CL 610: EXPERIMENTAL METHODS

Report on Experiment No 4: Osmometer

DATE: 28th JANUARY 2025

Instructor: Prof. Partha S. Goswami

TA: Ayush Ranjan

Department of Chemical Engineering

Indian Institute of Technology, Bombay

 Batch: T4

Work distribution

Name Roll Number Work done

Theory and Experimental Procedure, Sources of Error and

Sparsh Kushwaha 24M0403
Precautions
Observation Table, Graph, Calculations, Result and
Anita Rawat 24M0430
Discussion
Table of Contents

1. Aim
2. Experimental Apparatus
3. Reagents and Chemicals
4. Theory
5. Experimental Procedure
6. Observations and Observation Table
7. Plots
8. Calculations
9. Results and Discussion
10. Sources of Errors
11. Precautions
12. References
LIST OF FIGURES, TABLES AND PLOTS

Figures:

 Fig No 1: Vapor Pressure Osmometry

 Fig No 2: Osmometer with open bulb
 Fig No 3: Writing Observations during the experiment
 Fig No 4: Concentration calculations during the experiment

Tables:

 Table No. 1: Observed values of voltage for solution of concentrations

0.2, 0.3, 0.4, 0.5 and 0.6 mol/liter of Sodium Chloride during calibration
 Table No. 02: Concentration of solution and average signal/gain
 Table No. 03: Observed values of voltage for solution of concentrations 0.25,0.35 and 0. 45
mol/liter of Sodium Chloride
 Table No. 04: Conversion of concentrations
 Table No. 05: Molecular weight calculation for three concentrations of unknown solution

Plots:

 Plot No. 01: Concentration of solution vs average signal/gain, slope of the tread
line denotes Kcaliberated =188.76.
 Plot No. 02: Calculated molecular weight against respective concentrations.
 1. Aim

To determine the molecular weight of the given compound using Vapor Pressure Osmometry

2. Experimental Apparatus

1. Vapor Pressure Osmometer

2. 10 ml volumetric flask
3. Spatula
4. Weighing machine

3. Reagents and Chemicals

1. Sodium Chloride
2. Water

4. Theory

Vapor Pressure Osmometry is a technique used to find out the average molecular weight of a
compound based on the principle of vapor pressure lowering.

When the solute is non-volatile as compared to the volatile solvent in which it is dissolved, or
when the solution is very dilute, the vapor phase consists of solvent only and can be
approximated to an ideal solution. The pressure exerted on the ideal solution is governed by
the Raoult’s Law as below,

𝑃𝑠 = 𝑥𝑠 ∗ 𝑃𝑠0

Where Ps is the partial vapor of the solution, 𝑥𝑠 is the mole fraction of solvent and 𝑃𝑠0 is the
vapor pressure of the pure solvent at the given temperature.

The vapor pressure for pure substance depends on the temperature which is given by Antoine’s
equation, derived from the Clausius-Clapeyron relation. When a non-volatile solute, like salt,
is added to a solvent, Raoult’s law comes into the picture and the partial pressure of the solvent
in the surrounding atmosphere decreases because the mole fraction of solvent in the solution
decreases. As the vapor contains only the solvent, this is the same as the vapor pressure of the
solvent. Therefore, the vapor pressure of the solution decreases.

On placing a drop of solution in the pure solvent environment along with the solvent drop, there
is a vapor pressure difference which is compensated by the condensation of solvent vapor on the
solution drop. The ability of the solvent to vaporize from a solution containing non- volatile
solute decreases due to the availability of fewer solvent molecules available on the surface.

The temperature of the solution drop increases due to latent heat release during the
condensation of the solvent. The temperature difference corresponding to the vapor pressure
can be deducted from the Clausius-Clapeyron equation,

𝑃𝑠 ∆𝐻𝑣 1 1
𝑙𝑛 =− ( − )
𝑃𝑆0 𝑅 𝑇1 𝑇2

Where ∆𝐻𝑣 is the latent heat of vaporization of the solvent, T1 and T2 are the temperatures of
the pure solvent and solution respectively. As the concentration is very small, ∆𝑇 is small thus
𝑇1𝑇2 ≅ 𝑇12

𝑃𝑠 1 1
ln 𝑃𝑠𝑜 = ln xs=ln(1-x1)≈-lnx1= 𝑥1 + 2𝑥1 2 + 3𝑥1 3+ ⋯

Substituting in the former equation we get the ∆𝑇 in terms of the mole fraction of the solute.

In the osmometry setup, there is a thermistor with two beads, one of which is wetted with
solvent drop and the other with the solution drop, both the drops are maintained in the solvent
vapor environment. Condensation will lead to the relative increase in temperature of the
solution drop with respect to the pure solvent drop. The thermistor is connected to the
Wheatstone bridge arrangement of the osmometry. The increase in the temperature changes the
resistance which in turn disturbs the Wheatstone bridge which created minimal current flow
which generated a potential difference. This potential difference is recorded as the equilibrium
is reached.

The basic relation for molecular mass determination equals:

𝑚(𝑠𝑎𝑚𝑝𝑙𝑒)
𝑛(𝑠𝑎𝑚𝑝𝑙𝑒) { }
𝑥= = 𝑀(𝑠𝑎𝑚𝑝𝑙𝑒)
𝑚(𝑠𝑜𝑙𝑣𝑒𝑛𝑡) 𝑚(𝑠𝑜𝑙𝑣𝑒𝑛𝑡)
where,

n=number of sample molecules

m=mass of sample and solvent

M=molecular weight of the sample

The change in vapor pressure is proportional to the number of species present in the solution,
which is measured in terms of osmol units. Hence it is very similar to osmolality determination.
A sample of known molecular mass with different concentration, graph is plotted between the
voltage and concentration, the slope of the graph gives the Kcalibration by Molecular mass of
solute.

𝑀𝑉
𝐾𝑐𝑎𝑙𝑖𝑏𝑟𝑎𝑡𝑖𝑜𝑛 =
𝑐

Where

V=Potential difference

c=Molality of solute (mol/Kg)

M=Molecular weight of known sample (g/mol)

From the calibration graph Kmeasurement is found by determining potential difference for the
known concentration, Kmeasurement = Vsample/csample (in g/Kg), the molecular mass of the unknown
sample is determined by

Molecular weight of the sample= 𝐾𝑐𝑎𝑙𝑖𝑏𝑟𝑎𝑡𝑖𝑜𝑛

𝐾𝑚𝑒𝑎𝑠𝑢𝑟𝑒𝑚𝑒𝑛𝑡

The vapor pressure osmometer (Fig 2a) generally consists of six injection syringes, five of
which are connected to the left while one syringe is pointed to right. The top part through which
syringe is inserted is called head. A beaker inside filled with 25% water and rest with water
vapor is used to create the liquid vapor environment. The beaker together with the thermistor
is called cell. Generally, the cell temperature is maintained within the range of 20ᵒC-130ᵒC.
The head temperature is kept 5ᵒC above the cell temperature to preheat the syringe. The solvent
and solution drops are put on the thermistors which are connected to Wheatstone bridge that in
turn gives the potential difference. There is a wick inside the beaker which is used to increase
the liquid surface area for an optimum saturation of vapor in the cell. A hole is made in the
wick so that UV light can pass through it which falls on the thermistor and finally we can see
the liquid drop on the thermistor from the top after reflection.

Fig No 1: Vapor Pressure Osmometry

5. Experimental Procedure

Fig No 2: Osmometer with open bulb

a. First the syringes are rinsed properly. The syringes are rinsed at least 10-12 times.
b. The cells of the thermistor are washed using a syringe.
c. A filter paper of 2cm is cut and is placed inside the beaker. The beaker is filled with distilled water
which is 25% of the volume of the beaker.
d. The thermistor is then fitted inside this beaker which is then placed inside the osmometer.
e. Switch on the osmometer and allow the temperature of the head and cell to reach 62 and 60
degrees Celsius.
f. Insert the syringe in the openings above the osmometer so that the tip of the needle touches the
cell. Ensure that the syringe moves freely and smoothly.
g. A drop of water is made on both the cells and then left for at least 45 minutes. The system should
be heated for at least 45 minutes.
h. The concentration is to be converted in g/ml. The volume of the flask that is used is 10ml.
Two kinds of samples are made- calibration and measurement. Before starting press Auto-Zero
and allow the signal to be absolute zero.
i. Drops of the samples are inserted using a syringe from one end while the other end still has drop
of water and one syringe inserted completely.
j. There are two sets of syringes for the sample. Students can either use one each for calibration and
measurement or use them interchangeably. After every sample the syringes are to be washed 9-
10 times before using it for a new sample.
k. A new drop is created on one end then press start to start the timer and wait for two minutes. If
the timer is not showing two minutes student should run the timer accordingly the drop is allowed
to be heated for at least 2 minutes.
l. After the above step note down the gain and signal. This is followed by switching on the timer
using start stop and then gain is changed until overload is obtained. Repeat the same steps for both
calibrations followed by measurement.

Note: The temperature should remain constant during the course of conduction if temperature
changes the student must wait till it becomes constant to conduct the experiment. The change is
visible as 60+2 starts blinking in the osmometer.

6. Observations and Observation Table

Fig No 3: Writing Observations during the experiment

 0.2 mol/liter 0.3 mol/liter 0.4 mol/liter 0.5 mol/liter 0.6 mol/liter
Gain mV/ mV/ mV/ mV/
mV gain mV gain Mv gain mV gain mV mV/gain
1 47 47 63 63 66 66 85 85 117 117
2 98 49 123 61.5 133 66.5 173 86.5 246 123
4 198 49.5 146 36.5 266 66.5 347 86.75 496 124
8 402 50.25 493 61.625 533 66.62 694 86.75 995 124.3
16 815 50.93 988 61.750 1067 66.68 OVL OVL OVL OVL

32 OVL OVL OVL OVL OVL OVL OVL OVL OVL OVL

64 OVL OVL OVL OVL OVL OVL OVL OVL OVL OVL
128 OVL OVL OVL OVL OVL OVL OVL OVL OVL OVL
256 OVL OVL OVL OVL OVL OVL OVL OVL OVL OVL
Avg 49.336 56.875 66.460 86.250 122.075

Table No. 1: Observed values of voltage for solution of concentrations 0.2,0.3,0.4,0.5and 0.6 mol/liter of Sodium
Chloride

Note: During measurement of solution of concentration 0.4mol/lit, two drops were formed.

Concentration Average
(mol/lit) (Signal/gain)
0.2 49.336
0.3 56.875
0.4 66.460
0.5 86.250
0.6 122.075

Table No. 02: Concentration of solution and average signal/gain

 0.25 mol/liter 0.35 mol/liter 0.45 mol/liter
Gain mV/ mV/ mV/
mV gain mV gain mV gain
1 54 54 68 68 86 86
2 109 54.5 140 70 176 88
4 218 54.5 282 70.5 354 88.5
8 437 54.62 567 70.87 712 89
16 859 53.68 1138 71.125 OVL OVL
32 OVL OVL OVL OVL OVL OVL
64 OVL OVL OVL OVL OVL OVL
128 OVL OVL OVL OVL OVL OVL
256 OVL OVL OVL OVL OVL OVL
AVG 54.26 70.099 87.875

Table No. 3: Observed values of voltage for solution of concentrations 0.25,0.35 and 0.45 mol/liter of Sodium
Chloride
 7. Plots

140

120 y = 188.76x
R² = 0.9889
100
Average S/G

80

60

40

20

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7
Concentration (mol/lt)

Plot No.1: Concentration of solution vs average signal/gain, slope of the trendline denotes

Kcalibrated =188.76

Concentration vs Molecular weight

60

50
Molecular weight (gm/mol)

40

30

20

10

0
0 0.1 0.2 0.3 0.4 0.5
Concentration(mol/lit)

Plot No. 02: Calculated Molecular weight against respective concentrations.

8. Calculations

To make solution of 0.2 mole/liter it was converted to g/ml as the solution is made in 10 ml of
distilled water.
To convert 0.2 mole/liter to g/ml
1 liter of water is as good as 1kg of water; therefore 0.2 mole/liter is as good as 0.2 mole/kg
𝑊
=0.2
58.44
W=0.2*58.44=11.688g
1000 ml contains 11.688g
Therefore, for 10ml= 11.688/100=0.11688g/ml
Similarly, we can calculate for other concentrations

Fig No 4: Concentration calculations during the experiment

 Concentration (mole/liter) Concentration (g/ml)
0.2 0.11688
0.25 0.1461
0.3 0.1753
0.35 0.20454
0.4 0.23376
0.45 0.26298
0.5 0.2922
0.6 0.35064

Table No. 04: Conversion of concentrations

Calculation of Molecular weight of Sodium Chloride using three different concentrations

Average
Concentration M=Kcalibrated/Kmeasurement
Signal /
Sample (g/kg) Kmeasurement (g/mol)
Gain
Sodium 54.26
14.61 3.7138 50.832
Chloride 0.25
Sodium
70.099 20.454 3.4271 55.078
Chloride 0.35
Sodium
87.875 26.29 3.3425 56.472
Chloride 0.45
Average Molecular Weight 54.1275

Table No. 05: Molecular weight calculation for three concentrations of unknown solution

Error percentage calculation:

Molecular weight of unknown sample (Sodium Chloride here) = 58.44 g/mol

Calculated average molecular weight= 54.1275 g/mol

Percentage error = (58.44-54.1275) × (100/58.44) = 7.3793 %

9. Results and Discussion

 Kcalibrated obtained using solutions of different concentration of known molecular

weight, Kcalibrated= 188.76
 The slope of the tread line was 188.76 with an R2 value of 0.9889.
 The calculated average molecular weight from a known concentration is 54.1275 g/mol.
 The error percentage in the measurement of molecular weight was estimated to be
7.3793%.

10. Sources of Errors

1. There might be the presence of traces of droplets of the previous solution, due to
improper cleaning and leading to a difference in the concentration of the solution added
for analysis.
2. The error might occur due to improper contact of the droplet with the thermistor
3. Average drop size should be the same for all concentrations, else the potential
difference can vary.
4. Change of error in calibration of weigh scale and loss of water/NaCl while
preparation of solutions
5. Sufficient time to be given for reaching uniform equilibrium temperature in the
equipment
6. Chances of instrument error

11. Precautions
 The thermistor beads to be ensured clean before start of the experiment, the same to be
cleaned with water and acetone after the completion of experiment.
 The syringes to be thoroughly cleaned with water and specific concentration before
filling them, it is to be ensured there are no air bubbles in the syringe
 Precautions to be taken while adding the solution in thermistor, ensuring proper size of
the drop and drop to be stable, and doesn’t fall while taking the reading
 The beaker to be filled to less the 25%, such that overflow/ water touching the
thermistor beads can be avoided during the course of the experiment
 Ensure clean weighing scale, volumetric flask and other apparatus used such that proper
solution can be prepared.