Engineering chemistry
Laboratory Manual
INDEX
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3
INTRODUCTION
Apparatus :
In titrimetric analysis, while using the following apparatus, we should take some
precautions to minimize the practical errors.
1) Burette : Generally the burette has the capacity of holding 50 ml and graduated
1/10 of a milliliter and it will be graduated from the top to bottom and at the lower
end it is provided with stop cock to regulate the flow of solution.
a) The burette should always be kept in non – greasy condition. For this
condition, the burette is cleaned with chromic acid and then thoroughly washed
with tap water and then distilled water.Then the burette should be thoroughly
rinsed with little of solution which is to be filled in it and reject the rinsed
solution.
b) The burette is filled with the standard solution. The burette readings should be
noted with out parallax error and then it should be vertically clamped in a
burette stand.
c) While taking the readings it is better to hold a white paper behind the burette
readings and eye must be placed in the same line of the meniscus. Generally
the reading tangential to lower meniscus in the case of colourless or light
coloured solutions and upper meniscus incase of concentrated or deeply
coloured solutions, is taken as the burette reading.
2) Volumetric pipette : The pipette is a long narrow tube having cylindrical bulb in
the middle and tapping to a fine nozzle at its lower end and carrying a mark round
the glass tube above the bulb. The volume delivered between the upper mark and
lower tip is the volume being titrated. (Caution ! Don’t blow the last drop in the
nozzle of the pipette). With this we can transfer a definite volume of solution
from one flask to another. The pipette should be washed repeatedly with tap water
and then distilled water and then rinsed with a little of solution which is to be
transferred.
3) Graduated pipette : Another type of pipette used in the laboratory is the graduated
pipettes for transferring approximate volumes of reagents (such as acids, alkalis,
indicators etc.,) . These are graduated in 1/10 of a milliliter, for every milliliter.
These are available to measure 1.0 ml , 2.0 ml, 5.0 ml , 10.0 ml and 20.0 ml. An
advantage of these graduated pipettes is fraction of a ml can be measured and
transferred to the conical flask.
4) Measuring jar : This is cylindrical jar and provided with a round base at its one
end. It will be graduated from the bottom to top and has the capacity of holding
50 ml or 100 ml. and graduated in 1.0 ml units . This is only used for measuring
and transferring the approximate volumes of solutions (generally reaction medium
and other reagents), where accuracy is not important. This should be thoroughly
washed with chromic acid followed by tap water and distilled water. They are
also available in the following capacities 10 ml , 20 ml, 25 ml, 250 ml, 500ml and
1000 ml.
5) Conical flask or Erlenmayer flask : It is cone shaped flask and is used in titrations
as reaction flask. It is available in the volume range from 10 ml , 25 ml, 50 ml,
100 ml, 250 ml, 500 ml and 1000 ml. Generally 250 ml conical flasks are
6
recommended for class work. While titration is on, the neck of the conical flask
should hold using the right hand. It helps to make swirling motion of the solution
convenient by rotating the flask.
6) Distilled water bottle / Wash bottle : It is readily available in the range 500 ml,
750 and 1000 ml. it is made of pyrex glass or corning glass or polyethene. The
importance of using wash bottles is to get fine streams of water to wash down the
adhering droplets of the titrant in to the bulk of the titrand in the conical flask.
7) White glazed tile : It is white ceramic tile and helps to see the exact colour change
at the end point of the reaction by providing a glossy white back ground.
7
GENERAL INSTRUCTIONS
Before coming to the laboratory, understand the theory behind the reaction you are
going to carry out.
Keep the work - bench and sink neat and clean. Don’t allow filter paper, broken
bits of glass, sticks of matches etc., to lie on the table or in sink. Put these things
in the dustbin placed at the worktable.
Apparatus should be in non-greasy condition.
Keep the apparatus clean and properly arranged on the work - bench.
If any piece of apparatus is broken, report at once to the staff members / Lab
Assistant.
Once you have transferred a reagent from a reagent bottle, never pour it back even
if there is some excess.
Arrange reagent bottles in their proper places after use and see that they are
properly stoppered.
Handle reagent bottles / chemicals carefully.
Use only minimum possible quantity of chemicals / Reagents for any reaction.
Close the water tap immediately after use; do not waste water.
Precautions should be taken to avoid fire accidents.
After the class, before you leave the laboratory, wash the apparatus clean, wipe the
table and keep the apparatus in proper place.
8
2. Estimation of Sodium carbonate in Soda Ash.
Aim : Determination of the amount of sodium carbonate present in commercial soda
ash by using Standard Hydrochloric acid.
Theory : Sodium carbonate is a weak base has the formula Na2 CO3 and Hydrochloric
acid is a strong acid with the formula HCl. Sodium carbonate can be estimated
with a standard hydrochloric acid solution using acid-base indicator. These
two reacts as follows:
Na2CO3 + 2HCl 2NaCl + H2O + CO2
In this reaction salt and water are formed, which is an example of
neutralization reaction. All the reactants and products are colourless, so Methyl
Orange indicator is used to locate the end point of the reaction. The colour change of
methyl–orange is from yellow in alkaline medium to orange–red in acidic medium
(pH range 3.3 to 4.3). Sodium carbonate is supposed to decompose in aqueous
solution according to the following equation.
Na2CO3 + 2H2O 2NaOH + H2CO3
Methyl orange is not affected by the very weak carbonic acid formed in
solution.According to the above reaction equivalent weight of sodium carbonate is
equal to half of its molecular weight.
Procedure :
The given soda ash solution is made upto the mark of volumetric flask with
distilled water carefully. The flask is stoppered and shaken thoroughly about 3 to 5
minutes for complete homogenization.10.0 ml of the above solution is pipetted out
into a clean conical flask carefully and 50.0 ml of distilled water is added with
measuring jar. Two drops of methyl orange indicator is added directly to the of
contents of conical flask. The conical flask contents are titrated with standard
hydrochloric acid solution after noting the initial reading. The titration is continued
until the colour changes from yellow to pale red. The final reading of burette is noted.
A number of titrations are repeated for getting concurrent results. The results are
tabulated in Table No. I.
Table – I
Table– II
Percentage error table
Report:
Amount of sodium carbonate present in the given 100ml. of solution ----- gm.
***
10
Part – I :
Standardisation of potassium permanganate solution by using standard
solution of Mohr’s Salt.
Procedure : 10.0 ml of standard Mohr’s salt solution is pipetted out into a clean
conical flask carefully. 40.0 ml of distilled water and 5.0 ml of 1:1 dilute sulphuric
acid are added to the contents of the conical flask with a measuring jar. Then the
burette is filled with potassium permanganate solution after rinsing with the same
solution. Now the colourless conical flask contents are titrated with permanganate
solution after noting the initial reading of the burette, which coincides with the upper
meniscus. The titration is continued drop wise with constant shaking until a drop of
permanganate solution gives a colour change from colourless to pale pink, which is
the end point of the titration. The final reading of burette is noted with out parallax
error and results are tabulated in Table – I. A number of titrations are carried out until
2 or 3 concurrent readings are obtained.
11
Table – I
Titration of potassium permanganate solution with a standard
Mohr’s salt solution.
Normality of standard solution of Mohr’s salt ____________ N
Indicator : Self Indicator (Colour of the Potassium permanganate)
Colour change at the end point : Colourless to pale pink.
Calculations :
By the law of equivalence V1 N1 = V2 N2
Part – II :
Estimation of Ferrous iron present in a given 100 ml of ore solution by
titrating against a standard solution of potassium permanganate.
Procedure :
The given iron ore solution is diluted up to the mark of volumetric flask with
distilled water carefully and the flask is stoppered tightly. Then the solution is shaken
throughly about 3 to 5 minutes for complete homogenisation. 10.0 ml of above Iron
ore solution is pipetted out into a clean conical flask carefully. 40.0 ml of distilled
water and 5.0 ml of 1:1 dilute sulphuric acid are added to conical flask contents with a
measuring jar. Then the burette is filled with standard potassium permanganate
solution. Now the conical flask contents are titrated with permanganate solution after
noting the initial reading of the burette, which coincides with the upper meniscus.
The titration is continued by drop wise with constant shaking until a drop of
permanganate solution gives a clear cut colour change from colourless to pale pink,
which is the end point of the titration. The final reading of burette is noted with out
parallax error and the results are tabulated in Table – II. A number of titrations are
carried out until 2 or 3 concurrent readings are obtained.
12
Table – II
Titration of standard potassium permanganate solution with a unknown Iron
ore solution.
Normality of standard Potassium permanganate solution = ____________ N
Indicator : Self Indicator (Colour of the Potassium permanganate)
Colour change at the end point : Colourless to pale pink.
Calculations :
By the law of equivalence V3 N 3 =V4 N4
N3 = V 4 N 4 / V 3
Amount of Ferrous Iron present in 1 liter of solution = Normality of ferrous iron ore
solution X equivalent weight of ferrous iron = g
Amount of ferrous iron present in the given 100 ml of solution = amount present in 1
liter of solution / 10 = g
Table – III
Percentage Error Table
Report: The amount of ferrous iron present in the given 100ml. unknown
solution is g
***
13
4. Estimation of Calcium in port land cement
the reactants and products are colourless except potassium permanganate. When all
the oxalic acid has completely reacted, the excess trace amount of permanganate will
give the pink colour to the solution, which is the end point of titration. In other words
in this reaction no indicator is necessary, because potassium permanganate itself acts
as an indicator. Also one of the products that is Mn+2 ions are acting as a catalyst,
which catalyzes the preceding reaction. So it is an example of self indicator coupled
with auto catalytic type of reaction.
Part – I :
Standardisation of potassium permanganate solution by titrating against a
standard oxalic acid solution
Procedure :
10.0 ml of standard oxalic acid is pipetted out into a clean conical flask
carefully and to this 45.0 ml of distilled water followed by 5.0 ml of 1:1 dilute
sulphuric acid are added with a measuring jar. The burette is filled with potassium
permanganate solution after rinsing with the same. Now the conical flask contents are
heated to just boiling which will be indicated by commencement of bubbles from the
bottom of the flask. After noting the initial reading of the burette a small portion ( ~
0.5 ml ) of potassium permanganate is added to the hot solution of conical flask and
the flask is kept in undisturbed position until the permanganate solution is
decolourised to produce the sufficient amount of Mn+2 ions, which catalyse the
preceding reaction. Now the titration is continued while hot with permanganate
solution until the pale pink colour is obtained. The final reading of the burette is
noted which coincides with upper meniscus. A number of titrations are carried out
until 2 or 3 concurrent readings are obtained. The results are tabulated in table No - I.
15
Table – I
Titration of potassium permanganate solution with standard
Oxalic acid solution.
Calculations :
By the law of equivalence,V1 N 1 = V2 N 2
N2 = V1 N 1 / V2
Procedure :
The Potassium permanganate solution is standardised using standard oxalic
acid solution (refer Part-I of experiment No. 4). The given cement solution is diluted
upto the mark of volumetric flask with distilled water carefully. The flask is
stoppered tightly and is shaken thoroughly about 3 to 5 minutes for complete
homogenisation. 10.0 ml of cement solution is pipetted out into a clean conical flask
carefully and to this 45.0 ml of distilled water followed by 5.0 ml of 1:1 dilute
sulphuric acid are added. The burette is filled with standard potassium permanganate
solution. Now the conical flask contents are heated to just boiling. After noting the
initial reading of the burette a small portion( ~ 0.5 ml) of potassium permanganate is
added to the hot solution and kept it in undisturbed position until the decolourisation
of the permanganate solution. Now the titration is continued while hot with
permanganate solution until the colour changes from colourless to pale pink colour.
The final reading of the burette is noted. A number of titrations are carried out until 2
or 3 concurrent readings are obtained. The results are tabulated in Table – I.
16
Table – I
Titration of standard potassium permanganate solution with a unknown
cement solution.
Normality of standard solution of potassium permanganate _________ N
Indicator : Self Indicator (Colour of the Potassium permanganate)
Colour change at the end point : Colourless to pale pink.
Calculations :
By the law of equivalence, V1N 1 = V2 N 2
N 1 = V 2 N 2 / V1
The normality unknown cement solution = ________________ N
Table – II
Percentage Error Table
Report: The amount of calcium present in the 100 ml. of the given unknown cement
solution is g
***
17
5. Estimation of Hydrogen peroxide
Table – I
Titration of an unknown hydrogen peroxide solution
with standard potassium permanganate solution
Calculations : ( By weight )
Equivalent weight of hydrogen peroxide = Mol.wt./ 2= 34.02 / 2= 17.01
1 gr. Eq.weight of potassium permanganate= 1 gr.eq.weight of hydrogen peroxide. 1
gm. Eq.wt. of potassium permanganate dissolved in 1 lit.solution gives 1 normal
solution
1000 ml of 1 N solution of potassium permanganate = 17.01gm.of hydrogen peroxide
1ml of 0.1N solution of potassium permanganate = 0.001701 gm of hydrogen peroxide
10ml of hydrogen peroxide consumes‘X’ml of 0.1N potassium permanganate solution
Amount of hydrogen peroxide present in 1 lit. of solution = 100 x X x 0.001701
…………..gm.
Amount of hydrogen peroxide present in a given 100 ml of solution
=10x X x 0.001701 gm.
Table – II
Percentage Error Table
Report: The amount of hydrogen peroxide present in the 100 ml. of the given
solution is g
19
Procedure :
The given bleaching powder solution is diluted upto the mark with distilled
water carefully and stoppered well. The solution is shaken thoroughly for 3 to 5
minutes for complete homogenisation. 10.0 ml of well shaken bleaching powder
solution or suspension is pipetted out into a clean conical flask and to this 50.0 ml of
distilled water, 10.0 ml of 10% potassium Iodide solution are added using a
measuring Jar. Then the above solution is acidified by adding 10.0 ml of glacial
acetic acid and the flask is covered with watch glass for about 5 minutes for complete
liberation of iodine. The burette is filled with standard hypo solution and the initial
reading is noted. The brown coloured solution (liberated iodine) is then titrated with
standard hypo solution drop wise with constant shaking until the brown colour
becomes pale yellow. At this stage 1.0 ml of 1% freshly prepared starch solution is
20
added to this solution and the colour changes to blue. The titration is continued until
an excess drop of hypo solution changes the colour of the solution from blue to
colourless (disappearance of blue colour), which is the end point of the reaction. The
final reading of the burette is noted. A number of titrations are repeated until 2 or 3
concurrent readings are obtained. The results are tabulated in Table – I.
Table – I
Titration of bleaching powder suspension with a standard hypo solution.
Calculations :
Ca 2 pH 10 Ca pH 10 Ca
2
+ 2In-2 In2 + EDTA EDTA + 2In-2
Mg Mg Mg
unstable complex Stablecomplex Free indicator
Wine red in colour Colourless Blue in colour
The di-sodium salt of EDTA solution can be standardized by using standard zinc
sulphate solution in presence of ammonia – ammonium chloride buffer (pH 10) using
Table – I
Titration of standard EDTA solution with unknown water sample
Morality of standard solution of EDTA ____________ M
Indicator : Eriochrome Black – T.
Colour change at the end point : Wine red to blue
Calculations :
1 gram mol.weight of EDTA = 1 gram mol.weight of calcium carbonate
1 gram mol.weight of EDTA dissolved in 1000 ml of solution gives one
molar solution
1000ml of 1 M EDTA = 100 gr. of calcium carbonate
1.0 ml of 1 M EDTA = 0.1 gr of calcium carbonate
1.0 ml of 0.01 M EDTA = 0.001 gr of calcium carbonate
1.0 ml of 0.01 M of EDTA equivalent to 1.0 mg of calcium carbonate
equivalent hardness
50.0 ml of hard water samples consumes ‘x’ ml of 0.01 M EDTA solution
Report: The total hardness of the given water sample is mg/l or ppm.
***
23
Part – I :
Standardisation of Mohr’s salt solution by titration against a standard solution
of potassium dichromate.
Procedure :
10.0 ml of Mohr’s salt solution is pipetted out into a clean conical flask
carefully. 40.0 ml of distilled water, 5.0 ml of 1:1 dilute sulphuric acid and 3.0 ml of
syrupy phosphoric acid are added with measuring cylinder. One or Two drops
diphenyl amine indicator is added directly to the conical flask contents. The burette
is rinsed and then filled with standard potassium dichromate solution, the initial
reading is noted, which coincides with the lower meniscus, after removing the air gap
from the nozzle. Now the contents are titrated with potassium dichromate solution
with constant thorough shaking until the colour changes from colourless - pale green,
24
- dark green – bluish green to bluish violet, which is the end point of the reaction.
The final reading of the burette is noted without parallax error. A number of titrations
are carried out until 2 or 3 concurrent results are obtained. The results are tabulated in
Table No. 1.
Table – I
Titration of standard potassium dichromate solution with Mohr’s salt
solution.
Normality of standard solution of potassium dichromate ____________ N
Indicator : 1 % Diphenyl amine solution
Colour change at the end point : Bluish green to Bluish violet
Calculations :
By the law of equivalence, V1 N 1= V2 N 2
N1 = V2 N 2 / V1
The Normality of Mohr’s Salt solution = _____________ N.
Part – II :
Estimation of chromium (VI) in the given 100 ml of potassium dichromate
solution by titrating against a standard solution of Mohr’s salt.
Procedure :
The given potassium dichromate solution is diluted upto the mark of
volumetric flask with distilled water carefully. The flask is stoppered tightly and is
shaken thoroughly about 3 to 5 minutes for complete homogenization. 10.0 ml of
standard Mohr’s salt solution is pipetted out into a clean conical flask carefully. 40.0
ml of distilled water, 5.0 ml of 1:1 dilute sulphuric acid and 3.0 ml of syrupy
phosphoric acid are added with a measuring cylinder. One or Two drops diphenyl
amine indicator is added directly to the conical flask contents. The burette is filled
with the above potassium dichromate solution after rinsing with the same solution and
then initial reading is noted. Now the conical flask contents are titrated with
potassium dichromate solution with constant thorough shaking until the colour
changes from colourless - pale green, - dark green – bluish green to bluish violet,
which is the end point of the reaction. The final reading of the burette is noted
without parallax error. A number of titrations are carried out until 2 or 3 concurrent
results are obtained. The results are tabulated in Table No. II.
25
Table – II
Titration of potassium dichromate solution with a standard solution of Mohr’s
salt.
Calculations :
By the law of equivalence V3 N3 =V4 N4
N4 = V 3 N3 / V 4
Amount of chromium (VI) present in the given 100 ml solution = Amount present in 1
lit. of solution / 10 = g
Table – III
Percentage error table
Table – III
Percentage error table
Calculations :
By the law of equivalence V1 N1 = V 2 N2
N1 = Normality of Hypo solution = ?
V1 = Volume of Hypo solution = ml
N2 = Normality of copper sulphate solution = N
V2 = Volume of Copper sulphate solution = ml
N1 = V 2 N2 / V 1
Part II :
Estimation of copper in a copper ore by titrating against a standard
solution of Hypo via the liberation of Iodine through potassium Iodide.
Procedure :
The given copper ore solution (as sulphate) is diluted upto the mark of
volumetric flask with distilled water carefully. The flask is stoppered tightly and is
shaken thoroughly about 3-5 minutes for complete homogenization. 10.0 ml of the
copper ore solution is pipetted out into a clean conical flask carefully. To this sodium
carbonate solution is added by drop wise until the solution becomes turbid. Then
dilute acetic acid (1:1) is added by drop wise until the solution becomes clear. Then
10.0 ml of 10% potassium iodide solution is added to the conical flask contents with
gentle swirling and then flask is covered with watch glass immediately for one or two
minutes for complete liberation of iodine. The solution is then diluted with 30.0 ml of
distilled water and the resultant solution is dark brown in colour. The burette is filled
with standard Hypo solution and initial reading of the burette is noted. Now the dark
brown conical flask contents are titrated with Hypo solution by drop wise with
constant shaking until the colour of solution changes from dark brown – dark yellow –
yellow – pale yellow to wheatish yellow / straw yellow. At this stage 1.0 ml of
freshly prepared starch solution is added to wheatish yellow coloured conical flask
contents, the solution becomes blue in colour. Now the titration is continued drop
wise with thorough shaking until the blue colour just disappears (flesh white) which is
the end point of the reaction. The final reading of the burette is noted. A number of
titrations are carried out until 2 or 3 concurrent readings are obtained. The results are
tabulated in Table No-II.
29
Precautions :
1. After the addition of potassium iodide the flask is covered with watch glass
for about one / two minutes for complete liberation of Iodine.
2. Starch indicator should be added before the end point.
3.The minimum quantities of Na2 CO3 solution and CH3 COOH are to be added.
Table – II
Titration of standard Hypo solution with copper ore solution.
Normality of standard solution of Hypo ____________ N
Indicator : 1 %freshly prepared starch solution
Colour change at the end point : Blue to flesh white
Calculations :
By the law of equivalence , V3 N3 = V4 N4
N4 = V 3 N3 / V 4 .
The Normality of copper ore solution _____________ N.
Amount of copper present in the given 100 ml of copper ore solution = amount
present in 1 liter of the solution / 10 = g
Table – III
Percentage Error Table
Report: The amount of copper present in the given 100 ml of an unknown solution
is g.
30
Amount of copper sulphate present in the given 100 ml of copper ore solution =
amount present in 1 liter of the solution / 10 = g
Table – III
Percentage Error Table
Report: The amount of copper sulphate present in the given 100 ml of an unknown
solution is g.
31
9 (a). DETERMINATION OF VISCOSITY OF THE GIVEN LIQUID
Aim
To determine the viscosity of the given liquid using Ostwald’s viscometer.
Theory
The Ostwald’s viscometer method is based on Poseuille’s equation. This
relates the rate of flow of a liquid through a capillary tube with the coefficient of
viscosity expressed by the equation
r4 t
=
8vl
Where r = Volume of the liquid of viscosity flowing in time ‘t’ through a
capillary tube of radius ‘r’ and length ‘l’. p- hydrostatic pressure of the
liquid.
If t1 and t2 are the flow times required to flow for equal volumes of two liquids
through same length of capillary tube, then
1 Pt
1 1
2 P2 t 2
P = hdg
here h & g are same for the two liquids.
1 dt
11
2 d2t 2
d1 t1
1 x 2
d2 t2
Procedure
The viscometer is cleaned first with chromic acid, water and then with distilled
water. It is finally washed with alcohol and ether and then dried. A piece of clean
rubber tube is attached to the end ‘C’ of viscometer and is clamped vertically in air.
32
A sufficient volume of distilled water is introduced in one of the bulbs (B) so that the
bend portion of tube and half or a little more than half bulb (B) are filled up. With
the help of rubber tube attached to the upper arm of bulb (A) water is sucked until it
raises above the upper mark ‘C’ and is allowed to flow under its own weight. The
time of flow of water from ‘C’ to ‘D’ is counted by starting stopwatch as the meniscus
just passes lower mark ‘D’. The same procedure is repeated three times and the mean
values is determined. The viscometer is cleaned and dried. The same procedure is
repeated with the same volume of given liquid and the time of flow of liquid is
measured and the values are recorded in Table-1. The relative density of a given
liquid is measured using pycnometer.
Observations
1
2
3
4
1 dt
11
2 d2t 2
Where
1 = Viscosity of the given liquid = ?
2 = Viscosity of water= poise
d1 = density of the given liquid = gm/cm3
d2 = density of water = gm/cm3
Report
The relative viscosity of the given liquid with respect to water at room
temperature is ________poise.
33
Aim :
To determine the surface tension of the given liquid at room temperature by
stalagmometer.
Theory :
When a liquid is allowed to flow through a capillary tube, a drop is formed at
its lower end. It increases to a certain size and falls off. The size of the drop depends
on the radius of the capillary and the surface tension. The surface tension acting
along the circumference of the capillary tube supports the drop in the upward
direction.
The measurement of surface tension of a liquid is based on the fact that the
drop of the liquid at the lower end of capillary falls down when the weight of the drop
becomes equal to the surface tension. The surface tension of the given liquid is
determined relative to water at room temperature by using stalagmometer. The
number of drops for the same volume of water and the given liquid are counted and
let there be n1 and n2 respectively. Now if the densities of water and given liquid at
room temperature as determined separately using specific gravity bottle, then the
surface tension 2 of the given liquid can be calculated using the relationship.
1 n 2 d1
x dynes/cm
2 n1 d 2
Procedure
The stalagmometer is cleaned thoroughly first with chromic acid solution and
finally with distilled water and then dried. The lower end of stalagmometer is
immersed in a beaker containing distilled water. The water is sucked until the level
rises above the mark ‘C’ and the screw is tightened. The liquid is allowed carefully
so that the liquid drops start falling at an interval of about 2-3 sec. in successive drops.
Counting of the drops is started when the meniscus just reaches the upper mark ‘C’
and stopped when the meniscus just passes the lower meniscus ‘D’. The same
procedure is repeated thrice and the mean value is considered. The values obtained
are noted in Table 1. The stalagmometer is cleaned and dried. It is then filled until the
level rises above the upper mark ’C’ and the number of drops are counted as
described earlier. A specific gravity bottle is cleaned and dried. The density of the
given liquid is measured using the specific gravity bottle.
34
Table – I
1
2
3
1 n 2 d1
x
2 n1 d 2
n1 d 2 x xd
2 = x x 1 1 1 2
n 2 d1 n2 x d2
Precautions
1. The stalagmometer and the specific gravity bottle should be cleaned properly
and dried before use.
2. The stalagmometer should be fixed vertically.
3. The No. of drops must be between 15-20 per 3 minutes.
Report
The relative surface tension of the given liquid with respect to water at room
temperature is ___
35
Aim
To estimate the amount of given Mohr’s salt by titrating against standard
potassium dichromate solution potentiometrically.
Theory
It is very well known that the electrode potential of the electrode depends upon
the concentration of its ions in the solution so the potential of an indicator electrode
goes on changing with respect to a standard (reference) calomel electrode by the
change of concentration of ions during the titration. The equivalence point is
indicated by fairly a large change in electrode potential value. This can be found by
plotting a graph between the emf of the cell on Y axis and the volume of titrant and
added on X axis.
0.591 [oxidant]
E = Eo + log
n [reductant]
Procedure
10.0 ml of unknown Mohr’s salt solution is pipetted out in to a 100 ml beaker.
5.0 ml of 1:1 sulphuric acid and 35 ml of distilled water are taken in a measuring
cylinder and are transferred in to the beaker. The potentiometer is connected with an
indicator electrode (platinum) and a reference electrode (calomal) in proper direction.
The contents of the beaker are then titrated against standard dichromate solution. A
pilot titration is carried out by adding 1 ml portion of dichromate solution each time.
The solution is thoroughly mixed and the corresponding emf values are noted in table
No. 1. At the equivalence point a large change in potential is noticed. Similarly an
accurate titration is carried out by adding 0.1 ml portions of dichromate solution at the
vicinity of the equivalence point. The results are presented in table No. II. A graph is
drawn between volume of dichromate solution on X-axis and potentials on Y-axis for
the accurate titration.
Table I
Pilot titration of Mohr’s salt solution with standard solution of potassium
dichromate
10.0 ml Mohr’s Salt Solution + 5 ml of 1:1 H2SO4 + 35 ml water
Table II
Calculations
According. to law of equivalence, V1N1 = V2N2
V1= Volume of Mohr’s salt solution = 10.0 ml
N1 = Normality of Mohr’s salt solution =?
V2 = Volume of dichromate solution = ml
N2 =Normality of dichromate solution = 0.05N
V2 N 2
N1
V1
Normality of Mohr’s salt solution = N
Amount of Mohr’s salt in 1lit = Normality x Eq. wt.
= N1 x 392.2
N1 x 392.2
Amount of Moh r’s salt present in 100 ml = = gm.
10
Table– III
Percentage error table
Report
Amount of Mohr’s salt present in 100 ml of solution = g.
Precautions
1. The platinum electrode should be activated using spirit lamp before starting the
titration.
2. The solution should be thoroughly shaken with a stirrer each time.
37
10 (b). DETERMINATION OF STRENGTH OF HYDROCHLORIC ACID BY PH
METRIC METHOD
Aim
To determine the strength of hydrochloric acid with standard sodium hydroxide
by pH metric method.
Procedure
The unknown solution of hydrochloric acid is made up to the mark with
distilled water. 10.0 ml of the solution is pipetted out in to a clean beaker. 40 ml of
distilled water is added to this solution. Meanwhile the pH meter is switched on and
is allowed to stabilize for about 10 to 15 min. The instrument is calibrated with
standard buffers of pH 4 and 9.2. A standard solution of sodium hydroxide is taken in
a micro burette. A pilot titration is carried out by titrating the contents of the beaker
with 1 ml portions of sodium hydroxide each time. The solution is thoroughly mixed
and the corresponding pH values are noted in table I. Accurate titration is carried out
similarly with 0.1 ml portions of sodium hydroxide near the neutralization point. The
corresponding pH values are recorded in Table – II
Table I
1 0.5
2 1.0
3 1.5
38
Table II
1 0.5
2 1.0
3 1.5
Calculations
According to law of Equivalence, V1N1 = V2N2
V1 - Volume of sodium hydroxide = ml
N1 - Normality of sodium hydroxide = N
V2 - Volume of hydrochloric acid = ml
N2 - Normality of hydrochloric acid = ?
Table– III
***