UOP4 MKII Manual - SL Extraction

SOLID/LIQUID EXTRACTION UNIT
Instruction Manual
UOP4 MKII
ISSUE 16
November 2010
Table of Contents
Copyright and Trademarks ...................................................................................... 1
General Overview ....................................................................................................... 2
Equipment Diagrams................................................................................................... 3
Important Safety Information..................................................................................... 10
Introduction............................................................................................................ 10
General Safety Rules ............................................................................................ 10
The COSHH Regulations ...................................................................................... 14
Water Borne Hazards ............................................................................................ 15
Electrical Safety..................................................................................................... 15
Description ................................................................................................................ 17
Overview................................................................................................................ 17
Process Components ............................................................................................ 18
Console (Front Panel Components) ...................................................................... 21
Console (Rear Panel Components)....................................................................... 23
Console (Components on Underside) ................................................................... 24
Installation ................................................................................................................. 25
Advisory................................................................................................................. 25
Installation Requirements ...................................................................................... 25
Installation Process ............................................................................................... 26
Connection to Services.......................................................................................... 26
Using the Optional Educational Software and Data Logging Accessory ............... 28
Commissioning ...................................................................................................... 28
Electrical Wiring Diagram ...................................................................................... 30
Operation .................................................................................................................. 31
Operating the Software.......................................................................................... 31
Operating the Equipment....................................................................................... 41
Cleaning after use ................................................................................................. 49
Equipment Specifications.......................................................................................... 52
Overall Dimensions ............................................................................................... 52
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Table of Contents
I/O Port Pin Connections ....................................................................................... 52
Environmental Conditions...................................................................................... 53
Routine Maintenance ................................................................................................ 55
Responsibility ........................................................................................................ 55
General.................................................................................................................. 55
Configuration of the PID Temperature Controllers ................................................ 56
Recalibration of the Thermocouple Conditioning Circuits...................................... 58
Recalibration of the Conductivity Conditioning Circuits ......................................... 59
RCD Test............................................................................................................... 60
Laboratory Teaching Exercises................................................................................. 61
Index to Exercises ................................................................................................. 61
Introduction and Background................................................................................. 61
Nomenclature ........................................................................................................ 62
Graphs of Concentration ....................................................................................... 64
Exercise A: Batch Extraction - Open Loop................................................................ 65
Exercise B: Batch Extraction - Closed Loop ............................................................. 69
Exercise C: Single Stage Continuous Extract ........................................................... 73
Exercise D: Two Stage Continuous Extraction ......................................................... 79
Exercise E: Three Stage Continuous Extraction ....................................................... 86
Project Work.............................................................................................................. 93
Contact Details for Further Information ..................................................................... 95
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Disclaimer
This document and all the information contained within it is proprietary to Armfield
Limited. This document must not be used for any purpose other than that for which it
is supplied and its contents must not be reproduced, modified, adapted, published,
translated or disclosed to any third party, in whole or in part, without the prior written
permission of Armfield Limited.
Should you have any queries or comments, please contact the Armfield Customer
Support helpdesk (Monday to Friday: 0800 1800 GMT). Contact details are as
follows:
United Kingdom International
(0) 1425 478781 +44 (0) 1425 478781

(calls charged at local rate) (international rates apply)
Email: support@armfield.co.uk
Fax: +44 (0) 1425 470916
Copyright and Trademarks

Copyright 2009 Armfield Limited. All rights reserved.
Any technical documentation made available by Armfield Limited is the copyright

work of Armfield Limited and wholly owned by Armfield Limited.
Brands and product names mentioned in this manual may be trademarks or

registered trademarks of their respective companies and are hereby acknowledged.
1
General Overview
The extraction (leaching) of a substance from a solid material with the aid of a liquid
is a common process in chemical engineering which can be applied to appropriate
biological, inorganic and organic substances. A familiar activity which illustrates this
process is the making of tea or coffee, where hot water is used to perform the
extraction from tea leaves or coffee beans. Other examples are the extraction of
sugar from sugar beet using hot water and the extraction of oils from seeds using
organic solvents such as hexane, acetone or ether.
For the solid/liquid extraction process to be appropriate, the substance to be

extracted (tea) must be soluble while the solid phase (tea leaves) must be insoluble
in the chosen solvent (hot water). The appropriate solvent is introduced to the solid
material and the two remain in contact while the soluble component dissolves into the
solvent. The solvent containing the dissolved substance (the miscella) is then drained
from the insoluble solid. This is the basis of all solid/liquid extraction processes.
Further processing may be required to recover the extracted substance from the
solvent.
Before performing solid/liquid extraction the solid material must be prepared by

crushing, grinding or cutting, as appropriate, to allow adequate contact between the
solvent and the soluble component. The amount of preparation will depend on the
amount and distribution of the soluble component within the solid and the nature of
the solid (how easily diffusion can occur).
Numerous different types of solid/liquid extractors may be employed to perform the

basic task of introducing the solvent to the material to be extracted. The extraction
process may involve batch operation (fixed-bed) with the addition of open loop or
closed loop circulation of the solvent. Alternatively extraction may be a continuous
operation (moving-bed) with single or multi-stage processing involving co-current flow
or counter current flow of the solvent and the soluble material to be extracted. In
large scale industrial solid/liquid extraction systems economic factors frequently lead
to the use of the more sophisticated multi-stage counter current flow systems due to
their high extraction efficiency.
The Armfield UOP4 MkII is designed to demonstrate a simplified version of the

moving-bed leaching process used by many industrial solid/liquid extraction systems.
The process used is a continuous multi-stage process, which gives counter current
flow of the solvent and the solid phase. A batch extraction vessel is also incorporated
to allow demonstration of fixed-bed leaching with either open or closed loop
circulation of the solvent. The recommended process for the UOP4 MkII is the
extraction of Potassium Bicarbonate from a solid carrier of porous polymer pellets
using water as the solvent.
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Equipment Diagrams
Figure 1: Front View of UOP4 MKII Solid/Liquid Extraction Unit
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Armfield Instruction Manual
Figure 2: Side View of UOP4 MKII Solid/Liquid Extraction Unit
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Equipment Diagrams
Figure 3: UOP4 MKII Schematic Diagram Showing 3 Stage Process
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Figure 4: UOP4 MkII Console - Front View
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Equipment Diagrams
Figure 5: UOP4 MkII Console - Rear View
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Figure 6: PCB Connections
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Equipment Diagrams
Figure 7: Location of Temperature Calibration Potentiometers on PCB
Figure 8: Location of Conductivity Calibration Potentiometers on Conductivity Measurement PCB
9
Important Safety Information
Introduction
All practical work areas and laboratories should be covered by local safety
regulations which must be followed at all times.
It is the responsibility of the owner to ensure that all users are made aware of
relevant local regulations, and that the apparatus is operated in accordance with
those regulations. If requested then Armfield can supply a typical set of standard
laboratory safety rules, but these are guidelines only and should be modified as
required. Supervision of users should be provided whenever appropriate.
Your UOP4 MKII Solid/Liquid Extraction Unit has been designed to be safe in use
when installed, operated and maintained in accordance with the instructions in this
manual. As with any piece of sophisticated equipment, dangers exist if the equipment
is misused, mishandled or badly maintained.
Before proceeding to install, commission or operate the equipment described in this

instruction manual we wish to alert you to potential hazards so that they may be
avoided.
Although designed for safe operation, any laboratory equipment may involve
processes or procedures which are potentially hazardous. The major potential
hazards associated with this particular equipment are listed below.
INJURY THROUGH MISUSE
INJURY FROM ELECTRIC SHOCK
INJURY FROM ROTATING COMPONENTS
IRRITATION FROM DUST WHEN HANDLING DRY MATERIALS
BURNS FROM COMPONENTS AT HIGH TEMPERATURES
INJURY FROM INCORRECT HANDLING
DAMAGE TO CLOTHING
Accidents can be avoided provided that equipment is regularly maintained and

staff and students are made aware of potential hazards. A list of general safety
rules is included in this manual, to assist staff and students in this regard. The list is
not intended to be fully comprehensive but for guidance only.
Please refer to the notes overleaf regarding the Control of Substances Hazardous to
Health Regulations.
General Safety Rules

1. Follow Relevant Instructions
a. Before attempting to install, commission or operate equipment, all relevant

suppliers/manufacturers instructions and local regulations should be
understood and implemented.
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b. It is irresponsible and dangerous to misuse equipment or ignore instructions,

regulations or warnings.
c. Do not exceed specified maximum operating conditions (eg. temperature,

pressure, speed etc).
2. Installation
a. Use lifting tackle where possible to install heavy equipment. Where manual
lifting is necessary beware of strained backs and crushed toes. Get help from
an assistant if necessary. Wear safety shoes where appropriate.
b. Extreme care should be exercised to avoid damage to the equipment during

handling and unpacking. When using slings to lift equipment, ensure that the
slings are attached to structural framework and do not foul adjacent pipework,
glassware etc. When using fork lift trucks, position the forks beneath
structural framework ensuring that the forks do not foul adjacent pipework,
glassware etc. Damage may go unseen during commissioning creating a
potential hazard to subsequent operators.
c. Where special foundations are required follow the instructions provided and
do not improvise. Locate heavy equipment at low level.
d. Equipment involving inflammable or corrosive liquids should be sited in a

containment area or bund with a capacity 50% greater than the maximum
equipment contents.
e. Ensure that all services are compatible with the equipment and that
independent isolators are always provided and labelled. Use reliable
connections in all instances, do not improvise.
f. Ensure that all equipment is reliably earthed and connected to an electrical

supply at the correct voltage. The electrical supply must incorporate a
Residual Current Device (RCD) (alternatively called an Earth Leakage Circuit
Breaker - ELCB) to protect the operator from severe electric shock in the
event of misuse or accident.
g. Potential hazards should always be the first consideration when deciding on a

suitable location for equipment. Leave sufficient space between equipment
and between walls and equipment.
3. Commissioning
a. Ensure that equipment is commissioned and checked by a competent

member of staff before permitting students to operate it.
4. Operation
a. Ensure that students are fully aware of the potential hazards when operating
equipment.
b. Students should be supervised by a competent member of staff at all times

when in the laboratory. No one should operate equipment alone. Do not leave
equipment running unattended.
c. Do not allow students to derive their own experimental procedures unless

they are competent to do so.
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d. Serious injury can result from touching apparently stationary equipment when
using a stroboscope to `freeze rotary motion.
5. Maintenance
a. Badly maintained equipment is a potential hazard. Ensure that a competent

member of staff is responsible for organising maintenance and repairs on a
planned basis.
b. Do not permit faulty equipment to be operated. Ensure that repairs are carried
out competently and checked before students are permitted to operate the
equipment.
6. Using Electricity
a. At least once each month, check that ELCBs (RCCBs) are operating correctly
by pressing the TEST button. The circuit breaker must trip when the button is
pressed (failure to trip means that the operator is not protected and a repair
must be effected by a competent electrician before the equipment or electrical
supply is used).
b. Electricity is the commonest cause of accidents in the laboratory. Ensure that

all members of staff and students respect it.
c. Ensure that the electrical supply has been disconnected from the equipment
before attempting repairs or adjustments.
d. Water and electricity are not compatible and can cause serious injury if they
come into contact. Never operate portable electric appliances adjacent to
equipment involving water unless some form of constraint or barrier is
incorporated to prevent accidental contact.
e. Always disconnect equipment from the electrical supply when not in use.
7. Avoiding fires or explosion
a. Ensure that the laboratory is provided with adequate fire extinguishers

appropriate to the potential hazards.
b. Where inflammable liquids are used, smoking must be forbidden. Notices

should be displayed to enforce this.
c. Beware since fine powders or dust can spontaneously ignite under certain
conditions. Empty vessels having contained inflammable liquids can contain
vapour and explode if ignited.
d. Bulk quantities of inflammable liquids should be stored outside the laboratory

in accordance with local regulations.
e. Storage tanks on equipment should not be overfilled. All spillages should be

immediately cleaned up, carefully disposing of any contaminated cloths etc.
Beware of slippery floors.
f. When liquids giving off inflammable vapours are handled in the laboratory, the
area should be ventilated by an ex-proof extraction system. Vents on the
equipment should be connected to the extraction system.
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g. Students should not be allowed to prepare mixtures for analysis or other

purpose without competent supervision.
8. Handling poisons, corrosive or toxic materials
a. Certain liquids essential to the operation of equipment, for example mercury,

are poisonous or can give off poisonous vapours. Wear appropriate protective
clothing when handling such substances. Clean up any spillage immediately
and ventilate areas thoroughly using extraction equipment. Beware of slippery
floors.
b. Do not allow food to be brought into or consumed in the laboratory. Never use
chemical beakers as drinking vessels.
c. Where poisonous vapours are involved, smoking must be forbidden. Notices

should be displayed to enforce this.
d. Poisons and very toxic materials must be kept in a locked cupboard or store
and checked regularly. Use of such substances should be supervised.
e. When diluting concentrated acids and alkalis, the acid or alkali should be
added slowly to water while stirring. The reverse should never be attempted.
9. Avoiding cuts and burns
a. Take care when handling sharp edged components. Do not exert undue force
on glass or fragile items.
b. Hot surfaces cannot, in most cases, be totally shielded and can produce
severe burns even when not `visibly hot. Use common sense and think which
parts of the equipment are likely to be hot.
10. Eye protection
a. Goggles must be worn whenever there is a risk to the eyes. Risk may arise
from powders, liquid splashes, vapours or splinters. Beware of debris from
fast moving air streams. Alkaline solutions are particularly dangerous to the
eyes.
b. Never look directly at a strong source of light such as a laser or Xenon arc
lamp. Ensure that equipment using such a source is positioned so that
passers-by cannot accidentally view the source or reflected ray.
c. Facilities for eye irrigation should always be available.
11. Ear protection
a. Ear protectors must be worn when operating noisy equipment.
12. Clothing
a. Suitable clothing should be worn in the laboratory. Loose garments can cause
serious injury if caught in rotating machinery. Ties, rings on fingers etc. should
be removed in these situations.
b. Additional protective clothing should be available for all members of staff and
students as appropriate.
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13. Guards and safety devices
a. Guards and safety devices are installed on equipment to protect the operator.
The equipment must not be operated with such devices removed.
b. Safety valves, cut-outs or other safety devices will have been set to protect
the equipment. Interference with these devices may create a potential hazard.
c. It is not possible to guard the operator against all contingencies. Use common
sense at all times when in the laboratory.
d. Before starting a rotating machine, make sure staff are aware how to stop it in
an emergency.
e. Ensure that speed control devices are always set at zero before starting
equipment.
14. First aid
a. If an accident does occur in the laboratory it is essential that first aid

equipment is available and that the supervisor knows how to use it.
b. A notice giving details of a proficient first-aider should be prominently

displayed.
c. A `short list of the antidotes for the chemicals used in a particular laboratory
should be prominently displayed.
The COSHH Regulations

The Control of Substances Hazardous to Health Regulations (1988)
The COSHH regulations impose a duty on employers to protect employees and
others from substances used at work which may be hazardous to health. The
regulations require you to make an assessment of all operations which are liable to
expose any person to hazardous solids, liquids, dusts, vapours, gases or micro-
organisms. You are also required to introduce suitable procedures for handling these
substances and keep appropriate records.
Since the equipment supplied by Armfield Limited may involve the use of substances
which can be hazardous (for example, cleaning fluids used for maintenance or
chemicals used for particular demonstrations) it is essential that the laboratory
supervisor or some other person in authority is responsible for implementing the
COSHH regulations.
Part of the above regulations is to ensure that the relevant Health and Safety Data
Sheets are available for all hazardous substances used in the laboratory. Any person
using a hazardous substance must be informed of the following:
Physical data about the substance
Any hazard from fire or explosion
Any hazard to health
Appropriate First Aid treatment
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Any hazard from reaction with other substances
How to clean/dispose of spillage
Appropriate protective measures
Appropriate storage and handling
Although these regulations may not be applicable in your country, it is strongly

recommended that a similar approach be adopted for the protection of the students
operating the equipment. Local regulations must also be considered.
Water Borne Hazards

The equipment described in this instruction manual involves the use of water, which
under certain conditions can create a health hazard due to infection by harmful
micro-organisms.
For example, the microscopic bacterium called Legionella pneumophila will feed on
any scale, rust, algae or sludge in water and will breed rapidly if the temperature of
water is between 20 and 45C. Any water containing this bacterium which is sprayed
or splashed creating air-borne droplets can produce a form of pneumonia called
Legionnaires Disease which is potentially fatal.
Legionella is not the only harmful micro-organism which can infect water, but it
serves as a useful example of the need for cleanliness.
Under the COSHH regulations, the following precautions must be observed:
Any water contained within the product must not be allowed to stagnate, ie.
the water must be changed regularly.
Any rust, sludge, scale or algae on which micro-organisms can feed must be
removed regularly, i.e. the equipment must be cleaned regularly.
Where practicable the water should be maintained at a temperature below

20C. If this is not practicable then the water should be disinfected if it is safe
and appropriate to do so. Note that other hazards may exist in the handling of
biocides used to disinfect the water.
A scheme should be prepared for preventing or controlling the risk

incorporating all of the actions listed above.
Further details on preventing infection are contained in the publication The Control
of Legionellosis including Legionnaires Disease - Health and Safety Series booklet
HS (G) 70.
Electrical Safety
The equipment described in this Instruction Manual operates from a mains voltage
electrical supply. It must be connected to a supply of the same frequency and voltage
as marked on the equipment or the mains lead. If in doubt, consult a qualified
electrician or contact Armfield.
The equipment must not be operated with any of the panels removed.
To give increased operator protection, the unit incorporates a Residual Current

Device (RCD), alternatively called an Earth Leakage Circuit Breaker, as an integral
15
part of this equipment. If through misuse or accident the equipment becomes

electrically dangerous, the RCD will switch off the electrical supply and reduce the
severity of any electric shock received by an operator to a level which, under normal
circumstances, will not cause injury to that person.
At least once each month, check that the RCD is operating correctly by pressing the
TEST button. The circuit breaker MUST trip when the button is pressed. Failure to
trip means that the operator is not protected and the equipment must be checked and
repaired by a competent electrician before it is used.
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Description
Where necessary, refer to the drawings in the Equipment Diagrams section.
Overview
The heart of the solid/liquid extraction system is a continuously rotating extraction cell
divided into compartments. The raw material is fed into these compartments from the
input hopper using a screw feeder mechanism. The material is then passed under
three solvent sprinkler bars, one for each stage of the process, and the dissolved
product captured in the three collection troughs. Pumps are provided at each stage to
pump the product from the collection trough of one stage to the sprinkler of the next
stage. At the end of its cycle, the spent carrier material is dropped into a collection
tank aided by water spraying from a nozzle.
The system is configured as a three stage, counter current flow process, but may
also be configured as a one or two stage process for teaching purposes.
Full temperature control is provided at each stage of the process using the three
integrated PID controllers and related heating elements. Direct control is also
provided over the product feed rate, the cell rotation speed and the inter-stage pump
speeds.
In addition to the rotary cell, an independent vessel is provided which allows batch
extractions to be performed.
The unit is fully instrumented with each stage of the process equipped with sensors,
giving a temperature and a milli-volt conductivity probe output. When using the
standard water / Potassium Bicarbonate system, the sensor readings can be related
to the percentage weight of Potassium Bicarbonate in the solution using experimental
data.
All temperatures and voltage outputs from the conductivity probes, together with the
feed, extractor cell and individual pump rates can also be displayed on a computer
using the optional data logging package. Using this package it is also possible to
display and log the product concentration (when using the recommended materials).
The equipment is designed to teach all relevant aspects of solid/liquid extraction in a

simple and safe manner. It does not require the use of toxic, volatile or flammable
solvents, as it is designed to use water or water based solvents. This allows the
process to be made fully visible to students, allowing them to observe and
understand the details of the operation at every stage. There is no need for
expensive solvent recovery equipment such as a distillation column.
The recommended process for the UOP4 MkII is the extraction of Potassium
Bicarbonate (Potassium Hydrogencarbonate, chemical symbol KHCO 3 ) from a solid
carrier of porous polymer pellets (microporous Polyamide 6-pellets) using water as
the solvent. This combination of a non-toxic salt with water and an inert solid gives a
safe demonstration of the process and a simple measurement of the conductivity and
temperature at each stage in the process allows the changing concentration
(percentage weight) of the salt in the water to be determined. A quantity of porous
polymer pellets is supplied with the equipment. These plastic pellets are used as the
carrier for convenience and avoid dust, grit etc that could cause operational
problems. The plastic pellets can be reclaimed and reused.
The process can be monitored in real time using the displays on the console, which
show the conductivity probe output and temperature of the solvent at each of the
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stages. Using experimental data these values can be related to the percentage
weight of Potassium Bicarbonate in the solution. Alternatively the optional UOP4MkII-
303IFD Data logging and Educational Software Accessory may be used to
automatically log the measurements, perform the necessary calculations and present
the results in a real time graph.
If the UOP4 MkII is used with any other extractable material the relationships
between conductivity probe output, percentage weight and temperature will need to
be investigated by the user (refer to project work in the UOP4 MkII Teaching Manual
for further information). It may be possible to use other solid materials, but these
would need to be evaluated in conjunction with the rotating cell and the feed
mechanism. Materials must not be used that generate dust as this could settle in the
pipework causing blockages.
Figure 3 the schematic diagram shows the various stages of the process with the
solids and solvent (water) flowing counter-currently. In reality the solids rotate in a
circular path but for simplicity, the compartments of the rotor and the solvent
collecting troughs are shown in a straight line in the diagram.
Process Components
All the numerical references in this section relate to the equipment diagrams. The
letters a, b and c associated with each numerical reference refer to the three stages
of the process a = First stage, b= Second stage and c= Third/Final stage.
1. Framework
The equipment is fitted into a welded steel framework constructed from circular
section members and supported on adjustable feet.
2. Console
The metal console housing contains the majority of the electrical components
and electronic circuit boards. The rear panel incorporates the various
protection devices. The front panel incorporates the three PID controllers, the
measurement display and various control knobs and switches (see Description
of Console for further details).
3. Pumps (3a, 3b, 3c)
The three solvent stages are supplied by three peristaltic pumps, which have a
maximum capacity of approximately 13 l/hr. The rotary controls for varying the
speed of the pumps are on the front panel of the console.
4. Solvent Heaters (4a, 4b, 4c)
Each of the three solvent stages has a separate solvent heater which is
controlled using a PID controller on the console. The heater consists of a
cartridge element which is enclosed in a concentric tubular jacket through
which the solvent is circulated. The cartridge element is protected from over
temperature by a thermocouple which senses the internal temperature of the
element and a circuit which cuts the power if the temperature exceeds a pre-
set value, when this happens the over-temperature indicator on the console
flashes. The over-temperature protection automatically resets when the
cartridge element cools down.
5. Conductivity Probes C1, C2, C3, C4 and Temperature Sensors T1, T2, T3, T4
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Description
At each of the three stages where the solvent is being fed into the rotor the
concentration of the extracted Potassium Bicarbonate in the solvent is
monitored using a temperature sensor and a flow-through conductivity probe.
The temperature sensor is fitted in a quick release fitting which is mounted on
the top of the solvent heater. The glass conductivity probe on each of the
stages is positioned down stream of the temperature sensor and is connected
to the quick release fitting via a section of flexible tubing.
An additional temperature sensor T4 and conductivity probe C4 are

incorporated at the point where the final miscella exits the process.
Temperatures T1, T2 & T3 are indicated on the appropriate PID controller.
Temperature T4 and conductivities C1, C2, C3 & C4 are displayed on the

panel meter via a selector switch.
6. Solvent Sprinkler Bars (6a, 6b, 6c)
The solvent is delivered on to the top of the moving bed of solids through three
solvent sprinkler bars. The three sprinkler bars are positioned above the three
solvent collecting troughs and represent the three stages of the process.
The sprinkler bars are removable from the extraction cell to allow them to be
cleaned. A hexagon adjuster (Allen screw) on the top of the hub above each
bar clamps the bar in place.
7. Extraction Cell
The function of the extraction cell is to transport the solids, which are being
processed through the three solvent stages and to discharge the spent solids
into the extracted solids tank. The base of the extraction cell supports the rotor
that is driven by a geared motor located in the central hub. A clutch fitted
between the motor and the rotor protects the motor/gearbox if the rotor is
moved by hand or solid material jams between the rotor and the base. The
rotor is divided into compartments by vertical baffles that sweep the solid
material along as it rotates. The base incorporates a perforated stainless steel
mesh, directly below the rotor, to allow the solvent that has percolated through
the solid material being processed to drain into the solvent collection troughs
below. The speed of the rotor can be varied from zero up to approximately four
revolutions per hour using the rotary speed control on the console. The
compartments of the rotor should be filled to approximately between one-third
and half height by the feeder during normal operation.
The base of the extraction cell is mounted at three points to allow the whole
unit to be removed from the framework, if necessary. However, normal
cleaning can be carried out with the base retained in the frame. Two clamp
knobs on topof the central hub can be released, allowing the hub / rotor
assembly to be removed from the base. It will be necessary to remove the
Feeder and any flexible tubing / connecting leads before removing the hub /
rotor.
An aperture in the base of the extraction cell allows spent solid carrier to be
discharged into the extracted solids tank underneath. A spray nozzle mounted
above the rotor assists the discharge by washing the solids from the rotor. The
spray nozzle is adjustable in height and a pressure regulating valve mounted at
the rear of the extraction cell allows the spray pattern to be varied. These
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should be adjusted in combination to wash the spent solids into the extracted
solids tank without spraying excess water outside of the rotor.
8. Solvent Collection Troughs (8a, 8b, 8c)
As the solvent drains down through the stainless steel mesh it is collected in
three troughs which correspond to the three solvent stages. Once the fresh
solvent from the sprinkler bar in stage 1 has found its way into the first trough it
is pumped to the sprinkler bar of the second stage. Similarly, miscella draining
into the trough of the second stage is pumped to the sprinkler bar of the third
stage. Final miscella draining into the trough of the third stage is allowed to
flow into the final miscella tank by gravity.
Each of the three troughs incorporates a vent through the sidewall to ensure
consistent flow through the stainless steel mesh. In operation, the liquid level
inside each trough must not be allowed to cover the elbow on the end of the
vent tube inside the trough.
9. Filters (9a, 9b, 9c)
Filters are incorporated at the outlet from each of the solvent collection troughs
to prevent any solid particles from reaching the pumps, heaters or
instrumentation. It may be necessary to clean these filters after use to remove
any contamination. The correct procedure is described in the Routine
Maintenance section of this Product Manual.
10. Material Hopper and Feeder.
The solid material, which is to be extracted from in the process, is metered into
the compartments of the rotor using a spiral type conveyor. The depth of the
solids in the rotor can be controlled by adjusting the relative speeds of the
feeder and/or the rotor using the rotary controls on the front of the console.
It will be necessary to top up the hopper at regular intervals with fresh solid
material which has been suitably prepared. Preparation of the material is
described in the Operation section.
11. Fresh Solvent Tank
The fresh solvent (usually de-mineralised water) is stored in this tank. During
long runs it will be necessary to top-up this tank with de-mineralised water to
prevent the system from running dry. It is suggested that de-mineralised water
be used since hardness in tap water may form precipitates and salts in the tap
water may affect the conductivity measurements.
12. Extracted Solids Tank
The spent solids, having been leached of the soluble component, are
continuously discharged from the extraction cell as each compartment passes
an aperture in the base below the rotor. The solids, still wet with solvent, are
washed into the extracted solids tank using a spray of water. A connector with
integral filter, in the base of the tank, allows the water to flow to drain
continuously while retaining the solids inside the tank.
13. Final Miscella Tank
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Description
The liquid exiting the extraction process is called the final miscella. This is
solvent with the extracted material dissolved in it. The final miscella is collected
in the final miscella tank. It will be necessary to empty this tank periodically.
14. Batch Vessel
A clear acrylic batch vessel mounted on the support frame allows solid/liquid
extraction to be carried out on a fixed batch of material. The batch of material
is placed in a cloth bag that is supplied with the equipment. The bag is located
inside the batch vessel. Quick release connections at the top and bottom of the
vessel allow appropriate components in the system to be incorporated to allow
the demonstration of fixed-bed leaching with either open or closed loop
circulation of the solvent. In normal operation the solvent enters at the bottom
and flows upward through the vessel. A bypass valve at the bottom allows
solvent to be recirculated without passing through the vessel (used to allow the
temperature of the solvent to stabilise prior to extraction taking place).
The batch vessel also allows samples of different materials to be tested where
the material cannot be passed through the feeder and rotor arrangement.
Refer to the Operation section for further information.
Console (Front Panel Components)

All the references in this section relate to Figure 4 & 5 in the equipment diagrams.
15. Mains On/Off Switch
This switch is the on/off switch for all functions in the console and should
always be in the off position when the equipment is not in use. Before
switching the console on it is important to make sure that the three heater
switches are in the off position.
16. Feeder Speed Control and On/Off Switch.
This rotary potentiometer adjusts the speed of the Spiral feeder and is used to
vary the rate at which the material to be extracted is fed into the extraction cell.
An On/Off switch is provided to start and stop the feeder without the need to
change the speed setting.
17. Rotor Speed Control and On/Off Switch.
This rotary potentiometer adjusts the speed of the rotor. Varying the rotor
speed will have the effect of changing the time that each compartment spends
under each sprinkler bar and the time under the material feeder which fills the
compartments. An On/Off switch is provided to start and stop the rotor drive
without the need to change the speed setting.
18. Temperature/Conductivity Display and Selector Switch
This multifunction display can show either the reading of the temperature
sensor at stage four (T4 final miscella out) or any one of the four conductivity
probe readings (C1, C2, C3 and C4 in mV) as selected on the rotary switch.
Note: Temperatures T1, T2 & T3 are indicted continuously on the appropriate

PID controller.
19. Peristaltic Pump Speed Controls (19a, 19b, 19c)
21
These three rotary potentiometers adjust the rotational speed and therefore the
flow rate of the three peristaltic pumps. In operation, the three speeds will need
to be adjusted so that there is a constant flow of liquid from one stage to the
next without any of the stages running dry.
20. Heater On/Off Switches (20a, 20b, 20c)
These switches allow the individual solvent stage heaters to be switched off
when not required. Although the heaters are protected from overheating, they
should be switched off before the console is switched on and whenever there
is no fluid flow through the heaters.
21. Heater OVER TEMP indicators (21a, 21b, 21c)
The indicator operates when the temperature of the heater has exceeded the
upper level of the normal temperature range, this can happen when the flow of
liquid in the heater is intermittent or when the heater is switched on and the
solvent pump is switched off. When the indicator flashes the power to the
heater will be cut until the system detects that the temperature has declined
whereupon the system will automatically reset and the indicator will go out. To
prevent the heater from going into over temp mode it is important to make sure
that all of the heaters are switched off before turning on the console. The
heaters should only be turned on when there is a constant flow of liquid
through the heaters (for more details see Safe Operation).
22. PID Temperature Controllers (22a, 22b, 22c)
PID Controller
The PID controller has three keys that are used for adjusting the desired
temperature set point and for altering the configuration of the controller. The
configuration of each controller is set before delivery and should not require
adjustment. If for any reason, the user needs to restore the configuration or
wishes to alter it, the procedure and default settings are listed in the Routine
Maintenance section of this manual.
During normal operation the controller will display the process temperature (the
temperature of the solvent leaving the appropriate heater, measured by the
thermocouple located at the top of the heater). When power is supplied to the
heater, the control output indicator, located above and to the left of the digital
display on the PID controller, is illuminated.
22
Description
To check the current set point:
Press either the increase key or decrease key briefly.
The display will automatically return to the process temperature.
To change the current set point:
Press either the increase key or decrease key briefly. The current set
point will be displayed.
Press and hold the increase or decrease key as required until the
required value of the digit is displayed.
Note:
For optimum control of the temperatures within the process, without excessive
overshoot, the setpoint of each controller should be set to ambient temperature
when the equipment is first switched on with water flowing. Adjustment to the
required setpoint during operation will then give smooth control without
excessive overshoot.
Similarly it is suggested that the temperature of stage 1 should be allowed to

stabilise before increasing the setpoint of stage 2 and the temperature of stage
2 should be allowed to stabilise before increasing the setpoint of stage 3.
Console (Rear Panel Components)

All the references in this section relate to Figure 4 & 5 in the equipment diagrams.
23. Residual Current Device
If through misuse or accident the equipment becomes electrically dangerous

the RCD will switch off the electrical supply and reduce the severity of any
electric shock received by an operator to a level which, under normal
circumstances, will not cause injury to that person. The RCD is alternatively
called a Residual Current Circuit Breaker or RCCB. Refer to the Important
Safety Information.
24. Circuit Breakers (a, b, c & d)
There are four circuit breakers mounted on the rear of the console which
protect the electrical circuits within the console from excess current flow, as
follows:
a. HEAT 6 Amp breaker to protect the mains supply to the

heaters.
b. DC 4 Amp breaker to protect the DC power supply.
c. O/P 1 Amp breaker to protect the mains output socket
d. CONTROL 1 Amp thermal breaker to protect the mains supply to

the PID controllers (push to reset).
23
25. Mains Output Socket
The socket marked OUTPUT can be used to provide mains power at line
voltage to any additional instrumentation used with the equipment. This socket
is used to power the optional Armfield interface device IFD3 which is supplied
with the Educational Software and Data Logging Accessory UOP4MkII-303IFD.
The output current is limited to 1 Amp by a circuit breaker (24c).
26. Mains Input Socket
This socket is used to connect the console to the mains electrical supply using
the flexible mains lead supplied with the equipment. Ensure that the label fixed
above the socket matches the voltage and frequency of the mains electrical
supply before connecting the lead to the supply.
Console (Components on Underside)

27. I/O Port Socket
The data from the temperature sensors, conductivity probes and speed
settings for the pumps, feeder and rotor can be logged on a computer with the
aid of an Armfield interface device. The UOP4 MkII is linked to the interface
device using a ribbon cable that is plugged into the I/O Port socket on the
underside of the console. The ribbon cable / interface device is supplied as
part of the UOP4MkII-303IFD Educational Software and Data Logging
Accessory.
28. Feeder connector
A jack socket on the underside of the console allows the feeder to be

disconnected from the console when it is necessary to remove it for cleaning.
29. Extraction cell connector
A jack socket on the underside of the console allows the extraction cell to be
disconnected from the console when it is necessary to remove the hub of the
extraction cell for cleaning.
24
Installation
Advisory
Before operating the equipment, it must be unpacked, assembled and installed as
described in the steps that follow. Safe use of the equipment depends on following
the correct installation procedure.
Installation Requirements
Electromagnetic Compatibility
This apparatus is classified as Education and Training Equipment under the
Electromagnetic Compatibility (Amendment) Regulations 1994. Use of the apparatus
outside the classroom or similar such place invalidates the conformity with the
protection requirements of the Electromagnetic Compatibility Directive (89/336/EEC)
and could lead to prosecution.
Facilities Required
Installation may be completed using a basic tool kit.
The UOP4 MkII is designed for floor standing on a firm, level floor. When choosing a
location for the equipment, the need to gain access to items such as the solvent tank
for filling and the waste solids hopper for emptying will need to be taken into account.
Access to all four sides of the equipment should be allowed.
The unit requires connection to a mains electrical supply, a continuous supply of cold
water and connection to a floor drain.
Mains Electrical Supply

The equipment requires connection to a single phase fused electrical supply. Four
metres of cable is supplied with the equipment, terminated with a plug to suit the
mains input connector on the rear panel of the console. Three versions are available:
UOP4 MkII-A 220/240V/1ph/50Hz @ 13 Amps
UOP4 MkII-B 120V/1ph/60Hz @ 15 Amps
UOP4 MkII-G 220/240V/1ph/60Hz @13 Amps
Cold Water Supply

For reliable discharge of the spent solid carrier, a permanent connection to a cold
water supply will be required. The supply should be connected to the inlet on the
pressure regulator using / 12.7 mm ID hose (not supplied by Armfield). A source
of de-ionised water will also be required for preparing the salt solutions and for use
as the solvent when performing solid/liquid extraction.
Laboratory Drain
A suitable floor drain will be required to dispose of water from the equipment during
operation. The outlet in the base of the extracted solids tank should be connected to
the drain using / 12.7 mm ID hose (not supplied by Armfield). Note that water
drains from the tank under gravity and the drain connection must not therefore be
restricted.
25
Installation Process
All numerical references relate to the equipment diagrams.
The UOP4 MkII Solid/Liquid Extraction Unit is supplied fully assembled. The following
checks should be made to ensure that all electrical and fluid connections are intact
and the equipment is ready for commissioning following shipping and unpacking.
1. Ensure that all packaging has been removed, especially from the rotor of the
extraction cell (7) and the hopper/spiral feeder (10).
2. Connect the electrical mains lead supplied to the mains input socket (26) on
the rear of the console but do not connect it to the electrical supply at this
point.
3. Check that DC supply lead from hub of extraction cell is connected to socket
on underside of console.
Check that DC supply lead from motor on feeder is connected to socket on

underside of console.
4. Check that the system is connected as shown in Figures 1 and 3. When

correctly connected, fluid from the fresh solvent tank (11) should flow in the
following sequence:
First stage pump (3a on right-hand side) to first stage heater (4a) to first stage
sprinkler bar (6a furthest anticlockwise).
First stage solvent collection trough (8a) via filter (9a) to second stage pump
(3b middle) to second stage heater (4b) to second stage sprinkler bar (6b
middle).
Second stage solvent collection trough (8b) via filter (9b) to third stage pump
(3c left-hand side) to third stage heater (4c) to third stage sprinkler bar (6c
furthest clockwise).
Third stage solvent collection trough (8c) via filter (9c) then conductivity
electrode C4 and temperature sensor T4 to overflow into final miscella tank
(13).
5. Place the solid carrier (porous polymer pellets) and the filling tube/batch
sample cloth, supplied with the equipment, in a safe location ready for use.
The equipment is ready for connection to the appropriate services followed by

commissioning. See Connection to Services and Commissioning.
Connection to Services
Electrical Supply for Version UOP4 MKII-A
Before connecting the electrical supply ensure that the RCD/RCCB (23) and all
miniature circuit breakers (24a, 24b, 24c) are in the off (down position). Also ensure
that all rotary controls are set to minimum and all switches are set to off on the front
of the console.
The equipment requires connection to a single phase, fused electrical supply. The
standard electrical supply for this equipment is 220/240V, 50Hz. Check that the
26
Installation
voltage and frequency of the electrical supply agree with the label attached to the
supply cable on the equipment. Connection should be made to the supply cable as
follows:
GREEN/YELLOW - EARTH
BROWN - LIVE (HOT)
BLUE - NEUTRAL
Fuse Rating - 13 AMP
Electrical Supply for Version UOP4 MKII-B

miniature circuit breakers (24 a,b,c) are in the off (down position). Also ensure that all
rotary controls are set to minimum and all switches are set to off on the front of the
console.
standard electrical supply for this equipment is 120V, 60Hz. Check that the voltage
and frequency of the electrical supply agree with the label attached to the supply
cable on the equipment. Connection should be made to the supply cable as follows:
BROWN - LIVE (HOT)
BLUE - NEUTRAL
Electrical Supply for Version UOP4 MKII-G

miniature circuit breakers (24 a,b,c) are in the off (down position). Also ensure that all
rotary controls are set to minimum and all switches are set to off on the front of the
console.
standard electrical supply for this equipment is 220/240V, 60Hz. Check that the
voltage and frequency of the electrical supply agree with the label attached to the
supply cable on the equipment. Connection should be made to the supply cable as
follows:
BROWN - LIVE (HOT)
BLUE - NEUTRAL
The UOP4 MKII Solid/Liquid Extraction Unit is ready for commissioning.
Refer to the Operational procedures section for details on how to operate the
equipment and how to prepare samples of solid material ready for extraction.
27
Cold Water Supply

Set the pressure regulator to minimum before connecting it to the cold water supply
(pull the knob upwards then turn the knob fully anticlockwise). Connect a cold water
supply to the inlet on the pressure regulator using ID / 12.7 mm hose (not
supplied by Armfield). The hose must be secured to the pressure regulator using a
suitable hose clip (not supplied).
Drain Connection
Connect the drain in the base of the extracted solids tank to a suitable floor drain
using ID / 12.7 mm hose (not supplied by Armfield). Note that the tank drains
under gravity and the hose must not be restricted when the equipment is in use.
Using the Optional Educational Software and Data Logging

Accessory
An I/O Data Port connector (27) on the underside of the console allows the voltage
signals from each of the measurements to be connected to the parallel port of a
suitable PC using an Armfield IFD3 interface device. The interface device obtains its
power from a mains output socket (25) marked OUTPUT at the rear of the console.
This interface device together with the appropriate Windows based software is
available as an optional accessory to accompany the UOP4 MkII. The operation of
the interface is described in the instruction leaflet supplied with the IFD3. The
operation of the Windows based software is described in the help text included as
part of the software.
Commissioning
All numerical references relate to the equipment diagrams.
The following procedure is intended for initially checking that the equipment is
operating correctly after assembly. This procedure should be started with the mains
electrical supply disconnected.
1. Using the spirit level attached to the base of the extraction cell (7) alongside
the rotor, adjust the feet at the bottom of the frame (1) to level the equipment
in both axes.
2. Check that the mains switch on the front of the console (15) is in the OFF
position.
3. Check that all of the rotary controls on the console (16, 17, 19a, 19b, & 19c)
are set to ZERO (fully anti-clockwise).
4. Check that all three of the heater switches on the front of the console are
switched OFF (20a, 20b & 20c). Note that the heaters should only be
switched on when there is a consistent flow of liquid through the heaters. If
the heaters are switched on with no liquid flowing they will rapidly overheat
and cause the over temperature protection operate. This will reset
automatically when the heaters cool to a satisfactory temperature but will take
time.
5. Connect the mains electrical supply and check that it is switched on.
Check the operation of the RCD (23) by pressing the TEST button. The RCD
must trip when the button is pressed. If the RCD does not trip or it trips before
28
Installation
pressing the test button then it must be checked by a competent electrician

before the equipment is used.
6. Ensure that the RCD (23) and three miniature circuit breakers (24a, 24b &
24c) on the rear panel of the console are switched on.
7. Set the mains on/off switch (15) on the front of the console to the ON position.
8. With the heaters still switched off check that the displays on the three PID
controllers (22a, 22b & 22c) are illuminated and displaying the temperatures
at their respective sensing points (T1, T2 & T3) - initially at ambient
temperature until the equipment is operational.
The Temperature/Conductivity display (18) should also be illuminated. Set the

selector switch adjacent to the display to position T4 and confirm that the
reading is also of ambient temperature.
Note: At this stage the conductivity probes should contain no liquid and so will
not give a meaningful reading if the selector switch is set to positions C1, C2,
C3 or C4.
9. To test the operation of the spiral feeder (10), set the feeder speed on/off
switch (16) to the ON position then gradually turn the feeder speed control
clockwise. The spiral should rotate progressively faster as the control is
turned further clockwise. Once the feeder has been tested the control can be
turned back to zero and the switch set to the off position.
10. To test the operation of the rotor on the extraction cell (7), set the rotor speed
on/off switch (17) to the ON position then gradually turn the rotor speed
control clockwise. The rotor should turn progressively faster as the control is
turned further clockwise. Once the rotor has been tested the control can be
turned back to zero and the switch se to the off position.
Note: As the maximum rotational speed of the rotor is only 4 revolutions per
hour it will take some time for the rotation to be apparent.
11. To test the operation of the three peristaltic pumps:
Fill the Fresh Solvent Tank (11) with clean water.
Set the rotary speed control (19a) for the first stage pump (3a) to 80%.
Water should be ejected from the first stage sprinkler bar (6a) when the
pipework has primed.
When water has drained into the first stage solvent collection trough (8a) and a
level has been established, set the rotary speed control (19b) for the second
stage pump (3b) to 80%. When water has drained into the second stage
solvent collection trough (8b) and a level has been established, set the rotary
speed control (19c) for the third stage pump (3c) to 80%. Water should exit to
the final miscella tank (13) when the pipework has primed.
Note: For correct operation a water level of approximately 15 mm must be

maintained inside the solvent collection troughs for the first and second stages
(8a and 8b). The actual depth is not important but the relative speed of the
pumps must be adjusted to ensure that these troughs do not run dry. Similarly
29
these troughs must not overfill above the level of the elbow on the vent tube
that is mounted through the sidewall of the trough.
12. To test the operation of the PID controllers and heaters:
Ensure that water is flowing through the three stages of the system as
described above. It may be necessary to adjust the relative speed of the
pumps slightly to maintain a steady level in each of the solvent collection
troughs. (If any tank runs dry then the next stage will be starved.)
To avoid excessive overshoot when heating, initially adjust the setpoint of each
controller to match the temperature on the display. If necessary, refer to the
procedure for checking or adjusting the set point which is included in the
description of the PID controllers.
Switch on heater 1 (20a) then adjust the set point of the first stage controller
(22a) to 40oC and allow the temperature reading to stabilise at 40oC. Switch on
heater 2 (20b) then adjust the set point of the second stage controller (22b) to
45oC and allow the temperature to stabilise at 45oC. Switch on heater 3 (20c)
then adjust the set point of the third stage controller to 50oC and allow the
temperature to stabilise at 50oC.
13. To test the operation of the spray nozzle:
Ensure that a water supply is connected to the pressure regulator and that the
outlet in the base of the extracted solids tank is connected to a suitable drain.
Adjust the height of the spray nozzle so that the tip of the nozzle is above the
baffles inside the rotor but below the top edge of the rotor.
Adjust the pressure regulator to give a spray pattern that washes the walls of
the cells without excessive splashing or overspray (adjust the height of the
spray nozzle if necessary).
Check that water drains into the extracted solids tank and flows to drain via the
outlet.
Turn of the spray nozzle by turning the knob on the pressure regulator fully
anticlockwise.
Commissioning of the UOP4 MkII is complete.
Switch off each of the heaters and set each of the pump speed controls to zero then
switch off the main switch.
Electrical Wiring Diagram

Click on the relevant link to invoke the Wiring Diagram:
Wiring Diagram CDM27585 sheet 1
Wiring Diagram CDM27585 sheet 2
Printed Versions of this Instruction Manual

Please note, all wiring diagrams are appended at the rear of this manual
30
Operation
Where necessary, refer to the drawings in the Equipment Diagrams section.
Operating the Software

Note: The diagrams in this section are included as typical examples and may not
relate specifically to the individual product described in this instruction manual.
The Armfield Software is a powerful Educational and Data Logging tool with a wide
range of features. Some of the major features are highlighted below, to assist users,
but full details on the software and how to use it are provided in the presentations
and Help text incorporated in the Software. Help on Using the Software or Using the
Equipment is available by clicking the appropriate topic in the Help drop-down menu
from the upper toolbar when operating the software as shown:
Before operating the software ensure that the equipment has been connected to the
IFD5 Interface (where IFD5 is separate from the equipment) and the IFD5 has been
connected to a suitable PC using a USB lead. For further information on these
actions refer to the Operation manual.
Load the software. If multiple experiments are available then a menu will be
displayed listing the options. Wait for the presentation screen to open fully as shown:
Before proceeding to operate the software ensure that IFD: OK is displayed at the
bottom of the screen. If IFD:ERROR is displayed check the USB connection between
the IFD5 and the PC and confirm that the red and green LEDs are both illuminated.
If the problem persists then check that the driver is installed correctly (refer to the
Operation manual).
31
Presentation Screen - Basics and Navigation

As stated above, the software starts with the Presentation Screen displayed. The
user is met by a simple presentation which gives them an overview of the capabilities
of the equipment and software and explains in simple terms how to navigate around
the software and summarizes the major facilities complete with direct links to detailed
context sensitive help texts.
To view the presentations click Next or click the required topic in the left hand pane
as appropriate. Click More while displaying any of the topics to display a Help index
related to that topic.
To return to the Presentation screen at any time click the View Presentation icon
from the main tool bar or click Presentation from the dropdown menu as
shown:
For more detailed information about the presentations refer to the Help available via
the upper toolbar when operating the software.
Toolbar
A toolbar is displayed at the top of the screen at all times, so users can jump
immediately to the facility they require, as shown:
The upper menu expands as a dropdown menu when the cursor is placed over a
name.
The lower row of icons (standard for all Armfield Software) allows a particular
function to be selected. To aid recognition, pop-up text names appear when the
cursor is placed over the icon.
Mimic Diagram
The Mimic Diagram is the most commonly used screen and gives a pictorial
representation of the equipment, with continuously updated display boxes for all the
various sensor readings, calculated variables etc. directly in engineering units.
To view the Mimic Diagram click the View Diagram icon from the main tool bar
or click Diagram from the View drop-down menu as shown:
32
Operation
A Mimic diagram is displayed, similar to the diagram as shown:
The details in the diagram will vary depending on the equipment chosen if multiple
experiments are available.
In addition to measured variables such as Temperature, Pressure and Flowrate (from

a direct reading flowmeter), calculated data such as Motor Torque, Motor Speed and
Discharge / Volume flowrate (from pressure drop across an orifice plate) are
continuously displayed in data boxes with a white background. These are
automatically updated and cannot be changed by the user.
Manual data input boxes with a coloured background allow constants such as Orifice
Cd and Atmospheric Pressure to be changed by over-typing the default value, if
required.
The data boxes associated with some pressure sensors include a Zero button
alongside. This button is used to compensate for any drift in the zero value, which is
an inherent characteristic of pressure sensors. Pressing the Zero button just before
starting a set of readings resets the zero measurement and allows accurate pressure
measurements to be taken referenced to atmospheric pressure. This action must be
33
carried out before the motor is switched on otherwise the pressure readings will be
offset.
The mimic diagram associated with some products includes the facility to select
different experiments or different accessories, usually on the left hand side of the
screen, as shown:
Clicking on the appropriate accessory or exercise will change the associated mimic
diagram, table, graphs etc to suit the exercise being performed.
Control Facilities in the Mimic Diagram

A Power On button allows the motor to be switched off or on as required. The button
always defaults to off at startup. Clicking this button switches the power on (1) and off
(0) alternately.
A box marked Motor Setting allows the speed of the motor to be varied from 0 to
100% either stepwise, by typing in values, or using the up / down arrows as
appropriate. It is usual to operate the equipment with the motor initially set to 100%,
then reduce the setting as required to investigate the effect of reduced speed on
performance of the equipment.
When the software and hardware are functioning correctly together, the green LED
marked Watchdog Enabled will alternate On and Off. If the Watchdog stops
alternating then this indicates a loss of communication between the hardware and
software that must be investigated.
Details on the operation of any automatic PID Control loops in the software are
included later in this section.
Data Logging Facilities in the Mimic Diagram

There are two types of sampling available in the software, namely Automatic or
Manual. In Automatic logging, samples are taken regularly at a preset but variable
interval. In Manual logging, a single set of samples is taken only when requested by
34
Operation
the operator (useful when conditions have to be changed and the equipment allowed
to stabilize at a new condition before taking a set of readings).
The type of logging will default to manual or automatic logging as appropriate to the
type of product being operated.
Manual logging is selected when obtaining performance data from a machine where
conditions need to stabilize after changing appropriate settings. To record a set of set
of data values from each of the measurement sensors click the icon from the
main toolbar. One set of data will be recorded each time the icon is clicked.
Automatic logging is selected when transients need to be recorded so that they can
be plotted against time. Click the icon from the toolbar to start recording, click
the icon from the toolbar to stop recording.
The type of logging can be configured by clicking Configure in the Sample drop-
down menu from the upper toolbar as shown:
In addition to the choice of Manual or Automatic sampling, the parameters for

Automatic sampling can also be set. Namely, the time interval between samples can
be set to the required number of minutes or seconds. Continuous sampling can be
selected, with no time limit or sampling for a fixed duration can be set to the required
number of hours, minutes or seconds as shown:
Tabular Display
To view the Table screen click the View Table icon from the main tool bar or
click Table from the View dropdown menu as shown:
35
The data is displayed in a tabular format, similar to the screen as shown:
As the data is sampled, it is stored in spreadsheet format, updated each time the
data is sampled. The table also contains columns for the calculated values.
New sheets can be added to the spreadsheet for different data runs by clicking the
icon from the main toolbar. Sheets can be renamed by double clicking on the
sheet name at the bottom left corner of the screen (initially Run 1, Run 2 etc) then
entering the required name.
For more detailed information about Data Logging and changing the settings within
the software refer to the Help available via the upper toolbar when operating the
software.
Graphical Display
When several samples have been recorded, they can be viewed in graphical format.
36
Operation
To view the data in Graphical format click the View graph icon from the main
tool bar or click Graph from the View drop-down menu as shown:
The results are displayed in a graphical format as shown:
(The actual graph displayed will depend on the product selected and the exercise
that is being conducted, the data that has been logged and the parameter(s) that has
been selected).
Powerful and flexible graph plotting tools are available in the software, allowing the
user full choice over what is displayed, including dual y axes, points or lines,
displaying data from different runs, etc. Formatting and scaling is done automatically
by default, but can be changed manually if required.
To change the data displayed on the Graph click Graph Data from the Format
dropdown menu as shown:
37
The available parameters (Series of data) are displayed in the left hand pane as
shown:
Two axes are available for plotting, allowing series with different scaling to be
presented on the same x axis.
To select a series for plotting, click the appropriate series in the left pane so that it is
highlighted then click the appropriate right-facing arrow to move the series into one of
the windows in the right hand pane. Multiple series with the same scaling can be
plotted simultaneously by moving them all into the same window in the right pane.
To remove a series from the graph, click the appropriate series in the right pane so
that it is highlighted then click the appropriate left-facing arrow to move the series into
the left pane.
The X-Axis Content is chosen by default to suit the exercise. The content can be
changed if appropriate by opening the drop down menu at the top of the window.
The format of the graphs, scaling of the axes etc. can be changed if required by
clicking Graph in the Format drop-down menu as shown:
38
Operation
For more detailed information about changing these settings refer to the Help
available via the upper toolbar when operating the software.
PID Control
Where appropriate, the software associated with some products will include a single
or multiple PID control loops whereby a function on the product can be manually or
automatically controlled using the PC by measuring an appropriate variable and
varying a function such as a heater power or pump speed.
The PID loop can be accessed by clicking the box labelled PID or Control depending
on the particular software:
A PID screen is then displayed as shown:
39
The Mode of operation always defaults to Manual control and 0% output when the
software is loaded to ensure safe operation of the equipment. If appropriate, the
operator can retain manual operation and simply vary the value from 0 to 100% in the
Manual Output box, then clicking Apply.
Alternatively, the PID loop can be changed to Automatic operation by clicking the
Automatic button. If any of the PID settings need to be changed from the default
values then these should be adjusted individually before clicking the Apply button.
The controller can be restored to manual operation at any time by clicking the Manual
button. The value in the Manual Output box can be changed as required before
clicking the Apply button.
Settings associated with Automatic Operation such as the Setpoint, Proportional

Band, Integral Time, Derivative Time and Cycle Time (if appropriate) can be
changed by the operator as required before clicking the Apply button.
Clicking Calculations displays the calculations associated with the PID loop to aid
understanding and optimization of the loop when changing settings as shown:
40
Operation
Clicking Settings returns the screen to the PID settings.
Clicking OK closes the PID screen but leaves the loop running in the background.
In some instances the Process Variable, Control variable and Control Action can
be varied to suit different exercises, however, in most instances these boxes are
locked to suit a particular exercise. Where the variables can be changed the options
available can be selected via a drop-down menu.
Advanced Features
The software incorporates advanced features such as the facility to recalibrate the
sensor inputs from within the software without resorting to electrical adjustments of
the hardware. For more detailed information about these advanced functions within
the software refer to the Help available via the upper toolbar when operating the
software.
Operating the Equipment

Safe Operation
The UOP4 MkII is designed for safe operation and can be operated safely by a
person who fully understands the operation of the equipment. Before starting to
operate the equipment all operators should note the following important points:
1. Operators should avoid liquids getting on to the electrical parts of the system
since this could present an electric shock hazard and may trip the RCD.
2. Operators should not put their hands into the hopper (10) of the materials
feeder while it is switched on since the spiral is very highly geared and could
damage a persons fingers.
3. Operators should not put their hands into the rotor (7) when it is switched on.
Although the speed of rotation is extremely slow and incorporates a slipping
clutch, the rotor is very highly geared and could damage a persons fingers.
41
4. Although not toxic, the salt (Potassium Bicarbonate) and carrier (porous
polymer pellets) need to be handled with care. Operators should avoid
breathing in dust containing the Potassium Bicarbonate and should wear
gloves to avoid contact with the salt in powder form or in solution. If clothing is
contaminated with Potassium Bicarbonate it should be removed and any
areas of skin which have been in contact should be thoroughly washed with
clean water.
5. The heater (4a, 4b & 4c) in each stage of the process relies on flowing liquid
to carry the heat to the temperature sensor downstream which is used by the
PID controller to control the temperature. Each heater switch (20a, 20b & 20c)
must therefore be switched off until water is flowing continuously through the
appropriate heater. Over-temperature protection is fitted to each of the
heaters for safety but it is good practice and will save time if the heaters are
only switched after the system is primed and running. Over temperature
indicators (21a, 21b & 21c) flash when the temperature is excessive and
power to the appropriate heater has been cut. The protection will reset
automatically when the temperature of the heater returns to normal.
Preparation of Materials
Before starting to operate the equipment it will be necessary to prepare the solid
material (carrier) to be extracted from.
The recommended solid material for processing in the UOP4 MkII is Microporous
Polyamide 6-pellets. This is an inert, plastic material in pellet form that offers a
convenient porous carrier for the extractable material. A quantity of porous polymer
pellets is supplied with the equipment for use as the solid carrier. The plastic pellets
can be reclaimed and reused.
Note: Solid carrier material other than the porous polymer pellets supplied with the
equipment may contain dust, large particles or hard particles that could damage the
equipment. For this reason it is important to check the suitability of alternative
carriers before using them in the feeder or extraction cell.
The recommended material for extraction is a salt called Potassium Bicarbonate

(also called Potassium Hydrogencarbonate having the chemical symbol KHCO 3 ).
Other materials may be used if required but the conductivity change with
concentration will need to be defined by the user.
The laboratory teaching exercises and exercises using UOP4MkII-303IFD software

assume that Potassium Bicarbonate is used.
The solid carrier can be prepared for use in the UOP4 MkII as follows (3 litre batches
of material will be convenient to handle):
1. Ensure that the porous polymer pellets are thoroughly dry before attempting
to absorb the salt into them.
2. If the pellets are not dry spread them onto drying trays and allow to air-dry,
this process can be accelerated using an oven set to no more than 60C.
3. Measure a 3 litre batch of dry pellets.
4. Dissolve 500g of the extractable material (Potassium Bicarbonate) into 1.5

litres of water at room temperature.
42
Operation
5. Add the solution of Potassium Bicarbonate to 3 litres of dried porous polymer

pellets and stir the mixture until the pellets are thoroughly wetted out with the
solution.
6. Leave the pellets for approximately 24 hours to absorb the solution, stirring
the mixture periodically to distribute the solution evenly.
7. Spread the wetted out pellets on to drying trays. If there is a small amount of
unabsorbed solution it can be stirred into the pellets after it has been dried in
the next stage.
8. Finally dry out the pellets, this process can be accelerated using an oven set
to no more than 60oC.
9. Weigh the dried pellets and determine the proportion of Potassium

Bicarbonate by weight (ConcS). Because of the low density of the pellets the
ratio will be approximately 1:1.8 ie. 500 grams of KHCO 3 in a total weight of
900 grams of treated porous polymer pellets and ConcS = 55%.
10. Note: it is possible for the pellets to become electrostatically charged which
may result in pellets sticking to the hopper surface. Care should be taken in
storing the polymer to prevent electrostatic charging.
Calibration of Feed Pumps

The user will find it useful to calibrate the peristaltic feed pumps (3a, 3b & 3c) so that
the actual flow rate can be related to the setting of the rotary speed control (19a, 19b
& 19c). Although the three pumps are identical in specification it is advisable to carry
out a separate calibration for each as there may be slight differences due to
tolerances. To calibrate each pump the following steps should be followed:
1. Check that the heaters are switched off using the three switches (20a, 20b &
20c) on the front of the console. Disconnect the flexible tubes attached to the
pump making a note of the original connections
2. Connect a length of flexible tubing from a large beaker of water to the pump
inlet and a similar flexible tube leading from the pump outlet to a measuring
cylinder (typically 250 ml or 500 ml capacity).
3. Set the appropriate pump rotary speed control (19a, 19b or 19c) to setting
2.0.
4. Collect the water discharging from the pump for a timed period using the
measuring cylinder and stopwatch then calculate the volume flowrate as
follows:
5. Repeat the above step for settings of 4.0, 6.0, 8.0 and 10.0.
6. Draw a graph of flow rate (litres/hour) versus speed setting. The result should
be a straight line (the pumps will not operate at low settings of the speed
control).
7. Re-attach the flexible tubes from the pumps to their original positions.
43
8. Repeat the above steps for the two remaining pumps to produce similar
graphs for those pumps.
Copies of the three graphs produced using the above procedure should be kept with
the equipment for reference.
Calibration of Feeder
The user will find it useful to calibrate the feeder arrangement so that the actual
delivery of solid material can be related to the setting of the rotary speed control.
To calibrate the feeder the following steps should be followed:
1. Fill the hopper (10) with a dried sample of the solid carrier (porous polymer
pellets containing Potassium Bicarbonate) to be processed.
2. Rotate the rotor of the extraction cell until one cell aligns with the aperture in
the base. Ensure that the rotor and base are dry to prevent solid material from
adhering. Place a suitable receptacle beneath the shute on the underside of
the aperture to collect any solid discharging from it.
3. Switch on the feeder and set the feeder rotary speed control (16) to setting
2.0.
4. When the spiral has filled and solid is discharging at a steady rate, collect the
solid for a timed period using a stopwatch. Weigh the solid collected then
calculate the mass flowrate as follows:
5. Repeat the above steps for settings of 4.0, 6.0, 8.0 and 10.0.
6. Draw a graph of mass flow rate (kg/hour) versus speed setting. The result
should be a straight line (the feeder will not operate at low settings of the
speed control).
A copy of the graph produced using the above procedure should be kept with the
equipment for reference.
Calibration of Rotor Speed

The user will find it useful to calibrate the rotor so that the actual speed of rotation
can be related to the setting of the rotary speed control. For accurate results the rotor
should be calibrated under normal operating conditions containing wet material.
To calibrate the rotor the following steps should be followed:
1. Place a mark on the base of the extraction cell (7) adjacent to the wall of the
rotor.
2. Fill the hopper (10) with a dried sample of the solid carrier (porous polymer
pellets containing Potasium Bicarbonate) to be processed.
3. Switch on the rotor and set the rotor speed control (17) to setting 2.0.
44
Operation
4. Switch on the feeder and set the feeder rotary speed control (16) to setting
2.0.
5. Switch on the pumps (19a, 19b & 19c) and allow the system to stabilise.
6. Using a stopwatch record the time taken for one compartment to move past
the marks on the base. For accuracy repeat the measurement several times.
7. Calculate the rotor speed as follows:
8. Repeat the above steps for settings of 4.0, 6.0, 8.0 and 10.0.
9. Draw a graph of rotor speed (revs/hour) versus speed setting. The result
should be a straight line (the rotor will not operate at low settings of the speed
control).
A copy of the graph produced using the above procedure should be kept with the
equipment for reference.
Method for Setting the Temperature Controllers

Having selected a suitable temperature for the solvent in the three stages of the
process it will be necessary for the user to set this temperature on the three PID
controllers (22a, 22b & 22c). The operating range is between ambient and 55oC (it
will not be possible to control the temperature with a setting at or below the ambient
air temperature).
The set point of the controllers can be checked and changed as follows:
Make sure that the heaters are switched off using the three heater switches (20a,
20b & 20c) on the front panel of the console and then switch on the UOP4 MkII (15).
The digits on the three PID controllers should illuminate and, after an initial check,
display the temperature at the three sensing points.
To check the current set point:
Press either the increase key or decrease key briefly.
To change the current set point:
Press either the increase key or decrease key briefly. The current set point
will be displayed.
Press and hold the increase or decrease key as required until the required
value of the digit is displayed.
Note that the heaters should not be switched on until the flows of liquid in the heaters
are steady.
45
Note:
For optimum control of the temperatures within the process, without excessive
overshoot, the setpoint of each controller should be set to ambient temperature when
the equipment is first switched on with water flowing. Adjustment to the required
setpoint during operation will then give smooth control without excessive overshoot.
Similarly it is suggested that the temperature of stage 1 should be allowed to stabilise

before increasing the setpoint of stage 2 and the temperature of stage 2 should be
allowed to stabilise before increasing the setpoint of stage 3.
Method for Starting Up and Balancing the Three Liquid Stages

Before using the extractor system as a multi-stage process users may find it useful to
operate the three solvent stages independently from the rest of the system, this will
allow the user to master the techniques that will be needed to keep the three stages
running in balance. It is important to balance the stages since they cascade from one
to another. If one stage pump is running too fast relative to the other pumps there will
be a tendency for the trough which is supplying the pump to run dry and for the next
trough down the line to over flow. Out of balance running can lead to instability and
intermittent liquid flows can cause the heater protection circuits to operate.
Note: For correcty operation the first and second stage troughs must not be allowed
to run dry and the level must not be allowed to rise so that the elbow on the vent pipe
(mounted through the side wall of each trough) becomes submerged.
The objective of the following method is to fill the stage troughs to a depth of
approximately 15 mm of water and to set the stage pumps running so that the three
stages run in balance at the desired operating speed:
1. Check that the mains switch (15) on the front of the console is in the off
position.
2. Check that all of the rotary controls (16, 17, 19a, 19b & 19c) on the console
are set to zero (fully anti-clockwise).
3. Check that all three of the heaters are switched OFF using the switches (20a,
20b & 20c) on the front of the console.
4. Switch the on the mains power using the mains switch (15) on the front of the
console.
5. Switch the RCD/RCCB (23) and circuit breakers (24a, 24b, 24c & 24d) on the
back of the console to the on position.
6. Fill the fresh solvent tank (11) with clean water.
7. To save time, fill solvent collection trough one (8a) and solvent collection
trough two (8b) to a depth of approximately 20 mm by pouring water in
through the rotor.
8. Pour water into the third stage trough (8c) until the water level reaches the
point where it drains into the final miscella tank (13). Note that the final trough
will drain completely.
46
Operation
9. Prime each of the pumps (3a, 3b & 3c) in turn by setting the appropriate
speed control (19a, 19b or 19c) to maximum until water exits the appropriate
sprinkler bar (6a, 6b or 6c).
10. Once the system has been primed the three pumps can be adjusted to run at
the desired rate (eg. setting 5.0 on the potentiometer for half of maximum
flow). Water from the fresh solvent tank should now be cascading through the
three stages via the three pumps and troughs and then draining into the final
miscella tank.
11. After the system has been running for a while the levels in solvent collection
troughs one and two will indicate how well the flowrates in the system are
balanced. If the system is perfectly in balance then the levels in troughs one
and two will not have changed, however if the levels are changing an
alteration to the system will be needed. To make the necessary changes the
following steps can be followed:
12. Use the flow rate of pump 1 as the master setting for all of the solvent flows
by leaving the speed control (19a) fixed at the desired rate. The user will find
that this technique will greatly reduce any complexity involved in balancing
the system since it can now be balanced using alterations to the two other
pumps only.
13. Having set pump 1, work from right to left through the solvent stages when
making changes ie. first look at the trend/level in trough 1 (8a) and alter the
speed setting (19b) of pump 2 to change the trend. If the level in trough 1 is
falling reduce the speed of pump 2. Conversely, if the level in trough 1 is
rising increase the speed of pump 2. If the level has changed substantially
from the half full position temporarily set the speed to maximum or minimum
as appropriate then reset the speed to normal when the level has been
returned to half full. Note the change in pump speed necessary to restore the
balance.
14. Once pump 2 has been set to maintain the level in trough 1 the user can look
at trough 2 (8b). The control of the level in trough 2 is slightly different to that
in trough 1 since trough 2 has a variable flow of liquid into it (controlled by
pump 2) as well as a variable flow of liquid being removed from it (controlled
by pump 3). When the user adjusts the speed of pump 3 to maintain the level
in trough 2 it will be necessary to consider the effect of any changes that have
been made to the speed of pump 2 as well as any existing change in the
level. If for example trough 2 was maintaining its level before an increase in
pump 2 speed, it will be necessary to increase the speed of pump 3 by a
similar amount in order to compensate for the increased flow into the trough
from pump 2 .
15. The level in the final trough (8c) does not require any adjustment since this is
self-controlling.
The balancing procedure described above should be repeated as frequently as is

required. Users will find that as the balance becomes more precise, the period
between speed adjustments will become longer and the required adjustments will
become finer. Maintaining the balance will be easier if trends in the liquid levels are
spotted early and small adjustments are made to the flows to compensate.
47
Once the user has balanced the system it is possible to retain the approximate pump
settings for future use by making a note of the potentiometer settings (19a, 19b &
19c).
Method for Start Up and Operation

Once the points relating to safety (listed earlier) have been understood the operator
should read through all of the steps for operating the system listed below before
starting to use the system.
The first step in starting up the system is to balance the solvent stages at the
required flow rate as described in the previous section. Once the solvent system is
running in balance the procedure is as follows:
1. Switch on the extractor rotor and adjust the speed control (17) to give the
required rotational speed (typically two revolutions per hour). Note that at two
revs per hour it will take three minutes for one of the dividers in the rotary cell
to pass a fixed point.
2. Half fill the hopper (10) of the spiral feeder with untreated solid carrier (dry
porous polymer pellets).
3. Switch on the feeder and adjust the speed control (16) so that the
compartments of the rotary cell are filled to between one-third and half height
as they pass under the feeder. Note that the top surface of the solid will adopt
a saw tooth profile due to the action of the baffles.
4. As the filled compartments pass beneath the sprinkler bars (6c, 6b then 6a
because of the counter current operation) the balance in the collection
troughs will change because of hold-up in the material. Because of this the
speed of the second and third stage pumps will need to be adjusted regularly
during the first rotation to prevent any of the collection troughs from running
dry. Once all of the compartments in the system have been filled the balance
of the solvent system should progressively approach an equilibrium state and
adjustments to the pump speeds should be minimal.
When the solid material reaches the aperture in the base at the rear of the
extractor it will be necessary to turn on the spray nozzle so that the material is
washed into the extracted solids tank. Adjust the position of the nozzle and
pressure regulator as required to prevent overspray.
5. More experienced operators may wish to reduce the time taken to start up the
system filling all of the compartments of the rotary cell with untreated solid
carrier then wetting it with water by hand before balancing the pump settings.
6. Once the system has settled down and the solvent stages are running in
balance the PID heater controllers (22a, 22b & 22c) can be set to the desired
operating temperature (using the method described earlier) and switched on
(20a, 20b & 20c). For smooth control the setpoint of each stage should be
increased to the required value after the previous stage has stabilised.
7. The next stage in the start up procedure is to replace the carrier with pellets
containing Potassium Bicarbonate, this is done by simply filling the feeder
hopper with the treated solid carrier as the untreated material runs out.
8. Once the system has been started up as described above the parameters
such as the operating temperatures, solvent flow rate, solid feed rate and
48
Operation
rotor speed can be varied as required. Although the extraction process is

continuous and should settle to an equilibrium condition, the way in which this
condition is established is just as important as the final condition. Readings
should therefore be taken at regular intervals throughout the operation to
allow the transient responses to be studied.
When running the UOP4 MkII it is important that the user should carefully monitor the
process since the apparatus will need to be kept topped up with fresh solvent and
extractable material. The user will also have to empty the waste solids hopper and
check that the solvent stages remain in balance.
Shut Down Procedure

Shutting down the UOP4 MkII is a simple process which can be accomplished as
follows:
1. Switch off all three of the heaters using the switches on the control console
(21a, 21b & 21c).
2. Switch off the spiral material feeder (16).
3. Set the speed of the rotor to maximum (17) in order to empty the rotor of the
remaining solid materials.
4. Fill the fresh solvent tank (11) with clean water then set the speed of the
pumps to maximum (19a, 19b & 19c) to thoroughly flush the heaters,
temperature sensors, conductivity probes, sprinkler bars and flexible tubing.
5. When all of the solid material from the rotor has discharged into the extracted
solids tank (12) the rotor can be switched off (17) and the spray nozzle can be
turned off by setting the pressure regulator to minimum (knob full
anticlockwise).
6. When the heaters, sensors, flexible tubing etc have been thoroughly flushed
through with fresh water the pumps can be set to minimum (19a, 19b &19c).
7. Switch off the power to the unit using the switch (15) on the control console
and then switch off and unplug the mains supply.
Cleaning after use

After use all of the solid material and liquid solutions should be emptied from the
equipment before flushing the process pipework with clean water. Fill the Fresh
Solvent Tank with clean water then operate the three stages of the process with the
pumps at maximum speed to flush the system. Operation with the water at elevated
temperature will be beneficial (set point on each PID controller at maximum).
If the equipment will be operated within a few days of commissioning then the
pipework should remain filled with de-ionised water to prevent deterioration of the
electrodes inside the conductivity probes. After cleaning, fill the Solvent tank with de-
ionised water then pump this through the system to leave the probes filled.
If the equipment will not be operated for a longer period then the conductivity probes
should be removed from the pipework, flushed with de-ionised water then air-dried to
prevent deterioration of the electrodes inside the probes.
49
After prolonged use it may be necessary to flush the system with a weak acid to
remove any build up of the salt in the pipework etc. Refer to the Routine Maintenance
section for further details if this is necessary.
Periodically it will be necessary to clean the Feeder and Extractor Cell. Details of the
procedure for dismantling these components is given below. The general procedure
for cleaning the equipment is to disassemble the parts which need cleaning,
removing any electrical assemblies and then to wiping the non electrical parts with a
cloth soaked in warm soapy water (abrasive cleaners and volatile solvents should not
be used). Note that when cleaning the equipment operators should avoid contact with
the chemicals used and if necessary should wear protective gloves.
1. Cleaning of the extractor assembly:
a. To prevent damage to the sprinkler bars remove the quick release fitting from
the end of each sprinkler bar (push the grey collar against the body of the
fitting while pulling the fitting).
b. Unclamp the spray nozzle at the rear of the extractor, raise and rotate the
rigid tube so that the tip of the nozzle is clear of the rotor.
c. Disconnect the electrical cable to the feeder from the socket on the underside
of the console.
d. Remove the feeder by unscrewing the thumbscrews that secure it to the

frame. Carefully tip any remaining solid carrier into a suitable container.
e. Disconnect the electrical cable to the top of the central hub on the extraction
cell from the socket on the underside of the electrical console.
f. Remove the top of the extractor (including the hub and rotor as a complete
assembly) from the base by unscrewing the two fixing screws (large thumb
nuts) on top of the hub. The hub / rotor will simply lift away from the base
revealing the mesh that allows the solvent to drain into the troughs
underneath.
g. Carefully wipe the rotor with a damp cloth soaked in warm soapy water to
remove any contamination.
h. With the hub / rotor removed the mesh which supports the solid carrier can be
cleaned using warm soapy water Ensure that the central recess for the hub of
the rotor is clear of any solid particles.
i. The collection troughs can usually be cleaned adequately by pouring warm

soapy water through the mesh from above. However, if contamination is
severe, the mesh can be removed to gain acces to the troughs for more
thorough cleaning. The mesh should be lifted from the recess in the base,
starting at one end and taking care not to distort it. After cleaning, the troughs
and mesh should be dried using a soft cloth then reassembled by pressing
the mesh into the recess, again taking care not to distort the mesh. When
correctly assembled the mesh should be flush with the surrounding PVC
base.
j. While the feeder / extractor hub are removed the frame can be cleaned to
remove any dust or spillage using a damp cloth.
50
Operation
k. After cleaning, the extractor should be dried with a soft cloth and reassembled
as follows:
Locate the central hub in the central recess of the base and rotate the hub until
the dowel pin locates in the hole. Pass the two fixing screws through the two
holes in the top of the hub and tighten the screws to secure the hub to the
base. Reconnect the electrical cable to the base of the console. Refit the
feeder to the frame using the thumbscrews.
l. Reposition the spray nozzle with the tip of the nozzle inside the cells but clear
of the baffles.
m. Reconnect the flexible tubing to the spray bars on the extraction cell.
Refer to Figure 1 and 3 in the equipment diagrams for details of the

connections of the flexible tubing/sprinkler bars to the extractor.
2. Cleaning of Spiral Conveyor Assembly
a. Cleaning of the feeder will not usually be necessary when using the porous
polymer pellets supplied by Armfield. However, after prolonged use or in
unusual circumstances cleaning of the spiral conveyor and hopper will be
necessary. Remove any remaining material from the hopper by running the
conveyor or by tipping the material into a suitable container after removing the
assembly from the frame by unscrewing the thumbscrews.
b. Detach the drive motor from the rest of the assembly by undoing the four
caphead screws which secure the motor to the hopper. Pull the motor away
from the hopper to separate the link between the motor and the spiral.
Remove the drive coupling from the end of the spiral (where the motor was
fitted) by unscrewing the grub screw that retains the coupling.
c. Having removed the motor and drive coupling undo the three thumb nuts on
the other end of the tube containing the spiral and disassemble the remainder
of the conveyor.
d. After cleaning with warm water, the components of the conveyor can be dried
with a soft cloth and then reassembled. Assembly of the components is
simply the reverse of the disassembly.
51
Equipment Specifications
Overall Dimensions
Approximate overall dimensions of the equipment in millimetres are:
Height - 1520 mm
Width - 770 mm
Depth - 560 mm
I/O Port Pin Connections

To allow access to the measurement signals in applications other than when using
an Armfield IFD3, the connections to the 50 way connector (27) are listed below for
information:
Pin No Channel No Signal Function
Analog Outputs (0-5 V dc exported from socket):
Temperatures T1 to T4 (0-60 oC) and Conductivities

1 Ch 0 Signal
C1 to C4 (0-100 mS) via analog switch
2 Ch 0 Return
3 Ch 1 Signal Speed setting of feeder (0-100%)
4 Ch 1 Return
5 Ch 2 Signal Speed setting of rotor (0-100%)
6 Ch 2 Return
7 Ch 3 Signal Speed setting of pump 1 (0-100%)
8 Ch 3 Return
10 Ch 4 Return
12 Ch 5 Return
13-21 Not Used
Analog Inputs (0-5V dc input from socket):
52
Equipment Specifications
22-25 Not Used
Digital Outputs (0-5V dc):
Not Used
Digital Inputs (0-5V dc):
38 Ch 0 Analog switch
42 Digital Ground
43 Ch 4 Inhibit analog switch
44-46 Not Used
47 Digital Ground
48-50 Not Used
Environmental Conditions
This equipment has been designed for operation in the following environmental
conditions. Operation outside of these conditions may result reduced performance,
damage to the equipment or hazard to the operator.
a. Indoor use;
b. Altitude up to 2000 m;
c. Temperature 5 C to 40 C;
d. Maximum relative humidity 80 % for temperatures up to 31 C, decreasing

linearly to 50 % relative humidity at 40 C;
e. Mains supply voltage fluctuations up to 10 % of the nominal voltage;
f. Transient over-voltages typically present on the MAINS supply;
NOTE: The normal level of transient over-voltages is impulse withstand (over-

voltage) category II of IEC 60364-4-443;
g. Pollution degree 2.
Normally only nonconductive pollution occurs.
53
Temporary conductivity caused by condensation is to be expected.
Typical of an office or laboratory environment
54
Routine Maintenance
Responsibility
To preserve the life and efficient operation of the equipment it is important that the
equipment is properly maintained. Regular maintenance of the equipment is the
responsibility of the end user and must be performed by qualified personnel who
understand the operation of the equipment.
General
In addition to regular maintenance the following notes should be observed:
1. The equipment should be disconnected from the electrical supply when not in
use.
2. Check the operation of the RCD by pressing the TEST button. The RCD must
trip when the button is pressed. If the RCD does not trip or it trips before
pressing the test button then it must be checked by a competent electrician
before the equipment is used.
3. When the equipment is not in use the conductivity probes (C1, C2 and C3)
should ideally be left full of de-ionised water, this will help to maintain the
accuracy of the conductivity probes when returned to normal operation.
4. To preserve the life and the efficient running of the equipment it is important
to keep the equipment clean. Refer to the section Cleaning After Use for
further information.
5. After prolonged use it may be necessary to adjust the screws that limit the
vertical movement of the rotor. Adjustment will be necessary if there is
excessive vertical movement of the rotor allowing the solid carrier to escape
between the wall of the rotor and the base plate. The adjusting screws are
accesible by removing the top cover on the central hub after releasing the two
screws that secure the hub to the base. Note that if these screws are
overtightened the excessive friction will cause the protection clutch to slip
resulting in no drive to the rotor.
6. At regular intervals inspect the electrodes inside the conductivity probes (C1,
C2 and C3) for contamination. Contamination of the glass wall or metal
electrodes inside the probes indicates that salt is also contaminating the
pipework and needs to be removed for satisfactory operation of the
equipment. If there is a need to remove contamination then the system should
be flushed through with a solution of 0.1M hydrochloric acid at room
temperature, this will remove any contamination from the probes and
pipework. After flushing with acid the system should be thoroughly flushed
through with clean water to remove all traces of the acid.
If the probes are removed for cleaning then users should avoid using sharp
objects or abrasives to clean the probes since the coating of the electrode
plates and connecting wires in the probes may be damaged. The plated
surface of the electrodes and their connecting wires should be a uniform colour
and free from any blemishes or scratches since this can cause erratic
measurement results. If any damage to the coating is found it will be necessary
to replace the electrode.
55
7. At regular intervals inspect the filters (9a, 9b and 9c) for blockage of the wire
mesh. The filter can be opened for cleaning by unscrewing the two halves of
the body (lugs on each half of the body assist in opening the filter).
8. At regular intervals inspect the filter in the transparent bowl of the pressure
regulator for blockage. The filter can be removed for cleaning by unscrewing
the bowl from the body of the pressure regulator.
Configuration of the PID Temperature Controllers

If, for any reason, the configuration of the controller has been altered or corrupted it
will be necessary to restore the settings as follows:
a. Make sure that the heater switches on the front of the console are switched
off then switch on the console. After the initialisation checks each of the
controllers should display the process temperature.
b. To access the User Menu press the scroll key for 3 seconds then release the
key. The code for the first parameter will be displayed, alternating with the set
value. To change the value press the increase or decrease key as required to
achieve the requied value. When the value is set correctly press the scroll key
to check the other settings within the User Menu.
c. To access the Setup Menu press the scroll key and decrease key
simultaneously then release both keys. The code for the first parameter will
be displayed, alternating with the set value. To change the value press the
increase or decrease key as required to achieve the required value. When the
value is set correctly press the scroll key to check the other settings within the
Setup Menu.
d. Once the desired figure has been entered the scroll key will access the next
parameter for checking. The display will automatically revert to the sensed
temperature if no key is pressed for a period of approximately 2 minutes. To
return to normal operation immediately press the increase and decrease
keys simultaneously then release both keys.
The suggested values for the controller parameters are as follows:
CODE PARAMETER UNITS SETTING
USER MENU
o
A1.SP Alarm set point C 60
o
ShiF Shift process value C 0.0
o
Pb 1 Proportional band output 1 C 72.0
ti 1 Integral time Sec 28
td 1 Derivative time Sec 5

o
A1.Hy Hysteresis alarm 1 C 1
56
Routine Maintenance
PL 1 Power limit Output 1 100
SETUP MENU
FunC Function complexity level FuLL
Conn Communication interface type nonE
in 1 Input 1 Sensor type selection 0-1V
in1.u Input 1 unit selection Pu
dP 1 Input 1 decimal point selection no.dP
in1.L Input 1 low scale value 0
in1.H Input 1 high scale value 60
in 2 Input 2 Signal type selection nonE
out 1 Output 1 Function reVr
o1.ty Output 1 Signal type SSrd
CYC 1 Output 1 cycle time Sec 1
o1.Ft Output 1 Failure transfer mode BPLS
out 2 Output 2 Function nonE
A1.Fn Alarm 1 Function PV1.H
A1.nd Alarm 1 Operation norn
A1.Ft Alarm 1 Failure transfer mode on
A2.Fn Alarm 2 Function nonE
EiFn Event input function nonE
PVnd PV mode selection PV 1
FiLt Filter damping time constant Sec 0.5
SELF Self tuning function nonE
SLEP Sleep mode function selection nonE
SP.nd Set point mode selection SP1.2
SP1.L SP1 Low scale value 0
57
SP1.H SP1 High scale value 60
diSF Display format PV
SEL1 Select 1st parameter nonE
SEL2 Select 2nd parameter nonE
SEL3 Select 3rd parameter nonE
SEL4 Select 4th parameter nonE
SEL5 Select 5th parameter nonE
Maintenance of the UOP4 MkII does not require access to the electrical circuits or
components inside the console. However in the event of an electrical problem or
recalibration of the conditioning circuits, it may be necessary for a competent
electrician to gain access to the console as follows:
Ensure that the console is disconnected from the electrical supply (not just switched
off) before removing the cover from the console.
Unscrew the fixings, which retain the blue metal cover then carefully remove the
cover itself. It will be necessary to disconnect the earth lead attached to the cover.
An electrical wiring diagram showing the mains and DC electrical circuits inside the
console is included to assist in fault finding.
Recalibration of the Thermocouple Conditioning Circuits

This procedure requires access to the circuits inside the console and must be carried
out by a competent electrician.
The thermocouple conditioning circuits (which provide readings from the

thermocouples fitted to each of the stages) are located on a PCB inside the console.
These circuits are calibrated before despatch and should not require recalibration.
However, should recalibration become necessary the following procedure should be
used:
a. Ensure the equipment has been connected to the electrical supply and
switched on for at least 20 minutes before re-calibrating the temperature
conditioning circuits. Re-calibration can be effected using a thermocouple
calibrator or using the thermocouples themselves immersed in ice and hot
water (the PID controllers are limited to a maximum of 60oC).
b. Remove the blue cover from the console as described above then identify the
circuit board with the temperature adjustment potentiometers on it (see
Figures 6 & 7 in the equipment diagrams).
c. If using a thermocouple calibrator, disconnect the appropriate thermocouple

from the socket adjacent to the pump then connect the calibrator to the
vacant socket. If using ice and hot water, remove the thermocouple from the
quick release fitting by pushing back the grey collar while pulling the
thermocouple (do not remove the thermocouple by pulling the lead).
58
Routine Maintenance
d. To set the zero point on one of the temperature circuits the user should
connect the calibrator and set the output to 0oC or place the thermocouple
into a beaker of water and crushed ice as appropriate. Once the temperature
reading on the appropriate PID controller has stabilised the user should
identify the appropriate zero potentiometer (see Figure 7 in the equipment
diagrams) and adjust it to give a reading of 0oC.
e. To set the span of the thermocouple set the output from the calibrator to 60oC
or place the thermocouple into a beaker of hot water at approximately 60oC,
along with a thermometer. Once the temperature has stabilised the span
potentiometer should be adjusted to give the temperature of the liquid on the
relevant PID controller display.
f. Repeat the adjustment of the zero and span potentiometers until no further
adjustment is necessary.
g. Having calibrated one of the thermocouples, the process can be repeated for
any of the other thermocouples as necessary. When the calibration is
complete the thermocouples can be refitted to the equipment and the console
cover must be replaced.
Recalibration of the Conductivity Conditioning Circuits

This procedure requires access to the circuits inside the console and must be carried
out by a competent electrician.
The conductivity conditioning circuits (which provide readings from the four
conductivity probes fitted to each of the three solvent stages and the miscella
collection stage) are located on a single printed circuit board located inside the
console. These circuits are calibrated before dispatch and should not require re-
calibration. However, should re-calibration become necessary the following
procedure should be used:
a. Ensure the equipment has been connected to the electrical supply and
switched on for at least 20 minutes before re-calibrating the conductivity
conditioning circuits. Re-calibration can be effected using a reference solution
with a typical conductivity of 80 mS. It will be necessary to adjust the
temperature of the reference solution or adjust the actual conductivity reading
to compensate for any temperature difference from its calibration temperature
using the table supplied with the solution.
b. Remove the blue cover from the console as described above then identify the
circuit board with the conductivity adjustment potentiometers on it (see Figure
8 in the equipment diagrams).
c. Disconnect the four conductivity probes by unplugging connector 8 from the

conductivity circuit board. (Refer to Figure 8 in the equipment diagrams which
shows the position of conn 8.)
d. Connect an AC Volt meter (range AC mV) to one of the pairs of conductivity

probe pins on the circuit board (refer to Figure 8 in the equipment diagrams
which shows the position of the pins). Adjust potentiometer VR2 on the PCB
to give a reading of 50 mV (RMS) on the voltmeter (probe excitation voltage
for the four probes), then disconnect the voltmeter.
59
e. Reconnect the plug for the four probes and then carefully remove the probes
to be calibrated by disconnecting the flexible tubing and removing the glass
body from its support.
f. Fill a small beaker with the conductivity reference solution. Immerse the probe
to be calibrated and a suitable thermometer in the reference solution. It is
important to make sure that the conductivity probe is completely full of the
liquid and to allow the probe to soak in the solution for a few minutes to allow
the temperature to stabilise.
g. From the table supplied with the conductivity reference solution determine the
actual conductivity of the solution at the measured temperature. Set the
selector switch (on the front of the console) to display the conductivity of the
probe being calibrated. Adjust the appropriate potentiometer to give a reading
on the display to match the conductivity of the reference solution (to identify
the correct potentiometer refer to Figure 8 in the equipment diagrams).
Having calibrated one of the probes, the process can be repeated for any of the other
probes as necessary. When the calibration is complete the probes can be refitted to
the equipment and the console cover must be replaced.
RCD Test
Test the RCD by pressing the TEST button at least once a month. If the RCD button
does not trip when the Test button is pressed then the equipment must not be used
and should be checked by a competent electrician.
60
Laboratory Teaching Exercises
Index to Exercises
Exercise A: Batch Extraction - Open Loop
Exercise B: Batch Extraction - Closed Loop
Exercise C: Single Stage Continuous Extract
Exercise D: Two Stage Continuous Extraction
Exercise E: Three Stage Continuous Extraction
Project Work
When using the appropriate Armfield Teaching Software (optional accessory) the
Teaching Exercises may differ slightly and it is suggested that reference is made to
the help text incorporated in the software rather than this manual.
Introduction and Background

Solid liquid extraction appears to be a relatively simple process in which a solvent
percolates through a bed of solid particles, dissolving, and therefore extracting some
of the soluble component from the solid particles (the solid carrier).
The overall extraction process involves a series of steps, some of which are more
complex individual operations as follows:
a. Solvent is applied to the particles of solid that are to be extracted from.
b. The solvent permeates through the bed of solid particles.
c. The soluble component on the surface of the solid particles is washed off
easily by the solvent.
d. The soluble component contained within the solid particles is gradually

dissolved by the solvent. The solute created diffuses through the pores in the
solid to the outside of the particle.
e. The solute at the surface of the particle diffuses into the static layer of solvent
in contact with the particle.
f. The concentrated solute adjacent to the solid particles mixes with the main
bulk of the solution.
g. The final miscella (solvent containing the soluble component) is drained from
the bed of solid particles and collected for further processing.
h. The spent solid material is removed from the process.
In extraction processes the degree of extraction of the soluble component is heavily

dependent on the concentration of the solvent and the amount of the soluble
component present. When the solvent is fresh and there is a large amount of soluble
component available there will be a high degree of extraction. Conversely when the
solvent has a high solute content and the soluble component in the solid is low (solid
exhausted) a point can be reached where there is no net extraction taking place and
an equilibrium is reached.
61
There are two obvious ways in which an equilibrium state can happen:
a. The solvent can become saturated with the solute so that there is no longer
any net transfer of the soluble component to the solvent, regardless of the
amount of the soluble component available to be extracted. It is possible to
increase the extraction in this case by increasing the temperature, which
allows the solvent to absorb more solute. Alternatively the solute
concentration in the solvent can be reduced by adding fresh solvent. Note
that increasing the concentration of the soluble component in the solid by
adding fresh solids will have no effect if the solvent is saturated.
b. When the soluble component content of the solid material is low, a point may
be reached where the concentration of the solute at the surface of the
particles may have the same concentration as the main body of solvent. The
result is no net transfer of solute to the main body of the solvent. In this case
a temperature change will have little effect. To extract more solute it will be
necessary to generate a difference in concentrations. Adding fresh solvent
will reduce the concentration in the main body of solvent and so generate a
difference in concentration that will allow the solute to move from the solid
particles to the main body of solvent by osmosis. Alternatively increasing the
content of soluble component by adding fresh solids to the process will
increase the solute concentration in the contact solvent and so generate the
difference in concentration that is needed for transfer of the solute to the main
body of the solvent.
The principles outlined above refer to solid liquid extraction in general and can be
applied to both the continuous and batch configurations of the UOP4 MkII.
Nomenclature
Name Symbol Unit
Speed setting of first stage pump N1 % of max
Speed setting of second stage pump N2 % of max
Speed setting of third stage pump N3 % of max
Speed setting of feeder NF % of max
Speed setting of rotor NR % of max
Volume flowrate of final miscella F4 m3/hr
Mass flowrate of solvent in first stage

M1 kg/hr
(From N1)
Mass flowrate of solvent in second

M2 kg/hr
stage (From N2)
62
Laboratory Teaching Exercises
Mass flowrate of solvent in third

M3 kg/hr
stage (From N3)
Mass flowrate of solvent lost in the

ML kg/hr
process
Mass flowrate of solids into process

MS kg/hr
(From N4)
Output of KHCO 3 from process MO kg/hr
Temperature of fresh solvent

T1 C
entering stage 1
Temperature of first miscella entering

T2 C
stage 2
Temperature of second miscella

T3 C
entering stage 3
Temperature of final miscella exiting

T4 C
process
Temperature of solvent in fresh

TS C
solvent tank
Conductivity of solvent entering

C1 mS
stage 1

C2 mS
stage 2

C3 mS
stage 3
Conductivity of final miscella exiting

C4 mS
process
Initial conductivity of the solvent

(closed loop batch extraction only, Cinit MS
from C1)
Concentration of KHCO 3 in solid ConcS %wt
Concentration of KHCO 3 in first Conc2

%wt
miscella (From C2)
Concentration of KHCO 3 in second Conc3

%wt
miscella (From C3)
63
Concentration of KHCO 3 in final Conc4

%wt
miscella (From C4)
Percentage of KHCO 3 extracted from

%
solids
Specific heat of solvent Cp kJ/kgoC
Density of solvent kg/m3
Power input to first stage solvent

Q1 W
heater
Power input to second stage solvent

Q2 W
heater
Power input to third stage solvent

Q3 W
heater
Total power input to process Qt W
Graphs of Concentration
64
Exercise A: Batch Extraction - Open Loop
Objective
To demonstrate the operation of the batch extractor system when configured for
open loop extraction and to show how the concentration of solute in the solvent
changes with processing time.
Method
In open loop extraction fresh solvent is fed into the batch extractor vessel
continuously and the miscella leaving the process is monitored continuously. By
measuring the conductivity and temperature of the solvent stream at regular intervals
as it exits the extractor it is possible to monitor the extraction of the Potassium
Bicarbonate (KHCO 3 ) from the batch of material.
Equipment Required
UOP4 MkII Solid Liquid Extraction Unit
Solid carrier - porous polymer pellets containing Potassium Bicarbonate (prepared in

advance)
Stopwatch (not supplied)
Optional Equipment
None
Theory/Background
Open loop extraction on a batch of material is not a usual configuration but it
interesting to observe the effect when fresh solvent is fed continuously through the
batch of material and this concept can be applied to each individual stage in the
continuous process which will be studied in a later exercise. It is possible to make the
following observations about this configuration.
a. In most batch extraction systems both the concentration of the solvent and
the available soluble component reduce as the soluble component is
extracted by the solvent. Open loop batch extraction differs in that while the
available soluble component reduces, the concentration of solvent does not,
because of this there will always be a difference of solute concentration
between the contact solvent and the main body of the solvent (so long as
there is any soluble component left). The difference between the
concentrations means that in theory 100% extraction can be achieved.
b. In an open loop system the rate of extraction will be dependent on the solvent
temperature, the solvent flow rate and the amount of soluble material left in
the particles. The extraction rate will not be affected by changes in solvent
concentration as the process progresses because the solvent entering the
batch vessel is always fresh solvent. If the solvent flow rate and temperature
are constant the rate of extraction will be related to the amount of extractable
material remaining, thus the rate of extraction should progressively slow
down.
Because extraction commences as soon as the solvent contacts the solid particles it
will be necessary to preheat the solvent to the required operating temperature before
allowing it to flow through the batch extraction vessel. This simple precaution will
65
allow the transient changes in conductivity to be monitored throughout the process

without additional transients during start-up due to changing solvent temperature.
Equipment Set Up
a. Configure the system for open loop batch extraction as depicted in the flow
diagram below. Water from the fresh solvent tank is pumped upwards through
the first stage heater then passes upwards through the batch extractor before
overflowing to the final miscella tank.
Procedure
Start Up
a. Check that the UOP4 MkII is switched off, all switches are set to off and all
rotary controls are set to minimum on the front panel of the console.
b. Fill the fresh solvent tank with clean water.
c. Place the cloth over the batch vessel then insert the filling tube so that the
cloth lines the vessel. Pour the prepared solid carrier (porous polymer pellets
containing Potassium Bicarbonate) into the filling tube then gradually
withdraw the filling tube to leave the vessel full of the prepared solid carrier.
Ensure that the top of the sample does not protrude above the side tapping at
the top of the vessel.
d. Open the bypass valve (lever in line with valve body) at the base of the
extractor vessel to divert the solvent to the final miscella tank.
e. Plug in and switch on the UOP4 MkII. Adjust the setpoint of controller 1 to
match the temperature indicated on the display (to avoid excessive overshoot
when heating is required).
66
Exercise A
f. Set pump speed one to give the required flow rate (typically 5.0 on the speed
control, approximately 6 litres per hour).
g. Switch on heater ONE ONLY then adjust the set point on the stage 1
temperature controller to 40oC. Note that the heater must only be on when
there is a steady flow of liquid through the heater. Monitor temperature T1
(indicated on the stage 1 temperature controller) and wait until it has
stabilised. Once the temperature of the water has stabilised the extraction can
commence as follows.
Extraction
Before commencing the extraction it will be necessary to organise recording of the
required data. The following readings will be required:
T1 Temperature of solvent entering the batch vessel
T4 Temperature of solvent leaving the batch vessel
C1 Conductivity of solvent entering the batch vessel (will remain constant)
C4 Conductivity of solvent leaving the batch vessel
In manual operation it will be necessary to switch the multi function display on the
console between C1, C4 and T4 in order to take down these readings on a regular
basis (typically once per minute) as the process progresses. T1 is indicated
continuously on the stage 1 temperature controller.
Start the stopwatch as you close the bypass valve at the bottom of the extractor
vessel to feed the solvent upwards through the vessel. When the miscella (solvent
containing the extract) reaches the overflow at the top of the vessel it will flow into the
miscella tank (it may be necessary to disconnect the flexible tube briefly to allow the
tube to prime). Once the sensors have filled with liquid the data can be recorded at
regular intervals until the conductivity reading C4 falls towards to zero.
When the process has finished switch off the heater before the solvent pump.
If time permits the exercise can be repeated at different solvent flowrates or solvent
temperatures to investigate their effect on the rate of extraction. It will be necessary
to replace the exhausted solid carrier in the extractor with prepared solid carrier.
Presentation of Results and Analysis

The first stage in analysing the results is to turn the pairs of conductivity and
temperature readings (C4 C1 with T4) into values of percentage weight KHCO 3 ,
this is done by linear interpolating between points on the conversion graph which is
presented in Graphs of Concentration.
Having converted the values produce a graph showing the percentage weight of
extracted material in the miscella against time.
Note: When using the UOP4 MkII with the optional PC based interface and software
(UOP4MkII-303IFD) the conversion of the data and the plotting of the graph is carried
out automatically in real time.
Comment on the profile of the graph in relation to the theory of open loop extraction
eg.
67
a. Does the miscella concentration tend to zero with increasing time or does it
reach an equilibrium point?
b. Does the rate of extraction decrease as more of the soluble component is

extracted?
When considering the above it may be necessary to take into account factors such
as fluctuating temperature of the solvent or washing of soluble material from the
surface of the solid particles as the processing starts.
If results were obtained at different solvent flowrates or different solvent temperatures

compare the graphs of concentration against time and comment on the effect of
flowrate and/or temperature.
68
Exercise B: Batch Extraction - Closed Loop
Objective
To demonstrate the operation of the batch extractor system when configured for
closed loop extraction and to compare the results with predicted values.
Method
In closed loop extraction the solvent draining from the batch extractor is returned to
the inlet of the extractor so that the same solvent is continuously recycled. By
measuring the conductivity and temperature of the solvent stream at regular time
intervals it is possible to monitor the extraction of the Potassium Bicarbonate
(KHCO 3 ) from the batch of material.
Equipment Required

advance).
Measuring cylinder (not supplied)
Optional Equipment
None
Theory/Background
In closed loop batch extraction the fixed batch of extractable material is processed by
a fixed amount of solvent, which is continuously circulated through the extractor. It is
possible to make the following observations about this configuration.
a. In this system the solute concentration in the main body of the solvent rises
as the process proceeds and the solute content of the solvent in contact with
the particles declines progressively with time until they reach a similar
concentration and an equilibrium is found (assuming that the solvent does not
become saturated before equilibrium is reached).
b. When equilibrium is reached, the concentration of solute in the solvent will

depend on the volume of solvent used in the process and the amount of
soluble component initially in the solid.
c. The temperature of the solvent will have an effect on the speed of the
extraction but it will not have any effect on the final concentration.
d. The flow rate of the solvent will have an effect on the speed of the extraction
but it will not have any effect on the final concentration.
Equipment Set Up
Configure the system for closed loop batch extraction as depicted in the flow diagram
below. Water from the final miscella tank is pumped upwards through the first stage
heater then passes upwards through the batch extractor before overflowing back into
the final miscella tank for recirculation
69
Note: When operating with a small volume of solvent it may be easier to place a
small beaker, containing the solvent, inside the final miscella tank to increase the
depth of the solvent and submerge the end of the flexible tubing to the pump suction.
When setting up the closed loop batch configuration it will be necessary to choose
the volume of solvent to use in the loop. If a small volume of solvent is used the
concentration of KHCO 3 in the miscella will tend to be higher but the percentage
extraction will be lower. If the volume of the solvent is very low the solvent may
become saturated before equilibrium between the contact solvent and the main body
of the solvent is reached.
Method for choosing the volume of solvent
Choose an equilibrium concentration that is less than the saturation point at ambient
temperature (typically 7% wt).
E.g. With 700 ml of porous pellets in the batch extractor containing 117 gm of
Potassium Bicarbonate a solution of 7% by wt is achieved with a batch of 1.67 litres
of water.
Measure the mass of the solids that are to be processed in the batch extractor and
calculate the mass of KHCO 3 in the solids using the known proportions of the soluble
and non-soluble components (see Preparation of Materials).
Calculate the mass of water that would produce the required percentage weight
given the mass of KHCO 3 in the solids (this assumes that equilibrium is reached with
a uniform concentration in the contact solvent and the main body of the solvent).
Check that the calculated mass and therefore volume of water will fill the pump,
heater, flexible tubing, sensors, overcome the static hold up of the solids and be
enough for there to be a workable liquid level in the miscella tank. If there is not
enough water the planned percentage weight will need to be reduced.
70
Exercise B
Procedure
Start Up
Check that the UOP4 MkII is switched off, all switches are set to off and all rotary
controls are set to minimum on the front panel of the console.
Ensure that the flexible tubing connected to the pump suction is fully submerged in
the solvent and will not float to the top of the liquid causing intermittent liquid flows.
Place the prepared solid carrier in a measuring cylinder and note the level. Place the
cloth over the batch vessel then insert the filling tube so that the cloth lines the
vessel. Pour the prepared solid carrier into the filling tube then gradually withdraw the
filling tube to leave the vessel full of the prepared solid carrier. Ensure that the top of
the sample does not protrude above the side tapping at the top of the vessel. Note
the level of solid carrier remaining in the measuring cylinder to determine the amount
of solid carrier in the extractor.
Fill the final miscella tank, or beaker if appropriate, with the required volume of clean
water.
Open the bypass valve (lever in line with valve body) at the bottom of the extractor
vessel to divert the solvent back to the final miscella tank.
Plug in and switch on the UOP4 MkII. Adjust the setpoint of controller 3 to match the
temperature indicated on the display (to avoid excessive overshoot when heating is
required).
Set pump speed three to give maximum flow rate (typically 13.5 litres per hour) and
check that the volume of solvent available will be enough for the solvent loop to
operate when the batch extractor is introduced later on.
Switch on heater THREE ONLY then adjust the set point on the stage 3 temperature
controller to 40oC. Note that the heater must only be on when there is a steady flow
of liquid through the heater. Monitor temperature T3 (indicated on the stage 3
temperature controller) and wait until it has stabilised. Measure and record the initial
conductivity of the solvent Cinit indicated as C3. Once the temperature of the water
has stabilised the extraction can commence as follows.
Extraction
T3 Temperature of solvent entering the batch vessel
T4 Temperature of solvent leaving the batch vessel
C3 Conductivity of solvent entering the batch vessel
C4 Conductivity of solvent leaving the batch vessel
basis (typically once per minute) as the process progresses. T3 is indicated
continuously on the stage 3 temperature controller.
71
Start the stopwatch as you close the bypass valve at the bottom of the extractor
vessel to feed the solvent upwards through the vessel. When the miscella (solvent
containing the extract) reaches the overflow at the top of the vessel it will flow into the
miscella tank
Once the sensors have filled with liquid the data can be recorded at regular intervals
until the conductivity readings C3 and C4 are the same no further extraction is
occurring.
When the process has finished switch off the heater before the solvent pump.
If time permits the exercise can be repeated with a different initial volume of solvent
to investigate the effect on the final concentration. Different solvent flowrates or
solvent temperatures could also be tried to investigate their effect on the rate of
extraction. It will be necessary to replace the exhausted solid carrier in the extractor
with prepared solid carrier.
Results and Analysis

The first stage in analysing the results is to turn the pairs of conductivity and
temperature readings (C3 Cinit with T3 and C4 Cinit with T4) into values of
percentage weight KHCO 3 . This is done by linear interpolating between points on the
conversion graph which is presented in Graphs of Concentration.
Having converted the results produce a graph showing the percentage weight of
extracted material in the final miscella against time. Also produce a graph of
difference in percentage weight between solvent entering the batch vessel (Conc3
from C3) and solvent leaving the batch vessel (Conc4 from C4) against time.
Note: When using the UOP4 MkII with the optional PC based interface and software
the conversion of the data and the plotting of the graphs is carried out automatically
in real time.
Comment on the profile of the graphs in relation to the theory of closed loop
extraction eg.
a. Does the miscella concentration tend reach an equilibrium point as the

process proceeds?
b. How does the equilibrium concentration of the KHCO 3 compare with the
predicted value?
When considering the above it may be necessary to take into account factors such
as fluctuating temperature of the solvent or washing of soluble material from the
surface of the solid particles as the processing starts.
If results were obtained with a different initial volume of solvent or differing solvent
flowrate/temperature compare the graphs of concentration against time and comment
on the effect of volume, flowrate and/or temperature.
72
Exercise C: Single Stage Continuous Extract
Objective
To demonstrate the operation of the extractor when configured for single stage
continuous solid liquid extraction and to assess the efficiency of the process.
Method
By measuring the conductivity and temperature of the final miscella as it leaves the
process it is possible to find the percentage weight of extracted Potassium
Bicarbonate (KHCO 3 ) in the final miscella and therefore the degree of extraction
taking place. Similar measurements of the fresh solvent entering the process allow
the efficiency of the process to be investigated.
Equipment Required

advance).
Measuring cylinder, typically 250 ml (not supplied)
Optional Equipment
None
Theory/Background
When the system is configured for single stage continuous extraction the fresh solid
material is fed into the system using the spiral material feeder. The solid material is
moved through the system by the rotating cell and fresh solvent sprinkled onto it
continuously drains through it. (Refer to the flow diagram in Equipment Set-up
below.) Once the solid material has been processed it discharges into the extracted
solids tank. The miscella containing the soluble component is collected in the final
miscella tank.
Single stage continuous extraction is an open loop system and the rate of extraction
will be dependent on variables such as the solvent temperature, the solvent flow rate,
the solids feed rate, the amount of solute in the dry solid and the characteristics of
the contact between the solid particles and the liquid.
Because the extraction is continuous the process will stabilise after an initial period;
however, transient changes as the process starts up and stabilises will be of interest,
as well as the readings when steady state is achieved.
The % weight of KHCO 3 in the final miscella can be determined from measurements
of temperature and conductivity of the final miscella using the conversion graphs in
Graphs of Concentration.
When choosing the operating parameters of an extraction process the main

objectives are as follows:
a. To make the final miscella as concentrated as possible to minimise the cost

of further processing when recovering the soluble component from the
solvent.
73
b. To use the minimum amount of solvent to reduce operating costs.
c. To lose the minimum amount of solvent solvent retained in the solids after
processing
d. To maximise product output to process the required amount of product in

the minimum time.
e. To extract the maximum percentage of the valuable soluble component from

the feed any soluble component remaining in the solids after processing is
wasted.
f. To minimise the energy input to the process (operating at the lowest

practicable temperature) to reduce operating costs.
It is clear that all of these objectives are inter-related and that any attempt to
compare how a system performs with different combinations of settings would require
a comprehensive series of tests to determine the individual effects of each
parameter. Such a test is suggested in the Project Work section.
The efficiency of the process can be assessed by considering the following

parameters:
Concentration of the final miscella.
Amount of soluble component extracted.
Amount of soluble component remaining in the solids after processing.
Amount of solvent remaining in the solids after processing.
Energy required to perform the extraction.
Equipment Set Up
Configure the equipment for single stage continuous extraction as depicted in the
flow diagram below. Water from the fresh solvent tank is pumped upwards through
the first stage heater and sprinkled onto the surface of the solid material which is
moved beneath the sprinkler by the rotor. The miscella draining from the bottom of
the rotor is collected in the final miscella tank.
74
Exercise C
Configuration for Single stage continuous extraction
Procedure
Start Up
Fill the fresh solvent tank with clean water.
Fill the hopper of the spiral feeder with prepared solid carrier.
Plug in and switch on the UOP4 MkII. Adjust the setpoint of controller 1 to match the
temperature indicated on the display (to avoid excessive overshoot when heating is
required).
Set pump one to give the required flow rate (typically 5.0 on the speed control,
approximately 6 litres per hour).
When solvent appears at the sprinkler bar measure and record the temperature TS of
the solvent direct from the fresh solvent tank indicated on the stage 1 temperature
controller (T1) before the heater is switched on.
Switch on heater ONE ONLY then adjust the set point on the stage 1 temperature
controller to 40oC and allow the temperature to stabilise. Note that the heater must
only be on when there is a steady flow of liquid through the heater.
Monitor temperatures T1 and T4 (T1 indicated on the stage 1 temperature controller,

T4 indicated on the panel meter via the selector switch) and wait until the
temperatures have stabilised. Once the temperatures have stabilised the extraction
can commence as follows.
75
Extraction
T1 Temperature of solvent entering rotor
T4 Temperature of final miscella
C1 Conductivity of solvent entering the rotor (will remain constant)
C4 Conductivity of final miscella
basis (typically once per minute) as the process progresses.
Start the rotor cell and adjust the speed control to give the required rotational speed
(typically 5.0 on the speed control, approximately 2 revs per hour).
Turn on the spiral material feeder and adjust the speed control to give the required
depth of material in the cells of the rotor (typically 30 -50% full).
When the solid material reaches the aperture in the base at the rear of the extractor it
will be necessary to turn on the spray nozzle so that the material is washed into the
extracted solids tank. Adjust the position of the nozzle and pressure regulator as
required to prevent overspray.
Note: It will be necessary to refill the hopper with prepared solid carrier as the
exercise proceeds.
Start the stopwatch and commence recording the above readings when the first cell
containing the solid material reaches the sprinkler bar.
As the solvent extracts the KHCO 3 from the solid carrier the output from conductivity
probe C4 will rise and eventually stabilise.
Note: When the system has achieved steady state small cyclic variations will be
observed in the reading from conductivity probe C4 as the individual cells of the rotor
present fresh solid material to the solvent stream. This effect can be observed more
clearly when logging results continuously using the optional PC logging interface and
software (Armfield product code UOP4MkII-303IFD).
Readings at steady state

Once the system has reached steady state the following measurements should be
recorded:
Feeder speed setting NF %
Rotor speed setting NR %
Pump 1 speed setting N1 %

o
Temperature of solvent at stage 1 T1 C
76
Exercise C
Conductivity of solvent at stage 1 C1 mS

o
Temperature of final miscella T4 C
Conductivity of final miscella C4 mS
Using a measuring cylinder and stopwatch collect a timed sample of the final miscella
to determine the flowrate of solvent leaving the process (F4 litres/hr).
When shutting down the process switch off the heater before the solvent pump.
If time permits the exercise can be repeated at different solvent flow rates, or solvent
temperatures to investigate their effect on the rate of extraction and the efficiency of
the process.
Similarly, the effect of the solid feed rate and/or the rotor speed can be investigated.

From the measurements taken while the process was stabilising calculate the
concentration of the KHCO 3 in the final miscella by converting the readings of (C4
C1) and T4 into values of percentage weight KHCO 3 (using the conversion graphs in
Graphs of Concentration).
Plot the graph of percentage weight of extracted material in the final miscella against
time. Comment on the shape of the graph as the process stabilises.
Using the calibration graphs for the equipment where appropriate (refer to
Operational Procedures for details) convert the above measurements taken at steady
state as follows:
Mass Flowrate of solid material (from NF using calibration

MS kg/hr
graph)
Mass Flowrate of solvent entering the process (from N1

M1 kg/hr
using calibration graph)
Mass Flowrate of final miscella (= F4 x density of the

M4 kg/hr
solvent)
Loss of solvent in the process (= M1 M4) ML kg/hr
Concentration of KHCO 3 in the solid (from preparation data) ConcS %wt
Input of KHCO 3 to the process (= MS x ConcS/100) MI kg/hr
Concentration of KHCO 3 in the miscella (from C4 C1 and

Conc4 %wt
T4 using graph)
Output of KHCO 3 from the process (= M1 x Conc4/100) MO kg/hr
Percentage of KHCO 3 extracted from the solids (= 100 x %
77
MO/MI)
Energy input to the process (primarily heating of the

solvent) (= 0.277 x M1 x (T1 TS) x Cp)
Q1 Watts
Note factor of 0.2777 for M1 in kg/hr and Cp in kJ/kg/K
Comment on the efficiency of the process by considering the magnitude of the

calculated values obtained when the process has achieved steady state (the
appropriate parameters are suggested in the Theory section above).
If results were taken under different operating conditions compare the results and
comment on the effect of the changes on the efficiency of the process.
78
Exercise D: Two Stage Continuous Extraction
Objective
To demonstrate the operation of the solid liquid extractor when configured for two
stage continuous extraction in counter current flow, to determine the contribution of
each stage in the extraction process and to compare the results with those obtained
from the single stage exercise.
Method
By measuring the changes in conductivity and temperature of the streams of solvent
at each stage of the process it is possible to find the percentage weight of extracted
Potassium Bicarbonate (KHCO 3 ) in the solvent streams. From this data the user can
determine the degree of extraction that is taking place at each stage.
Equipment Required

advance).
Measuring cylinder, typically 250 ml (not supplied)
Optional Equipment
None
Theory/Background
When the system is configured as a two stage counter current flow extractor the
fresh solid material and the fresh solvent are fed into the system from opposite ends
of the process (refer to the flow diagram below). The solid material is moved through
the system by the rotating cell and the solvent effectively flows through the material
in the opposite direction being pumped to the sprinkler bars in the first and second
stages.
Once the solid material has been processed it discharges into the extracted solids
tank. The miscella containing the soluble component is collected in the final miscella
tank.
In the counter current arrangement the most concentrated solids are processed by
the least concentrated solvent and vice versa. This arrangement is used in industrial
processing because it is generally more efficient than co-current operation. Similarly
two-stage extraction is more efficient than single stage extraction.
Two stage continuous extraction is an open loop system and the rate of extraction
Because the extraction is continuous the process will stabilise after an initial period
however, transient changes as the process starts up and stabilises will be of interest
79
The % weight of KHCO 3 in the first miscella and final miscella can be determined
from measurements of temperature and conductivity of the appropriate miscella
using the conversion graphs in Graphs of Concentration.


solvent.
processing

the minimum time.

wasted.

parameter. Such a test is suggested in the Project Work section.

parameters:
Equipment Set Up
Configure the system for two stage continuous extraction as depicted in the flow
diagram below. Water from the fresh solvent tank is pumped upwards through the
first stage heater and sprinkled onto the surface of the solid material which has
already been processed and moved beneath the sprinkler by the rotor. The first
miscella draining from the bottom of the rotor is pumped upwards through the second
stage heater and sprinkled onto the surface of the dry unprocessed solid material.
The final miscella draining from the bottom of the rotor is collected in the final
miscella tank. The flow of solvent and solid material is countercurrent.
80
Exercise D
Configuration for two stage continuous countercurrent extraction
Procedure
Start Up
Fill the solvent tank with fresh water.
Fill collection trough one (right-hand side) to approximately 20mm depth by pouring
water through the mesh at the base of the rotor.
Pour water into collection trough two (middle trough) until the water drains through
the pipework into the final miscella tank.
Set the speed of pump one to maximum to purge air from the first stage of the
process. When water drips from the first sprinkler bar stop the pump. Set the speed
of pump two to maximum to purge air from the second stage of the process. When
water drips from the second sprinkler bar stop the pump. After priming it may be
necessary to top up the level of water in the first trough to return it to 20mm depth.
Note: the final trough will always run empty.
Once the system has been primed the two pumps can be switched on and adjusted
to run at the desired solvent flow rate (typically setting 4.0 on the speed controls).
The solvent stage system should now be taking liquid from the fresh solvent tank,
cascading it through the two stages via the two pumps and troughs and then draining
it into the final miscella tank.
After the system has been running for a while any imbalance in the stages will be
indicated by a change in level in the first stage collection trough. If the level is falling
reduce the speed of pump two. If the level is rising increase the speed of pump two.
81
Do not adjust the speed of pump one during the exercise. It will be necessary to
check the level at regular intervals and to make small adjustments when required.
Adjust the setpoint of controllers 1 and 2 to match the temperature indicated on the
display (to avoid excessive overshoot when heating is required).
(typically 5 on the speed control, approximately 2 revs per hour).
Put some untreated solid carrier in the hopper of the spiral material feeder.
depth of material in the cells of the rotor (typically 30 - 50% full).
Note: It may be necessary to refill the hopper with untreated solid carrier until the
system has stabilised and extraction can commence.
Allow the cells of the rotor to fill with untreated solid carrier. When the dry material
passes beneath the sprinkler bars it may be necessary to make small adjustments to
pump two to maintain the level in collection trough one.
Measure and record the temperature TS of the solvent direct from the fresh solvent
tank indicated on the stage 1 temperature controller (T1) before the heater is
switched on.
Once the system has settled down and the solvent stages are running in balance
switch on heater ONE then adjust the set point on temperature controller ONE to
40oC. When T1 has stabilised switch on heater TWO then adjust the set point of
temperature controller TWO to 40C. Note that no heater should be switched on until
there is a steady flow of liquid through the heater.
Monitor temperatures T1 and T2 (indicated on the appropriate temperature controller)

and wait until the temperatures have stabilised. When the temperatures have
stabilised the extraction can commence as follows.
Extraction
required data. The following readings will be required to show the transient response
as the system stabilises:
T1 Temperature of solvent entering the first cell of the rotor
T2 Temperature of miscella entering the second cell of the rotor
T4 Temperature of final miscella leaving the second cell
C1 Conductivity of solvent entering the first cell of the rotor (will remain
constant)
C2 Conductivity of miscella entering the second cell of the rotor
82
Exercise D
C4 Conductivity of final miscella leaving the second cell
console between C1, C2, C4 and T4 in order to take down these readings on a
regular basis (typically once per minute) as the process progresses. T1 and T2 are
indicated continuously on the appropriate temperature controllers.
Allow the hopper to empty of untreated solid carrier then fill the hopper with solid
carrier containing the KHCO 3 just as the untreated solid carrier runs out. Start the
stopwatch when the hopper is filled.
Note: It will be necessary to refill the hopper with treated solid carrier as the exercise
proceeds.
As the solvent extracts the Potassium Bicarbonate from solid carrier the outputs from
conductivity probes C2 and C4 will rise and eventually stabilise. Once the system has
reached a steady state the appropriate temperatures and the conductivities can be
recorded.
observed in the readings from conductivity probes C2 and C4 as the individual cells
of the rotor present fresh solid material to the solvent stream. This effect can be
observed more clearly when logging results continuously using the optional PC
logging interface and software (Armfield product code UOP4MkII-303IFD).

recorded:

o
o
o
83
the process.

concentration of the KHCO 3 in the first miscella and final miscella by converting the
readings of C2 C1 with T2 and C4 C1 with T4 into values of percentage weight
KHCO 3 (using the conversion graphs in Graphs of Concentration).
Plot the graph of percentage weight of extracted material in the first miscella and final
miscella against time. Comment on the shape of the graphs as the process
stabilises. What is the contribution of each stage in the process?
state as follows:
Mass Flowrate of solid material (from NF using

MS kg/hr
calibration graph)
Mass Flowrate of solvent entering the process

M1 kg/hr
(from N1 using calibration graph)
Mass Flowrate of final miscella (= F4 x density of

M4 kg/hr
the solvent)
Concentration of KHCO 3 in the solid (from

ConcS %wt
preparation data)
Concentration of KHCO 3 in the first miscella (from

Conc2 kg/hr
C2 C1 and T2 using graph)
Concentration of KHCO 3 in the final miscella (from

Conc4 %wt
Output of KHCO 3 from the process = M1 x

MO kg/hr
Conc4/100)
(= 100 x
Percentage of KHCO 3 extracted from the solids %
MO/MI)
Energy input to stage 1 of the process (primarily

heating of the solvent) (= 0.277 x M1 x (T1 TS) x Q1 Watts
Cp) Note factor of 0.2777 for M1 in kg/hr and Cp in
84
Exercise D
kJ/kg/K

heating of the solvent) (= 0.277 x M2 x (T2 T4) x
Cp)
Note factor of 0.2777 for M2 in kg/hr and Cp in Q2 Watts

kJ/kg/K. Note as temperature of fluid entering the
second stage heater cannot be directly measured
and T4 is taken to be equivalent temperature.
Total energy input to process (= Q1 + Q2) Qt Watts

appropriate parameters are suggested in the Theory section above). Compare the
results obtained with those for single stage extraction (Exercise C) and comment on
the effect of the second stage in the process.
85
Exercise E: Three Stage Continuous Extraction
Note: It is suggested that operators have performed Exercise D (two stage
continuous extraction) and understand the technique for balancing the individual
stages before attempting to operate the more complex three stage process described
in this exercise.
Objective
To demonstrate the solid liquid extractor when configured for three stage continuous
extraction in counter current flow, to determine the contribution of each stage in the
extraction process and to compare the results with those obtained from the single
and two stage exercises.
Method
By measuring the changes in conductivity and temperature of the streams of solvent
at each stage of the process it is possible to find the percentage weight of extracted
Potassium Bicarbonate (KHCO 3 ) in the solvent stream at each stage. From this data
the user can determine the contribution that each stage is making in the extraction
and the degree of extraction that is taking place.
Equipment Required

advance).
Measuring cylinder approximately 250 ml (not supplied)
Optional Equipment
None
Theory/Background
The three-stage process is similar to the two-stage process demonstrated in Exercise
D with solvent and solid material passing continuously through the process in
opposite directions. The additional stage improves the efficiency of the process but
the balancing of the stages is made more difficult because the flow of solvent in the
later stages are both affected by the flow of solvent in the first stage and the flow of
solvent in the second stage is also affected by the flow of solvent in the third stage.
In the counter current arrangement the most concentrated solids are processed by
the least concentrated solvent and vice versa. This arrangement is used in industrial
processing because it is generally more efficient than co-current operation. Similarly
three-stage extraction is more efficient than two-stage extraction.
Three stage continuous extraction is an open loop system and the rate of extraction
Because the extraction is continuous the process will stabilise after an initial period
however, transient changes as the process starts up and stabilises will be of interest
86
Exercise E
The % weight of KHCO 3 in the first miscella, second miscella and final miscella can
be determined from measurements of temperature and conductivity of the
appropriate miscella using the conversion graphs in Graphs of Concentration.


solvent.
processing

the minimum time.

wasted.

parameter. Such a test is suggested in the Project Work section of this instruction
manual.

parameters:
Equipment Set Up
Configure the system for three stage continuous extraction as depicted in the flow
diagram below. Water from the fresh solvent tank is pumped through the first stage
heater and sprinkled onto the surface of the solid material which has already been
processed twice. The solid material is moved beneath the sprinklers by the rotor. The
first miscella draining from the rotor is pumped through the second stage heater and
sprinkled onto the surface of the solid material which has been processed once. The
second miscella draining from the rotor is pumped through the third stage heater and
sprinkled on the dry unprocessed solid material. The final miscella draining from the
rotor is collected in the final miscella tank. The flow of solvent and solid material is
countercurrent.
87
Configuration for three stage continuous countercurrent extraction
Procedure
Start Up
Fill the fresh solvent tank with clean water.
Fill collection troughs one (right-hand side) and two (middle) to 20mm depth by
pouring water through the mesh at the base of the rotor.
Pour water into collection trough three (left-hand trough) until the water drains
through the pipework into the final miscella tank.
Set the speed of pump one to maximum to purge air from the first stage of the
process. When water drips from the first sprinkler bar stop the pump. Set the speed
of pump two to maximum to purge air from the second stage of the process. When
water drips from the second sprinkler bar stop the pump. Set the speed of pump
three to maximum to purge air from the third stage of the process. When water drips
from the third sprinkler bar stop the pump.
After priming it may be necessary to top up the level of water in the first and second
troughs to return them to 20mm depth. Note: the final trough will always run empty.
Once the system has been primed the three pumps can be switched on and adjusted
to run at the desired solvent flow rate (typically setting 4.0 on the speed controls).
The solvent stage system should now be taking liquid from the fresh solvent tank,
cascading it through the three stages via the three pumps and troughs and then
draining it into the final miscella tank.
88
Exercise E
After the system has been running for a while any imbalance in the stages will be
indicated by a change in level in the first and/or second stage collection troughs.
Check the right-hand trough (stage 1) first. If the level is falling reduce the speed of
pump two. If the level is rising increase the speed of pump two. Now check the
middle trough (stage 2). If the level is falling reduce the speed of pump three. If the
level is rising increase the speed of pump three. Do not adjust the speed of pump
one during the exercise. It will be necessary to check the levels at regular intervals
and to make small adjustments when required.
Adjust the set point of controllers 1, 2 and 3 to match the temperature indicated on
the corresponding display (to avoid excessive overshoot when heating is required).
(typically 5.0 on the speed control, approximately 2 revs per hour).
Put some untreated solid carrier in the hopper of the spiral material feeder.
depth of material in the cells of the rotor (typically 30 - 50% full).
Note: It may be necessary to refill the hopper with solid carrier until the system has
stabilised and extraction can commence.
Allow the cells of the rotor to fill with untreated solid carrier. When the dry material
passes beneath the sprinkler bars it may be necessary to make small adjustments to
pump two and pump three to maintain the correct levels in the troughs.
Measure and record the temperature TS of the solvent direct from the fresh solvent
tank indicated on the stage 1 temperature controller (T1) before the heater is
switched on.
Once the system has settled down and the solvent stages are running in balance
switch on heater one then adjust the set point on temperature controllers one to
40oC. When T1 has stabilised switch on heater two then adjust the set point on
temperature controller 2 to 40C. When T2 has stabilised switch on heater three then
adjust the set point on temperature controller 3 to 40C Note that no heater should
be switched on until there is a steady flow of liquid through the heater.
Monitor temperatures T1, T2 and T3 (indicated on the appropriate temperature

controller) and wait until the temperatures have stabilised. When the temperatures
have stabilised the extraction can commence as follows.
Extraction
required data. The following readings will be required to show the transient response
as the system stabilises:
T1 Temperature of solvent entering the first cell of the rotor
T2 Temperature of first miscella entering the second cell of the rotor
89
T3 Temperature of second miscella entering the third cell of the rotor
T4 Temperature of final miscella leaving the third cell
C1 Conductivity of solvent entering the first cell of the rotor (will remain
constant)
C2 Conductivity of first miscella entering the second cell of the rotor
C3 Conductivity of second miscella entering the third cell of the rotor
C4 Conductivity of final miscella leaving the third cell
console between C1, C2, C3, C4 and T4 in order to take down these readings on a
regular basis (typically once per minute) as the process progresses. T1, T2 and T3
are indicated continuously on the appropriate temperature controllers.
Allow the hopper to empty of untreated Porosolid carrier then fill the fill the hopper
with solid carrier containing the KHCO 3 just as the untreated solid carrier runs out..
Start the stopwatch when the hopper is filled.
Note: It will be necessary to refill the hopper with treated solid carrier as the exercise
proceeds.
As the solvent extracts the Potassium Bicarbonate from the solid carrier the outputs
from conductivity probes C2, C3 and C4 will rise and eventually stabilise. Once the
system has reached a steady state the appropriate temperatures and the
conductivities can be recorded.
observed in the readings from conductivity probes C2, C3 and C4 as the individual
cells of the rotor present fresh solid material to the solvent stream. This effect can be
observed more clearly when logging results continuously using the optional PC
logging interface and software (Armfield product code UOP4MkII-303IFD).
recorded:

o
o
90
Exercise E
o
o
the process.

concentration of the KHCO 3 in the first miscella, second miscella and final miscella
by converting the readings of C2 C1 with T2, C3 C1 with T3 and C4 C1 with T4
into values of percentage weight KHCO 3 (using the conversion graphs in Graphs of
Concentration).
Plot the graph of percentage weight of extracted material in the first miscella, second
miscella and final miscella against time. Comment on the shape of the graphs as the
process stabilises. What is the contribution of each stage in the process?
state as follows:
Mass Flowrate of solid material (From NF using

MS kg/hr
calibration graph)
Mass Flowrate of solvent entering the process (from

M1 kg/hr
N1 using calibration graph)
Mass Flowrate of final miscella (= F4 x density of the

M4 kg/hr
solvent)
Concentration of KHCO 3 in the solid (from preparation

ConcS %wt
data)
91
Concentration of KHCO 3 in the first miscella (from C2

Conc2 kg/hr
C1 and T2 using graph)
Concentration of KHCO 3 in the second miscella (from

Conc3 kg/hr
Concentration of KHCO 3 in the final miscella (from C4

Conc4 %wt
C1 and T4 using graph)
Output of KHCO 3 from the process (=M1 x Conc4/100) MO kg/hr
Percentage of KHCO 3 extracted from the solids (= 100

%
x MO/MI)

heating of the solvent) (= 0.277 x M1 x (T1 TS) x Cp)
Q1 Watts
Note factor of 0.2777 for M1 in kg/hr and Cp in kJ/kg/K

heating of the solvent) (= 0.277 x M2 x (T2 T4) x Cp)
Note factor of 0.2777 for M2 in kg/hr and Cp in kJ/kg/K.
Q2 Watts
Note temperature of fluid entering the second stage
heater cannot be directly measured and T4 is taken to
be equivalent temperature.

heating of the solvent) (= 0.277 x M3 x (T3 T4) x Cp)
Note factor of 0.2777 for M3 in kg/hr and Cp in kJ/kg/K.
Q3 Watts
Note temperature of fluid entering the third stage
heater cannot be directly measured and T4 is taken to
be equivalent temperature.
Total energy input to process(= Q1 + Q2 + Q3) Qt Watts

appropriate parameters are suggested in the Theory section above). Compare the
results obtained with those for single stage extraction (Exercise C) and two-stage
extraction (Exercise D). Comment on the effect of the third stage in the process.
92
Project Work
For simplicity in operation the following trials can be performed using the open loop
batch arrangement as described in Exercise A or the single stage continuous
arrangement as described in Exercise C.
Investigate the Effect of Temperature

Repeat extractions at different solvent temperature but fixed solvent flow rate (also
solid feed rate if continuous operation) to establish the effect on the rate of extraction.
Plot a graph of extraction rate against temperature to determine the optimum
temperature for extraction. (Remember: increased temperature means increased
operating costs and possible damage to the product being extracted.)
Investigate the Effect of Solvent Flowrate

Repeat extractions at different solvent flowrates but fixed temperature (also fixed
solid feed rate if continuous operation) to establish the effect on the rate of extraction.
Plot a graph of extraction rate against flowrate to determine the optimum flowrate for
extraction. (Remember: reduction in flowrate will give increased concentration but
reduced throughput.)
Investigate the Effect of Solid Feed Rate (only continuous operation)

Repeat extractions at different solid feed rates but fixed temperature and solvent
flowrate to establish the effect on the rate of extraction. Plot a graph of extraction rate
against feed rate to determine the optimum feed rate for extraction. (Remember:
partial extraction from a solid requires more throughput of solid and therefore
increased cost for the same gain.)
Investigate the Effect of Co-Current Flow of Solids and Liquids

The quick release fittings and flexible tubing used on the UOP4 MkII will allow the
pumps, sprinkler bars and solvent collection troughs to be reconnected so that the
movement of the solvent is in the same direction as the solids (co-current operation).
The results can be compared with those obtained in counter-current operation to

demonstrate the effect of direction.
As described in the teaching exercises there are many parameters which will affect
the efficient operation of a solid liquid extraction process, some of which are listed
above as individual project work.
The effect of changing these parameters and their effects when combined can be
investigated by performing a series of trials while varying each parameter in turn then
changing parameters in combination.
Using Alternative Solids

Solid materials other than porous pellets / Potassium Bicarbonate can be used in the
UOP4 MkII provided that they are compatible with the equipment.
When using porous polymer pellets prepared with salts other than Potassium
Bicarbonate it will be necessary to investigate the dependence of concentration on
conductivity and temperature.
When using solid carrier other than the porous polymer pellets supplied by Armfield,
it will be necessary to use the batch extraction vessel unless the material is suitable
for use in the feeder and rotor cell. Hard materials, large particles or dusty material
93
MUST NOT be fed through the spiral feeder or extraction cell as these may damage
the equipment.
Investigate the Effect of Preparation of the Solid Feed

Before performing solid/liquid extraction the solid material must be prepared by
crushing, grinding or cutting, as appropriate, to allow adequate contact between the
solvent and the soluble component. The amount of preparation will depend on the
amount and distribution of the soluble component within the solid and the nature of
the solid (how easily diffusion can occur). The effect of such preparation can be
investigated by comparing extractions under the same conditions of flowrate and
temperature but different degrees of preparation, eg. the extract from roast coffee
beans ground to different grain sizes can be compared using a colorimeter to
measure the change in tint.
Using Alternative Solvents (must be water based)

Alternative solvents can be evaluated in the system provided that they are
compatible with the materials of construction, namely PVC, Acrylic and
Polypropylene.
The solvents used must not be flammable or hazardous to the operator.
A typical solvent would be a 10% mixture of Ethanol and water.
Where the change in conductivity is small an alternative means of checking the

extraction will be necessary, eg. using a refractometer.
94
Contact Details for Further Information
Main Office: Armfield Limited
Bridge House
West Street
Ringwood
Hampshire
England BH24 1DY
Tel: +44 (0)1425 478781

Fax: +44 (0)1425 470916
Email: sales@armfield.co.uk
support@armfield.co.uk
Web: http://www.armfield.co.uk
US Office: Armfield Inc.
436 West Commodore Blvd (#2)

Jackson, NJ 08527
Tel: (732) 928 3332

Fax: (732) 928 3542
Email: info@armfieldinc.com
95

UOP4 MKII Manual - SL Extraction

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SOLID/LIQUID EXTRACTION UNIT

General Overview ....................................................................................................... 2

Important Safety Information..................................................................................... 10

General Safety Rules ............................................................................................ 10

The COSHH Regulations ...................................................................................... 14

Water Borne Hazards ............................................................................................ 15

Process Components ............................................................................................ 18

Console (Front Panel Components) ...................................................................... 21

Console (Rear Panel Components)....................................................................... 23

Console (Components on Underside) ................................................................... 24

Installation Requirements ...................................................................................... 25

Installation Process ............................................................................................... 26

Electrical Wiring Diagram ...................................................................................... 30

Operating the Software.......................................................................................... 31

Operating the Equipment....................................................................................... 41

Cleaning after use ................................................................................................. 49

Overall Dimensions ............................................................................................... 52

I/O Port Pin Connections ....................................................................................... 52

Routine Maintenance ................................................................................................ 55

Configuration of the PID Temperature Controllers ................................................ 56

Recalibration of the Thermocouple Conditioning Circuits...................................... 58

Recalibration of the Conductivity Conditioning Circuits ......................................... 59

Laboratory Teaching Exercises................................................................................. 61

Index to Exercises ................................................................................................. 61

Introduction and Background................................................................................. 61

Graphs of Concentration ....................................................................................... 64

Exercise A: Batch Extraction - Open Loop................................................................ 65

Exercise B: Batch Extraction - Closed Loop ............................................................. 69

Exercise C: Single Stage Continuous Extract ........................................................... 73

Exercise D: Two Stage Continuous Extraction ......................................................... 79

Exercise E: Three Stage Continuous Extraction ....................................................... 86

Contact Details for Further Information ..................................................................... 95

United Kingdom International

(0) 1425 478781 +44 (0) 1425 478781

Fax: +44 (0) 1425 470916

Copyright and Trademarks

Any technical documentation made available by Armfield Limited is the copyright

Brands and product names mentioned in this manual may be trademarks or

For the solid/liquid extraction process to be appropriate, the substance to be

Before performing solid/liquid extraction the solid material must be prepared by

Numerous different types of solid/liquid extractors may be employed to perform the

The Armfield UOP4 MkII is designed to demonstrate a simplified version of the

Figure 1: Front View of UOP4 MKII Solid/Liquid Extraction Unit

Figure 2: Side View of UOP4 MKII Solid/Liquid Extraction Unit

Figure 3: UOP4 MKII Schematic Diagram Showing 3 Stage Process

Figure 4: UOP4 MkII Console - Front View

Figure 5: UOP4 MkII Console - Rear View

Figure 6: PCB Connections

Figure 7: Location of Temperature Calibration Potentiometers on PCB

Figure 8: Location of Conductivity Calibration Potentiometers on Conductivity Measurement PCB

Before proceeding to install, commission or operate the equipment described in this

INJURY THROUGH MISUSE

INJURY FROM ELECTRIC SHOCK

INJURY FROM ROTATING COMPONENTS

IRRITATION FROM DUST WHEN HANDLING DRY MATERIALS

BURNS FROM COMPONENTS AT HIGH TEMPERATURES

INJURY FROM INCORRECT HANDLING

Accidents can be avoided provided that equipment is regularly maintained and

General Safety Rules

a. Before attempting to install, commission or operate equipment, all relevant

b. It is irresponsible and dangerous to misuse equipment or ignore instructions,

c. Do not exceed specified maximum operating conditions (eg. temperature,

b. Extreme care should be exercised to avoid damage to the equipment during

d. Equipment involving inflammable or corrosive liquids should be sited in a