THE COPPERBELT UNIVERSITY

SCHOOL OF MINES AND MINERAL SCIENCES

CHEMICAL ENGINEERING LAB MANUAL

CE 330

Compiled by: A.N. Mugala, P. Chipili & J. Musonda

Approved by: ---------------------------------------------

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Table of Contents

Laboratory safety, rules and regulations 3

General rules 3
Laboratory safety rules 4

Safety agreement 6
Responsibility of students 7

Experiment 1: Investigation of flow patterns 8

Experiment 2: Viscosity of a fluid by Ostwald’s viscometer method 10
Experiment 3: Investigating heat transfer in a Liebig condenser 13
Experiment 4: Calibration of a flowmeter 15
Experiment 5: Variation of flow rate with pressure head 20
Experiment 6: Variation of pressure with height of fluid 21
Experiment 7: Constant area fin 22
Experiment 8: Flow measurements (weirs) 24

Experiment 9: Friction losses in pipe system 25

Experiment 10: Mass transfer in agitated vessels 26
Experiment 11: Screen analysis 28
Experiment 12: Determination of copper by electrolysis 30

Experiment 13: Determination of optimum flocculation dose for raw water. 32

Experiment 14: Solubility curve for a ternary system of liquids 34

Experiment 15: Efflux time from a tank 37

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LABORATORY SAFETY, RULES AND REGULATIONS

Laboratory safety is the top priority and this requires every person in the laboratory to observe
safe practices at all times!

General Rules
1. Students must abide by the dress code while working in the laboratory.
2. Laboratory coat must be worn all the time when working in the laboratory.
3. Only closed toe shoes are allowed in the laboratory. Do not wear sandals, slippers and
high heeled shoes inside the laboratory.
4. Students with long hair must get their hair well confined when doing laboratory work.
5. Bags and other belongings must be kept at the designated places.
6. Always wear proper eye protection in chemical work, handling and storage areas.
7. Never engage in horseplay, pranks or other acts of mischief in chemical or biological work
areas.
8. Always know the hazards associated with the materials that are being utilized in the lab.
9. Properly label chemical waste with specific contents. Keep label attached to the container at
all times. Always replace old and deteriorated labels.
10. Keep chemical waste containers closed.
11. Do not use cell phones, Bluetooth and MP3 players while working in the lab.
12. Never leave an open flame unattended. Know the location of the nearest fire extinguisher.
Never leave an experiment unattended while it is being heated or is rapidly reacting.
13. Do not keep or work with flammable substances near a flame.
14. Never remove chemicals, biological agents or any other laboratory related item from the
laboratory without proper authorization.
15. Foods, drinks and smoking are strictly prohibited inside the laboratory.
16. Food or drinks and chemicals should not be stored in the same refrigerator.
17. Noise must be kept to the minimum as a courtesy to respect others.
18. Students are not allowed to work alone without the supervision of laboratory
instructor/officer.
19. There must be at least 2 persons present in the laboratory at same time.

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 20. Students are not allowed to bring any outsiders (non-registered parties) into the
laboratory.
21. Any unauthorized experiment without the knowledge of laboratory instructor is
prohibited.
22. All instruments and equipment must be handled with care.
23. Remove clutter and practice good housekeeping.
24. Workspace has to be cleaned and tidied up after the experiment is completed. Instruments
and equipment must be returned orderly after use.
25. Students are strictly prohibited to take any equipment or any technical manuals out of the
laboratory without the permission of laboratory instructor/officer.
26. Students are required to instill an instinctive awareness towards property value of
laboratory equipment and to be responsible when using it. Any damages can jeopardise
the success of not only the individual work but also the university.
27. Do not attempt to remove and dismantle any parts of the equipment from its original
design without permission.
28. Keep equipment back from the edge of the lab bench to prevent spillage.
29. Report any accident immediately, however minor or irrelevant you might think it might be.
30. Students shall be liable for damage of equipment caused by individual negligence. If any
damage has occurred, an investigation will take place to identify the causes and the
names of the involved students will be recorded for faculty attention.
31. Please check the notice board regularly and pay attention to laboratory announcements.
32. Disciplinary action shall be taken against those students who fail to abide by the rules and
regulations.

Laboratory Safety Rules

 It is always a good practice and the responsibility of an individual to keep a tidy working
condition in laboratory.
 It is important for each student to follow the procedures given by the laboratory instructor
when conducting laboratory experiment.
 Before any experiment starts, students must study the information / precaution steps and
understand the procedures mentioned in the given laboratory sheet.

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 Students should report immediately to laboratory instructor/officer if the laboratory
equipment is suspected to be malfunctioning or faulty.
 Student should report immediately to the laboratory instructor/officer if discovered any
damages on equipment or any hazardous situation.
 Students should report immediately to the laboratory instructor/officer if any injury
occurred.
 If there is a tingling feel when working with electrical devices, stop and switch off the
devices immediately. Place a warning note before reporting to the laboratory
instructor/officer and wait for further instruction.
 Do not work with electricity under wet condition in laboratory. Electric shock is a serious
fatal error due to human negligence and may cause death.
 Students are required to wear goggles, gloves, apron and mask when handling corrosive
or active chemical agents.
 Hazardous chemical agents must be properly stored and labeled in a designated place.
Students must acquire and study the material safety data sheet of a particular chemical
agent before using it.

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SAFETY AGREEMENT
I have studied; I understand and agree to follow the safety regulations required for this course. I
have located all emergency equipment and now know how to use it. I understand that I may be
dismissed from the laboratory for failure to comply with stated safety regulations.

Signature …………………………
Name………………………………
Computer No……………………..
Date………………………………..
Course……………………………..
Department……………………….
Supervisor…………………………

Person (s) who should be notified in the event of an accident:

……………………………………..
……………………………………..
……………………………………..
……………………………………..

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RESPONSIBILITY OF STUDENTS

 Attendance is compulsory. Attendance shall be taken during the laboratory session.

 Please sign your attendance when you attend the laboratory session.
 laboratory report can only be accepted for submission if the student has attended the
laboratory session.
 Student must be punctual to attend laboratory session.
 Students who are late for more than 30 minutes will be barred from attending the
laboratory session. Only students with valid reason of medical basis or unforeseen
circumstances can be considered to apply for laboratory replacement.
 Students are expected to study the lab sheet before the laboratory session start.
 Student must understand all the safety measures / precaution steps before starting any
experiment.
 Student must complete the experiment within the allocated duration of laboratory session.
 Students are responsible for the condition of their working area at the end of each
laboratory session. All power to the equipment and instruments should be turned off, and
cooling water flows should be shut off. Glassware used should be cleaned and dried.
 Students have to pass up their experiment results to laboratory staff on the same day after
every experiment. A copy of the experimental result (with chop) must be attached
together with the laboratory report.
 Fabricating results and plagiarism are strictly prohibited. Strict action will be taken if
student is found fabricating results or copy from others.
 Students have to pass up their laboratory report two weeks after the date of experiment to
laboratory staff.

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EXPERIMENT 1:

TITLE: INVESTIGATION OF FLOW PATTERNS

AIM

To demonstrate laminar and turbulent flow patterns

To demonstrate the relationship between Re and water velocity

INTRODUCTION

In this experiment, water is discharged from a constant head device through a circular glass pipe
of known diameter. Water flow rate is varied and the flow pattern within the glass pipe is
observed, by injecting a fine tracer stream of colored liquid into the water. In this way the
relationship between pipe diameter, flow rate and flow pattern is investigated.

PROCEDURE

 Assemble the apparatus as shown in the diagram above.

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  Open inlet until apparatus is about 275mm filled with water.
 Ensure steady state conditions are achieved at this flow rate.
 Collect water in a calibrated receiver over a period of time.
 Measure the internal diameter of the glass pipe line
 Introduce some drops of KMnO4 and make observations.
 Repeat steps (2) and (6) a number of different flow rates

RESULT ANALYSIS

 Report flow regimes under different flow rates

 Draw a graph of Re Vs Velocity (m/s) and comment on the graph
 Explain which kind of flow is encouraged by increases in the flow rate, viscosity and pipe
diameter.

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EXPERIMENT 2

TITLE: VISCOSITY OF A FLUID BY OSTWALD’S VISCOMETER METHOD

PRINCIPLE
Viscosity is the property of a fluid that determines its resistance to flow. For example, it is an
indicator of flow ability of a lubricating oil; the lowest the viscosity, the greater the flow
ability. It is mainly due to the forces of cohesion between the molecules of lubricating oil.
Absolute Viscosity may be defined as “the tangential force per unit area which is required to
maintain a unit velocity gradient between two parallel layers. Its Unit is centi stokes (cSt).
Viscosity generally decreases with increase in temperature. The maintenance of viscosity
over the range of temperature is called the viscosity Index (V.I). A relatively small change/no
change in viscosity with temperature is indicated by high viscosity index whereas low
viscosity index shows relatively large change in viscosity with temperature Note: There is a
direct correlation between molecular structure of lubricating oil with its viscosity and
viscosity index. A high viscosity index is exhibited by those lubricating oils which have
linear or rod like shape molecules with high molecular weight. This is due to the greater
intermolecular forces of attraction. Viscosity of lubricating oil is inversely proportional to the
temperature i.e. with increase of temperature, viscosity decreases. This is due to the decrease
in intermolecular attraction. At higher temperature, oil must have sufficient viscosity to carry
loads. Kinematic viscosity is calculated by multiplying the time in seconds by the viscometer
constant while Dynamic viscosity is calculated by multiplying the kinematic viscosity by the
specific gravity of the oil at the same temperature.

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PROCEDURE:

The experimental set up is as shown,

1. Slowly pour the sample of oil under test through the tube marked L to fill up the bulb of
the Ostwald viscometer marked A up to the level marked G.
2. Place the viscometer in a water bath set at 40ºC and allow equilibrium to be attained
within 30 minutes.
3. Using a suction pump, fill up the bulb marked C to a height above E.
4. Remove the pump and allow the oil to fall freely to E
5. Using an accurate timer, note down the time in second it takes the sample to fall from E
to F.
6. Repeat the process 5 times and calculate the mean time.
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7. NB It is very important that the temperature is kept constant. Otherwise the results will be
rendered inaccurate due to temperature fluctuation.

Results and Analysis

(a) Kinematic viscosity

Kinematic viscosity @ 40ºC = _____________________________________

(b) Dynamic viscosity

(c) Dynamic viscosity @ 40ºC = __________________________________

Questions

1. In detail, explain the significance of viscosity of fluids.

2. Briefly explain the effect of temperature on viscosity

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EXPERIMENT 3

TITLE: INVESTIGATING HEAT TRANSFER IN A LIEBIG CONDENSER

AIM:

 To determine the duty of the heat exchanger

 To estimate the heat transfer coefficient for the setting

INTRODUCTION

A heat exchanger, transfers heat from a hot fluid to a cooler fluid. In this experiment, a
laboratory water cooled Liebig condenser to reduce the temperature of a stream of hot liquid is
used.

APPARATUS

PROCEDURE

 Fit a laboratory condenser with thermometers at each inlet and outlet.

 Pass the hot liquid which is to be cooled through the central ‘tube’ of the heat exchanger.
Pass the cooling water through the outer ‘shell’ in a counter-current direction.
 Adjust the flow rates of both liquid streams to give a temperature drop of at least 5 oc for
the hot liquid.

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  When conditions are steady, record the hot liquid inlet temperature T 1 and outlet
temperature T2, also the cooling water inlet temperature t1 and the outlet temperature t 2.
 Measure the mass flow rate of the hot liquid and cooling water through the heat
exchanger.
 Measure the length and average diameter of the ‘tube’ across which the heat transfer
takes place.

ANALYSIS OF RESULTS

 Calculate the heat lost by the hot liquid and the heat gained by the cold water.
 Calculate the overall heat transfer coefficient.

NOTE

The duty of the heat exchanger (Q) for the hot liquid is described by the equation:

Heat transfer per hour (Q)/KJhr-1 = Mass flow per hour/Kghr -1 x Specific heat capacity of
liquid/KJKg-1 K-1 x Temperature change (T1-T2)/K

The performance of a heat exchanger is described by the equation:

Where U is the heat transfer coefficient.

The area of the heat transfer surface (A/m2) is calculated from the tube length (l/m) and the
average diameter (dav/m)

∆tm, the log mean temperature difference across the heat exchanger is calculated from t 1,t2,T1 and
T2

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EXPERIMENT 4

TITLE: CALIBRATION OF A FLOWMETER

INTRODUCTION

1. Efficient operation and control of processes involving fluid flow requires flowmeters of
acceptable accurancy, reliability and adequate methods of calibrating them and recalibrating
them. To be adequate, the method of calibration must involve an independent determination of
the rate of flow of higher accuracy than that with which the flow meter may be read. Then it is
possible not only to determine the ‘time’ flow rate corresponding to each flow meter scale
reading but also to estimate random of readings.

2. This experiment is an exercise in the initial calibration of a ‘Rotameter’flowmeter for the

measurement of the volumetric rate of water at room temperature.

EXPERIMENT EQUIPMENT

3. The ‘Rota meter’ Flow meter has two components, a straight glass tube about 300mm long
and of diameter suitable for the flow and a ‘rotor’ within the tube. The tube has a slight, but
accurate taper in its bore and is marked with a uniform scale with its zero near the small bore
end. The rotor has its main body of a cylinder whose length is about equal to its diameter, which
is some 80% of the tube diameter. At its base the cylinder tapers in a con,its top extends as a
thin, sharp edge disc with a diameter barely less than the minimum bore of the tube, just beneath
the disc there is a circlet of angled vanes which cause the rotor to spin as fluid flows past it.

4. In use the Rota meter tube is mounted vertically with the smaller bore at the lower end and the
flow upwards. For zero flows the rotor at the lower end with the flow upwards. For zero flow the
rotor rests on a spring top at the lower end of the tube. For a finite flow rate the fluid has to pass
through the annulus between the rotor and the tube wall. The consequent higher flow velocity
round the rotor, especially high in the very small gap round the edge of the disc at the top of the
rotor, combines with the effects of viscosity and turbulence to produce a pressure drop across the
rotor which varies directly with flow rate, intensity of turbulence and viscosity of the fluid and
inversely with the size of the annular gap. In this dynamic state three forces are acting on the
rotor.

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(i) Its weight acting downwards

(ii) Its buoyancy, acting upwards and equal to the weight of the fluid displaced by the volume of
the rotor.

(iii) An upward force due to the difference in fluid pressure across the rotor, which depends on
fluid density, viscosity and the size of the annular gap.

As the flow rate is increased from zero, the rotor will remain on its stop until the pressure force
becomes greater than the weight of the rotor minus its buoyancy force. The rotor will then rise up
the tube until the annular gap has increased (due to the taper in the tube bore) and so reduces the
pressure force to the point where the three forces are in equilibrium. The rotor then becomes
stationary at a position which can be defined conveniently by the tube scale reading indicated by
the sharp edge of the disc at the top of the rotor. It follows that there is a unique scale reading for
a specific flow rate of a fluid of specific density and viscosity so that the scale may be calibrated
for flow rate. It must be noted however that separate calibrations must be made for each fluid for
which the flow meter is used and that these calibrations cannot extend to zero flow rate.

(iv) This analysis has ignored the fact that the pressure drop across the rotor will depend not only
on the size in the area of the annular gap, It also depends on the shape of the gap which varies
with any eccentricity, or alignment of the axis of the rotor in relation to the axis of the tube, so
that the flow meter scale reading could be subject to random variations for a constant flow rate.
Errors of this kind are minimized by the spin produced by the circlet of angled vanes on the rotor
which generates a tendency to a concentric alignment of the rotor.

(v) The calibration Rig has, as its main components, the Rota meter mounted vertically over a
sink and a constant Head Tank higher than the rotameter.The constant head tank is a small open
container with three tubes leading from its base:-

a. The inlet tube connected to a water tap

b. The outlet tube connected to the bottom of the Rota meter tube.

c. The overflow tube draining into the sink.

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The level of the free surface if the water in the open tank is maintained at a constant level, either
by a weir which screens the overflow tube from the other tubes or by extending the overflow
tube up into the tank so that it acts as a combined weir and overflow. By adjusting the setting of
the tap feeding the inlet tube, so that the inflow matches the outflow to the Rota meter plus a
small steady overflow to the sink, the flow rate to the Rota meter can be varied over a wide range
whilst isolating the feed pressure to the rig from any fluctuations of mains pressure. Transparent
flexible pipes make all connections in the rig and the rate of flow through the system is
controlled by a screw clamp used to construct the cross-sectional area of the flexible pipes
connected to the Rota meter to achieve the desired flow rate. A compensating adjustment of the
supply tap is required from time to time to avoid flooding of the constant head tank.

(vi) The independent Determination of the rate of flow is made by measuring the volume of
water discharged from the outlet pipe of the Rota meter during a known time interval, using a
measuring cylinder and stop watch as recording instruments, the experimental conditions being
such that the rate and hence the flow meter scale reading is constant over discharge period.

REQUIREMENTS TO BE SATISFIED BY THE EXPERIMENT

The Results required from this experiment are:-

1. A calibration Graph relating the scale reading of the Rotameter to the Volumetric flow rate of
water at room temperature over the full scale range of the Rotameter.

2. An assessment with details of the arguments on which it is based, of the accuracy of flow rates
determined by the rotameter and of your calibration graph.

3. An assessment in similar terms of the adequacy of the method of calibration.

4. A report of your actual experimental procedure including a record of all measurements made
in their chronological sequence.

5. Sketches, broadly to scale and with key dimensions shown so that a reader could use them to
duplicate your experiment,

i. The calibration rig.

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ii. The construction of the constant head tank.

iii. The rotor in the rotameter tube with a precise indication of how its positioned relative to the
scale with readings.

6. Any other information considered relevant.

EXPERIMENTAL PROCEDURE.

(i) Check that the calibration rig is correctly set up and soundly assembled and that it can be used
satisfactorily. The rotameter on the combustion unit in the chemical engineering may also be
used.

(ii) Plan sequence of experimental measurements which will satisfy the requirements specified.
In making allowances for experimental conditions likely to affect the precision ,reliability and
general usefulness of your results, you may wish to consider amongst other things:-

 The effects of parallax, unsteadiness or misalignment of rotor

 On the observation of flow meter reading, the effects of fluctuations of water level in the
constant head tank, air bubbles in the pipes, variation of rig geometry
 On the steadiness of the pressure head in the rig, the alignment of the rotameter tube with
vertical
 The effects of the method of starting and stopping flow into the independent flow
measurement system on quantity recorded an d its synchronization with stop watch
reading and any effects on steadiness of flowmeter reading
 The dependence of overall accuracy of the independent flow measurement on the relative
accuracies and sizes of time interval and volume discharged.

(iii) Carry out the planned sequence of experiments subject to the need to modify the plan, if
it proves inadequate.

(iv) Record all your observations quantitative and qualitative clearly and simply as the are
made.

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Note that you are not required to reproduce your report information available in this
experiment brief. This may be attached as an appendix to the report and referred to as
necessary.

DATA ANALYSIS

 Prepare a plot of gallons per minute (GPM) versus rotameter reading (g/s) on
rectangular coordinates.
 Determine the constants in the linear regression equation.
Q=mR+b
Where,
Q = Flow rate, GPM
R = Rotameter setting, percent of scale.
m and b are the regression constants.
 Compare your best results with the manufacturer’s specification.
 Calculate the correlation coefficient for your measured data.

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 EXPERIMENT 5

TITLE: VARIATION OF FLOW RATE WITH PRESSURE HEAD

APPARATUS

One litre, three holed cylindrical plastic bottle, Thermometer, 30cm rule, A set of capillary
tubes of varying lengths and bores (if possible), Stop watch, 250ml measuring cylinder

PROCEDURE

 Measure the following dimensions of the capillary tube ( i) Diameter (ID) (ii) Length
 Stabilize the fluid level in the bottle to a constant head, by manipulating the overflow
tube and the fluid supply flow rate.
 Using the stop watch and the measuring cylinder, determine the volumetric flow rate
through the capillary tube at the constant head.
 Measure the fluid temperature.
 Adjust the overflow tube to a new level and repeat parts (a) to (d)

TREATMENT OF DATA

 Calculate the following parameters

 Velocity at each head.
 Reynolds number at each head.
 Establish the following relationship on a graph paper.
 Head vs Velocity
 Reynolds number and flow rate
 Discuss your results in relation to those in the literature in the the library under similar
conditions.

RECOMMENDATIONS

Recommend any improvements that can made to this experiment.

CONCLUSION

Make conclusions about the experiment

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EXPERIMENT 6

TITLE: VARIATION OF PRESSURE WITH HEIGHT OF FLUID

THEORY

Set out a suitable theory

APPARATUS

 Measuring cylinder
 Meter rule or travelling microscope
 Weighting scale

METHOD

 Set up the apparatus

 Using the beam balance, weigh the empty measuring cylinder.
 Fill the empty measuring cylinder with water to 3cm level.
 Using the beam balance, weigh the the measuring cylinder with water in it.
 Add more water to the measuring cylinder to a different level (6cm) and take the overall
weight.
 Repeat step five (5) and take weights at five additional points.
 Using a vernier caliper, measure the diameter of the measuring cylinder.

RESULTS

 Set out a table of results to include, Wt of container, Wt of container with fluid,Wt of

fluid, Height of fluid and pressure.
 Plot a graph of pressure of fluid versus height of fluid.

CONCLUSION

 From the plotted graph develop a relationship between pressure of fluid and its height and
evaluate whether it agrees with the theory.
 Make conclusions.

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EXPERIMENT 7

TITLE: CONSTANT AREA FIN

AIM: To determine the the heat transfer coefficient between the ambient air and the fin.

MATERIALS

Copper wire, Thermometer, Micrometer Screw gauge, Meter rule and a Water bath

THEORY

The temperature profile along a fin of length L and diameter D is:

T(x)-T∞/To-T∞=Cosh.m (L-x)/Cosh.mL………….(1)

For a cylindrical fin m2 = 4h∞/KD, K = Conductivity of the fin (e.g. Copper wire).The
experiment attempts to determine h∞ by iteration method.

PROCEDURE

 Fix the copper wire in a water bath so that it stands upright.

 Fill the water bath to the brim and heat the water between 60oC and 70oC.
 Measure the fin base temperature (the temperature of the fin just above the surface of the
water).
 Measure the ambient air temperature T∞.
 Measure the temperature T(x),at x distance from the fin base [mark a cut for x on fin].
 Repeat step five (5) for three (3) times.

RESULTS

To=? T∞=? D=?

Run Distance (x) T (x)

1
2
3

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NOTE

The value of X should be constant but not T(X) due to infinitesimal variations in T∞, which
has been assumed constant.

ANALYSIS OF RESULTS

Guess the initial value of h∞ [use the literature value of h∞ between atmospheric air and a
vertical rod of diameter D]

The value of h∞ which makes LHS=RHS of equation (1) is the correct value [h∞: 0 < h∞ < 10

WRITE UP

 Why should the water bath not be heated above 70oC?.

 What are the short comings of this experiment?.
 How can you improve the experiment in order to sufficiently achieve its objectives?.
 Find the formula and use it to confirm the h∞ value found by iteration.

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EXPERIMENT 8

TITLE: FLOW MEASUREMENTS (WEIRS)

THEORY: SET OUT A SUITABLE THEORY.

APPARTUS

 A pump, a pipe delivery system, a tank with suitable weir.

METHOD

 Switch the power.

 Plug in the speed control for the pump.
 Set the speed as required beginning with low speed.
 Take readings of weir depth o the fluid and weir fluid width.
 Repeat at different speeds and different levels of fluid,(about 5 to 6 times).

ANALYSIS OF RESULTS

 Evaluate flow rates at chosen speeds

 Plot graphs flow versus depth and flow versus width of fluid.
 Do these results agree with theory?
 Draw conclusions.

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EXPERIMENT 9

TITLE: FRICTION LOSSES IN PIPE SYSTEM

THEORY: SET OUT A SUITABLE THEORY

APPARATUS

 A pipe line with suitable fittings and enlargement or contractions,elbows,T-junctions etc

METHOD

 Explore the chosen pipe system and identify the fittings,elbows,T-Junctions etc.
 Take the length of the pipe system.
 Evaluate the friction loss for system.

ANALYSIS OF RESULTS

 Table out your results as much as you can.

 Do these results agree with the theory?
 Draw conclusions.

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EXPERIMENT 10

TITLE: MASS TRANSFER IN AGITATED VESSELS

AIM: To measure mass transfer coefficients as a function of extent of agitation for the
transfer of solid salicylic acid into water. Further to correlate the mass transfer coefficient
with operating and system variables.

EXPERIMENTAL PROCEDURE

Vessels are carefully filled with a known amount of distilled water. The stirrers are set at
different speeds of rotation and the amount of salicylic acid going into solution is measured
as a function of time by titrating 10ml of samples (taken at intervals) with 0.1mol/L of
sodium hydroxide solution.

 Fill each of the vessels to just above the baffle with distilled water, noting how much
water it takes.
 Then from right to left, the stirrer speeds should be 100rpm, 200rpm and 300rpm.
 Take samples at 5min, 10min and 15min of titration.
 Continue the experiment until the points collected are good enough to form a linear
graph.

ANALYSIS OF RESULTS

 The rate of mass transfer is given by, where k is the mass

transfer coefficient, A is the area of solid ring/tablet and V is volume of solution, is
the interfacial concentration (saturated) with value of about 0.0163 kmol/m3, is
concentration at time t.Use integrated form of equation to derive k at each stirring
speed.
 The Gilliland and Sherwood equation correlates mass transfer data of the type being
studied.

where k is m.t.c,Ɩ is diameter of the mixing tank d is the

molecular diffusivity (see Reid and Sherwood for D of say benzoic acid in water if that for

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salicylic acid cannot be found), and µ and ρ are viscosity and density of solution (take as
water),R is speed of rotation of stirrer and d is impeller diameter.

If Danckwerts theory applies, exponent b= 0.5 and unknowns in the above equation are k and
exponents c. Plot data to obtain values for these quantities.

In conjunction with writing up your report, take the opportunity of doing some reading on
theories of mass transfer.

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 EXPERIMENT 11

TITLE: SCREEN ANALYSIS

AIM:

To separate the given sample into fractions after thoroughly mixing, by using a set of
standard Tyler screens and weighing the retained fractions.

APPARATUS: Tyler screens, mesh # 70,100,140,200,270 and 325, pan, cover, fine brush,
weighing balance and sieve shaker.

METHOD: Arrange the screens in the following order; at the bottom the pan, 325mesh, next
270 and so on, with largest mesh size at the top (70).A sample of about 200g is taken (after
carrying out the procedure for thoroughly mixing to ensure a representation of sample, (see
method recommended) and accurately weighed. The sample is then placed on the top screen
(70 mesh) and the set of screens shaken for about 10-15 minutes. After this period the
fraction remaining at each screen is shaken off (carefull, do not damage screens) and weigh.
The results are tabulated as shown and graphs plotted of (1) cumulative weight (net) size in
microns (2) weight % retained against size in microns or mesh No. Weight sample taken =
200g

Size micron Tyler Mesh Wt Retained (g) %Wt Retnd. Cuml.wt% Retnd Cuml.wt% passing

212 70
150 100
106 140
75 200
55 270
45 325
Pan

From the graph of Cuml.wt % passing against screen size in microns, find the 80% passing
size.

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EXPERIMENT 12

TITLE: DETERMINATION OF COPPER BY ELECTROLYSIS

THEORY

A method by which reactions are carried out in solutions of electrolytes or in molten salts by
use of electricity. One or several reactions occur at each electrode when current flows
through the cell. Reduction - a reaction in which electrons are consumed occurs at the
electrode called the cathode while oxidation occurs at the anode. The method involves the
decomposition of copper atoms in a sample by treating it with a mixture of nitric and
sulphuric acids. The solution containing the electrolytic acid is electrolyzed at 2-amps and
the copper is deposited onto a platinum cathode. The increase in weight of the platinum
electrode is recorded and the percentage copper content in the sample is calculated.

APPARATUS

Electrolytic machine, 200ml Pyrex beaker, measuring cylinders (5ml, 10ml, 25ml), wash
bottle, analytical balance, spatula, hot plate, platinum electrodes, oven.

REAGENTS

Conc. sulphuric acid, Nitric acid, Isopropyl alcohol, Urea salt, distilled water.

PROCEDURE

 Weigh between 1-1.5g of the pulverized and sieved sample and transfer to a 200ml
beaker.
 Add 25ml-30ml of water and then 10ml of concentrated sulphuric acid and heat to boiling
for five (5) minutes.
 Cool the solution and add 5ml of concentrated nitric acid and then dilute with water to
about 150ml mark.
 Add 0.2g of urea crystals and dissolve with no spillages.
 Electrolyses to deposit the copper on a clean pre-weighed platinum electrode for 1.5 hrs
at 2-amps.

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 Continue electrolyzing until the blue color disappears, then add 15ml of water into the
electrolyte and continue the process so that the rise in volume of the solution could
confirm further electrolysis or not.
 After complete deposition has been confirmed with the current still flowing, remove the
solution carefully while rinsing the electrodes with a stream of water.
 The deposited copper will blacken and become oxidized if the current is broken
(switched off) before the electrodes are completely removed out of the solution and well
rinsed.
 Switch off the current, remove the electrode from the electrolytic machine, rinse with
water, then finally dip the electrode into the isopropyl alcohol and dry them in an oven at
105 to 110oc for 2-3 minutes.
 Cool the platinum electrode and take the final weight using the analytical balance.
 Clean the platinum electrode, so as to remove the deposited copper by immersing it in the
cleaning chemical solution provided (nitric acid).Ensure that all the deposited copper is
completely dissolved and then finally rinse with plenty of tap water.
 Rinse the platinum electrodes with plenty of tap water, then immerse them in isopropyl
alcohol and dry them in an oven for 2-3 minutes.

CALCULATIONS

% Cu in sample = [Wt of cathode +Cu]-[Wt of cathode]/ [Wt of original sample]

 What is the colour of the solution after adding H2SO4 acid to the sample? Write a
chemical balanced equation for this reaction.
 What chemical reactions take place at the cathode and anode during electrolysis?
 Why is platinum used in this process?
 Where in Zambia is electrolysis applied?
 What safety precautions would apply to a real process?
 What environmental concerns or precautions would apply to a real process?
 Name the chemical used to clean the deposited copper from the platinum cathode and
write a balanced chemical reaction involved in the cleaning process.

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EXPERIMENT 13

TITLE: DETERMINATION OF OPTIMUM FLOCCULATION DOSE FOR RAW

WATER.

INTRODUCTION

The removal of fine suspended matter is of primary importance in the treatment of water for
domestic usage. Aluminium sulphate (Alum) by virtue of its large positive charge is able to
neutralize the negative charges tend to keep the particles of finely divided solids fully dispersed,
but small additions of alum (20-40 ppm) to the water enables coagulation to occur and by
frequent collisions with other particles a ‘ floc’ is formed, which collects the fine solids largely
responsible for the water’s coloured or turbid appearance.

Sodium aluminate acts in a similar fashion. Dosing with alum is a very flexible procedure and is
thus able to cope with the ever-changing quality of raw water due to seasonal variations.

NOTE

Describe the purpose of Jar testing and summarise the theoretical background. Expound on the
information that is presented in this handout.

REQUIREMENTS

Jar test apparatus, aluminium sulphate, pond water, pipette, Erlenmeyer flasks, methyl orange
indicator, 600 mL beaker, volumetric flasks, burettes, 0.02N sulphuric acid.

METHOD

 Add 500mL of raw water to four separate 600mL beakers.

 Pipette 2.5mL, 3.0mL,3.5mL and 4mL alum solution to the four beakers
(25; 30; 35; 40 ppm alum)
 Place the beakers on the Jar test apparatus and stir at 160 rpm for 2 minutes.
 Reducing stirring rate to 40 rpm and maintain at this speed for 20 minutes.
 Switch off flocculator and allow to precipitate to settle for atleast 20 minutes.
 Record

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 (a) Best floc

(b) Quickest settling time.

(c) Clarity of supernatant

 Determine the pH of each treated water sample.

 Measure the alkalinity of the sample with the largest alum concentration.

DATA ANALYSIS

Plot turbidity and pH as a function of coagulant dose.

QUESTIONS

What is the best coagulant dose?

Why did the pH change?

Why did the alkalinity change with dose?

Compare the measured alkalinity change with that of the theoretical alkalinity change
requirements.

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EXPERIMENT 14

TITLE: SOLUBILITY CURVE FOR A TERNARY SYSTEM OF LIQUIDS

OBJECTIVES

 To determine the solubility curve and tie lines for a ternary system of two immiscible
liquids and a third liquid which is miscible with each of them

INTRODUCTION

Acetic acid is one of the most widely used carboxylic acids. It is used in many reactions, for
example in synthesis of acetic esters, or it can be used as a solvent, for example in the
manufacture of cellulose acetate or pharmaceutical products. Acetic acid biosynthesis produces
important quantities of aqueous solutions from which acetic acid should be economically
recovered.

For acetic acid concentrations lower than 40% w/w the liquid-liquid extraction can be
appropriate process.

Acetic acid is an important laboratory reagent as well as solvent for carrying reaction since it
remains unchanged by oxidizing and reducing agents. It is used for coagulation of rubber latex,
for curing fish and meat, for the manufacture of vinyl acetate, poly-vinyl acetate etc.

In this study, in order to obtain data for solubility curve for a ternary system and tie lines, water
and n-butanol solvent of known mixture was titrated with a third component acetic acid to the
point of the first disappearance of permanent turbidity.

Note

Provide suitable theory

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EXPERIMENTAL WORK

APPARATUS AND CHEMICALS

125mL Erlenmeyer flasks, 2mL and 5mL pipettes, 2 burettes and holders. Distilled water, n-
butanol and glacial acetic acid

PROCEDURE

 Prepare the titration mixtures as in the table below:

No WATER (mL) n-BUTANOL (mL)

1 18 2
2 16 4
3 12 8
4 8 12
5 5 15
6 4 16
7 2 18

 Add acetic acid into No 1 binary mixture drop by drop until the first disappearance of
turbidity. Record the titration volume.
 Repeat this procedure for other binary mixtures.
 Calculate the composition of these ternary systems in terms of weight by weight percent
%.
 Plot the curve of the ternary acetic acid – n-butanol-water mixture using both right and
equilateral triangles.
 Draw tie lines in this solubility curve using the data below.
 Determine the Nernst diagram (Equilibrium curve)

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n-BUTANOL PHASE WATER PHASE

AA (%) W% BTA (%) AA (%) W (%) BTA (%)

4.5 10.0 85.5 3.5 86.0 10.5

10.0 12.5 77.5 7.5 81.0 11.5

14.5 17.0 68.5 10.5 77.5 12.0

15.5 24.0 60.5 13.5 69.0 17.5

Where :

AA = Acetic acid

W = Water

BTA = n-Butanol

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EXPERIMENT 15

TITLE: EFFLUX TIME FROM A TANK

OBJECTIVE

 To study the measured efflux time (drainage time) from tanks.

INTRODUCTION

Chemical processes can be classified under two broad categories which relate to their operation,
namely continuous or batch. In some large industrial plants combinations of both operations are
encountered. Most operations the student is exposed to one of continuous type but this should not
imply that batch operations are unimportant. In the pharmaceutical industry, for example, nearly
all chemical synthesis are carried out using batch processes. Good engineering control and
planning for these operations are critical for pollution prevention. Examples of batch operations
commonly encountered are emptying of hoppers containing solids i.e. coal, ore and grain
hoppers, and the discharging of tanks, i.e. reaction vessels, and liquid storage tanks. This
experiment deals with the emptying of a tank containing water and comparing the experimental
data with theoretical equations.

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37
NOTE : Provide suitable theory

PROCEDURE

 Attached the desired exit pipe to the quick opening valve.

 Fill the tank to a level slightly above the highest mark on the level scale.
 Reset the timers and start them all simultaneously.
 Open the quick-action valve.
 Stop the first timer when the liquid level falls to the first (highest) mark on the level
scale.
 Stop a timer as the liquid level falls past preselected uniformly spaced marks on the level
scale.
 Record the times.
 After the liquid has drained out, close the valve and refill the tank.
 Reset the timers, and repeat the experiment as needed.

DATA ANALYSIS

The principle variables in this study are tank diameters, pipe diameter, and pipe length.

Examine the following correlations for your system:

 Correlate the level in the tank H in inches, with the time of flow.
 At the lowest flow rate, estimate the Reynolds number at the pipe exit.
 Use the applicable equation and compare your measured data with the relationship by
linearization.
 Use linear regression analysis to determine the slope and compare the measured slope to
the theoretical slope given by the applicable equation.

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