Division: ___ Roll No.

: _______ Date of Performance:

__________
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Expt. No.: 01: ALKALINITY OF WATER SAMPLE.

Aim: To determine alkalinity of water sample.

Apparatus: Burette, Pipette, 250 ml conical flask, Beaker.
Chemicals: H2SO4, Phenolphthalein, Methyl Orange indicator, K2CO3,
Water sample.

Theory: Alkalinity of water is due to the presence of hydroxides,

carbonates and bicarbonates of elements such as calcium,
magnesium, sodium, potassium and ammonia. Knowledge of
alkalinity of water is helpful in controlling rate of corrosion, caustic
embrittlement, deposition of scales, precipitation of sludge,
neutralizing acids and treatment of water.
Alkalinity is a quantitative capacity of water to neutralize acid
to a specific pH and it is expressed in CaCO 3 scale. Alkalinity can be
estimated by the titration of alkaline water sample against standard
acid using phenolphthalein and methyl orange as indicators. The
chemical reactions involved are:

1. Ca (OH) 2 + H2SO4 CaSO4 +2H2O

2. 2CaCO3 + H2SO4 CaSO4+ Ca (HCO3)2
3. Ca (HCO3) 2 + H2SO4 CaSO4 + 2CO2 + 2 H2O

The titration of water sample against a standard acid upto

phenolphthalein end point shows the completion of hydroxide + ½ of
the normal carbonate present. The titration of the water sample till
methyl orange end point marks the completion of the reactions 1, 2
and 3. The amount of an acid used after the phenolphthalein end

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point corresponds to ½ of normal carbonate + all the bicarbonates.
The total alkalinity is represented by the total amount of acid used.

Procedure:
Part A : Standardization of H2SO4
1. Weigh exactly 0.345 gm of K2CO3 on clean watch glass.
2. Dissolve it in water and dilute the solution up to the mark
in a 250 ml volumetric flask, obtain homogeneous solution.
3. Fill burette with 0.02N K2CO3 solution. Take out 10 ml of this
solution in a conical flask.
4. Add 2 drops of methyl orange indicator.
5. Titrate it against given H2SO4 till the colour changes from
yellow to red.
6. Take two more readings by adding 1 ml more in the same
solution i.e. for 11ml and 12ml.
7. Find out exact Normality of H2SO4.

Part B : Estimation of Alkalinity

1. Pipette out 10 ml of water sample in a conical flask.
2. Add 1-2 drops of phenolphthalein indicator.
3. Fill the burette with 0.02N H2SO4.
4. Titrate the content of conical flask with 0.02N H 2SO4 untill
the pink colour just disappears. This is phenolphthalein
end point (P).
5. To the same solution add 2 drops of methyl orange and
continue the titration with 0.02N H2SO4 till the colour
changes from light yellow to red. This is methyl orange end
point (M).
6. Take three readings and find out C. B. R.

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Observations and observation table:
Part A : Standardization of H2SO4
Burette–1 : 0.02N K2CO3 solution
Burette-2 : Given H2SO4 solution
Indicator : Methyl orange
End Point : Yellow to red.

Observation Table 1 :

Burette –1 10 ml 11 ml 12 ml

Burette-2 X1 ml = X2 ml = X3 ml =

Calculations:
K2CO3 = H2SO4
N 1 V1 = N 2 V2
0 .02 x 10
N2 ’ = =
X1
0 .02 x 11
N2’’ = =
X2
0 .02 x 12
N2’’’ = =
X3
N2’ + N2’’ + N2’’’
Mean Normality =
3

Exact Normality of H2SO4 = ………….N

Part B : Estimation of Alkalinity
Burette : 0.02N H2SO4
Pipette : 10 ml, Alkaline water sample
Indicator : Part (a) Phenolphthalein,
Part (b) Methyl orange
End-Point : (a) Pink to colourless.
(b) Yellow to red.

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Observation Table 2 :

Burette reading, ml
End Point C.B.R., ml
I II III
P
M

Calculations:

1) Volume of sample taken for titration = 10 ml.

2) Total alkalinity in terms of CaCO3
ml of H2SO4 used in total titration x N of H2SO4 x 50000

= ml of sample taken
ml of sample
taken

= mg/L

Result: Alkalinity of given water sample is mg/L

Signature of the Teacher

Marks Total
with date

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Division: ___ Roll No.: _______ Date of Performance:
__________
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Expt. No.: 02: HARDNESS OF WATER

Aim: Determination of temporary and permanent hardness in given

water sample.
Apparatus : Borosil beaker 250 ml, Volumetric flask 250 ml, Pipette
25 ml, Funnel, Burette, Glass rod.
Chemicals : Water sample, Na2EDTA Solution, ZnSO4 Solution, EBT
Indicator, Conc. HCl, 1:1 Ammonia solution, NH4Cl.

Theory: Water sample that does not produce lather with soap is
known as hard water. On heating it leaves deposits of scales on the
walls of the container. The hardness is due to the presence of
dissolved bicarbonates, sulphates, chlorides and nitrates of
magnesium and calcium. For determining suitability of water for
domestic and industrial purpose, type of hardness and hence
magnitude of hardness is important. To determine total hardness of
given water sample, Disodium salt of ethylene diamine tetra acetic
acid is used as it forms strong 1:1 complex divalent metal ions.
In this complexometirc titration, Eriochrome black T is used as
an indicator. This indicator forms less (w.r.t. metal ion–EDTA
complex) stable wine red coloured complex with metal ion which
dissociates on titration with EDTA solution.

Structure of Disodium Salt of EDTA:

NaOOC-H2C CH2-COOH
.. .. ..
N-CH2-CH2-N
HOOC-H2C CH2-COONa
It can be shortly written as Na2H2Y.

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Reactions:
1) Ionization of Na2H2Y in water
Na 2H2Y→ H2Y2 -+ 2Na+
2) Formation of metal indicator complex (wine red indicator)
M2++HIn2-→ MIn- + H+
3) Formation of metal EDTA complex
MIn- + H2Y2- → MY22- +HIn2- + H+

Procedure :
Part A: Standardization of Na2EDTA solution.
1. Prepare 0.01M ZnSO 4 solution by dissolving and diluting
0.718 gm of ZnSO4 in 250 ml volumetric flask with distilled
water.
2. Fill the burette-1 with 0.01M ZnSO4 and burette-2 with given
Na2EDTA solution.
3. Take 10ml ZnSO4 solution from burette-1 in conical flask.
4. Add 5 ml buffer solution (pH= 10) and 2 - 3 drops of EBT
indicator. Solution will turn wine red.
5. Titrate it against Na2EDTA solution.
6. Colour change will be wine red to blue. Note down this
burette reading as X1 ml.
7. To the same solution in conical flask, add 1ml ZnSO4 solution
from burette-1(total burette reading becomes 11 ml) titrate
this solution against Na2EDTA solution from burette-2 till a
blue colour is obtained. Note down this burette reading as X 2
ml.
8. Again to the same solution in conical flask take out 1ml
ZnSO4 solution from burette-1. Repeat the procedure. Note
down this burette reading as X3 ml.

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 9. Find out exact Molarity (M2) of Na2EDTA solution.
Part B: Determination of Total Hardness
1. Fill burette-1 by water sample and take 10 ml of water sample
from it in conical flask.
2. Add 5 ml buffer solution (pH=10) and 5 drops of EBT
indicator, colour of the solution will be wine red.
3. Titrate it against Na 2EDTA solution from burette-2.
Colour change will be wine red to blue. Note down this
burette reading as Y1 ml.
4. To the same solution in conical flask, add 1ml water sample
from burette-1 (total burette reading becomes 11 ml) titrate
solution against Na2EDTA solution from burette-2 till a blue
colour is obtained. Note down this burette reading as Y2 ml.
5. Again to the same solution in conical flask take out 1 ml
water sample from burette-1. Repeat the procedure. Note
down this burette reading as Y3 ml.

Part C: Determination of permanent hardness

1. Take exactly 50 ml hard water in 100 ml beaker and boil
gently for 1 hour, cool it and filter into 50 ml volumetric
flask
2. Make the volume upto the mark by addition of distilled
water. Take out entire solution into 250 ml beaker and fill
the burette-1 by this water sample. Repeat the procedure
to obtain V1,V2,V3 ml.

Observations and observation table:

Part A : Standardization of Na2EDTA solution
Burette-1 : ZnSO4 solution.
Burette-2 : Na2EDTA solution.
Indicator : EBT indicator

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End point : Wine red to blue.

Observation Table 1:

Burette –1 10 ml 11 ml 12 ml
Burette-2 X1 ml = X2 ml = X3 ml =

Calculations:
ZnSO4.7H2O = Na2EDTA
M 1 V 1 = M2 V 2

0.01× 10
------------ = M2 ’ -------------------------(1)
X1

0.01× 11
------------ = M2”-------------------------(2)
X2

0.01× 12
------------ = M2’”-------------------------(3)
X3

M2 ’ + M2”+ M2’”
M 2 = -------------------- = -----------------------
3

Morality of Na 2EDTA = M2 = M

Part B: Determination of total hardness

Burette-1: Water sample.
Burette-2: Na2EDTA solution.
Indicator: EBT indicator
End point: Wine red to blue.

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Observation Table 2:

Burette –1 10 ml 11 ml 12 ml
Burette-2 Y1 ml = Y2 ml = Y3 ml =

Structure:

The complex made by EDTA with Ca+2 ion

Calculations:
Part B: Determination of total hardness
1 M of Na 2EDTA = 1 M of CaCO3
1000 ml 1 M Na 2EDTA = 100 g CaCO3 = 105 mg CaCO3

Y ×M
1 2 × 105
Y1 ml M 2 M Na 2EDTA = = ---------- mg
--------------------------

1000

10 ml of water sample = ------------ mg CaCO3

1000 ml of water = -------------------- mg/L CaCO3

Y2 × M2 × 105
Y2 ml M2M Na2EDTA = --------------------------- = ----------------- mg
1000

11ml of water sample = ------------ mg CaCO3

1000 ml of water = -------------------- mg/L CaCO3

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 Y3 × M2 × 105
Y3 ml M2M Na2EDTA = --------------------------- = ------------- mg
1000
12ml of water sample = ------------ mg CaCO3
1000 ml of water = -------------------- mg/L CaCO3

Mean total hardness = --------------- mg/L CaCO3

Given water sample contains (A) = ----------------- mg/L CaCO3
Part C: Determination of permanent hardness
Burette-1: Treated water sample.
Burette-2: Na2EDTA solution.
Indicator: EBT indicator
End point: Wine red to blue.

Observation Table 3:

Burette –1 10 ml 11 ml 12 ml
Burette-2 V1 ml = V2 ml = V3 ml =

1 M of Na2EDTA = 1 M of CaCO3
1000 ml 1 M Na 2EDTA = 100 g CaCO3
V1 × M2 × 105
V1 ml M 2 M Na2EDTA = -------------------------- = mg
1000

10ml treated water sample contains = ------------ mg CaCO3

1000ml treated water sample contains = ------------ mg/L CaCO3

V × M × 105 2 2
V2 ml M 2M Na 2EDTA = = -------------- mg
---------------------------

1000
11ml treated water sample contains = ------------ mg CaCO3
1000ml treated water sample contains = ------------ mg/L CaCO3

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 V3 × M2 × 105
V3 ml M 2M Na 2EDTA = --------------------------- = -------------- mg
1000
12ml treated water sample contains = ------------ mg CaCO3
1000ml treated water sample contains = ------------ mg/L CaCO3

Treated water sample contains (B) = ------------- mg/L CaCO3

Result :

1.Exact molarity of Na2EDTA solution(M2) M

2. Total Hardness (A) mg/L
3. Permanent Hardness (B) mg/L
4. Temporary Hardness (A-B) mg/L

Signature of the Teacher

with date
Marks Total

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 A Journal of Engineering chemistry, SCOE, Pune-41
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BLANK

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Division: ___ Roll No.: _______ Date of Performance:
__________
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Expt. No.: 03: CHLORIDE ION CONTENT.

Aim: To determine chlorine content in a given water sample by

Mohr’s Method.
Apparatus : Burettes, Conical flask, Measuring cylinder, etc.
Chemicals: Silver nitrate solution (0.01M approx), 0.1M NaCl
solution, Potassium chromate indicator (K2CrO4), Water
sample, etc

Theory: Chlorides are present in water usually as NaCl, MgCl2, and

CaCl2. Although chlorides are not harmful as such, their
concentrations over 250 ppm impart a peculiar taste to the water
thus rendering the water unacceptable for drinking purposes.
Further, existence of unusually high concentrations of chloride
in a water sample indicates pollution from domestic sewage or from
industrial wastewaters. Salts like MgCl2 may undergo hydrolysis
under the high pressure and temperature prevailing in the boiler,
generating hydrochloric acid which causes corrosion in boiler parts.
Chlorides in the form of MgCl2 and CaCl2 cause permanent hardness
and are a source of trouble not only at our house hold but also in
industries.
By Argentimetric method chloride ions in a water sample, which is
neutral or slightly alkaline can be determined by titrating it against
standard silver nitrate solution using potassium chromate indicator.
The pH should be in between 7-8. As at higher pH,

Ag+ + OH- AgOH

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And at lower pH, K2CrO4 indicator is converted to KHCrO4. As KHCrO4
is weak in nature, concentration of CrO4-- decreases and therefore,
higher concentration of Ag+ is needed for the solubility product of
Ag2CrO4 to be exceeded.
Ag+ react with Cl- and CrO4 --
when AgNO3 solution is released
from the burette to the sample solution, which has Cl-.
Ag+ + Cl- AgCl (White ppt)
2 Ag+ + CrO4- Ag2CrO4 (Red ppt)
Red colour formed because of formation of silver chromate
disappears as the solution contains high concentration of Cl-
Ag2CrO4 + 2 Cl- 2 AgCl + CrO4- -
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 AgCl. One extra
drop of AgNO3 at this point reacts with Potassium chromate and
reddish coloured silver chromate is formed.
2 AgNO3 + K2CrO4 Ag2CrO4 + 2KNO3

Procedure:

Part A: Standardization of AgNO3 Solution

1. Fill burette-1 with standard 0.1M NaCl solution and burette-2
with AgNO3 solution.
2. Take out 10 ml standard 0.1M NaCl solution from burette-1
in a clean conical flask resting on a white tile.
3. Add 1ml of K2CrO4 indicator solution.
4. Then start adding AgNO3 solution slowly from burette;
swirling the liquid constantly.
5. During addition of AgNO3 solution reddish brown coloured
precipitate formed which disappears immediately.

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 6. Continue the addition of AgNO3 solution untill a faint reddish
brown coloured precipitate formed persists.
7. During titration brisk shaking is essential.
8. Repeat the titration procedure to take further two readings
for 11 and 12ml.

Part B: Estimation of Chloride ion content from water sample

1. Fill burette-1 with given water sample and refill burette-2
with AgNO3 solution.
2. Repeat the procedure as per part A (2 to 8), taking given
water sample instead of NaCl solution.

Observations and observation table:

Part A: Standardisation of 0.01M AgNO3 solution
Burette-1: 0.1 M NaCl solution
Burette-2: 0.01 (approx) M AgNO3 solution
Indicator: 1ml K2CrO4 solution
End point: Yellow to faint reddish brown coloured ppt.

Observation Table 1:

Burette –1 10 ml 11 ml 12 ml
Burette-2 X1 ml = X2 ml = X3 ml =

Calculations:
M 1 V 1 = M2 V 2

0.01× 10
M2 ’ = ------------ -------------------------(1)
X1

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 0.01× 11
M2” = ------------ -------------------------(2)
X2

0.01× 12
M2 ’” = ------------ -------------------------(3)
X3

M2 ’ + M2”+ M2’”
M 2 = -------------------- = -----------------------
3

Morality of AgNO3 = M2 = -------------- M

Part B: Estimation of Chloride ions from water sample

Burette-1: Water sample
Burette-2: Std.AgNO3 solution
Indicator: 1ml K2CrO4 Solution.
End point: Yellow to faint reddish brown coloured ppt.

Observation Table 2:

Burette –1 10 ml 11 ml 12 ml
Burette-2 Y1 ml = Y2 ml = Y3 ml =

Calculations:

1000 ml 1M AgNO3 = 35.5 gm of Cl‾ ions.

Y1 x M2 x 35.5
Y1 ml M2 Molar AgNO3 = ------------------ = ------------- g of Cl‾ ions.
1000

10 ml contains -------- g of Cl‾ ions x 1000= ---------- mg of Cl‾ ions.

1000 ml contains ------ mg of Cl‾ions x 100 = ---------- mg of Cl‾ ions.

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 Y2 x M2 x 35.5
Y2 ml M2 Molar AgNO3 = ------------------ = ------------- g of Cl‾ ions.
1000

11 ml contains -------- g of Cl‾ ions x 1000= ---------- mg of Cl‾ ions.

1000 ml contains ----- mg of Cl‾ions x (1000/11)= ------mg of Cl‾ ions.

Y3 x M2 x 35.5
Y3 ml M2 Molar AgNO3 = ------------------ = ------------- g of Cl‾ ions.
1000

12 ml contains -------- g of Cl‾ ions x 1000= ---------- mg of Cl‾ ions.

1000 ml contains------mg of Cl‾ions x (1000/12)=-------mg of Cl‾ ions.

Mean = ---------------------- = -------------- mg/L

Chlorine content in given water sample is ------------ mg/L.

Result: The Chloride ion content in given water sample is

--------mg/L.

Signature of the Teacher

Marks Total with date

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Division: ___ Roll No.: _______ Date of Performance:
__________
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Expt. No.: 04: PROXIMATE ANALYSIS

Aim: Estimation of moisture, ash and volatile matter in a given coal

sample by Proximate Analysis.
Apparatus: Silica and Porcelain crucible, pair of tongs, Muffle
furnace and Oven etc.
Chemicals: Coal sample

Theory: Proximate analysis is a determination of moisture content,

volatile matter and ash content to find fixed carbon content. This
gives information about the practical utility of coal.
The moisture, which is lost on air-drying, is called free moisture. It
depends on the factor such as size of the coal and its rank,
treatment given to the coal, the degree of drying and the nature of
its surface. Whereas internal moisture depends on maturity (age or
degree of coalification). The moisture present in the fuel reduces the
calorific value and hence its presence is undesirable.
The volatile matter is a complex mixture of gaseous and liquid
products resulting from the decomposition of coal substance. A high

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volatile matter containing coal burns with a long flame, high smoke
and has low calorific value. Hence its presence is desirable.
The ash content is an unwanted, noncombustible matter, which
reduces the calorific value of coal. Moreover, ash causes the
hindrance to flow of air and heat, thereby lowering the temperature.

Procedure:
Part A: Moisture Content - Take some known quantity of powdered
coal sample in previously weighed porcelain crucible. Heat the
sample in an electric oven at about 1100C for about an hour. Take
out the crucible, cool it in dessicator and weigh it. Repeat the
procedure of heating, cooling and weighing the crucible till constant
weight is obtained. Note down constant weight.

Part B: Volatile matter content - After determination of moisture,

the dried sample of coal content is heated in a muffle furnace
mentioned as 925 ± 20 0C for exactly seven minutes. The coal
sample is taken in a crucible and heated. After heating, the crucible
is removed from muffle furnace with the help of long legged tong
carefully. It is first put on a cooled iron plate and then transfered the
warm crucible in a dessicator. Once it attains room temperature, it is
finally weighed.

Part C: Ash content – After determination of volatile matter,

moisture, the dried sample of coal content is heated in a muffle
furnace mentioned at about 700-8000C for an hour. The crucible is
taken out, cooled and weighed. Repeated ignition, cooling and
weighing the crucible till constant weight is obtained.

Observations and calculations:

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Part A : Moisture Content
Sr.No. Description Value (g)
1 Weight of empty crucible W1=
2 Weight of crucible and coal W2=
sample
3 Weight of coal (W2−W1)=
4 Weight of crucible and coal after W3=
heating
5 Loss in weight of coal after (W2−W3)
heating

Loss in weight due to heating = moisture content present in the

sample

Loss in weight
% of moisture = -------------------------- X 100
Weight of coal

(W2−W3)
= -------------------------- X 100
(W2−W1)

Part B: Volatile matter content-

Sr.No. Description Value (g)

1 Weight of empty crucible W4=
2 Weight of crucible and coal W5=
sample
3 Weight of coal (W5−W4)=
4 Weight of crucible and coal after W6=
heating
5 Loss in weight of coal after (W5−W6)=
heating

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 Loss in weight
% of V.M. = (----------------------- X 100) - (% moisture)
Weight of coal

(W5−W6)
= -------------------------- X 100
(W5−W4)

Part C: Ash content-

Sr.No. Description Value (g)

1 Weight of empty crucible W7=
2 Weight of crucible and coal W8=
sample
3 Weight of coal (W8−W7)=
4 Weight of crucible and coal after W9=
heating
5 Weight of ash after heating (W9−W7)

Weight of ash
% of Ash = -------------------------- X 100
Weight of coal

(W9 − W7)
= ------------------- X 100
(W8 − W7)

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Result:
1. Percentage of moisture
Percentage of volatile
2.
matter
3. Percentage of ash

Marks Total Signature of the Teacher

with date

Division: ___ Roll No.: _______ Date of Performance:

__________
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Expt. No.: 05: CONSTRUCTION OF PHASE
DIAGRAM

Aim: To construct a phase diagram for a binary system, naphthalene

and benzoic acid and find the melting and eutectic
temperatures.
Apparatus: Paraffin bath, hard glass test tubes, corks,
thermometer, stirrer stopwatch etc.
Chemicals: Naphthalene, Benzoic acid, water, paraffin oil etc.

Theory: The mixture of solids, which has the same overall

composition as the liquid phase has, is called eutectic solid mixture.

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The liquid phase of an identical composition and in equilibrium with
the eutectic solid mixture is called eutectic liquid mixture. A eutectic
mixture has the lowest freezing point of all the possible mixtures of
the components involved. Liquid mixtures of naphthalene and
benzoic acid of varying composition are allowed to cool. The
temperature at which the separation of solid phase just starts
(freezing point) and the temperature at halt for various mixtures are
noted. The temperature halt for all the mixtures will be the same
because the composition of solid phase (eutectic) is same in all the
cases. A graph is plotted between the composition of mixture and
freezing point and eutectic point is noted.

Procedure: Prepare the following compositions by taking weighed

amounts in properly labelled test tubes.

Sample No. 1 2 3 4 5 6 7 8 9 10 11
Naphthalen 10 9 8 7 6 5 4 3 2 1 0
e
Benzoic 0 1 2 3 4 5 6 7 8 9 10
acid
Melt the first sample (pure naphthalene) by placing the test tubes in
the hot liquid paraffin bath. When all the crystals have melted,
remove the test tube from the bath. Wipe it clean Place the test tube
in large boiling tube, which acts as an air jacket. Fix a thermometer
and a stirrer into the tube through the cork. Allow the temperature to
fall slowly. The boiling tube can be clamped in a beaker containing
water to ensure uniform cooling. Stir thoroughly and record the
temperature after every half-minute.
Note the temperature at which crystals begin to separate from the
molten mass. Temperature remains constant at this stage and the
whole mass solidifies. Temperature again starts dropping; continue

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to record three more temperature readings. Similarly, repeat the
determination with other mixture.
Record the freezing point and temperature halt for every sample.

Observations:

Sample No. Naphthalene:Benzoic acid Freezing Temperature

point halt
1 10:0
2 9:1
3 8:2
4 7:3
5 6:4
6 5:5
7 4:6
8 3:7
9 2:8
10 1:9
11 0:10

Diagram:

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Calculations:
Plot a graph between composition of naphthalene and freezing
temperature by taking percent composition on X-axis and
temperature on Y-axis. This will be the phase diagram for the above
system. From the graph, find out the freezing /melting temperature
of the benzoic acid and naphthalene and eutectic temperature of the
mixture.

A B

Temp.
C
Eutectic point

Composition

BLANK SPACE TO PRINT GRAPH IN BLUE COLOUR

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Result
:

Melting point of benzoic acid is

1.
2. Melting point of naphthalene is
3. Eutectic point of benzoic acid: naphthalene
system

Signature of the Teacher

Marks Total
with date

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