FACULTY OF ENGINEERING AND THE BUILT ENVIRONMENT

DEPARTMENT OF CHEMICAL, METALLURGICAL AND MATERIALS

ENGINEERING

STUDENT LABORATORY GUIDE

NAME OF COURSE: CHEMICAL PLANT IIIB

NQF NQF
QUALIFICATION & SAQA ID COURSE CODE
LEVEL CREDITS

Diploma in Chemical Engineering

6 0.083 CMP33BT
SAQA ID No.:1799

COMPILED BY: VT Hlongwane& JM Mosesane

2015

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 ©COPYRIGHT: Tshwane University of Technology

Private Bag X680

PRETORIA

0001

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Printed and distributed by:

FACULTY OF ENGINEERING AND

BUILT ENVIRONMENT

Tshwane University of Technology

Private Bag X680

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0001

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 1. EXAMPLE OF A PRACTICAL REPORT WRITING

It is important that the writer(s) of an engineering report keep in mind the

needs and interests of the anticipated readers of the report. The laboratory
report should be written with the same professionalism that would be used to
present the results of a major industrial project. The people who will read it,
and need to draw conclusions from it, can be expected to have technical
training, but probably would not be familiar with the details of the work.

A good report of technical work quantitatively states significant results of

experiments and computations and explains how they were obtained, what they
mean, and how they are useful. The report should be clear, concise, and
accurate. Often the structure of the report must conform to specific
conventions. A format for laboratory reports that is to be used in this course is
given below.

1. Title Page

The title of the report is followed by names of the authors and laboratory group,
the date of submission, and identification of the institution or organization
supporting the work (Tshwane University of Technology, Department of
Chemical & Metallurgical Engineering, CMP33BT).

2. Abstract

The abstract is a tightly written summary, typically 100 to 300 words long. This
section is important because it is the first impression your report will make to a
reader, and it could very well be the only part of it he or she will read! (Because
of its importance, it is a significant part of the overall grade.) The abstract should
be written as “stand alone” section of just text. Its independence means that
the use of symbols, tables, and graphs as well as literature references should
be avoided. A good abstract states the principal objective of the investigation,
describes the methodology used and summarizes the results and conclusions
in statements as quantitative and as general as possible.

The abstract should provide ranges of the experimental parameters (e.g. the
Reynolds number was varied from 100 to 10000), report the most important
results and state how these values compare to expected (i.e., literature) ones.
(e.g., “values for the friction factor in the laminar flow regime were consistently
15% higher that the predictions of Poiseuille flow”). If the value of a single
variable or a short list of numbers is given, the numbers should give the
uncertainty (e.g., … solubility at 25C was 25± 3 moles/liter) and of course units
should be included.

We recommend that you write the abstract last, when your thoughts are most
clearly in focus (i.e., you know all the answers and thus know what to say!).

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3. Table of Contents

A Table of Contents should be included in the report, including a listing of the

Abstract. Appendices should also be listed. All pages should be numbered,
including tables, figures, and appendices.

4. Introduction

The purpose of the Introduction is to place the work in the perspective of prior
work including key literature references, demonstrate its importance, and state
the specific objectives. The Introduction should not exceed two pages.

5. Theory

This section is a short, concise statement of the essential empirical and

theoretical relations to be used in interpreting the data or to be tested by the
data. Equations are usually stated with a reference, along with the pertinent
assumptions and limitations. Brief manipulations may be appropriate, but long
derivations are relegated to an appendix. The physical significance of equation
parameters should be pointed out.

6. Experimental

A. Apparatus

The objective of this section of the report is to describe the experimental

set-up in enough quantitative detail to enable the reader to completely
understand the experiment. Ranges of independent variables are
cited. The model and supplier of any unique equipment should be
cited. Also, a schematic diagram of the experimental apparatus should
be included.

B. Procedure

The objective of this section of the report is to describe the materials and
methods used to obtain the experimental data. Emphasis is placed on
general procedures that are not routine

7. Results

The data, or a representative fraction of them, must be included in this section.

They should be presented graphically. If there are only a few (i.e. 2-3)
numbers, these could put into a table if they can be understood. Data are often
not presented in raw form, but are reduced and shown in the way most clearly
supporting the conclusions. Representation of scatter in data is essential. For
example, the experimentally determined heat transfer coefficient is
meaningless unless it is accompanied by units and an estimated
uncertainty. Comparison of data with theoretical predictions and/or previously
published values should be included whenever possible. This may require
searching for information in reference books or research articles. Comment

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 briefly on unique aspects of the results, in particular its accuracy. Also
comment on the range of the variables covered.

Each graph or diagram is assigned a number (e.g., Figure 1) and should have
a caption that is descriptive of the information contained in the figure. A
restatement of the information on the axes is not an acceptable title.

8. Discussion

All important interpretations which follow from the results and the underlying
theory are logically and quantitatively compared in the Discussion section. The
positive conclusions, comparison with literature data, and the significance
applicability, and reproducibility of the results are stressed. Quantitative
statements about the accuracy and precision of the results are
required. However, when a detailed error analysis is essential to the work, it
should be relegated to an Appendix.

9. Conclusions and Recommendations

This section is a summary of the most significant conclusions developed in the

preceding section. Quantitative statements are best. Useful recommendations
to improve the experiment and to extend the work to other systems, should be
included here.

10. Literature Cited

Only references cited in the report are to be listed is this section since it is not
a bibliography covering all references but only the most pertinent
ones. Footnotes on individual pages of the report are not to be
used. References cited in the text of the final project report should give the last
name of the author (both authors when only two; first author et. al. when more
than two) and the corresponding page numbers. An example is given below.

“The Reynolds number can be interpreted as the ratio of inertial to viscous

forces at work in the fluid (Denn 37-39).”

References are to be listed in alphabetical order according to author or

equivalent and should not be numbered. Use Chemical Abstracts Service
Source Index journal abbreviations. For the previous example the citation
would be the following:

Denn, M. M. “Process Fluid Mechanics”; Prentice-Hall; New Jersey, 1980

Typical citations for a journal are given below.

Danckwerts, P. V.; Sharma, M. M. Chem. Eng. (London) 1966, 202, 244.

Danckwerts, P. V. Chem. Eng. Sci. 1979, 34, 443.

11. Nomenclature

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 Symbols used in the report are defined immediately after they are presented
the first time. This section of the report lists all of the symbols used. Units
should be included.

12. Appendices

The appendices contain material of secondary importance: sample

calculations (a sample of all calculations done for the experiment must be
included in the report), error analysis, derivation of theoretical relations, and
perhaps graphs, calibration curves and/or schematics. Note that the
appendices should be named in the order of which they appear in the final
project report. In other words Appendix A should be the first appendix referred
to in the text of the report.

2. PRACTICAL

SCREENING AND SIEVE ANALYSIS

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INTRODUCTION

Sieve analysis is accomplished by passing a known weight of sample material

successively through finer sieves and weighing the amount collected on each sieve to
determine the percentage weight in each size fraction. Sieving is carried with wet or
dry materials and the sieves are usually agitated to expose all the particles to the
openings. When applied to irregular shaped particles, sieving is complicated by the
fact that a particle with a size near that of the nominal aperture of the test sieve may
pass only when presented in a favourable position. Sieving is also complicated by the
presence of “near size” particles which cause “blinding”, or obstruction of the sieve
apertures and reduce the effective area of the sieving medium. Blinding is very serious
with test sieves of very small aperture size.

THEORETICAL ANALYSIS

Sieving may be divided into two stages; the elimination of particles considerably
smaller than the screen apertures, which should occur fairly rapidly and the gradual
process rarely reaching final completion.Both stages require the sieve to be
manipulated in such a way that all the particles have opportunities for passing the
apertures, and so that any which blind the aperture may be removed from it.Ideally,
each particle should be presented individually to an aperture, as it is permitted for the
largest aperture sizes, but for most sizes it is impractical.The effectiveness of a sieving
test depends on the amount of material put on the sieve and the type of movement
imparted to the sieve.Basically, if the charge is too large, the bed of material will be
too deep to allow each one a chance to meet an aperture in the most favourable
position for sieving in a reasonable time.The sample must contain enough particles to
be representative of the bulk, so a minimum size of sample is specified.In some cases,
the sample will be divided into a number of charges if the requirements for preventing
overloading are to be satisfied.

EXPERIMENTAL PROCEDURE

1. Arrange the sieves chosen for the test in a stack, or nest accordingly.
2. Put a tight fitting pan or receiver pan below the bottom sieve and place the lid on
top.
3. Weigh the desired amount of material and place in the top sieve of the nest.
4. Place the nest in the sieve shaker, ensuring it is tightly secured.
5. The duration of screening can be set on the shaker.
6. After the required time, take the nest apart and weigh the amount retained on each
sieve.
7. Most of the near mesh particles which block the openings can be removed by
inverting the sieve and tapping the frame gently.

PRESENTATION OF RESULTS

The results can be tabulated as follows:

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 Sieve size Sieve Sieve Nominal Cumulative Cumulative
range (μm) fractions fractions aperture % %
weight (g) weight
Size (μm) undersize oversize
(%wt)

Total

i) Draw the distribution curve

ii) Draw the cumulative undersize and oversize curves
iii) Find D50 from yours graphs

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 FIXED AND FLUIDISED BED EXPERIMENT

1. Introduction

Chemical engineering operations commonly involve the use of packed and fluidized beds. These are devices in
which a large surface area for contact between a liquid and a gas (absorption, distillation) or a solid and a gas or
liquid (adsorption, catalysis) is obtained for achieving rapid mass and heat transfer, and particularly in the case
of fluidized beds, catalytic chemical reactions. You will find a good deal of information about flow through
packed and fluidized beds in the book by McCabe, Smith, and Harriott (2001) and Perry’s Handbook (1997).
Here, only a brief summary is given. First, let us consider flow through a packed bed.

2. Objectives

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 2.1 Determination of the bed porosity.

2.2 Pressure drops through beds of various packing materials will be measured and correlated with bed
properties and flow rates by means of existing models. These pressure drops will be measured using
two modes:

2.2.1 Fluidization with water and

2.2.2 Fluidization with air.

3 Theoretical background

3.1 Packed Beds

A typical packed bed is a cylindrical column that is filled with a suitable packing material. You can learn about
different types of packing materials from Perry’s Handbook. The liquid is distributed as uniformly as possible at
the top of the column and flows downward, wetting the packing material. A gas is admitted at the bottom, and
flows upward, contacting the liquid in a countercurrent fashion. An example of a packed bed is an absorber. Here,
the gas contains some carrier species that is insoluble in the liquid (such as air) and a soluble species such as
carbon dioxide or ammonia. The soluble species is absorbed in the liquid, and the lean gas leaves the column at
the top. The liquid rich in the soluble species is taken out at the bottom.

From a fluid mechanical perspective, the most important issue is that of the pressure drop required for the liquid
or the gas to flow through the column at a specified flow rate. To calculate this quantity we rely on a friction factor
correlation attributed to Ergun. Other fluid mechanical issues involve the proper distribution of the liquid across
the cross-section, and developing models of the velocity profile in the liquid film around a piece of packing
material so that heat/mass transfer calculations can be made. Design of packing materials to achieve uniform
distribution of the fluid across the cross-section throughout the column is an important subject as well. Here, we
only focus on the pressure drop issue.

The Ergun equation that is commonly employed is given below.

3.1.1

Here, the friction factorfp,for the packed bed, and the Reynolds number Rep, are defined as follows.

 P DP  3
fp =   3.1.2
H us2 1 − 

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 DP us 
Re p = 3.1.3
(1 −  ) 

The various symbols appearing in the above equations are defined as follows:

 p= pressure drop
H = length of the bed

Dp = equivalent spherical diameter of the particle defined by:

6 (volume of the particle/surface area of the particles)

P = density of the fluid

 = dynamic viscosity of the fluid

 s = superficial velocity (  /A where Q is the volumetric flow rate of the

fluid and A is the cross-sectional area of the bed)

 = porosity of volume fraction of voids of solid bed (  is the ratio of

void volume to the total volume of the bed).

Sometimes, we may use the concept of the interstitial velocity Vi , which is related to the superficial velocity by
VS
Vi = . The interstitial velocity is the average velocity that prevails in the pores of the column.


Two simpler results, each obtained by ignoring one or the other term in the Ergun equation also are in use. One
is the Kozeny-Carman equation, used for flow under very viscous conditions.

150
fp = Re  1 3.1.4
Re p

The other is the Burke-Plummerequation, used when viscous effects are not as important as inertia.

f p = 175
. Re p  1000 3.1.5

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It is suggested that the student simply use the Ergun equation. There is no need to use these other two approximate
results, even though they continue to be reported in textbooks.

When a fluid flows through a bed of particles in a tube, it will exert a drag force upon the particles resulting in a
pressure drop across the bed. As the fluid’s superficial velocity is increased, pressure drop is magnified. In
an unrestrained bed that has fluid flowing upwardly through it, a condition will be reached where, with
increasing fluid velocity, the drag forces will cause the bed to expand. This expansion allows the particles to
offer less resistance to the fluid flow. When the drag force is sufficient to support the weight of the particles in
the bed, the bed is said to be fluidized. The fluid/solid system shows fluid-like properties, and the bed can be
made to flow from one vessel to another. The pressure drop across the bed,  p, then remains constant (even
with further increase in the fluid velocity) and equal to the effective weight of the bed per unit area:

 P = g (1 −  )(  p −  f )  h 3.1.6

g = gravitational acceleration

 = porosity or volume fraction of voids of solid bed

 P = pressure drop across the bed

 p = density of particles

 f = fluid density

h = length of the bed

As the gas velocity, u, is raised beyond that required to bring the bed to a

Fluidized condition, Umf, the equation 1.2.4 becomes:

 P = g (1 −  mf )(  p −  f )hmf 3.1.7

 mf = minimum porosity at incipient fluidization

Typically, for a bed of small particles ( Dp  01

. mm ), the flow conditions at this stage are such that the
Reynolds number is relatively small (Re  10) that we can use the Kozeny-Carman Equation, applicable
to the viscous flow regime, for establishing the point f onset of fluidization. This yield:

(  p −  f )  g  Dp2  mf3
U mf =  3.1.8
150 1 −  mf

When the superficial velocity u is equal to Umf, we refer to the state of the bed as one of incipient
fluidization. The void fraction,  , at this state depends upon the material, shape, and size of the
particles.

For nearly spherical particles (small),  is in the range 0.40 – 0.45, increasing with particle size.

For large particles (Dp ≥ 0.1 mm), inertial effects are important, and the full Ergun equation must be
use to determine u. When in doubt, use the Ergun equation instead of a simplified version of it. Now,

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 we consider the condition we must impose on the superficial velocity so that particles are not carried
out with the fluid at the exit. This would occur if the superficial velocity is equal to the settling velocity
of the particles. Restricting attention to small particles so that stokes law can be used to calculate their
settling velocity, we can write:

U settl =
( p )
−  f  g  Dp2
3.1.9
18

If we now use result for the minimum fluidization velocity for the case of small particles, given above,
we see that the ratio.

U settl 25 1 − 
=  3.1.10
U mf 3 3

For  lying in the range 0.40 – 0.45, this yields a ratio ranging from 50 to 78.

Since, not all particles are of the same size and that is only an average size, we see that fine particles
are likely to be carried out in the situation.

For materials which have no internal porosity, the voidage can be estimated from the density of the
solid  p and the density of the b :

b
 = 1− 3.1.11
p

b
 mf = 1 −
mf
3.1.12
p

mass of particle of the bed

b =
mf
volume of the bed at U mf

3.2Fluidized Beds

A fluidized bed is a packed bed through which fluid flows at such a high velocity that the bed is loosened and the
particle-fluid mixture behaves as though it is a fluid. Thus, when a bed of particles is fluidized, the entire bed can
be transported like a fluid, if desired. Both gas and liquid flows can be used to fluidize a bed of particles. The
most common reason for fluidizing a bed is to obtain vigorous agitation of the solids in contact with the fluid,
leading to excellent contact of the solid and the fluid and the solid and the wall. This means that nearly uniform
temperatures can be maintained even in highly exothermic reaction situations where the particles are used to
catalyze a reaction in the species contained in the fluid. In fact, fluidized beds were used in catalytic cracking in
the petroleum industry in the past. The catalyst is suspended in the fluid by fluidizing a bed of catalytic particles
so that intimate contact can be achieved between the particles and the fluid. Nowadays, you will find fluidized
beds used in catalyst regeneration, solid-gas reactors, combustion of coal, roasting of ores, drying, and gas
adsorption operations.

4. Observation on Solid Bed

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We consider the behavior of a bed of particles when the upward superficial fluid velocity is gradually increased
from zero past the point of fluidization, and back down to zero.

At first, when the flow rate is zero, the pressure drop is zero, and bed has a certain height. As we proceed along
the right arrow (Fig.1) in the direction of increasing superficial velocity, the pressure drop gradually increases
while the bed height remains fixed. This is a region where Ergun equation for a packed bed can be used to relate
the pressure drop to the velocity. When Umf is reached, the bed starts expanding in height while the pressure
drop levels off and no longer increases as the superficial velocity is increased. This is when the upward force
exerted by the fluid on the particles is sufficient to balance the net weight of the bed (W) and the particles begin
to separate from each other and float in the in the fluid.

As the velocity is increased further, the bed continues to expand in height, but the pressure drop stays constant;
infect, with reference to eqn 3.1.6, the increasing of h is compensated by a decreasing of  .

It is possible to reach large superficial velocities without having the particles carried out with the fluid at the exit.
This is because the settling velocities of the particles are typically much larger than the larger than the largest
superficial velocities used. Now if trace our path backward, gradually decreasing the superficial velocity, we find
that the behavior of the bed follows the reverse arrow in the figure above. A bed of particles, left alone for a
sufficient length of time, becomes consolidated, but it is loosened when it is fluidized. After fluidization, it settles
back into a more loosely packed state; this is why the constant bed height on the return loop is larger than the
bed height in the initial state. This effect is called “hysteresis effect”.

If we now repeat the experiment by increasing the superficial velocity from zero, we’ll follow the lower curve in
both directions.

5. THE PACKED AND FLUIDISED BED APPARATUS

5.1 DESCRIPTION

The apparatus contains two vertical cylinders made of Plexiglas as experimental sections with a bed of chosen
granular material. Air flows through one of the cylinders, water through the second. At the lower end of
cylinders is a distribution chamber and a stainless steel sintered plate distributor which supports the bed. This
system ensures uniform fluid flow into the bed without causing excessive pressure drop.

Upon leaving the bed, air and water passes through a stainless steel sintered plate; a centrifugal pump
provides the flow of water.

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The flow rates can be measured with two variable-area flow meters. Two differential pressure manometers
are used to measure the pressure the pressure drop across the fluidized beds. If the pressure in the air
distribution chamber rises 0.5 bar above atmosphere.

Possible causes of an excessive pressure in the distribution chamber are:

• Using a bed of dense, fine or strongly cohesive particles

• The upper stainless steel sintered plate of air is blocked by entrained particles.

In addition to the supplied material, any dry and free flowing granular material of a suitable density and size
may be introduced into the chambers creating many interesting demonstrations.

6. Presentation of Results

Sample presentation of fluidisation with water.

Sample 400  600  m glass microspheres, 2.5g/m1

 b
1.5 g/m1

 0.4

Q u dP H Observation

(1/h) (cm/s) (mmwc) (mm)

12 0,22 14 100

14 0,26 23 100

16 0,29 74 100 First movement of particles

18 0,33 76 100 Fluidization

20 0,37 76 102

22 0,40 77 104

24 0,44 77 105

26 0,48 75 107

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30 0,55 77 111

40 0,73 77 118

50 0,91 77 125

60 1,10 77 135

70 1,28 78 145

80 1,46 77 155

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