Page 1
Scirocco 2000
user manual
INSTRUMENTS
Page 2
Page 3
Scirocco 2000
User Manual
MAN0386 Issue 1.0 March 2007
Page 4
© Malvern Instruments Ltd. 2007
Malvern Instruments makes every effort to ensure that this document is correct. However, due to
Malvern Instruments’ policy of continual product development we are unable to guarantee the
accuracy of this, or any other document after the date of publication. We therefore disclaim all
liability for any changes, errors or omissions after the date of publication.
No reproduction or transmission of any part of this publication is allowed without the express
written permission of Malvern Instruments Ltd.
Head office:
Malvern Instruments Ltd.
Enigma Business Park,
Grovewood Road,
Malvern,
Worcestershire WR14 1XZ
United Kingdom.
Tel + [44] (0)1684-892456
Fax + [44] (0)1684-892789
Windows 2000 and XP are registered trademarks of the Microsoft Corporation.
Tygon is a registered trademark of Norton Co.
Perlast is a registered trademark of Precision Polymer Engineering.
Printed in England
Page 5
Table of Contents
Part 1 - Operator’s Guide
Introduction to this manual
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1
Access to the instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-2
Assumed information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
Where to get help. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
Hardware features
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
What the dispersion unit does . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
How the dispersion unit works . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-2
How the dispersion unit is controlled . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Features of the Scirocco 2000. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Scirocco 2000 with hopper . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-12
Software features
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
Making a measurement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
Manually controlling the dispersion unit . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2
Writing an SOP for the dispersion unit . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6
Making a measurement
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1
Dry powder measurement guidelines . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1
Making a measurement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-2
Scirocco 2000 Page i
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Table of Contents Scirocco 2000
Part 2 - Appendices
Specification
Specification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-1
Chemical compatibility
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-1
Components in contact with sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-1
Regulatory statements
CE Declaration of Conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-2
Index
Page ii MAN 0386
Page 7
Part 1 Operator’s Guide
Page 8
Page 9
Introduction to this manual
Introduction
This manual covers the operation of the Scirocco 2000 sample dispersion unit:
Instrument Model number
Scirocco 2000 (stainless steel venturi) ADA2000
Scirocco 2000 (ceramic venturi) ADA2001
Hopper for Scirocco 2000 option DPF2267
This manual is a supplement to the following manuals:
1
Mastersizer 2000 User Manual (termed “the main User Manual”).
Mastersizer 2000 Essentials Manual (termed “the Essentials Manual”).
This dispersion unit manual focuses on some specific issues of the dispersion unit
that are not covered by the above manuals. It aims to:
Describe what the dispersion unit is and explain in simple terms how it works.
Identify the physical features of the dispersion unit.
Describe the software and explain how to use the dispersion unit to make a
measurement on the system.
Warning!
The dispersion unit or the samples to be measured may be hazardous if
misused. Users must read the Health and Safety information in the
Essentials Manual before operating the system.
We recommend that users who have never operated a Malvern particle analyser
before read this manual fully before starting the first measurement.
Scirocco 2000 Page 1-1
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1
Chapter 1 Introduction to this manual
Those who are more familiar with particle size analysers may wish to jump straight
to Chapter 4 of the main User Manual which gives details on making measurements. However, the importance of sample preparation before measurement cannot be overstated so we recommend reading the chapter on sample preparation
(Chapter 8 of the main User Manual) as a priority.
Warning!
Static discharge can occur around the exit and feed pipe regions of the unit
under certain combinations of material, flow rate and humidity. If this is a
concern in your application, contact your Malvern supplier.
Access to the instrument
Within this manual, reference is made to the various people who will have access to
the dispersion unit. The following is a list of these people and their responsibilities:
Malvern personnel
Malvern personnel (service engineers, representatives, etc.) have full access to the
dispersion unit and are authorised to perform all service procedures that may
require the removal of the covers.
Supervisor
The supervisor is the person responsible for the management/safety of the dispersion unit and of its operation. The supervisor is responsible for the training of the
operators. The supervisor can perform all user maintenance routines identified in
Chapter 4 of the Essentials Manual, including changing the fuses.
Warning!
The supervisor/operator must never remove the covers of the instrument
or dispersion unit. Removal of the covers by unauthorised personnel will
invalidate the warranty of the dispersion unit.
Operator
An operator is a person trained in the use of the dispersion unit. The operator can
perform all user maintenance routines identified in Chapter 4 of the Essentials
Manual, except for changing the fuses.
Page 1-2 MAN 0386
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Introduction to this manual Chapter 1
Warning!
Failure to follow this guideline could result in exposure to hazardous
voltages.
Assumed information
Naming convention
Within this manual:
The Mastersizer 2000 optical bench is referred to as “the optical bench” or “the
instrument”.
The sample dispersion units are referred to in full (“the Scirocco 2000”) or as
“the dispersion unit”.
The combination of the optical bench, one or more dispersion units and the
computer is referred to as “the system”.
The hopper-equipped Scirocco 2000 is identified as a “hopper instrument”.
Menu commands
Menu commands from the Malvern software are referred to in the form main
menu-menu item. As an example, the command Configure-New SOP refers to
selecting the New SOP item in the Configure menu. The same rules apply for
sub-menus of sub-menus, so that Tools-Options-Instrument Port refers to the
Instrument Port item in the Options sub-menu, which itself is a sub-menu of
the Tools menu. Menu commands are always shown in bold text.
Where to get help
Full details on where and how to obtain help can be found in Chapter 1 of the
main User Manual.
The Essentials Manual gives information on the following:
Site requirements.
Health and Safety.
Maintenance.
Installation (in case the system has to be moved after its initial installation by
Malvern Instruments personnel).
Scirocco 2000 Page 1-3
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Chapter 1 Introduction to this manual
Page 1-4 MAN 0386
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Hardware features
Introduction
This chapter describes the physical features of the dispersion unit. It covers:
What the dispersion unit does.
How the dispersion unit works.
How the dispersion unit is controlled.
The physical features of the Scirocco 2000 in detail.
The Scirocco 2000 with hopper option.
2
What the dispersion unit does
The sole purpose of any sample dispersion unit is to prepare the sample and then
deliver it to the optical bench so that it can be measured.
The Scirocco 2000 allows the Mastersizer 2000 to be used for particle-in-gas particle sizing (in the majority of cases the gas will be air).
The materials used in the manufacture of the dispersion unit maximise the range of
samples which can be handled. Variable air pressure allows a wide range of particle
sizes and densities to be suspended and delivered to the optical bench.
Scirocco 2000 Page 2-1
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2
Chapter 2 Hardware features
How the dispersion unit works
This diagram shows the features of the dispersion unit:
2
1
3
The dry powder sample is manually placed in the sample tray with the air supply
and vacuum extraction system connected. When the sample tray is vibrated the
sample travels down the tray until it eventually falls into the main feed mechanism.
The rate at which the sample is fed is governed by the amplitude of vibration on the
sample tray (controlled from the software) and also by the gap between the feed
gates
on the sample tray.
At the entrance to the main feed mechanism is a wire sieve filled with ball bearings
. The ball bearings smooth the flow of sample and also help to break up loose
agglomerates within the sample.
As the sample falls through the sieve it is accelerated by compressed air within a
venturi where agglomerates are dispersed. The sample is then directed through the
air cell
fitted to the Mastersizer, where it is measured and then collected by the
vacuum extracting system at the rear of the air cell.
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Hardware features Chapter 2
How the dispersion unit is controlled
The dispersion unit is controlled using a single software dialogue with sliders for
the air pressure, sample tray vibration feed rate, and (for hopper instruments) the
hopper feed rate. (Chapter 3 has details.) When controlled through a Standard
Operating Procedure (SOP), the software tells the user what value to set for each
parameter.
The system automatically detects which dispersion unit and cell are connected. If
more than one dispersion unit is connected, the system will detect all dispersion
units connected but only the dispersion unit that has its cell installed on the optical
bench will be “active”.
Features of the Scirocco 2000
The illustration below identifies the main features of the dispersion unit:
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Chapter 2 Hardware features
Sample tray area
The sample tray area is where the sample is added to the dispersion unit. Sample
feeds down the sample tray as it is vibrated. Three sizes of sample tray are available
for different applications. More details of the sample tray area are given below.
Status indicator
The status indicator illuminates in one of three colours when the dispersion unit is
powered up:
Green if the dispersion unit is functioning correctly and its cell has been
loaded into the optical bench (i.e. the dispersion unit is “active”).
Amber if the dispersion unit is functioning correctly but its cell has not been
loaded into the optical bench (i.e. the dispersion unit is at “standby”).
Red if the dispersion unit detects an error. If an error message does not appear
on the screen, selecting Configure-Accessories will display the dispersion
unit control dialogue which should show the error.
Sample area lid
The sample area lid is primarily a safety feature that reduces the sound emissions
from the dispersion unit. The lid must be locked using the central catch to ensure
that sound emissions are reduced to an adequate level.
The lid is interlocked so the dispersion unit automatically returns to standby mode
if it is opened during a measurement. Unless there is a hopper, it is therefore
important that the sample is added to the sample tray before the measurement is
started. With hopper instruments, the sample can be added to the hopper as the
measurement proceeds.
Rear panel
The rear panel contains all services and communication connectors for the dispersion unit. More details are given later in this chapter.
Sample exit port
This is the port where the sample leaves the dispersion unit. It is connected to the
air cell via a flexible tube. The tube must be removed from this port if the cell is to
be stored in the cell holder. This prevents damage to the ceramic outlet nozzle.
Air cell
The air cell is used to confine the sample as it passes through the analyser beam in
the optical bench. More details are given later in this chapter.
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Hardware features Chapter 2
Vacuum switcher box
The vacuum switcher box is a control box used to turn on the primary vacuum unit
for the dry cell and the secondary vacuum unit used for cleaning. The switcher box
is controlled from the software. More details of its features are given below.
Vacuum unit
The vacuum unit removes the sample from the cell exhaust once it has been measured.
Sample tray area
The sample tray area holds a vibrating tray that holds the sample. Sample feeds
down the sample tray as it is vibrated. This illustration shows the main features:
21
4 3
ill 4942
Sample tray
The sample tray receives the sample to be measured. Three sample trays are available for the Scirocco. Each type is individually encoded so that, when it is attached to
the dispersion unit, it is automatically detected and reported in the sample records.
The three tray types are:
General purpose tray – the standard tray provided with the Scirocco
2000, this has an adjustable slit to regulate the flow of sample. This is most
suitable for free-flowing materials and materials having broad size distributions (greater than 1 to 300 microns) where larger samples need to be
measured to obtain statistical significance.
Micro volume tray – this is designed for pharmaceutical materials where
very little material is available. The smallness of the tray removes the temptation to overload it. The tray has a single slit width which is recorded in
the sample details and in the SOP.
Scirocco 2000 Page 2-5
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Chapter 2 Hardware features
This tray is not suitable for samples having broad size distributions unless
several repeat measurements are made. Repeat measurement tests need to
be carried out to determine the exact number of repeat measurements to
give the required standard of repeatability.
Small volume tray – if the small size of the micro volume tray proves to
be a problem in terms of repeatability, the small volume tray provides a
compromise. Again, it has a fixed width slit to eliminate one source of
method variation.
Gates
The gates of the general purpose tray are used as a method of controlling the flow
rate of the sample by varying the aperture between them. The gates are locked in
position by the knurled locking screws.
On hopper instruments the sample tray has a one piece guillotine style gate controlling the flow rate of the sample. To adjust this loosen the M3 Allen screws that
secure the gate then move the gate up or down to the desired position. Use a
1.5mm Allen key to adjust this, securing the screws afterwards.
Sieve
The ball bearings in the wire sieve at the entrance to the feed mechanism smooth
the flow of the sample as they effectively store the sample within the array for a
short period. The ball bearings also break up loose agglomerates in the sample.
One fine and one coarse sieve are provided with the dispersion unit.
Tray locking screw
The sample tray is locked in position by tightening the locking screw.
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Hardware features Chapter 2
Rear panel
This illustration shows the main features of the rear panel:
6
1
5 3
Mains power supply
4
2
ill 4979
The mains power supply is a standard IEC socket that supplies mains power to the
dispersion unit. The connector also houses the dispersion unit’s fuses and on/off
switch.
Auxiliary connector
The auxiliary connector is connected to the vacuum switcher box.
Accessory comms “in” connector
The communications cable from the optical bench or from another dispersion unit
connects here.
Accessory comms “out” connector
If more than one dispersion unit is connected to the system and this is the first dispersion unit in-line, a communication cable will be connected from here to the
“accessory comms - in” connector of the second dispersion unit.
Caution!
A termination plug must be fitted to this connector if this is the only dispersion unit connected or it is the last dispersion unit in the line.
Scirocco 2000 Page 2-7
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Chapter 2 Hardware features
Air in connector
The compressed air line is connected to this. The compressed air is used to disperse
the sample. The input range is from 6-8 bar.
Caution!
The dispersion unit may be permanently damaged if the compressed air
line is not clean, dry and free from oil (see the Site Requirements for
details).
Vacuum monitor connector
The vacuum monitor connector is connected to the rear of the air cell and used to
detect whether the vacuum unit is working. This is a safety device - it ensures that
the sample will not be fed into the system until the vacuum unit is capable of safely
taking it away. Do not apply a pressure greater than +0.3 bar g to this input.
Air cell
Caution!
The air cell is an optical device. Treat it carefully as you would an expensive camera. Scratches to the surfaces of the cell may affect performance.
The cell passes the sample through the analyser beam of the optical bench so that it
can be measured. The cell windows are part of the optical path of the system and
should be kept clean and free from scratches at all times. Refer to Chapter 4 for
details of cleaning/maintaining the cell.
The cell is encoded so the system detects and identifies it when it is loaded into the
optical bench. This diagram shows the features of the cell:
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Hardware features Chapter 2
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3
8
4
INSTRUMENTS
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1
2
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Noise protection box
This dampens any noise emissions from the air cell.
Sample inlet
The sample tube from the dispersion unit is connected to this inlet
Locking handle
The cell locking handle must be rotated anti-clockwise to lock the cell in place on
the optical bench. To remove the cell, disconnect the sample inlet tube from the
sample inlet, rotate the handle clockwise and lift the cell clear.
Warning!
Never attempt to lift the optical bench by the locking handle of the cell.
See the Health and Safety information for correct moving techniques.
Cell shroud
The cell shroud prevents stray light entering the measurement area and affecting a
measurement. More importantly, it stops human access to laser radiation. The system should never be used if the cell shroud is damaged.
Cell windows
The cell windows allow the analyser beam of the optical bench to pass through the
cell and hence the particle field. The cell windows can be removed to allow clean-
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Chapter 2 Hardware features
ing (the cell window tool used to remove the window is located within the cell
holder). The cell windows are delicate and should be treated with caution - refer to
the Essentials Manual for details on cleaning these windows.
Vacuum monitor connector
A tube from this connector attaches to the vacuum monitor connector on the rear
panel of the dispersion unit. This senses whether the vacuum unit is working. This
is a fail-safe device that prevents the sample being fed until the vacuum unit is on,
allowing the powder to be safely disposed of.
Earth lead
This earth lead must always be connected. It prevents the particles being charged.
Exhaust connector
The vacuum tube from the vacuum unit is connected here. A vacuum unit must be
used to prevent samples being discharged into the laboratory.
Cell holder
The Mastersizer system allows more than one sample dispersion unit to be connected at once. The cell holder provides a convenient storage location for the cell
(and the window removal tool) if another dispersion unit is being used.
The cell holder has a special fixing located on the left of the optical bench especially
for air cells. See
for details on how to fit the holder.
Disconnect the sample tube to the cell before storing the cell in the cell holder.
Cell holder fixing
There is a fixing plate under the cell holder which can be extended by undoing the
two hand screws and sliding the plate out. Re-tighten the hand screws to lock the
plate in place.
The cell holder can then be attached to the left side of the optical bench by locating
the fixing plate onto the two lugs on the underside of the optical bench.
Page 2-10 MAN 0386
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Hardware features Chapter 2
Vacuum switcher box
This diagram shows the features of the vacuum switcher box:
4 3
1
“From dry power feeder” connector
2
ill 4941
This connector connects to the dispersion unit’s Auxiliary connector. The vacuum
unit is controlled via this connector.
Fuse holder
This holds the vacuum switcher box fuse. Any replacement fuse must be of the
correct type and value (see the cover of the vacuum switcher box for details).
Mains inlet socket
The mains power supply is a standard IEC socket that supplies mains power to the
switcher box.
Mains outlet socket
The mains power outlet is connected to the vacuum unit.
Warning!
The warning symbol near this socket is there to warn that this power
socket is switched on and off by computer control. The operator must be
aware that this power socket may be powered unexpectedly.
Scirocco 2000 Page 2-11
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Chapter 2 Hardware features
Scirocco 2000 with hopper
The hopper instrument is a modified version of the Scirocco 2000, specifically
designed for the needs of customers in the cement and bulk chemical industries. Its
features are shown below:
2
1
3
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Changes from the standard Scirocco 2000 are:
New lid assembly
This has an integral hopper assembly and an auxiliary vacuum exit.
Hopper assembly
The hopper assembly is in the sample lid that sits above the sample tray. This comprises a sample funnel and a cascade assembly:
Sample funnel – two sample funnels which fit into the hopper assembly are
available, with fine or coarse meshes suitable for use with different sizes of
sample.
The sample is placed on a mesh inside the funnel and vibrated by a motor fitted
under the lid, so a steady stream of sample is deposited on the sample tray.
Cascade assembly – this is fitted beneath the funnel. It controls the rate at
which sample is delivered to the sample tray.
As with the sample tray feed rate, the vibration rate of the hopper can be set from
the SOP, allowing different feed rates to be used for different samples.
Auxiliary vacuum port
The auxiliary vacuum port allows a secondary vacuum cleaner to be attached to the
unit in order to remove any excess sample from the sample tray at the end of the
measurement.
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Hardware features Chapter 2
One piece sample tray
Similar in application to the general-purpose tray described earlier, this tray has a
narrow sample area to guide the sample directly towards the sieve. A one-piece
'guillotine' style gate controls the sample flow.
Vacuum switcher box
Hopper instruments use a larger switcher box. This has a second mains power
outlet socket, required for connecting the second vacuum unit used to remove any
excess sample from the sample tray after the measurement has finished.
Scirocco 2000 Page 2-13
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Chapter 2 Hardware features
Page 2-14 MAN 0386
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Software features
Introduction
This chapter describes the features of the software which are specific to the dispersion unit. It covers:
Making a measurement – the basics of making a measurement using the dis-
persion unit.
Manually controlling the dispersion unit.
Writing an SOP for the dispersion unit.
3
Making a measurement
Making a measurement is fully documented in Chapter 4 of the main User Manual. Refer to that manual for details.
The dispersion unit can either be controlled manually or automatically by running
a Standard Operating Procedure (SOP). The system automatically detects which
dispersion unit and cell is connected. If more than one dispersion unit is connected, the system detects all dispersion units connected, but only the dispersion
unit that has its cell installed on the optical bench will be “active”.
Scirocco 2000 Page 3-1
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Chapter 3 Software features
Manually controlling the dispersion unit
All Scirocco 2000 functions can be controlled directly from the Dry Accessory
dialogue (accessed by selecting Configure-accessories). The dialogue is shown
below:
4
5
2
1
3
This example shows the hopper-equipped version of the dialogue. The dialogue
allows the user to alter, by using the relevant slider bar, the Air Pressure, sample
tray vibration Feed Rate, and (for hopper instruments) the Hopper Feed rate.
The dialogue also allows the user to turn on the feed mechanism and air pressure.
Status indicators give information such as whether the tray lid is open/closed and
which sample tray is fitted, as well as reporting any errors.
Air pressure control
The Scirocco 2000 uses compressed air to transport and suspend the particles of the
sample as they pass through the air cell. High air pressure settings can also help
break up agglomerates. The air pressure can be controlled up to a pressure of 4 bar.
The optimum air pressure setting depends on your sample, so a few trial measurements are recommended. A typical starting air pressure is between 1 and 3 bar. If
the sample is fragile, for example freeze dried coffee, use a lower pressure. If the
sample is dense or cohesive, use a higher pressure.
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If the air pressure is set too high this may physically change the particle size, giving
an incorrect result.
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Software features Chapter 3
Use one of the following methods to ensure that the correct air pressure is being
used:
Perform a number of measurements at different air pressures and look for a
‘plateau’ of stable results. Choose the lowest air pressure commensurate with a
stable result.
If the sample can be recovered after measurement, and shows no significant
change when re-measured, the air pressure is acceptable.
If the sample can also be measured using a wet dispersion unit, and there is no
significant difference in the result, the air pressure setting is acceptable.
The air pressure control will not operate until the Air flow radio button is selected
from the Mode area of the dialogue.
Feed rate control
The Scirocco 2000 uses a vibrating tray to feed the sample into the dispersion system. The rate at which sample is fed is governed by the vibration amplitude and the
type of tray fitted.
Adjust the feed rate to produce a steady flow of sample into the dispersion system
and to obtain the optimum sample concentration through the measurement cell. If
the feed rate is too high, the sample concentration may become too high and any
agglomerates may not disperse correctly. If the feed rate is too low, the concentration may become too low and/or the sample flow may become intermittent. The
General Purpose tray has an adjustable slit to help maintain a steady sample feed.
Sample concentration is monitored using the obscuration reading in the Meas-
urement Display dialogue.
The feed rate control will not operate until the Feed radio button is selected from
the Mode area of the dialogue.
Mode selection
The Scirocco 2000 is turned on/off using the mode buttons: Standby, Air flow
and Feed. The status line describes the current state of the Scirocco 2000. The buttons operate as follows:
Standby – sets the unit into an inactive mode. The unit may be automatically
set to this mode if an error condition is detected.
Air flow – turns on the vacuum and checks the minimum vacuum level is
reached, then checks the air pressure is correct and turns on the air flow.
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Chapter 3 Software features
A progress bar indicates the state of the air control sequence. The segments
have the following meaning:
Segment 1 Unit in standby mode
Segment 2 Waiting for vacuum confirmation
Segment 3 Waiting for air pressure confirmation
Segment 4 Not used
Segment 5 Air flow on.
Feed – turns on the vibration of the tray. If the air flow is not already on, the
vacuum and air flow are turned on first. The associated indicator is illuminated
green when the requested vibration level is reached.
Error indicators
Any error detected by the system will return the unit to standby mode. Malfunctions are shown by red illuminated indicator boxes. The type of error will also be
displayed in the status area of the dialogue.
The system monitors the operation of the following devices:
Device Fault condition Possible cause
Vacuum No vacuum detected. Fuse blown in switcher box.
Vacuum unit not switched on.
Cable to switcher box not fitted.
Vacuum unit pipe not connected.
Power cable to switcher box not fitted.
Insufficient vacuum (e.g. clogged bag).
Lead to vacuum unit not fitted.
Sense tube between air cell and
dispersion unit not fitted.
Air Pressure Air pressure not within
10% of full scale pressure (i.e. ±0.4 bar of
requested pressure).
Vibrator Monitored level not
within 10% of requested
level.
Tray Invalid tray code. No tray fitted.
Air supply not on, or pressure low.
Air supply pipe not connected.
Air supply pipe blocked.
Tray jammed.
Hardware failure.
Tray fitted incorrectly (not screwed in).
Tray detection hardware failure.
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Software features Chapter 3
If an error is not corrected by the above suggestions, contact the local Malvern representative.
Sample tray and lid indicators
These indicators display which sample tray is fitted and whether the lid is open.
Hopper Feed control
The hopper is a pre-disperser. Its purpose is to deliver a steady amount of powder
to the sample tray, so that the amount of powder passing through the venturi
remains roughly constant. This prevents surges in obscuration and poor dispersion
caused by passing too much material through the venturi system.
Approximate starting hopper feed rates are 40% to 45% for a material such as
cement, but every product is different so the appropriate SOP settings may differ.
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Chapter 3 Software features
Writing an SOP for the dispersion unit
An SOP can be configured to control all settings for the dispersion unit automatically. When an SOP is run, the software will (depending on how the SOP has been
set up) automatically set the air pressure and feed rates to a pre-defined setting and
run through a measurement sequence. The SOP will even report if the wrong cell
or dispersion unit is fitted.
The SOP Wizard is described in full in the main User Manual. There are ten
dialogues in all but here we just describe those which have parameters specific to
the Scirocco 2000. These are the Sampler Selection, Sampler Settings and
Measurement Cycles dialogues.
Ensure that all systems an SOP is distributed to have the dispersion unit connected.
Sampler Selection dialogue
The Sampler Selection dialogue is shown below.
1
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Software features Chapter 3
Select the dispersion unit to use from the drop down list . All dispersion units
available are listed, even those that are not attached to the system. This enables an
SOP to be written remotely from the system.
Under the Sample handling unit options specify the type of venturi fitted.
There are two types:
Metal – suitable for most applications.
Ceramic – for abrasive materials.
Note
The unit’s A/B identity must be set for the correct venturi. It must be set to
i
A for a metal venturi and B for ceramic. On older systems this switch was
not used; if in doubt, select Original Configuration to disable the venturi type check. Contact the Malvern representative if required to switch
between the types of venturi.
Sampler Settings dialogue
The Sampler Settings dialogue controls the feed rate and air pressure settings for
the dispersion unit. This dialogue changes depending on the dispersion unit
selected in the Sampler Selection dialogue. This diagram shows the dialogue for
the Scirocco 2000:
1
2
3
4
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Chapter 3 Software features
i
Tray selection
This lists all the sample trays available. All systems the SOP is distributed to must
have the tray selected in the list fitted.
Vibration Feed Rate control
The Scirocco 2000 uses a vibrating tray to feed the sample into the dispersion system. The rate at which sample is fed is governed by the vibration amplitude and the
type of tray fitted.
Adjust the feed rate to produce a steady flow of sample into the dispersion system
and to obtain the optimum sample concentration through the measurement cell. If
the feed rate is too high the sample concentration may become too high and any
agglomerates may not disperse correctly. If the feed rate is too low the concentration may become too low and/or the sample flow may become intermittent. The
General Purpose tray has an adjustable slit to help maintain a steady sample feed.
Sample concentration is monitored using the obscuration reading in the Meas-
urement Display dialogue.
Dispersive Air Pressure control
The Scirocco 2000 uses compressed air to transport and suspend the particles of the
sample as they pass through the air cell. High air pressure settings can also help
break up agglomerates. The air pressure can be controlled over the range 0 to 4 bar
(atmospheric pressure is approximately one bar).
The optimum air pressure setting depends on the sample, so a few trial measurements are recommended. A typical starting air pressure is between 1 and 3 bar. If
the sample is fragile, for example freeze dried coffee, use a lower pressure. If the
sample is dense or cohesive use a higher pressure.
If the air pressure is set too high this may physically change the particle size, giving
an incorrect result. One of the following methods may be used to ensure that the
correct air pressure is being used:
If the sample can also be measured using a wet dispersion unit, and there is no
significant difference in the result, the air pressure setting is acceptable.
Perform a number of measurements at different air pressures and look for a
‘plateau’ of stable results. Choose the lowest air pressure commensurate with a
stable result.
Note
Application Notes available at www.Malvern.com describe the process
of method development for dry powder dispersion.
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Software features Chapter 3
Hopper Feed Rate (hopper instruments only)
The hopper is a pre-disperser. Its purpose is to deliver a steady amount of powder
to the sample tray, so that the amount of powder passing through the venturi
remains roughly constant. This prevents any surging in obscuration, and any poor
dispersion caused by passing too much material through the venturi system.
Aim to set a rate that delivers a steady amount of powder:
1. Initially set the Vibration Feed Rate to an appropriate value (around 30%).
2. Change the Hopper Feed Rate until enough material to produce a steady line
of powder is passed down the tray. This is then the rate to use in an SOP.
Approximate starting Hopper Feed Rates are 40% to 45% for a materials such as
cement, but every product is different so the appropriate SOP settings for specific
products may differ.
Scirocco 2000 Page 3-9
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Chapter 3 Software features
Measurement Cycles dialogue
The Measurement Cycles dialogue allows the system to be set up to perform
multiple measurements of a sample. It also defines the cleaning sequence used after
a measurement has been completed.
Excess sample often remains on the tray and has to be removed manually. The
Cleaning section of the dialogue enables this excess sample to be fed through the
system into the vacuum cleaner. In a hopper-equipped Scirocco, the excess sample
can be withdrawn directly from the sample tray into a second vacuum unit attached
to the sample lid.
The cleaning cycle becomes active when the Cleaning required check box is enabled. The user must then set:
The Clean Duration, the time beyond the measurement period during which
the vibrating tray, compressed air supply and vacuum cleaner are left running
in order to clear the sample from the tray.
The Vibration Feed Rate to use during the clean cycle.
The Dispersive Air Pressure required to convey the sample through the cell
during cleaning.
In addition, if a second vacuum cleaner has been installed on a hopper Scirocco,
selecting the Second vacuum fitted option triggers the second vacuum cleaner at
the end of the sample measurement and remove all excess sample directly from the
sample tray during the clean procedure.
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Software features Chapter 3
The Advanced - Measurement dialogue
The system can be configured to measure only when certain obscuration conditions are met. Open the Advanced - Measurement dialogue by clicking the
Measurement button on the Measurement dialogue.
1
2
3
4
The Advanced - Measurement dialogue allows configuring of Obscuration
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limits and Autostart, Obscuration Filtering (where measurements are only
taken when obscuration lies between certain limits) and Red Only Measure-
ment. These are described in Chapter 9 of the main User manual, but this section gives additional information specific to dry powder measurements.
The tabs on the dialogue are:
Obscuration limits
Check the Use default limits box to set the limits to default values of between
0.5% and 6% for a dry dispersion unit. Select the Raise alarm... box to flag when
integrated obscuration is out of range.
This tab only defines the limits - the Obscuration filtering tab imposes the
defined limits.
Scirocco 2000 Page 3-11
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Chapter 3 Software features
Note
Application Notes available at www.Malvern.com describe the process
i
of method development for dry powder dispersion, including selection of
obscuration limits.
Autostart
Autostart is used to ensure that no measurements are started until the dispersion is
stable. Dry measurements always exhibit a range of fluctuation so the Autostart
feature is not generally used for these.
Obscuration filtering
This facility is particularly useful when the sample concentration is liable to some
degree of fluctuation as is often the case with dry powder measurements. Selecting
the Only include snaps with values within obscuration limits check box
effectively turns on the obscuration limits set in
For dry powder measurements practical limits are 0.5% and 6% but exact settings
can only be found by experimentation.
In the event that a totally inappropriate feed rate is set so that the obscuration seldom (if ever) falls within the desired limits, a time-out allows the user to exit the
measurement. Do not set this so long as to give the measurement routine the
appearance of having hung up, but it should be sufficiently long to allow a fair
chance of sample of the required concentration passing through the measurement
zone.
above.
The user is strongly advised to adjust the feed rate so that the obscuration falls
between the preset limits for the duration of the measurement.
If a measurement times out the number of measurement snaps is recorded e.g. it
will be reported that “1760 of 2000snaps” were captured.
Red Only Measurement
The options on this tab are not available as the blue light source is not used for dry
powder measurements.
Page 3-12 MAN 0386
Page 39
Making a measurement
Introduction
This chapter describes how to make a measurement using a Scirocco 2000. It covers:
Dry powder measurement guidelines.
Making a measurement – important differences from the procedure described
in Chapter 4 of the main User Manual.
Dry powder measurement guidelines
4
To obtain good repeatable dry powder measurements, ensure that the individual
particles are well dispersed in the air flow and that they are transported through the
measurement region at a suitable steady rate and concentration.
The energy used to disperse the particles is mainly controlled by the air pressure.
The concentration is largely determined by the rate at which powder is fed into the
air stream.
The ease of dispersion varies greatly between materials. Cohesive materials such as
magnesium stearate require much more dispersion energy than free flowing samples such as glass beads. The same material can vary with humidity, temperature
and degree of compaction.
However, do not always simply use the maximum dispersing energy. Many pharmaceutical and food materials are fragile, as are substances like raw ceramics. Too
much energy will break up the primary particles.
Some cohesive materials may be compacted onto surfaces by high pressure and
flake off as agglomerates.
Scirocco 2000 Page 4-1
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4
Chapter 4 Making a measurement
Control of concentration is also important. Too little sample means measuring
mainly background noise. Too much sample means the measurement is distorted
by multiple scattering.
Making a measurement
Making manual and SOP measurements using the Scirocco 2000 is basically the
same as discussed in Chapter 4 of the main User Manual, but with two important differences:
As the lid to the sample tray is interlocked for safety, if the lid is opened during
a measurement, the dispersion unit automatically shuts down to its standby
mode. Because of this, the sample must be added to the sample tray before the
measurement is started.
Secondly, the Add sample tab of the measurement display is not typically
used. Instead, obscuration triggering is used to start a measurement. Obscuration triggering is where a measurement is only started when the obscuration of
the sample is between two preset values.
To make a basic manual measurement:
1. Open the lid to the sample area and add the sample to the sample tray. Add the
sample to the centre of the tray, especially for free-flowing samples, to prevent
the sample from self-feeding.
2. Close and lock the lid.
3. Alter the air pressure and feed rate setting by selecting Configure-Accesso-
ries... and moving the appropriate slider. Note that the air or feeder will not
actually start until the Airflow or Feed radio buttons are selected in the Mode
section of the dialogue. Position the control dialogue to the left of the screen
where it can be seen and readily accessed.
4. Select Measure-Manual to display the Measurement display. The system
will automatically measure an electrical background, align the system and then
measure the optical background.
5. Select the Options button to change any settings for the measurement.
Choose:
The Material tab to define the sample that is being measured.
The Measurement tab to set the measurement time.
Press the Measurement button in the Measurement tab to set the
obscuration settings.
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Making a measurement Chapter 4
6. In the Advanced - Measurement dialogue, shown below, select the Only
include measurements with values within obscuration limits check box.
Set the obscuration limits (typically set these to between 0.5% and 6%):
Select OK.
7. Press the Next button in the Measurement display to access the Add sample
tab. This tab is not be needed as the measurement will be started by obscuration triggering. Press the Next button again to view the Measure sample tab.
8. Press the Start button to start the measurement. The software now waits for
the sample to start feeding.
9. Select the Air flow radio button. The vacuum unit will automatically come on
and then, after a five second wait, the air line will be turned on automatically.
10. Select the Feed radio button in the Dry sampler control dialogue. The sam-
ple will start to move down the tray. The software will only make a measurement when the measured obscuration is between the set obscuration limits.
Once the measurement is complete, the results will be saved to a measurement file.
Scirocco 2000 Page 4-3
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Chapter 4 Making a measurement
To make a basic SOP measurement:
1. Open the lid to the sample area and adding the sample to the sample tray. Close
and lock the lid.
2. Select Measure-Start SOP. A dialogue appears asking you to select an SOP.
Select an SOP and press the Open button. The measurement is automatically
made.
Page 4-4 MAN 0386
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Part 2 Appendices
Page 44
Page 45
Specification
Specification
Dispersion type Dry, with controllable airflow, controllable feed rate, and
interchangeable feed trays automatically sensed by the
system.
Typical applications Dry powders, pharmaceutical excipients, fillers, cements,
flour, powder coatings.
Modes of operation Automatic via SOPs.
Manual via computer operating dialogues.
Weight 21.3kg.
Dimensions Width: 352mm
Height: 332mm
Depth: 355mm
Power 100-120V / 200-240 V AC, 50/60Hz, 240VA.
Maximum particle
size
2000 microns, depending on particle shape and density.
A
Scirocco 2000 Page A-1
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A
Appendix A Specification
Page A-2 MAN 0386
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Chemical compatibility
Introduction
The Scirocco 2000 is manufactured from materials that are considered to give the
widest protection from chemical attack. However, it is important to check that any
sample you may use is chemically compatible with the materials that they will come
into contact with within the dispersion unit.
This appendix lists all materials that come into contact with the sample in the normal operation of the dispersion unit.
B
Components in contact with sample
Component Materials
Tray & venturi 316 stainless steel and ceramic
Sieve and ball bearings 316 stainless steel
Sample pipes to cell Tygon™
Cell Glass, 316 stainless steel
Vacuum hose PVC
Cell elbow 316 stainless steel
Vacuum retaining pipe 316 stainless steel
Scirocco 2000 Page B-1
Page 48
B
Appendix B Chemical compatibility
Page B-2 MAN 0386
Page 49
C
Regulatory statements
This appendix presents regulatory information.
Scirocco 2000 Page C-1
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C
Appendix C Regulatory statements
CE Declaration of Conformity
The CE badge on this product, shown below, signifies conformance to European
Commission Directives.
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Index
A
Advanced - Measurement dialogue
Air cell
details
2-8
overview 2-4
Air flow radio button 4-3
Air in connector 2-8
Air pressure
control
3-8
faults 3-4
guidelines 4-1
optimum 3-8
setting 4-2
software control 3-2
Airflow mode 3-3
Autostart 3-12
C
CE Declaration
C-2
Cell holder 2-10
Cell shroud 2-9
Cell windows
cleaning
2-8
function 2-9
Chemical compatibility B-1
Cleaning required check box 3-10
Cleaning sequence 3-10
Communications cable 2-7
Concentration
importance of
4-2
optimising 3-8
Controlling the accessory
manually
3-2
D
Dispersion units
chaining
2-7
Dry Accessory dialogue 3-2
Dry powder guidelines 4-1
3-11, 4-3
E
Earth lead
2-10
Error indicators 3-4
Exhaust connector 2-10
F
Features overview
2-2, 2-3
Feed mode 3-4
Feed rate
changing
4-2
control 3-8
software control 3-3
G
Gates (sample tray)
2-6
H
Help
1-3
Hopper
cascade assembly
2-12
sample funnel 2-12
vibration rate 2-12
Hopper feed rate
purpose
3-9
software control 3-5
Hopper instruments
definition
1-3
overview 2-12
vacuum switcher box 2-13
L
Locking handle
2-9
M
Mains power supply
2-7, 2-11
Making a measurement 3-1
Manual control 3-2
Manual measurement
procedure
4-2
Measurement Cycles tab 3-10
Scirocco 2000 Page i
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Index Scirocco 2000
Measurement display
when appears
4-2
Measurement guidelines 4-1
Measurement snaps 3-12
Measurements
manual and SOP
3-1, 4-2
Menu commands 1-3
Micro volume tray 2-5
Model number 1-1
Modes
Standby, Airflow and Feed
Multiple accessories 2-7
N
Noise protection box
2-9
O
Obscuration
in Measurement Display
to control measurement 3-11
Obscuration filtering 3-12
Obscuration limits 3-11
Obscuration triggering 4-2
Operator functions 1-2
P
Particle size (maximum)
A-1
Power requirement A-1
R
Rear panel
details
2-7
overview 2-4
Regulatory statements C-1
S
Sample area lid
2-4
Sample concentration 3-8
Sample exit port 2-4
3-8
3-3
Sample tray
(hopper instruments)
2-13
faults 3-4
function 2-5
indicator 3-5
micro volume tray 2-5
overview 2-2
selection 3-8
small volume tray 2-6
Sample tray area
details
2-5
overview 2-4
Sample tray lid
interlock
4-2
Sampler Selection tab 3-6
Sampler Settings tab 3-7
Sieve
function
2-6
Small volume tray 2-6
Software features 3-1
SOP control 3-6
SOP measurement procedure 4-4
Specification A-1
Standby mode 3-3
Status indicator 2-4
Supervisor functions 1-2
V
Vacuum
faults
3-4
second unit (hopper instruments) 2-12, 3-10
Vacuum monitor connector 2-8, 2-10
Vacuum switcher box
connector
2-7
details 2-11
fuse 2-11
overview 2-5
Vibrator faults 3-4
Page ii Scirocco 2000
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