W2 W 2- W 1= W w W3 W3-W1= Ws
Density (gm/cc)
Relative density, or specific gravity, is the ratio of the density (mass of a unit volume) of a
substance to the density of a given reference material. Specific gravity usually means relative
density with respect to water. It is unitless.
m
Density ρ = v , where m = mass of liquid, V = volume of liquid
ms
v
ρs mw
Therefore relative density of solution = ρw = v
ms
ρw
As v is same for both liquid, therefore ρs = mw
5% solution 1
10% solution 1
15% solution 1
Unknown 1
solution
2
ρs t s
Therefore, ηs = ρw t w ηw where ηs = viscosity of sugar solution
ηw = viscosity of water
ρw = density of water
Precautions:
The viscometer should be clamp in a vertical position and its height must remain
constant each time when it is clamped.
EXP. NO. – 11
Theory: Saponification value of oil is defined as the number of milligram of KOH needed to saponify
one gram of oil. Saponification is in fact the alkali hydrolysis of oil and fat. A fat is mixer of various
glycerides, the esters of glycerols with higher fatty acid like steric acid Palmitic acid etc. It reacts with
alkali under goes hydrolytic decomposition and converts into soap and glycerol.
O H O
O +3 NaOH soap
C17H31 – C – O – C – H HEAT +
O C 3H8O3
C17H31 – C – O – C – H glycerol
fat
So if an excess of alkali is made to react with a known amount of the oil sample, some of the alkali will
be used up for saponification, depending upon the amount of which the saponification value of oil can be
found out by titrating excess alkali against a standard acid solution.
Chemicals required:
Procedure:
1. Standardise the aicoholic (N/20) KOH solution against standard (N/20) oxalic acid:
Take an aliquot of 25 ml of the standard (N/20) oxalic acid in a 250 ml conical flask, add 2-3 drops of
phenolphthalein indicator, dilute to 50 ml and titrate with the (N/20) KOH solution up to a red end
point.
Calculation:
Strength of standard oxalic acid solution = (0.3/ 0.3152) (N/20)
25×0. 3
Therefore, Exact strength of (N/2) KOH solution = ( V1×0. 3152 ) (N/2)
Take an aliquot of 25 ml of the standard (N/20) HCl acid in a 250 ml conical flask, add 2-3 drops of
phenolphthalein indicator, dilute to 50 ml and titrate with the standard (N/20) KOH solution up to a red
end point.
Calculation:
V2×0 . 3
Therefore, Exact strength of (N/2) HCl solution = ( 2×V1×0 . 3152 ) (N)
1 to 2 ml of oil sample is introduced into a 250 ml round bottom flask or a conical flask. 25 ml 1 (N)
alcoholic KOH is added to it. This is fitted with long air condenser and refluxed in boiling water for
an hour to complete the saponification. It is then titrated; at hot condition against a standard (N/2)
HCL using few drops of phenolphthalein indicator till a distinct pink color disappears.
A blank titration is performed without taking oil into flask and required amount acid is noted down.
Calculation:
( V4−V3 )×V2×0 .3
¿
2×0 .3152×V1 ml of (N)KOH
Discussion : Discuss why your sap value might have deviated from the true value of 254 also discuss
about the change in sap value if we use NaOH instead of KOH
QUESTION:
Experiment No:13
Theory:
The Nerst distribution law states that at constant temperature, when different quantities of a
solute are allowed to distribute between two immiscible solvents I contact with each other, then at
equilibrium the ratio of the concentration of the solute in two solvent layers is constant.
When a solute is shaken in two immiscible liquids, then the solute is found to be distributed between the
liquids in a definite manner, if the solute is soluble in each of the solvent. According to distribution law,
C1
K
the distribution co-efficient at a particular temperature is given by C2 where C and C represents
1 2
the concentration of solute in solvent 1 and 2 respectively, when in solution phase solute molecules are in
same state of association.
Now, if water and n-butanol are taken as the pair of two immiscible solvents and acetic acid as the solute
then as acetic acid retains its normal molecular weight in both the solvents, so the expression for partition
co-efficient will be
K=
Apparatus:
Stoppered bottles
Volumetric flask
Conical flask
Burette
Pipette
Materials Required:
NaOH solution
Acetic acid
N-Butanol
Distilled water
Phenolphthalein indicator
Procedure:
1. A standard oxalic acid solution of (N/10) was prepared and NaOH solution was
standardized against standard oxalic acid solution using phenolphthalein indicator.
2. In bottle 1, 20 ml acetic acid, 490 ml water and 490 ml n-butanol was added. Similarly
in bottle 2, 40 ml acetic acid , 480 ml water and 480 ml n-butanol was added.
3. Stoppered bottles were shaken for one hour and allowed to stand till the two liquid
layers separated.
4. Definite volume of aqueous layer and organic layer from each of the two bottles were
taken out and standardized against NaOH solution Using Phenolphthalein as indicator.
Experimental Results:
Table 1: Composition of materials in each bottle
Bottle 1 Bottle 2
Weight to be
Initial weight(gm) Final weight(gm) Weight taken(gm) Strength
taken(gm)
w
W1 W2 W1-W2 = w 1.575
1.575 (N/10)
Burette reading
Volume of Strength of
No. of Volume of Strength of
oxalic acid NaOH
observation Initial(ml) Final(ml) NaOH (ml) oxalic acid
(ml) solution
Table 4: Standardization acetic acid in aqueous layer and n-butanol layer by NaOH
solution
5
Organic layer
5
2
5
Aqueous layer
5
Calculation:
K=
Precaution:
During withdrawing aliquot one layer must not be contaminated with the other.