KENULE BEESON SARO WIWA POLYTECHNIC BORI

SCHOOL OF ENGINEERING

CHEMICAL ENGINEERING TECHNOLOGY DEPARMENT

CHEMICAL LABORATORY 1

CHE 214

PRACTICAL MANUAL
 Experiment 1
Heat of Solution
AIM: To find the most effective deicing agent.

INTRODUCTION
The enthalpy of solution, enthalpy of dissolution, or heat of solution is the enthalpy change
associated with the dissolution of a substance in a solvent at constant pressure resulting in infinite
dilution. The enthalpy of solution is one of the three dimensions of solubility analysis. Solubility is
the amount of a particular substance that can dissolve in a particular solvent; it is usually given in
mol/Kg.
For a given solute, the heat of solution is the change in energy that occurs as one mole of the solute
dissolves in a solvent. During the dissolving process, solutes either absorb or release energy.
If solutes absorb energy from the solvent as they dissolve, the solution gets colder and the reaction
is endothermic. If solutes release energy to the solvent as they dissolve, the solution gets warmer
and the reaction is exothermic. By using a titration method to determine the solubility and
measuring the change in the temperature of the solution during the dissolving process, we
calculated the heat of solution.
Solutions are very common in nature. In order for any reaction to occur there must be a change in
energy. The ease of dissolution is dependent on the temperature of the system and type of solution,
being endothermic or exothermic. Generally, when dissolution occurs, the entropy of the system
increases. It is important to determine the heat of solution (enthalpy change) this is because a
change in enthalpy takes account of energy transferred to the environment through the expansion of
the system under study.
The total enthalpy, H, of a system cannot be measured directly. Thus, change in enthalpy (ΔH), is a
more useful quantity than its absolute value. The change ΔH is positive in endothermic reactions,
and negative in exothermic processes. Enthalpy is a thermodynamic potential. It is a state function
and an extensive quantity. The enthalpy is the preferred expression of system energy changes in
many chemical, biological, and physical measurements, because it simplifies certain descriptions of
energy transfer.

THEORY
The heat of solution or enthalpy of solution is one of the three dimensions of solubility analysis. It
is the change in enthalpy associated with the dissolution of a solvent at constant pressure resulting
in infinite dilution, thus as one mole of the solute dissolves in the solvent. In the process, energy
can either be absorbed or released; it is expressed in kJ/mol at constant temperature, with positive
values indicating endothermic values and negative values indicating energy released or exothermic
energy. Dissolving a gas in liquid solvent releases energy, as heat, into the surroundings in an
exothermic reaction. The temperature of the solution decreases as energy leaves the system;
therefore solubility of a gas increases with a decrease in temperature of solution. On the other hand,
when the solution is heated, the reverse reaction occurs and gas evolves. Enthalpy of hydration is
one of the most common types of heat of solution. A substance, commonly a salt is dissolved in
water. When completely dissolved, the heat of solution is at its maximum. Dissolution of a solute
can occur in three steps:
1. Breaking of solute-solute attraction (endothermic)
2. Breaking of solvent-solvent attractions (endothermic)
3. Forming solvent-solute bonds (exothermic)

The sum of the individual enthalpy changes of each step is the overall value of the enthalpy change.
Stronger bonds are formed in solutions with negative enthalpy changes and these solutions tend to
have a lower vapour pressure. A negative enthalpy indicates that a solute is easily dissolved in the
solvent. (Wikipedia enthalpy change of solution; (University, 2005))
Three conditions are fulfilled in the process, as mentioned before, the pressure remains constant,
there is expansion against the atmosphere and work is done, and the temperature remains constant.
The enthalpy of solution is only valid for dissolution of a pure substance into another pure
substance. Enthalpies of solution of most substances can be measured directly when the resulting
solution is liquid. A constant temperature can be maintained if the solute is dissolved slowly.
(Bookrags, 2006)
When a solid is dissolved in a solvent in which it is soluble, it dissolves until saturation is reached
at a certain temperature. It is necessary to determine the amount of solute dissolved and the nature
of solid phase in equilibrium with the solution when performing solubility measurements.
Solubility depends on temperature; it increases with temperature in an endothermic reaction and
decreasing with increase in temperature in exothermic reactions. The well-known van’t Hoff
equation relates the equilibrium constant of a reaction, K, to the enthalpy change of that reaction,
∆H°:

dlnK ∆ H °
=
dT RT ²
A similar equation can be derived relating the solubility of a solid to its enthalpy of solution:

S
dln ⦋ ⦌
S° ∆H°
=
dT RT ²

Where S is the solubility in moles per kilogram, S°= 1 mol/kg, T is the temperature in degrees
Kelvin and ∆H° is the standard enthalpy of solution. (Department of Chemical Engineering, 2011)

MATERIALS
 50 mL beaker
 120 mL of distilled water
 Graduated cylinder
 Thermometer (Celsius)
 Stopwatch (use phone)
 3 spatulas, one spatula per salt (5 grams)

digital scales, one per salt

 5g of Sodium Chloride, NaCl
 5g of Calcium Chloride, CaCl₂
Control: 30 mL of distilled water which has no salt added, that is stirred for 2 minutes. Take the
initial and final temperature.

SAFETY
 WEAR GOGGLES AND AN APRON AT ALL TIMES
 HANDLE ALL GLASSWARE CAREFULLY
 DO NOT MIX THE DIFFERENT SALTS TOGETHER
 CLEAN UP ALL SPILLS IMMEDIATELY
 NO FOOD OR DRINKS ALLOWED IN THE LAB
 WASH HANDS AFTER CLEANUP IS COMPLETE

PROCEDURE
1. Measure out 30 mL of distilled water using the graduated cylinder.
2. Pour the 30 mL of distilled water into the 50 mL beaker.
3. Using the thermometer, record the initial temperature of the water ℃. Record data in data
table 1.
4. Place empty weigh boat on the digital scale and zero the scale
5. Using the spatula, measure 5g of sodium chloride into the weigh boat..
6. Pour the sodium chloride into the beaker containing 30 mL of distilled water
7. Stir solution constantly using the thermometer for two minutes with the stopwatch (on
phone).
8. Record the final temperature of the water using the thermometer (℃) in data table 1.
9. Discard of the solution in the labeled waste beaker in the hood.
10. After data has been recorded, clean the weight boat, beaker, and the thermometer, with the
Alconox soap and water.
11. Completely dry all materials using paper towels.
12. Repeat steps 1-11 using calcium chloride instead of the sodium chloride.
13 Repeat steps 1-3 and 7-11 to find the control.

RESULTS

Data Table 1: The effect of Salt (g) on the Change in Temperature (℃) of Water
Initial Temperature Final Temperature Change in Temperature
Type of Solute
(℃) (℃) (℃)
Sodium Chloride
Calcium Chloride
Distilled Water
(Control)

Calculation
The Change in Temperature is calculated by subtracting the initial temperature by the final
temperature.

Formula: Final Temperature-Initial Temperature=Change in Temperature

Conclusion
 EXPERIMENT 2
Batch sedimentation

AIM:
1. To carry out sedimentation studies by varying sedimentation rate with concentration and
with height of suspension.

INTRODUCTION

The world today is one where materials need to be extracted from time to time in order that
they become stand-alone. Most often than not, process industries would always be saddled with
the responsibility of separation. The Batch sedimentation phenomenon has been a widely used
method in the separation of flocculated suspension into concentrated sediment and a clear
liquid. Sedimentation is one major form of separation also known as settling, and may be
defined as the removal of solid particles from a suspension by settling under gravity.

Theory:
Sedimentation is a process used widely in the clarification of water and wastewater. Particles settle from
suspension in different ways, depending on the concentration of the suspension and the characteristics of
the particles. The simplest type of sedimentation is the settling of a dilute suspension of particles that have
little or no tendency to flocculate. In these circumstances, the prediction of clarification rates and their
scale-up to plant design is relatively straightforward. For higher concentrations where inter-particle effects
become significant and where agglomeration may take place, different regimes of settling rate occur,
known as ‘zone’ settling (Fig 1). Information from batch tests for such systems forms a vital part of the
search for the optimum design and operation of industrial sedimentation tanks. Suspensions containing
different concentration of sediments are being studied and the differences in sedimentation rate observed
by measuring the changes in height of the various solid/liquid interfaces with respect to time are plotted in
Figure 2.

Figure 1. Settling regimes Figure 2. Typical sedimentation curves

There are two basic types of settling that takes place, hindered settling and free settling. Hindered settling
occurs when the concentration of the solution is high enough for there to be significant interaction between
the particles. The frictional force exerted at a given velocity of the particles relative to the fluid may be
greatly increased as a result of modifications to the flow pattern. Free or particulate settling occurs when
the concentration of the solution is low and the particles are sufficiently far apart to freely settle regardless
of their nature. Faster settling particles may collide with slower moving ones where they may cohere or
continue downward at their own settling velocity. The cohered particles settle at a rate greater than that of
the individual particles and there is a gradual transition from particulate settling into zone settling regime
where the particles are forced to settle as a mass. The settling rate of the mass is a function of the solids
concentration. The sedimentation velocities of the particles tend to decrease steadily as the concentration
of the suspension is increased.
For concentrated suspensions there are two main types of settling Type 1 and Type 2 (Fig
3). In Type 1 settling, the suspension settles into four zones, a clear liquid zone, a constant
composition zone, a variable composition zone and sediment. In Type 2 settling, there are only
three zones with the constant composition zone absent. When the suspension is first allowed to
settle, there is a brief period of acceleration, followed by the constant downward movement of the
interface between the clear liquid and the suspension. The sediment accumulates at the bottom of
the vessel. When the interface approaches the layer of sediment, its rate of fall decreases until the
critical settling point is reached i.e. when the direct interface is formed between the sediment and
the clear liquid. Further sedimentation results in the agglomeration of the sediment and the
increased upward movement of the liquid.

Figure 3. Sedimentation of concentrated suspensions

(a) Type 1 settling (b) Type 2 settling

The final consolidation of the sediment is the slowest part of the process because the
displaced fluid has to flow through the small spaces between the particles. As consolidation occurs,
the rate falls off because the resistance to the flow of liquid progressively increases. The porosity of
the sediment is smallest at the bottom because the compressive force due to the weight of particles
is greatest and because the lower portion was formed at an earlier stage in the sedimentation
process.
 For batch settling carried out in vertical tubes the main factors which affect the process are
the height of the suspension, the diameter of the vessel, and the volumetric concentration.
Generally the height of the suspension does not affect the rate of sedimentation or the consistency
of the sediment obtained. However if the position of the interface is plotted as a function of time for
two or more different height, then it is seen that they vary by a constant factor.
If the ratio of the diameter of the vessel to the diameter of the particle is greater than about
100, the walls of the container appear to have no effect on the rate of sedimentation. For smaller
values, the sedimentation rate may be reduced because of the retarding influence of the walls. As
already indicated, the higher the concentration, the lower is the rate of fall of the sludge line
because the greater is the upward velocity of the displaced fluid and the steeper are the velocity
gradients in the fluid.

Figure 4. Layers that form in the batch sedimentation

The uses of sedimentation in industry fall into the following categories: (1) solid–liquid
separation (2) solid‒solid separation (3) particle-size measurement by sedimentation and other
operations such as mass transfer, washing, etc. In solid‒liquid separation, the solids are removed
from the liquid either because the solids or the liquid are valuable or because these have to be
separated before disposal.
If the primary purpose is to produce the solids in a highly concentrated slurry, the process is
called thickening. If the purpose is to clarify the liquid, the process is called clarification. Usually,
the feed concentration to a thickener is higher than that to a clarifier. Some types of equipment, if
correctly designed and operated, can accomplish both clarification and thickening in one stage.
Materials and Apparatus:
A. Materials:
Soil, water
B. Apparatus:
Sedimentation Study apparatus, graduated cylinder, triple beam balance, stopwatch,
beaker, seive
Procedure:
1 The cylinders of the sedimentation study apparatus should be cleaned first and checked to see if
there is any leakages.
2 The soil should be dry and sieve into fine particles.
3 weighed the fine soil particles into 10, 20 and 30 grams using the triple beam balance
.4 placed the fine soil into a beaker and add 1 L of water. shook the solution to obtain a
homogeneous composition.
5 transferred the suspension into the sedimentation apparatus cylinder making sure that no fine
soil was left on the beakerm. Shook the cylinder again so that some of the soil that settled was
diffused throughout the suspension again.
6 placed the cylinder back to the sedimentation study apparatus and start the timer . Switch on the
backlight for easier reading and record the height of sedimentation by varying the time.

Data and Results:

Table 1. Height of sedimentation at different times of three concentrations of solids

Height of Sedimentation (mm)

Time (min) 1 2 3
(10g/1L) (20g/1L) (30g/1L)
 1 2 3

Initial wt. of solid(g) 10 20 30

Concentration,(g/li)

Final Height of Sediment, (mm)

calculations:
calculate the concentration of the slurry and record the final height of the sediment.

Conclusion:
 Experiment 3
Drag Coefficient of a Sphere

Title: Drag Coefficient of Spheres

AIM: To measure the drag coefficient of a sphere as a function of Reynolds number.
Introduction
Drag is the force acting opposite to the relative motion of the object moving in a fluid medium.
The drag force on a body consists of two components. One component is pressure drag, which is
caused by the air particles being more compressed on the front- facing surface of the body and
more spaced out on the back surfaces of the body. The other component of drag is the friction drag,
which is caused by the friction of the fluid applied against the surface of the moving body. This
experiment will show how thedrag force (F D ) is a dependant on the speed of the moving body (v),
the size of the moving body (A) and the density of the fluid medium that the body is moving
through (ρ f ). The drag force can be defined as follows: FD=CD1 2ρf v2 A

Experimental Setup and Theory

As an object falls through a fluid, whether it be water or air, it will naturally experience a gravity
force pulling it down, but less intuitive, it will experience a drag force and possibly a buoyant force
opposing the downward motion. Both the gravity and buoyant force is a constant, but the drag
force is directly related to velocity. Figure 1 shows the force balance acting on the object as it falls.

Figure 1: Force balance of a falling object.

The experimental apparatus used to perform this laboratory exercise is shown below in Figure 2.
Figure 2: Experimental test apparatus.

The Drag Coefficient

When a fluid flows past a solid body, or the body moves through the fluid (e.g., Figure 12.1), the
force
(FD) exerted on the body by the fluid is proportional to the relative rate of momentum (mass flow
rate × velocity = ρV 2A) transported by the fluid. This can be expressed in terms of a dimensionless
drag coefficient (CD), which is defined by the following equation:

FD CD
= ρV ² (1)
A 2
Here
ρ is the density of the fluid
V is the relative velocity between the fluid and the solid body
A is the cross-sectional area of the body normal to the velocity vector V. For example, for a sphere
of diameter d it is πd2/4
Each force acting on the body had to be calculated in order to determine the drag coefficient acting
on the cylinder. First the buoyant force for a sphere is calculated using Equation (1).

F B=Vρ g (2)
Next the force of the weight is calculated using Equation (2).

F W =mg (3)
Finally the drag force is evaluated. Equation (4) shows that the drag force is directly related to the
velocity of the sphere.

1
F D = ρAC D V 2
2 (4)
From Figure 1 it is possible to notice that the weight force minus the buoyant force is equal to the
drag force acting on the body. Therefore, Equation (4) can be rewritten to express the drag force in
terms of the buoyant and weight forces, when the sphere has reached terminal velocity.
 1
F W −F B= ρAC D V 2
2 t (5)
The drag coefficient acting on the sphere can therefore be calculated once the terminal velocity is
FD
known using the equation: CD =
½ ρAV ²
(6)
Since the drag coefficient is calculated for the sphere, it is also important to know the Reynolds
number for the sphere so the data can be compared to theoretical published values. Equation (7) is
the equation for calculating the Reynolds number.

ρ Vd
Re =
d μ (7)

APPARATUS/ MATERIALS:
Drag coefficient apparatus, metal spheres, Vanier caliper, cylinder, meter rule, and engine oil.
Procedure
1.Measure the diameter and obtain the mass of all three spheres. Record these values
2.Place one sphere at the top of the tube and prepare to start the timer.
3.Release the spheres into the tubes.
4.Start the timer when the sphere reaches the first O-Ring.
5.Stop the timer when the sphere reaches the bottom. Record the time.
6.Retrieve the sphere using magnet.
7.Repeat steps 2 to 6 for the other two spheres.
8.Retrieve the spheres.
9.Repeat step 7, two more times to have a total of three trials for each sphere.
Results
Table 1: Experimental results of the spheres engine oil.

Spheres Mass (kg) Time 1 (s) Time 2 (s) Time 3 (s) Avg. Time (s)

Table 2: Areas and terminal velocities for each spheres.

Terminal
Velocities
Spheres Area (mm2) Vt (m/s)

Table 3 Drag Coefficient, Drag Force and Reynolds Numbers for each spheres.

Spheres Drag Coefficient (CD) Drag Force (FD) Reynolds Number

(Red)
Calculations:
1. First, the velocity should be calculated as a function of time. Since the ball needs to be traveling
at terminal speed in order to perform the correct force balance, the velocity had to be determined.
Equation (8) is the velocity in terms of time.
h(m)
Vt = (8)
t (s )

2. Calculate the areas of the spheres using the equation

πd ²
4
3 calculate drag coefficient(CD) using equation (6)
4 calculate drag force (FD) using equation (4)
5 calculate Reynolds number using equation (7)

3
NOTE: Volume of a sphere is calculated using V ¿ πr², Density of engine oil SAE 40 is
4
3
872.5kg/m
 9.000
8.000
7.000
6.000
5.000
CD

4.000
3.000
2.000
1.000
0.000
0.00E+00 1.00E+04 2.00E+04 3.00E+04 4.00E+04 5.00E+04

Experimental Theoretical

Figure 3: Drag coefficient versus Reynolds number.

Conclusions
 Experiment: 4

Heat Transfer in Natural Convection

Aim:- To determine the surface heat transfer coefficient for a vertical tube losing
heat by natural convection.
INTRODUCTION
There are certain situations in which the fluid motion is produced due to change in density resulting
from temperature gradients. The mechanism of heat transfer in these situations is called free or
natural convection. Free convection is the principal mode of heat transfer from pipes, transmission
lines, refrigerating coils, hot radiators etc.
The movement of fluid in free convection is due to the fact that the fluid particles in the immediate
vicinity of the hot object become warmer than the surrounding fluid resulting in a local change of
density. The colder fluid creating convection currents would replace the warmer fluid. These
currents originate when a body force (gravitational, centrifugal, electrostatic etc) acts on a fluid in
which there are density gradients. The force, which induces these convection currents, is called a
buoyancy force that is due to the presence of a density gradient within the fluid and a body force.
Grashoffs number a dimensionless quantity plays a very important role in natural convection.

Theory:
When a hot body is kept in still atmosphere, heat is transferred to the surrounding
fluid by natural convection. The fluid layer in contact with the hot body gets
heated; rise up due to the decrease in its density and the cold fluid rushes in to take
place. The process is continuous and the heat transfer takes place due to the relative
motion of hot cold fluid particles.
The heat transfer coefficient is given by:

q – q1
h = ----------------------................................................(1)
As x (Ts – Ta)

Where, h = Average surface heat transfer coefficient (W/ m 2 0C)

q = Heat transfer rate (Watts)
As = Area of heat transferring surface = π. d. l (m2)

Ts = Average surface temperature

(T1 + T2 + T3 + T4 + T5 + T6 + T7)
0
= C
7

Ta = Ambient temperature in the duct = T8 0C

q1 = Heat loss by radiation = σ . A. ε . (T 4s – T 4a)

Where, σ = Stefan Boltzmann constant = 5.667 x10-8 W/m2.K4

A = Surface area of pipe = (0.05966) m2 = πDL
 ε = Emissive of pipe material = 0.6
Ts and Ta Surface and ambient temperatures in 0K respectively

The surface heat transfer coefficient, of a system transferring heat by natural convection depends
on the shape, dimensions and orientation of the fluid and the temperature difference between heat
transferring surface and the fluid. The dependence of ‘h’ on all the above-mentioned parameters is
generally expressed in terms on non- dimensional groups as follow

n
hxL g. L3. β. ∆T Cp. •
--------- = A x --------------------- x ------------......................................(2)
k v2 k

hxL
Where, ----------......................................is called the Nusselt number,
k

g.L3. β. ∆T
-----------------................................is called to Grashof Number and
2
v

Cp. •
----------- ………… is the Prandtl Number
k

A and n are constants depending on the shape and orientation of the heat transferring
surface.
Where, L = A characteristic dimension of the surface.
K = Thermal conductivity of fluid.
v = Kinematics Viscosity of fluid.
• = Dynamic Viscosity of fluid.
Cp = Specific heat of fluid.
 = Coefficient of volumetric expansion for the fluid.
g = Acceleration due to gravity.
∆T = [Ts – Ta]

1
For gases,  =------------------/ 0 k
(Tf + 273)

(Ts + Ta)
Tf =
2

For a vertical cylinder losing heat by natural convection, the constant A and n of
equation(2) have been determined and the following empirical correlation obtained.

hxL
..........................................
--------- = 0.59(Gr. Pr) 0.25 for 104 < Gr. Pr < 108 (3)
k

hxL
--------- Specification:

1. Diameter of the tube (d) = 38 mm

2. Length of tube (L) = 500 mm
3. Duct size 200mm x 200mm x 800mm. Length
4. Multichannel Digital Temperature Indicator 0 – 300 0C using Chromel /
Alumel thermocouple.
5. Ammeter 0 – 2 Amp. and Voltmeter 0 – 200 Volts.
6. Dimmerstat 2 Amp. 240 Volts.

Schematic Diagram:
...............................................................
= 0.13(Gr. Pr) 1/3 for 108 < Gr. Pr < 1012 (4)
k
L = Length of the cylinder.
All the properties of the determined at the mean film temperature (Tf).
 Procedure:

1. Put ON the supply and adjust the dimmerstat to obtain the required heat
input – (Say 40W, 60W, 70W etc)
2. Wait till the steady state is reached, which is confirmed from temperature
reading- (T1 to T7)
3. Measure surface temperature at the various point i.e. T1 to T7.

4. Note the ambient temperature i.e. T8

5. Repeat the experiment at different heat inputs (Do not exceed 80w)

RESULTS:

1. O. D. Cylinder = 38mm.
2. Length of cylinder = 500mm.
3. Input to heater = V x I Watts

Observations Table:

Sr. No. Volt Amp TEMPERATURE, 0C

T1 T2 T3 T4 T5 T6 T7 T8

Calculations:
1) Calculate the value of average surface heat transfer coefficient,
neglecting end losses using equation (1).

2) Calculate and plot (fig. 4) the variation of local heat transfer coefficient
along the length of the tube using:
q
T = T1 to T7 and h = --------------------
As (Ts + Ta)
3) Compare the experimentally obtained value with the prediction of the correlation
equations (3) or (4).

Note – The heat loss due to radiation and conduction is not considered,
but they are present, which give different between actual and theoretical
values.

Results and Discussion:

Some typical results are shown in fig. 4 and 2 different heater

inputs. The heat transfer coefficient is having a maximum value at the
beginning as expected because of the just starting of the building of the
boundary layer and it decreases as expected in the upward direction due
to thickening of layer and which is laminar one. This trend is
maintained up to half of the length (approx.) and beyond that there is
little variation and turbulent boundary layers. The last point shown
somewhat increase in the value of heat transfer coefficient which is
attributed to end loss causing a temperature drop.

The comparison of average heat transfer coefficient is also made with

predicted values are somewhat less than experimental values due to the heat
loss by radiation.

Therefore, Heat loss by radiation = σ. A. ε. (Ts 4 – Ta 4)

Where, σ = Stefan Boltzmann constant = 5.667 x 10-8 W/

m2
K4 A = Surface area of pipe = 0.59 m2
ε = Emissivity of pipe material = 0.6
Ts and Ta = Surface and ambient temperature in K respectively.

Conclusion: Heat coefficient for a vertical tube losing heat by natural convection is found
out to be__________