1r Semestre

2017-2018

Manual de Laboratorio
OPERACIONES UNITARIAS I INQ0330L
UNIVERSIDAD SAN FRANCISCO DE QUITO
EXPERIMENT 1:

MECANICAL DISINTEGRATION OF SOLIDS AND SCREENING.

Introduction

Even though solids are not as studied as liquids and gases, they have various applications on applied research
and industry. Their handling, size and characterization must be studied to make the best use of them. Solid raw
materials have to be prepared in order to increase superficial area for a variety of purposes (Reactions, storage,
other applications). Mechanical disintegration of solids studies equipment designed to achieve this purpose.
Once the solids have been broken, they have to be classified depending on the size needed. Screening is an
operation designed to separate different solid fractions. In this practice, we will define which types of equipment
exist to disintegrate solids, operate this equipment and classify particles with a screening system.

Objectives

Analyze experimentally the effect of grinding on solids and how it can be improved.

Determine which factors define the screening operation and how these variables can be managed to obtain
better sieving.

Pre-Lab 1

How many types of mechanical disintegrators exist? When are they used?

List 1 example of each mechanical disintegrator and its use on industry

What is a sieve?

What is the relationship between the capacity, efficiency and mesh size in a sieving operation?

What are the common standards to classify mesh size? Which is the difference between each type?

Theoretical Background

Mechanical disintegration of solids

Screening

Granulometry

Experimental work

Materials

Armfield CEN Solids Handling Study Bench

A granular solid
Procedure

Check all electrical connections of the equipment. Make sure there are no wires without connection.

Weight 200 g of the solid selected and 1 kg of ceramic balls (size assigned). Register those values.

Analyze the solid with the sieve system. Register the values obtained for each sieve.

Add the solid along with the ceramic balls into the mill and close the system.

Switch on the ball mill drive at the lowest speed and increase to the highest speed, run for 20 minutes.

Remove the sample form the ball mill and analyze with the sieve shaker.

Weight the material retained in each sieve and register its value.

Data Collection

Before ball milling

Initial sample weight:

Table 1. Experimental data before milling operation

Sieve Aperture Sieve Weight Weight of Material in Sieve, Weight Retained

kg Percentage

Observations
After ball milling

Sample weight:

Table 2. Experimental data after milling operation

Sieve Aperture Sieve Weight Weight of Material in Weight Retained

Sieve, g Percentage

Observations

Data Analysis

Plot a bar graph in order to analyze the difference between the initial and final size of the solid and discuss yours
and your classmates results in order to identify the effect of the size of the balls on the operation.
EXPERIMENT 2: FILTRATION.

Introduction

Filtration is a fluid-solid operation used to separate liquids and gases from solids in order to use any of them on
a subsequent process. Filtration is a complementary operation used a variety of industries around the world.
Although there are different kinds of filters (the selection depends on the final goal of the operation or product
to obtain), this operation has main concepts that have to be studied in order to make the best selection. In this
experiment, we will review different types of filters and observe their similitudes, differences and operation.

Objectives

Define the main parts of a filtration system

Observe and analyze differences and similitudes of 2 different types of filters.

Pre-Lab 2

In terms of filtration, what is retention, permeability and capacity?

Which conditions does a filter need to satisfy in order to have a feasible operation? (3 conditions)

Which characteristics does a filtering medium need for being useful for a given operation?

Which types of filter exist depending on their function?

Theoretical Background

Filtration

Filtering medium

Experimental work

Materials

2 types of sand (provided by the professor)

Ruler

Marker

Chronometer

Vacuum flask

Filtration funnel
Procedure

Slow sand filters efficiency comparison.

Choose a sand layer height and put it on the filtration container. Assure that the sand layer is homogeneous
and doesnt have air cavities.

Start time readings when you start pouring the water sample. Try to make sure that the sample is poured in
the filtration area as homogeneous as possible.

Annotate all observations and how long the system took to filtrate.

Combine both sand layers and repeat the procedure.

Cake filtration: effect of pressure

Place a circle of filtering paper on a filtration funnel and set it on a vacuum flask.

For the first experiment, pour the water sample and observe the filtration process. Annotate all variables that
intervene on this process and filtration time. Also, observe the quality of filtration.

For the second experiment, repeat again the first indications but this time use the vacuum pump.

Data Collection

Table 3. Experimental data for slow sand filters comparison.

Filter Layer Sample Sample Flux Speed

Sand Type Time [s]
Number Height [cm] Inlet [cm3] Outlet [cm3] [cm3/s]
Coarse
1
Fine
Coarse
2
Fine
Coarse
3
Fine

Observations
Table 4. Experimental data for cake filters and the effect of pressure.

Operation Solid initial Sample inlet, Sample outlet, Solid final Time, s
weight, g cm3 cm3 weight, g

Atmospheric

Vacuum

Observations

Data Analysis

Plot a graph showing the relation between sand types, height and flux speed.

Plot a graph showing liquid retention vs pressure applied.

Draw conclusions based on the graphs and analyze the factors involved in the operation. Explain how this factors
could affect the selection of a filtering process on an industry
EXPERIMENT 3: SEDIMENTATION.

Introduction

Sedimentation refers to a separation operation in which solids can be separated from a liquid or other
solids. The basic principle of sedimentation is that an insoluble solid in a liquid will experiment a
gravitational force that will pull the solid to the bottom of the container in which it resides. In addition
to the force of gravity, other techniques include the use of centrifugal force or electromagnetism to
produce sufficient pull to force solids to deposit in the bottom of a container. The gravitational pull
that each solid particle will experiment will depend on its size and density so, over time, bigger and
more dense particles will sediment before smaller or less dense solids. In this experiment we will
observe how turbulence and particle size affect the sedimentation speed in an Imhoff cone.

Objectives

Observe the variables that affect sedimentation operation and how can we improve it.

Analyze the effect of particle removal on waste water treatment.

Pre-Lab 3

What is the difference between clarification and thickening?

What are the 4 part of a sedimentation system?

What is the difference between coagulation and flocculation?

Which unit is used to measure turbidity?

Theoretical Background

Sedimentation

Types of sedimentation

Critical Velocity

Drag coefficient

Experimental work

Materials

Imhoff cones

Chronometer

Stirring Rod
Procedure

Stir the sample on the container for homogenization purposes.

Pour the sample into the Imhoff cone. After you are done, start the stopwatch. Allow the sample to rest for 45
min.

After the 45 min, have passed, gently stir the liquid fraction to help precipitate remaining suspended solids.

Allow the system to rest for 15 more minutes. After this, read the amount of settled solids at the bottom of the
cone.

Data Collection

Table 5. Experimental data for slow sand filters comparison.

Initial Sample weight, kg Height of solids collected, cm Final Sample Weight, kg

Observations
EXPERIMENT 4: SHELL AND TUBE HEAT EXCHANGERS

Introduction

Heat exchangers are the most important industrial application of energy transport around the world. It is present
in almost every industry since it allows to reutilize heat and optimize energy consumption. Heat exchangers
require application of conduction and convection principles combined with momentum transport and
mechanical design. There are many heat exchangers configurations, and each one of them has a specific
application; but the one that is most frequently used, due to its characteristics and high efficiency, is the shell
and tube heat exchanger. In this experiment, we will understand how this heat exchanger operates, its energy
balance and the influence of the direction in which the currents flow.

Objectives

Analyze all the factors that influence heat exchange on an equipment

Understand and observe the operation of a laboratory shell and tube heat exchanger.

Analyze the effect of co current and counter current flows on a heat exchanger.

Theoretical Background

Heat Exchanger

Types of heat exchange equipment (3 types)

Logarithmic Mean Temperature Difference (LMTD)

Overall heat transport coefficient (U)

Fouling Factor

Co current and counter current operation

Pre-Laboratory 4

Create a table to compare heat exchangers characteristics using the types listed on Theoretical Background
section

How do we measure the fouling coefficient and how do we incorporate them to the overall heat transfer
equation?

Search how a MLTD graphic look for counter current and co current profiles. Graph both profiles.

Which do you think will have more impact on the operation? Justify your answer
Experimental work

Materials

Armfield HT30X Heat Exchanger Service Unit

Armfield HT33 Shell and Tube Heat Exchanger.

Procedure

1. Check the equipment for any visible damage.

2. Secure the water connections. After this plug in the equipment.
3. Turn on the workbench. Open the cold water inlet.
4. Turn on the pump and heater. Set the hot water temperature to 40 oC. Make sure there is sufficient
water in the heating tank to proceed with the experiment.
5. Wait until the heater reaches the set temperature.
6. Take note of both the hot and cold water temperatures at the point of entry and exit of the heat
exchanger.
7. Take note of the hot and cold water flux.
8. Change the cold water flow by opening or closing the cold water valve. Repeat steps 6 and 7 when the
equilibrium is reached.
9. Change the entry position of the cold water to change the direction of the water flow. Repeat steps 6-
8.

Observations
Data Collection

Table 6. Experimental data for shell and tube heat exchanger in co-current flow

Experiment Number
Variable
1 2

Hot volume flowrate (qvh), [m3/s]

Cold volume flowrate (qvc), [m3/s]

Hot fluid temperature inlet (T2), [oC]

Hot fluid temperature outlet (T1), [oC]

Cold fluid temperature inlet (T3), [oC]

Cold fluid temperature outlet (T4), [oC]

Table 7. Experimental data for shell and tube heat exchanger in counter current flow

Experiment Number
Variable
3 4

Hot volume flowrate (qvh), [m3/s]

Cold volume flowrate (qvc), [m3/s]

Hot fluid temperature inlet (T2), [oC]

Hot fluid temperature outlet (T1), [oC]

Cold fluid temperature inlet (T4), [oC]

Cold fluid temperature outlet (T3), [oC]

Table 8. Additional data for shell and tube heat exchanger

Specific heat of hot fluid (Cph), [kJ/kg K]

Specific heat of cold fluid (Cpf), [kJ/kg K]

Density of hot fluid (h), [kg/m3]

Density of hot fluid (c), [kg/m3]

Inner tube internal diameter (di), [m]

Heat transmission length (L), [m]

Calculations and Data Analysis

Calculations

Hot mass flow

qmh = qvh h [15]

Cold mass flow

qmc = qvc c [16]

Amount of heat transferred

Q = qmh Cph (T1 T2) = qmc Cpc (T4 T3) [17]

Transversal area

A = di L [17]

Logarithmic Mean Difference of Temperature counter current (LMDT)

(14)(23)
LMDT = (14) [18]
ln((23))

Logarithmic Mean Difference of Temperature co current (LMDT)

(13)(24)
LMDT = (13) [19]
ln((24))

Overall heat transport coefficient

Q
U= [20]
A LMTD

Data Analysis

Table 7. Results of shell and tube heat transfer calculations

Variable Co current 1 Co current 2 Counter current 1 Counter current 2

Q, [W]

LMDT, [OC]

U, [W/m2 OC]

For better results analysis, plot the following graph:

A bar chart that compares concurrent and counter current results (Q, LMDT, U) (6 charts)
EXPERIMENT 5: EVAPORATION

Introduction

Most of the times, unit operations are believed present only on big industries, but they are present in daily
operations like cooking. The differences between both scenarios are two: the purpose and the scale of operation.
Concentration of solutions (goes from the preparation of a soup to the concentration of large amounts of sodium
hydroxide) is a very important liquid-phase separation process present on several chemical and food industries
around the world. This process is represented on the Evaporation operation.

In this exercise, a process variable identification and relationship will be done along with an equipment
recognition and operation.

Objectives

Analyze and identify which variables influence on the process of evaporation.

Observe what components are part of an evaporation equipment

Theoretical background

Evaporation

Types of evaporators

Single effect evaporator

Multiple effect evaporator

Boiling point rising of solutions

Dhrings rule (Charts)

Vaccum System

Pre lab 5

When Dhrings rule is not a factor on the evaporation process? Explain with an example

Considering the concepts above, why the term distilled water is a wrong expression? How would be the
correct expression for distilled water?

Draw a scheme of a rice pan, annotate all the inputs and outputs and solve a mass balance for 200 g of rice
(consider that the rice/water ratio is 1:2).

Materials

Rising Film Evaporator UOP20-X-PHW

Procedure

Equipment Start-up

CHECK ALL WATER AND ELECTRIC CONECTIONS BEFORE PROCEDING.

Turn on the laboratory pump and open the evaporators water valve inlet.

Go to the Evaporators console and turn on breakers 31 (Main Power) and 32 (Control Board).

Turn on breakers 35 (1st effect) and 36 (1st effect pump).

Turn on switch 51 to turn on the hot water circulator system. Check that there are no leaks. Set the hot water
temperature to 110 oC.

Open the copper sulfate tank feed valve, and turn on Pump 46. Set the pump to speed marker 4.

Open V16 (refrigerating water inlet) and set the flux to 3 L/min under control 48.

Let the system stabilize for 15 min. Annotate values.

Turn on breaker 33 (Vacuum pump). Annotate values.

Reading procedure.

Take temperatures T4(Feed prior the evaporator), T6(Vapor generated), T2 (Concentrated Product), T11
(Heating Steam)

Take conductivity readings (C1 and C2).

Annotate the vacuum pressure.

Turn off breaker 33. Measure how much concentrated product and vapor condensate the evaporator
produced.

Observations

Data Collection
Table 8. Experimental data

Reading (before turning Reading (after turning

Variable
on the vacuum) on the vacuum)

Vacuum Pressure, mbar

Temperature 2 (T2) [OC]

Temperature 4 (T4) [OC]

Temperature 6 (T6) [OC]

Temperature 11 (T11) [OC]

Conductivity 1 (C1) [mS]

Conductivity 2 (C2) [Ms]

Feed, (F) [mL/min]

Concentrated Product, (L)[mL/min]

Condensate Steam (V), [mL/min]

If additional data is required, please list it as a different table with the title Additional data.

Calculations and Data Analysis

Calculations

Concentration
1
0.44113 0.67231
(%) =[ ]
1.24064

Heating Steam Requirement

+
=