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MAN 0101
Issue1.3
August 1997
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.
Spring Lane South,
Malvern.
Worcestershire. WR14 1XZ
U.K.
Tel + [44] (0) 1684-892456
Fax + [44] (0) 1684-892789
Printed in England
CONTENTS
Contents
Chapter 1 - Introduction to this manual
Welcome
1-1
1-1
1-2
Assumed information
1-3
Windows terms
1-3
Menu commands
1-5
1-5
Other reading
1-7
2-1
A typical system
2-1
2-2
The transmitter
2-2
2-4
The receiver
2-7
2-10
2-10
2-11
Modes of operation
2-15
Menu mode
2-15
Easy mode
2-15
Program mode
2-16
Getting help
2-16
G E T T I N G
S T A R T E D
Page i
CONTENTS
G e t t i n g
S t a r t e d
On-line help
2-16
2-17
2-17
2-17
2-18
Status line
2-19
Reporting Problems
2-19
3-1
3-1
3-2
3-4
3-6
3-6
The presentation
3-6
3-7
3-8
3-8
Page ii
Introduction
4-1
4-1
Sample preparation
4-2
4-2
4-3
4-3
4-5
As general advice
4-5
M A N
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CONTENTS
Avoiding lens cut off (Vignetting)
4-5
4-6
Making a measurement
4-6
Instrument preparation
4-6
4-8
4-8
4-10
4-11
4-11
4-13
5-1
5-1
5-3
5-3
5-5
5-6
Selecting a presentation
5-7
Special Presentations
5-8
5-8
6-1
Views
6-1
Reports
6-3
6-4
Understanding printing
6-6
6-7
G E T T I N G
S T A R T E D
Page iii
CONTENTS
G e t t i n g
S t a r t e d
6-7
6-7
6-8
6-9
6-9
7-1
Fundamental concepts
7-1
7-1
Equivalent spheres
7-2
7-3
7-4
8-1
Setting up a sequence
8-1
9-1
Representative sampling
9-1
9-2
9-3
Page iv
9-3
9-5
Surfactants
9-5
Admixtures
9-6
Slurries
9-6
9-6
M A N
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CONTENTS
Samples with unstable concentrations
9-7
Bubbles
9-7
9-8
10-1
Killing channels
10-1
10-1
10-3
10-4
10-4
10-6
10-7
Blending results
10-8
Multiple modifications
10-9
10-9
Chapter 11 - Maintenance
Introduction
11-1
11-1
Replacing fuses
11-2
11-3
11-4
11-4
11-6
11-7
Appendix A - Specification
Introduction
A-1
G E T T I N G
S T A R T E D
Page v
CONTENTS
G e t t i n g
S t a r t e d
A-1
A-2
A-4
A-5
A-6
B-1
B-1
B-1
B-1
Spray measurements
B-2
C-1
D-1
D-1
Page vi
Introduction
E-1
E-1
E-1
E-1
E-2
E-2
M A N
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CONTENTS
Appendix F - Malvern addresses
Malvern subsidiaries
F-1
G-1
G-1
G-1
Test conditions
G-1
EMC performance
G-2
G-3
G-3
Test conditions
G-3
EMC performance
G-3
G E T T I N G
S T A R T E D
Page vii
CONTENTS
Page viii
G e t t i n g
S t a r t e d
M A N
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CHAPTER 1
Welcome
Welcome to the Malvern Mastersizer Getting started manual. By now you
should have installed your system by following the instructions in the installation
manual.
This manual is designed to give a brief overview of what the Mastersizer can do
and how to do it. Obviously, all the features of the Malvern Mastersizer can not
be given within this manual. More detailed information is given in other manuals,
such as the Software Reference manual. After reading this Getting Started manual
you will be able to; identify the main features of the system, understand the basic
measurement technique, perform a simple measurement and analyse the data.
If you have never operated a Malvern Mastersizer before it is recommended that
you read this manual fully before you start your first measurement.
Warning
The Mastersizer or the samples to be measured may be dangerous if misused.
You must read the Health and safety booklet before operating the system.
Instrument.
Ref. Number.
MAM 5000
MAM 5002
MAM 5004
MAM 5005
G E T T I N G
S T A R T E D
Page 1.1
CHAPTER 1
Malvern personnel
Malvern personnel (service engineers, representatives etc.) have full access
to the instrument and are authorized to perform all service procedures that
may require the removal of the transmitter and receiver covers.
Supervisor
The supervisor is the person responsible for the management/safety of the
instrument 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 11, including changing the fuses.
The supervisor must on no circumstances remove the covers of the
transmitter or receiver and should only remove the sample area cover when
using the Mastersizer for spray measurements.
Operator
An operator is a person trained in the use of the instrument. The operator
can perform all user maintenance routines identified in chapter 11 except
for changing the fuses.
The operator must on no circumstances remove the covers of the
transmitter or receiver and should only remove the sample area cover when
using the Mastersizer for spray measurements.
Warning
Failure to follow these guidelines could result in the emission of laser
radiation. Laser radiation can be harmful to the body and can cause
permanent eye damage.
Page 1.2
MAN
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CHAPTER 1
Assumed information
For clarity this manual will assume that you have a standard bench Mastersizer S.
If there are any operational procedures that differ for the long bench Mastersizer
S or the Mastersizer X then alternative information will be given.
Most samples measured on the Mastersizer are those dispersed in a liquid. For
this reason all references to a sample preparation accessory within this manual will
refer to the Automated Sample Dispersion Unit. If you are using any other
accessory then consult its manual for details of operation, installation etc.
Within this manual it will be assumed that the flow cell is to be used. Again, if
this is not the case for your particular installation consult the accessory manuals
for details on installation and use of the cell you do have.
Within this manual the Mastersizer system will be referred to as the Mastersizer
or the system unless the information given is for a particular instrument.
Windows terms
It is important that you understand some Windows terms before reading further.
(Note that US spelling is used for some terms for compatibility)
Program - The Mastersizer software - it can also mean the Mastersizer Basic
program used within the main Mastersizer software.
Cursor or Pointer - The graphic - usually a pointer that is moved on the screen
by operation of the mouse.
Icon - The graphic on the desktop that represents a program.
Click - The mouse button is depressed and released. If this is not qualified with a
button description then assume it is the left button. Clicking a button means
click the left mouse button when the cursor is over the button.
Double-click - Press and release the mouse button twice in quick succession. If
this is not qualified with a button description then assume it is the left button.
Use the Mouse icon in the Control Panel of Program Manager to change the
double-click speed.
Dialogue Box - A window containing controls. The OK button accepts
changes in the dialogue box. The Cancel button closes the dialogue without
accepting the changes.
Control - This can mean a graphic on a dialogue like a button, listbox,
textbox etc.
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Page 1.3
CHAPTER 1
Press or Select - This means click the mouse over a control or use the
accelerator key (the underlined letter) or use the Tab key to move the focus to a
control then use the Enter key. Menu items can be selected using the cursor
keys in the same way.
ILL 1992
Button - This acts like a real-life button. Click to carry out an action. A typical
button is shown below.
ILL 1993
ILL 1994
Check Box - A button that can be toggled on and off. A check box is show below.
ILL 1995
Text Box or Edit Box - A box you can type text or values into. A text box is
shown below.
ILL 1996
List Box - A box containing a list of options. Some List Boxes allow multiple
entries to be selected.
ILL 1997
Drag - An action with the mouse which involves moving the mouse while
holding down the left mouse button. This is used for moving icons or making
multiple selections in a list box.
Page 1.4
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CHAPTER 1
Menu commands
Menu commands from the Malvern software are referred to in the form main
menu-menu item. As an example, the command File-Save Sample refers to
selecting the Save Sample item in the File menu. The same rules apply for
sub-menus of sub-menus, so that Edit-Copy-Data refers to the Data item in
the Copy sub-menu, which itself is a sub-menu of the Edit menu. Menu
commands are always shown in bold text.
G E T T I N G
S T A R T E D
Page 1.5
CHAPTER 1
Page 1.6
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CHAPTER 1
Other reading
More detail on the subjects within this manual can be found in the following
manuals:
Title
Ref. number
MAN 0102
MAN 0103
MAN 0104
G E T T I N G
S T A R T E D
Page 1.7
CHAPTER 1
Page 1.8
MAN
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CHAPTER 2
Introduction
By now you should have connected up the system by following the instructions
within the system and accessory installation guides.
Spend some time to familiarise yourself with all the physical features of the
system by reading the following sections. It is probable that you will not use all of
the features described as some are used for specific accessories or applications
only. This chapter is only intended to give you a guide to identify the features. A
description of how the system actually works and how to use it will follow in the
next few chapters.
This chapter is divided into three sections. Section one will identify the main
modules of a typical system. Section two will examine the features of the optical
unit in more detail. Finally the third section will identify the main features of the
Malvern software in more detail. Information on the sample preparation
accessories can be found in their own manuals.
A typical system
The diagram below shows a typical system with its key features of the optical unit
, one or more sample preparation accessories and a computer system .
3
E N
T S
ILL 1805
I N
S T
R U
M
The optical unit is used to collect the raw data that is used to measure the size of
a sample.
The sole purpose of the sample preparation accessory is to prepare the sample
and then deliver it to the optical unit so that it can be measured. Malvern makes
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G e t t i n g
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many sample preparation accessories to handle all forms of sample, including dry
powders, aerosols and samples dispersed in a liquid. You may have many sample
handling accessories or none at all depending on your particular requirements.
Consult the individual accessory manuals to identify the features of the sample
preparation accessories.
The computer system is a stand alone computer that runs the Malvern
software. It is the Malvern software that analyses the raw data from the optical
unit to give the size of the particles. Once completed the result can be further
analysed or reports printed etc.
The following section gives a more detailed overview of the features of the optical
unit.
ILL 3208
The transmitter
The transmitter contains the laser and electronics that produces the laser beam
that is used in the measurement of the sample.
The main features of the transmitter are on the transmitter end panel. Use the
figure below to identify these features and their function.
Page 2.2
M A N
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CHAPTER 2
FUSE
5 10
5A
0V
260V~
~
pec
rkin
g Th
ay
eW
ILL 3209
Ma
LV out connector
Connector that carries the low voltage power supply to the receiver.
Fuse holder
Fuse for the optical unit. Read the health and safety manual before attempting to
change the fuse.
Interlock connector
Laser interlock connector that shuts off the laser if any of the optical unit safety
interlocks are defeated. This connector must be connected to allow the system to
work.
Remote connector
Connection for an external laser interlock that turns the laser off when the
interlock is defeated. The usual form of this interlock is a switch on the door to
the room in which the system is installed that switches the laser off if the door is
opened. See appendix C for details.
If a remote interlock is not used then a shorting plug is connected to allow the
laser to be powered. The system will not work without a shorting plug or a
remote interlock connection.
G E T T I N G
S T A R T E D
Page 2.3
CHAPTER 2
G e t t i n g
S t a r t e d
Page 2.4
ILL 3210
M A N
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Warning!
The sample area coremoved for spray measurements. Read the safety manual
before removing the sample area cover.
Unless you are performing spray measurements do not attempt to remove the
sample area cover.
Beam expander
The beam expander is used to increase the diameter of the laser beam. Once the
laser beam has been expanded it is known as the analyser beam.
'
Note
The beam expander is actually part of the transmitter optics but has
been included here for clarity.
Range lens
The purpose of the range lens is to collect the laser light that has been scattered
from the sample and focus it onto the detector electronics.
Both the Mastersizer X and Mastersizer S have a number of range lenses available,
with each lens covering a different size range of particles. A list of lenses available
and their corresponding size range is given below.
Mastersizer X
Mastersizer S
Lens
Size range
Lens
Size range
45mm
0.1 - 80m
300RF
0.05 - 880m
100mm
0.5 - 180m
300mm
0.5 - 880m
300mm
1.2 - 600m
1000mm*
4.2 - 3480m
1000mm*
4.2 - 2000m
* The 1000mm range lens are available on long bench versions only.
G E T T I N G
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Page 2.5
G e t t i n g
CHAPTER 2
'
Note
S t a r t e d
The range lens is actually part of the receiver assembly but has been
included here for clarity.
Caution!
The optical unit will not operate correctly if more than one range lens is
mounted at any one time.
Sample cell
The sample to be measured is passed through the analyser beam by propelling the
sample through a cell. Malvern make various forms of cell to cope with different
types of material. One exception to using a cell is the case of spray measurements
where an aerosol is sprayed directly though the analyser beam.
There are three types of cell available:
Stirred cell. This is the simplest form of cell and is designed for samples
dispersed in a liquid. The sample and its liquid dispersant are placed into
the cell and the solution is kept in suspension by magnetically rotating a
stirrer bead within the cell.
Flow cell. A flow cell is also used for samples dispersed in a liquid. The
sample and dispersant are kept in suspension by an external accessory that
then pumps the solution through the flow cell.
Air cell. An air cell is used when measuring dry powders. The sample is
blown or dropped through the air cell by an external accessory.
Page 2.6
M A N
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Warning!
Always replace the accessory panels after the accessory has been removed.
Never run the system with the panels and accessory removed.
The receiver
The final part of the optical unit is the receiver unit. The receiver collects and
stores the information received from the scattering of the analyser beam as it
passes through the sample. Once the data has been collected it is sent to the
computer system for analysis.
The main component of the receiver is the detector (sometimes called the diode).
The detector is actually made up of a number of photo-diode elements that are
arranged in a radial pattern. The detector is not visible in normal use.
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S T A R T E D
Page 2.7
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G e t t i n g
S t a r t e d
Caution:
The detector is the most delicate (and expensive) component of the system. In
normal use the detector is safely contained within the covers of the receiver
unit. However, the Mastersizer X moves the detector within the covers. If the
diode was in the position required for the 45mm range lens then the detector
can be touched if the range lens was removed. On no circumstances touch or
clean the detector.
ILL 1808
The main features of the receiver unit are on the receiver end panel. Use the
figure below to identify the features on the receiver end panel and their function.
Page 2.8
M A N
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L.V. In connector
Connector that carries the low voltage power supply into the receiver.
Features to are usually used when performing spray measurements.
Abort connector
The abort connector is used to stop the experiment triggered using the Exp.
trigger above.
G E T T I N G
S T A R T E D
Page 2.9
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G e t t i n g
S t a r t e d
ILL 1867
When the Mastersizer software is installed the Mastersizer program group shown
below will appear in the Program Manager window.
There are three program icons within the program group. The first is the main
Mastersizer program icon. To enable the Mastersizer software, double click on
this icon.
The second icon is the presentation generator program. This is a program that is
usually run from the Mastersizer software but can be run independently by
double clicking this icon. The presentation generator calculates new
presentations that are used in the analysis of the measurement data.
Presentations are discussed in detail later in this manual.
The final icon is the Bitmap Editor. This program allows you to create your own
icon bitmaps.
Page 2.10
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ILL 1812
Menu bar
The menu bar contains the main menu headings for all Mastersizer functions.
There are several ways to select an item from the menu bar:
Using the mouse.
To select an item from the menu bar use the left mouse button to click
once on the menu item. The menu list will drop down. You can then select
the item from the menu list by clicking once on the item.
Using the keyboard.
To select an item from the menu bar using the keyboard, hold down the
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G e t t i n g
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Alt key and press the letter which is underlined in the item required. For
example to use the Measure menu hold down Alt and press m. Whenever
you use a key in this way it does not matter if you use upper or lower case.
M or m would both work.
Again a menu list will drop down. To select an item from the list type the
letter that is underlined. For example, typing d will select the Document...
item to enter sample details.
Using keyboard accelerators.
To the right of a menu item name there may also be a note of the
accelerator for this item. This is a key or combination of keys which can be
used to by-pass the menus. For example you can press Ctrl and N together
to select Measure-Document... without having to use the main menu and
drop down menu.
The items which end with a row of dots (...) will cause dialogue boxes to appear.
Those with no dots will cause an immediate action. For example Document...
displays a dialogue for you to enter details but Clean would cause the sample
handling unit to begin a cleaning sequence without any further action.
Some items are shown in grey. This indicates that the choice is not currently
available. For example, the Clean item may be grey because no sample handling
unit is installed and the Background, Inspect and Sample items may be grey
because these operations may not be performed until the system has been aligned.
Button Bar
Calculate
Button
The Easy button bar (or toolbar) contains a selection of buttons which you can
use to perform the most popular operations. Each button will have its equivalent
commands within the menu bar. For example using the calculate button is
equivalent to using the Calculate result... menu item from the Measure menu.
A button may represent more than one command, for example pressing the setup
button will automatically run you through the three Setup menu items;
Setup-Hardware, Setup-Analysis and Setup-Presentation.
Setup
Button
Page 2.12
The default button bar set when the Mastersizer software is first installed is:
M A N
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ILL 1810
CHAPTER 2
A - Setup
C - Document
D - Align Optics
E - Measure Background
F - Inspect Result
G - Calculate Result
H - Save Record
I - Print
J - Setup Sequence
K - Start Sequence
L - Clear Graph
M - Graph Scale Up
O - Exit Mastersizer
To help you identify a menu button a short description of the action of the button
is displayed in the status bar when the cursor is moved over the buttons - (The
cursor also changes to a picture of a hand when over a button).
As with the menu bar, if a button is not available it will be shown in a lighter
colour to show it is disabled. i.e.:
ILL 1811
The keyboard can be used to select Easy buttons by using the key combinations
which appears underneath each button. Because space is limited some of the text
has been abbreviated, for example A+S+1 means hold down the Alt and Shift
key while typing 1.
It is possible to customise the button menu to suit your own needs. See
Control-Easy Buttons in the software reference manual to change the layout of
the buttons and the pictures that are used. You can also hide the key description
which appears below the buttons.
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Table pane
The table pane is used to show the result information in tabular form. Other
information relevant to the measurement will also be shown. The type of
information displayed in the table pane is determined by the view. The software
has a list of standard views that can be easily changed by the user. Custom views
can be created by the advanced user.
To select a view, either select the View menu item or move the mouse cursor to
any part of the table pane and press the right mouse button. This action will
display a pop-up menu which shows you the selection of views available. Once
selected the table and graph pages will immediately update. See chapter 6 for
details of the views available.
Double-clicking the left mouse button in the table pane has the effect of
temporarily expanding that page to fill the window. Double-click again to restore
the split screen. Scroll bars appear on the table pane if the pane is too small to
show the whole table.
Graph pane
When a different view is selected the graph pane automatically changes to
represent the data in the table. The graph pane always shows the same result but
there are options to change the way it is displayed, for example the graph can be
shown as a histogram, oversize plot, undersize plot, frequency plot or the result
can be over-plotted on a graph of previous measurements.
The form of each graph may be modified by clicking the right mouse button over
the graph pane (or by selecting the Setup-Graph menu item). This produces a
dialogue that allows plot styles, axes and colours to be changed. See
Setup-Graph in the software reference manual for more information.
Query Cursor
If the left mouse button is pressed with the cursor over a graph the query cursor
appears.
Moving the query cursor over the graph displays information about the graph at
the co-ordinates of the cursor. A typical message would be:
x = 2.84 m, y = 11.8% (59.1%).
This means at this point of the graph that 59.1% of the sample is below 2.84
microns and that 11.8% of the sample is in that particular size band.
Double-clicking the left mouse button in the graph pane has the effect of
temporarily expanding that pane to fill the window. Double-click again to restore
the split screen. The graph will automatically fit the graph pane.
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Splitter bar
The splitter bar allows you to change the proportions of graph and table panes i.e.
to make the graph or table pane bigger or smaller.
Splitter Bar
Cursor
To move the split between graph and table panes using the mouse, move the
cursor onto the splitter bar - the arrow cursor will change to a double-headed
arrow. Now, hold down the left mouse button and drag the bar to the new
position. Release the mouse button when the desired position is reached.
The splitter bar may also be controlled from the keyboard or from the menus.
Status bar
The status bar is split into two parts. The left hand section is used to show the
status of the software. It usually shows the message Ready - Press F1 for Help. This
will change to inform you when the system is loading or saving files, calculating,
etc. As a menu is selected or the cursor moves over a toolbar button help
information is shown.
The right hand part of the status bar shows the instrument status. The instrument
status bar shows Instrument Ready if the optical unit is correctly connected and
switched on and Instrument NOT READY otherwise. The instrument status bar
will also show the progress of a measurement.
Modes of operation
The Malvern software has three main modes of operation, Easy, Menu and
program mode, which are summarised below.
Menu mode
Menu mode is the use of the menu bar and its options to control the Mastersizer.
Using the menus gives you access to all functions of the software. For full details
of all the options in menus see the software reference manual.
Easy mode
The Easy button bar (or Toolbar) provides a simple way to select frequently used
actions. For most samples a full analysis of a sample can be made by using the
buttons. The buttons can be used by relatively inexperienced operators.
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Program mode
The program mode uses the built-in program language Malvern Basic to allow
you to build complex measurement sequences with prompts to enter values,
perform actions, etc. and detailed checking of error conditions. Such programs
may be run individually, assigned to single key operations or set up to run
automatically when the software starts.
The Malvern basic language is an advanced feature that is usually used by the
more experienced user.
The full details of programming in the Malvern Basic language are given in the
Malvern Basic manual.
The three modes above are designed so they can be used in conjunction with each
other. You may find that you only need to use the easy mode buttons or just the
menu items but it is possible to use all modes in a single measurement. For
example you may align the system by pressing the align button from the button
bar, but then follow by measuring the background by using the menu item
Measure-Background.
Always remember, as with most modern Windows programs, there is usually
more that one way to operate the software. A function like printing a report for
example can be done in several ways; by using the print option in the File menu,
pressing the print button in the button bar or using the keyboard by pressing
F11.
Once you have gained experience in the operation of the Mastersizer it will be
normal for you to set up automatic sequences of measurements that will
automatically go from one procedure to the next, pausing only for you to enter
details. To do this you set up a measurement sequence. The software also
allows manual control of each stage. Even in manual control the system will take
you from one stage to the next logical stage using a single key action. The system
also locks-out actions that may lead to invalid measurements and gives warnings if
measurements are not within accepted limits.
Getting help
On-line help
Microsoft Windows contains a help program which can give information on using
Windows itself and on programs that use Windows. As well as leafing through the
manuals to find out how to do something you can also refer to the on-line Help
Page 2.16
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system. Almost all the software reference manual is available on the Help system
and in some cases is easier to search than the manual.
When the Help cursor is active clicking the left mouse button over a component
of the Mastersizer window will show help on that component. If a menu is
selected or a button in the toolbar is clicked then help will appear on that
command.
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you may find it useful to make the help window always stay on top of the
Mastersizer window.
The Help window has a row of buttons below the menu for the most used
actions:
Contents - Pressing this button send you to the main contents page.
Search - Selecting this displays the search dialogue - Searching Help.
. Type the first few letters of the item to search for in the text box. The list
box scrolls to show the item.
. Double-click the item in the list or press Show Topics. The list box at the
bottom of the dialogue shows one or more topics.
. Select the topic in the bottom list box. Double-click or press Go To.
. The help window changes to the topic.
Back - Pressing this button moves you to the last help topic displayed.
History - This button displays a window showing a list of help topics visited.
Double-click an item to go back to that topic.
<< and >> - These are the browse buttons - click these to see related topics
to the current one.
Glossary - Shows a list of glossary items. Click these to see the descriptions.
Page 2.18
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Help Jump
Cursor
The cursor also changes when it moves over certain graphics and buttons.
Clicking these items show more information about them.
Status line
When a menu is selected or the mouse cursor moves over a toolbar button the
status line at the bottom of the Mastersizer window will show information on the
command.
Reporting Problems
Before reporting a problem please check the relevant sections of the user and
reference manuals, or any accessory manuals, which may have an answer. If the
problem persists try to give as much detail as possible.
If there is a problem in the software try to give information that will allow the
engineers at Malvern to reproduce the conditions. If the problem is in the result
or the analysis the Malvern engineers will require a copy of the Data report.
A list of the Malvern subsidiaries can be found in appendix F.
G E T T I N G
S T A R T E D
Page 2.19
CHAPTER 2
Page 2.20
G e t t i n g
S t a r t e d
M A N
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CHAPTER 3
Introduction
After reading this chapter you will have a basic idea of the operating procedures of
the Mastersizer and in particular:
. Know the basic operating principles of the Mastersizer.
. Know the simple steps involved in making a measurement and analysing
the data. More detail will be given in later chapters.
G E T T I N G
S T A R T E D
Page 3.1
CHAPTER 3
G e t t i n g
S t a r t e d
Obscuration = 10.3 %
Data
Background
4500
4000
3500
3000
2500
2000
1500
1000
500
16
24
32
ILL 1857
0
40
Detector Number
Each bar in the histogram represents the light scattering from one of the
detector elements.
The detector takes a snap-shot of the scattering pattern. Obviously this
snap-shot will only capture the scattering pattern from the particles that
where passing through the analyser beam at that particular time. Taking
only one snap-shot may not give you a representative reading of the
scattering pattern. To overcome this the Mastersizer takes many snap-shots
(known as sweeps) and averages the result. Typically over 2000 sweeps are
made for each measurement, with each sweep taking 2mS.
. Secondly, once the measurement is complete the raw data contained in the
measurement can be analysed by the Malvern software using one of the
theories above.
The measurement data is analysed by first selecting a presentation. A
presentation is a predicted scattering pattern from theoretical particles. The
software has many presentations on disc that represent particles of different
materials suspended in different dispersants. You will choose the
presentation that matches the sample and dispersant you are measuring.
Page 3.2
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The presentation data is then made to fit the measurement data - this will
give you the final size distribution.
Once the data has been analysed the information can be displayed in various ways.
Usually the display will show you a graph of the result and a table showing the
same information in a tabular form. The graph below shows four of the more
common graph types for displaying the result.
Volume %
20
100
90
80
70
60
10
50
40
30
20
10
100.0
Particle Diameter ( m.)
ILL 1869
0
10.0
The histogram displays the result in the form of in band percentages. i.e. each
bar in the graph represents a size band of particles (52 - 59 microns for example)
and the height of the bar represents the percentage of the sample that is within
that band. The histogram graph uses the left scale. Unless you change the size
bands, the initial analysis uses the size bands that are set by the physical design of
the detector.
The undersize plot displays the result in the form of % of sample below a
certain size of particle. For example by reading the values from the graph you
may be able to determine that 10% of the sample is under 23 microns etc. (the
exact value can be read from the table that will accompany the graph). The
undersize plot is read from the right hand scale on the graph. The undersize plot
is calculated from the initial size bands by fitting a curve to the analysis data so
that values within a size band may be read.
The oversize plot is similar to the undersize plot except that the result is in the
form % of sample above a certain size of particle. For example by reading the
values from the graph you may be able to determine that 90% of the sample is
above 23 microns etc.
The frequency curve is calculated by differentiating the undersize curve. The
frequency curve is particularly useful for displaying the results to show the
G E T T I N G
S T A R T E D
Page 3.3
CHAPTER 3
G e t t i n g
S t a r t e d
modes or peaks in the graph. Several peaks in the graph indicate that there are
distinct sizes of particles within the sample. This at a glance inspection of the
results will be difficult if the result was shown as an undersize or oversize plot.
Another use for the frequency curve is to compare results from different
measurements - over-plotting results can be done using other graph types but the
graph may become confusing.
It is usual for the operator to use the software to setup a sequence that will
automatically go through the procedures above in one go. There is a large choice
of options when setting up a sequence, for example, you can easily arrange for the
Mastersizer to measure a single sample many times, each time analysing the
measurement data (using a pre-chosen presentation), saving the result and
over-plotting each result on a graph.
Alternatively you can go through each stage individually. Before you setup a
sequence it is important to understand the procedures in each stage. The
following section explains these procedures
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'
Note
G E T T I N G
S T A R T E D
Page 3.5
CHAPTER 3
G e t t i n g
S t a r t e d
The presentation
As stated earlier, the Mie theory needs to know specific information about the
structure of the sample and the medium it is suspended in so that it can calculate
exactly how light passes through them. The specific information required is the
relative refractive index of the particle to be measured, the particle adsorption
Page 3.6
M A N
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CHAPTER 3
(imaginary refractive index) and the refractive index of the medium that the
particle is suspended in (dispersant).
Once the Malvern software knows this information it can calculate the expected
scattering pattern from these particles. This scattering pattern is known as the
presentation. The presentation is identified by a label of the form 3OHD.
The details of how these codes are made up will be discussed later.
There are three ways of selecting a presentation.
. The easiest way is to use one of the four default or system presentations. These are;
Fraunhofer (3$$D). This is the presentation that is used when you wish
to use the simpler Fraunhofer model.
Standard - Wet (3OHD). This is a presentation that takes a middle of
the road value for the refractive index and adsorption of the sample and
assumes that the particle is suspended in water.
Standard - Dry (3RHA). This presentation is the same as standard-wet
except assumes that the particle is suspended in air.
Reference Reticle (3$$1). This is the presentation that is used when the
Diffraction Reference Reticle accessory is used to validate the system.
Obviously this will only be used if you have the accessory. Read the
Diffraction Reference Reticle accessory manual for further details.
. For a more accurate choice you can enter the refractive index of the particle
etc. and the software can then find the nearest match from the many precalculated presentations stored on the computer.
. Thirdly, if you require an exact presentation you can again enter the particle
details and then ask the software to generate the exact presentation.
You may ask yourself If I can generate the exact presentation why bother with a
default or near-match choice. Firstly, generating the exact presentation takes
time. Secondly, for most samples using either the standard-wet or standard-dry
presentations are more than sufficient. Choosing another presentation is only
required in specific circumstances, such as the majority of particles being under
10 microns in size. Details of choosing the correct presentation are given in
chapter 5. Until you know more about choosing a presentation it is
recommended that you use one of the two standard presentations.
G E T T I N G
S T A R T E D
Page 3.7
CHAPTER 3
G e t t i n g
S t a r t e d
Page 3.8
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Sample file:
Monday.SAM
Record Number
Run Number
10
11
12
As can be seen, the run number is reset after each batch of 3 samples. So, for
example, to see the data for the second sample taken two hours into Monday, you
will open record number 5 from the MONDAY.SAM sample file.
G E T T I N G
S T A R T E D
Page 3.9
CHAPTER 3
Page 3.10
G e t t i n g
S t a r t e d
M A N
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Making a measurement
CHAPTER 4
Introduction
It is usual for the operator to use the software to setup a sequence that, once set
up, will automatically go through the procedures of measuring the sample,
analysing the data and saving the results by simply pressing a single button.
However, it is important to know the individual stages that are involved. This
chapter is concerned with the measurement of the sample - the next chapter will
give the practical details on analysing the data.
In chapter 3 the section How to make a measurement gave a brief overview of
the stages involved in making a measurement. These stages where:
. Setup the system.
. Document the sample.
. Align the optics.
. Measure the background.
. Add the sample.
. Measure the sample.
This chapter will explain the practical steps of each of these stages. It has been
found that the best way to learn how to measure a sample is to actually make a
measurement on a system. To get the most benefit from this chapter it is advised
to read through the chapter first and then to go through a second time following
the instructions to make a measurement on the system.
To do this you will need a suitable sample to measure and a suitable dispersant to
disperse it in. Either ordinary dairy cream or a PVA glue dispersed in water are
readily available samples and dispersant that should give you good predictable
results.
By the end of this chapter you will have gained the practical knowledge that is
needed to perform a measurement, such as which range lens to choose or how to
prepare the sample etc. This knowledge will allow you to understand the
procedures involved in setting up a measurement sequence.
GETTING STARTED
Page 4.1
Getting Started
CHAPTER 4
Sample preparation
Firstly the most important thing to consider is the preparation of your sample
before it is measured. A representative sample must be taken. Dry powders, for
example, tend to separate out if stored for some time or vibrated. The larger
particles tend to rise to the top and the smaller particles collect at the bottom of
the container. If you were to take the sample from the top of the container it will
not contain the smaller particles, giving you a biased measurement. The sample
should be correctly mixed before a measurement is taken.
Wet samples have also to be correctly dispersed in a liquid dispersant. Using the
wrong dispersant can cause the sample to stick together in lumps, float on the
surface or even dissolve. The sample and dispersant should be checked to see if
they are suitable before a measurement is made. There are many ways to prepare
your sample to ensure a perfect measurement.
Details on sample preparation are given in chapter 9.
'
Note
It has been found that over half the problems encountered in measuring
the sample have been caused by bad sample preparation. It should be
obvious that if you make a bad measurement that no amount of
analysing will give you a good result.
Page 4.2
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Mastersizer X
NOTE'
Each lens can be
identified by removing
the front lens cap. The
name of the lens is
engraved on the lens
ring.
Mastersizer S
Lens
Size Range
Lens
Size Range
45mm
100mm
300mm
1000mm*
0.1 - 80 m
0.5 - 180 m
1.2 - 600 m
4.0 - 2000 m
300RF
300mm
1000mm*
0.05 - 880m
0.5 - 880m
4.2 - 3480m
GETTING STARTED
Page 4.3
CHAPTER 4
Getting Started
20
100
90
80
70
60
10
50
40
30
20
10
0
0
100.0
1000.0
ILL 1870
10.0
The graph shows that the distribution is cut off at the large size end. Clearly there
is a significant amount of material at sizes above 900m. Not only is this material
missed in the measurement but the light scattered by that material also distorts
the measurement of the material which is in the range. For such a material, the
4-3500m range (1000mm lens on the Mastersizer S) would be more suitable as
shown in the second graph below.
10
100
90
80
70
60
50
40
30
20
10
0
100.0
1000.0
10000.0
ILL 1871
0
10.0
Page 4.4
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CHAPTER 4
As general advice:
. Spray measurements should only be performed on the 300mm or
1000mm* lens.
. Samples dispersed in a liquid should initially be tried using the 45mm lens
on the Mastersizer X or the 300RF lens on the Mastersizer S. If the size
range of the sample is then found to be outside the ranges for these lenses
then try another lens.
Mastersizer X
Mastersizer S
Lens
Lens
100mm
300mm
1000mm*
24
84
290
300mm
1000mm*
36
290
GETTING STARTED
Page 4.5
Getting Started
CHAPTER 4
The lens cut off point is only an issue when using the Mastersizer for spray
measurements. Other forms of measurement use a cell to confine the samples
within the measurement zone.
'
Note
Making a measurement
We shall now go through the practical steps in making a measurement.
Instrument preparation
By now you should have connected the system by following the instructions in
the installation manual and the dispersion unit manual (We are assuming that you
are using Automated Sample Dispersion unit - if not consult the manual of the
accessory that you do have). Check that:
. The computer, optical unit and dispersion unit are connected and switched
on.
. For this measurement the 300RF lens (Mastersizer S) or the 45mm lens
(Mastersizer X) is fitted and both lens caps are removed.
. The beam expander is fitted and the lens cap removed.
Page 4.6
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CHAPTER 4
. The flow cell is fitted and the pipes are connected to the dispersion unit according to the instructions in the Automated Sample Dispersion Unit manual.
Before you begin a measurement you will have to tell the computer about the
physical features that you have just set up, i.e. which lens and sample accessory
you are using. These details are entered by filling in the Setup Hardware
dialogue.
This only needs to be done once and will only have to change if you change a lens
or an accessory. The computer will remember the setup if you save the
configuration. You will be automatically asked if you wish to save the
configuration when you exit the software.
. Select Hardware from the Setup menu. The dialogue below will appear.
2
ILL 2055
NOTE'
It is not essential for the
operation of the system to
change the name of the
sample unit - it is
recommended however as
the name of the sample
. Change the range lens setting by clicking on the arrow and selecting
300RF for the Mastersizer S or 45mm for the Mastersizer X.
. Change the sample unit by clicking the arrow and selecting Auto Sample Dispersion Unit. If you do not have a Automated Sample Dispersion
Unit then select the option for the accessory you do have.
. Select OK.
Remember to save the configuration when prompted to do so when exiting the
software!
GETTING STARTED
Page 4.7
CHAPTER 4
Getting Started
An alternative to
selecting
Measure-Document is
to press the document
ILL 2056
button.
. Within the box labelled Sample name type in a name for the measurement. The name can be up to 20 characters. For this demonstration type
Cream or PVA glue depending on the sample you have chosen.
. The Notes section can take up to 4 lines of text that describes your measurement. For example, type in Water dispersant. Using Automated Sample
Dispersion Unit - pump speed 75% stirrer 50%, ultrasound 20%
. Select OK.
Page 4.8
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ILL 2057
CHAPTER 4
The ease of use of the Malvern software is demonstrated with these windows. It is
of course possible to perform each of these tasks individually by first selecting
Align from the Measure menu, aligning the system, then closing down the align
window and then opening the next window, etc. A far easier way is to use the
Next button. Pressing the Next button will take you automatically to the next
logical dialogue in the sequence. Continually pressing the Next button will take
you through the complete measurement sequence.
The Next button is one of four buttons in the measure window that allow easy
control of the measurement sequence. A quick summary of these four buttons are
shown below.
Start. The Start button starts the measurement (either align,
background, inspect or sample). When the start button is selected it
will change to say stop, allowing you to stop the task at any point. When
the task is completed the button will change back to start.
Close. The Close button will close down the current measure dialogue
and return you to the main screen.
Next. As described above, the Next button will take you to the next logical
step in the measurement sequence.
Previous. Pressing the Previous button will take you back to the previous
measurement window. For example, if you pressed the Previous button
while in the Measure-background window it will take you back to the
Measure-Align window, allowing you to re-align the system if you
require.
Two other features of the Measure windows are the live display and the laser
power bar .
GETTING STARTED
Page 4.9
CHAPTER 4
Getting Started
The live display shows the scattering pattern that is detected by the detector. As
stated earlier, the detector is actually made up of series of photo diodes, arranged
in a radial structure. The individual diodes are numbered, with the diode at the
centre being numbered zero. The live display shows the scattering pattern from
diode 1 outwards.
NOTE'
An alternative to
selecting
Align-Measure
from the menus is to
select the align
button.
The laser power bar gives an indication of how well the system is aligned. The
laser power bar gives a reading from the central detector (detector zero). The bar
is colour coded to give a visual indication of the laser power, if the bar is green
then the laser power is acceptable. If red then the laser power is too low. The laser
power bar is linked to the laser power reading that shows the laser power as a
percentage.
The rest of this section will take you through the rest of the measurement
sequence using the measure windows.
'
Instead of manually
doing an alignment
you may chose to
enable the
Intelligent Align
control in the Set
Alarm Limits
dialogue. This
automatically
The laser must be aligned centrally on the detector. An alignment must be made
whenever any of the optics (the cell, range lens, beam expander etc) are removed
or replaced. An alignment should also be made after the system has been first
switched on and had time to stabilise its temperature. If an alignment has not
been made the software will not allow you to go on to the other measurement
dialogues by greying out the options.
. Select Align from the Measure menu. The dialogue below will appear.
1
performs an
alignment before
each background
measurement if it
senses that the
alignment has
degraded. A good
alignment must still
be performed
manually at the start
of the session or
ILL 2058
whenever a range
lens is changed.
. Select the Start button and the instrument will automatically align. The
Start button will change to Stop. When the alignment is complete the
button will change back to Start. Alignment usually only takes a few sec-
Page 4.10
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CHAPTER 4
onds to complete, but if the system is badly out of alignment it may take up
to two minutes.
When aligned the laser power reading should show a value greater than 75.
. From the Measure-align dialogue press the Next button. The Measurebackground dialogue shown below will appear.
ILL 2059
button.
. Press the Start button and the background measurement will automatically
start. Messages will appear on the right hand status line to show the progress of the measurement. The Start button will change to Stop while
the measurement takes place, allowing you to stop the measurement if you
need to. When the button changes back to Start the measurement is complete.
GETTING STARTED
Page 4.11
CHAPTER 4
Getting Started
The system measures whether the concentration is suitable by monitoring the
obscuration of the beam caused by the sample being added to the dispersant.
The obscuration is simply the fraction of light lost from the analyser beam
when the sample is introduced. For example an obscuration of 30% means that
30% of the analyser beam (recorded during the background measurement step)
has been lost to either scattering or absorption.
The Measure-inspect dialogue will tell you the exact concentration of the
sample within the dispersant and whether it is ideal, too low or high etc. The
obscuration bar ( in the figure below) gives a visual indication of the
concentration of the sample. If the bar is green then the concentration is in the
correct range. If orange then it is approaching the correct range and if red then the
concentration is out of range. The exact obscuration is given at the bottom left of
the dialogue ( in the figure below). The instrument has a wide range of
concentrations that are ideal and thus concentrations do not have to be precise.
The range of concentrations over which the instrument can be used can be
conveniently expressed in obscuration terms as below.
Obscuration ranges
Range %
Bar colour
Notes
<5%
5 - 10 %
Red
Orange
10 - 30 %
30 - 50 %
Green
Orange
>50 %
Red
Before you add the sample to the system it is usually best to pre-disperse the
sample within a little of the dispersant to form a slurry. To do this add a small
amount of your sample (in this demonstration use either ordinary dairy cream or
PVA glue) to a small beaker and add water. Use a pipette to thoroughly mix the
sample. When you come to measure your own samples, other than cream or PVA
glue, it will be of great benefit to read chapter 9 on sample preparation.
Page 4.12
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NOTE'
If you are not in the
Measure-background
dialogue you can select the
Measure-inspect dialogue
by selecting Inspect from
the Measure menu or
alternatively you can select
ILL 2066
. Press the Start button and the instrument will start to measure the obscuration. The Start button will change to Stop while the measurement takes
place, allowing you to stop the measurement if you need to.
. Using the pipette add the sample to the dispersion unit. Add a few drops at
a time and allow the sample to be thoroughly mixed within the dispersant.
Look at the obscuration bar. The objective is to add enough sample to turn the
bar green (giving a value of between 10 and 30%) on the readout .
Once you are satisfied that the sample concentration is in the correct range you
can continue to the final stage of the measurement.
Caution
Do not spill any dispersant or sample onto the surfaces of the cover. It has been
found that certain substances can cause permanent damage to the covers. All
spillage should be scrupulously cleaned up immediately.
. From the Measure-Inspect dialogue press the Next button. The dialogue
below will appear.
GETTING STARTED
Page 4.13
CHAPTER 4
NOTE
Getting Started
'
ILL 2060
Measure menu.
. Press the Start button and the measurement will start. The Start button
will change to Stop allowing you to stop the measurement if you require.
Once the measurement is complete the button will change back to say
Start.
The measurement is now complete. The next procedure to follow is the analysis
of the data you have just measured. This is described in the next chapter. At this
point you have the option of saving your measurement data - for this
demonstration though we will carry on with the analysis and save the result later.
The dialogue at present will still show the Measure-Sample dialogue. It is
possible to press the Next button that will take you to the next logical step in the
procedure - analysis of the data. At this point it is not recommended as it will
analyse the data using the parameters of the last sample analysed. It will be of
more benefit to you to follow the procedure in the next chapter that will explain
the setup of the analysis.
To close down the Measure-Sample dialogue press the Close button.
Page 4.14
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Analysing the
measurement data
CHAPTER 5
Introduction
This chapter describes the analysis of the measurement data. There are three steps
involved; choosing the analysis mode, choosing a presentation and finally telling
the software to calculate the result. It should be remembered that the
measurement data is never changed during the analysis. This allows the operator
to re-analyse the measurement data using different choices of analysis mode or
presentation.
Normally you would probably choose the analysis mode and presentation before
you made the measurement so that when the measurement was complete you
would only have to select the Next button to analyse the result. However for this
demonstration it will give you a better understanding of the way the system
operates by selecting the options now.
Again you will gain most benefit if you were to analyse actual data on the system.
It is recommended that you read through this chapter once then go through a
second time following the instructions to analyse the data you measured in the
previous chapter.
By the end of this chapter you will gain the practical knowledge that is needed to
choose the correct analysis mode and presentation.
G E T T I N G
S T A R T E D
Page 5.1
CHAPTER 5
The choice of which model to use is very simple - unless you definitely know
that the result graph will be of a particular shape always use the polydisperse
model.
So, when will you use the other modes?
The multimodal model assumes that there are a few distinct sizes of particles
within the sample. For example your sample may be made up of predominantly
10 micron, 50 micron and 100 micron particles. You will use the multimodal
model only if you are sure that your sample is made up of distinct sizes.
The monomodal model is very similar to the multimodal model but will assume
that there is only one size of particle in the sample. Typically this will be used for
measuring standards such as latex samples that have been specially made to be
of a known size. Again, only use this model if you definitely know that the
sample is made of single sized particles.
Very polydisperse is only used on the Mastersizer X and is a special purpose
model that is similar to polydisperse but provides a smoother analysis for samples
which have a broad size distribution extending over the majority of the size range
covered by the range lens in use. You will typically use this analysis mode for
measuring dry materials such as cement or soil.
Compressed range analysis has a reduced upper size limit and is meant for use
with dry powder and spray measurements. The compressed range analysis
disables the use of Kill Data low. This analysis is only used on the Mastersizer S.
ILL 2061
. Select Analysis from the Setup menu. The screen below will appear.
. Make your choice of analysis from the Analysis model section of the dialogue box. For this demonstration select polydisperse.
. All other choices on the screen, such as kill data and Particle density are
for the advanced user only.
. Select OK.
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Remember - unless you definitely know that the result graph will be of a
particular shape always use the polydisperse model.
G E T T I N G
S T A R T E D
Page 5.3
CHAPTER 5
chosen to give the widest choice of popular values. There are many reference
books available that state the refractive indices of materials.
Instrument
First
Relative
Second
Relative
Third
Dispersant
Fourth
character
particle
character
refractive
character
refractive
characte
index
refractive
index
index (real)
(imaginary)
Mastersizer X
0.5
Mastersizer S
0.75
0.0001
1.2
1.001
0.0003
1.3
1.002
0.001
1.33
1.003
0.003
1.4
1.005
0.01
1.5
1.007
0.03
1.6
1.01
0.1
1.7
1.015
0.3
1.02
1.03
1.045
1.065
1.095
1.15
1.2
1.3
1.45
1.65
1.95
2.35
The third character represents the imaginary refractive index of the sample, (this
is effectively its absorption). If the particle has an imaginary refractive index of
0.003 then the third character will be E, if it has a value of 0.1 then the third
character will be H etc. Choosing the value for the imaginary refractive index can
be difficult as the value has to be calculated by performing an experiment.
Page 5.4
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However, in most cases the value can be guessed with very little effect on the
result. In practice you will probably only use two values; if the sample is
transparent (glass beads for example) then there will be no absorption so the value
will be 0 (A on the grid), otherwise use 0.1 (H on the grid) as the absorption
value. If you feel you need a more accurate value then it can be calculated by
following the procedure in appendix D.
Finally the fourth character gives the refractive index of the dispersant the sample
is suspended in. As an example, if the sample is suspended in air then the fourth
character will be A (refractive index of air is 1) or if the sample is suspended in
water then the fourth character will be D (refractive index of water is 1.33). Again,
there are many reference books available that state the refractive indices of
materials.
In very rare circumstances you may find that the choice of presentation is critical
to the results and the values on the Malvern presentation grid are not accurate
enough. In this situation a presentation can be generated that use the exact figures
for the refractive index etc.
ILL 1872
This screen gives you three ways to select a presentation. These options are:
. The simplest way to select a presentation is to select one of the system presentations . There is a choice of four presentations usually you will only
use one of the two standard presentations.
. Secondly, if you know the Malvern presentation code you can choose from
the Select by code section . This lists all available codes that are currently on the system.
G E T T I N G
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. The right side of the screen gives the option of selecting or generating a
custom presentation. The list gives a choice of four of the custom presentations available. Selecting the Request button will allow you to select another custom presentation from those currently available.
There is also an option for you to enter the refractive indices of a new sample and
dispersant. When these details have been entered the software will give you the
option to:
. Use a presentation that is the closest match from the existing presentations.
. Calculate a new presentation based on the values within the Malvern presentation grid.
. Calculate a new presentation based on the exact values entered.
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The following is general advice on how important the choice of presentation is:
. If the ratio of the refractive index of the particle and the refractive index of
the dispersant is greater that 1.2 and the size of the particles are over 10 microns then the choice of presentation is not important.
. If the ratio of the refractive indices is between 1.1 and 1.2 and the particle
size is over 1 micron then the presentation is important.
. If the ratio of the refractive indices is under 1.1 or the size of the particles is
under 1 micron then the presentation is critical. Contact Malvern for an appropriate model matrix.
. If the ratio of the refractive indices is under 1.1 and the size of the particles
is under 1 micron then the presentation is critical. Contact Malvern for advice.
The absorption of the particles also plays a role, the higher the absorption, the less
critical is the optical model. However the above advice is good for any absorption.
It should be clear to the user that for liquid sprays in gaseous atmospheres, and for
dry powders the optical model dependence is not strong due to the high
differential of the refractive indices involved. For these types of experiments the
user will not find the choice of presentation is not critical and the standard
presentation will be entirely adequate.
It is worth pointing out in many cases it is possible to choose a different
dispersant to create a high differential refractive index where difficulties are being
experienced with the normal choice.
Selecting a presentation
For this demonstration we will assume that the system presentations are adequate.
Details on selecting a custom presentation can be found in the Software reference
manual.
$ To select a presentation
. Select Presentation from the Setup menu. The dialogue below will appear.
. The sample you have just measured is dispersed in water so you will select
the Standard - Wet system presentation .
. Select Load from the dialogue box .
The software will load the selected presentation and return to the main screen.
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ILL 2062
Special Presentations
The system presentations contains two special presentations, Fraunhofer 3$$D
and Reference Reticle 3$$1. There is also a third special presentation, 3$$A, that
can be found when you select a presentation by using the Select by code facility.
The two presentations 3$$A and 3$$D on your disc are the Fraunhofer
presentations for samples dispersed in air with refractive index 1.0 (3$$A) and
dispersed in water with refractive index 1.33 (3$$D). These are provided to allow
the Mastersizer to be compared with other instruments that only provide the
simpler Fraunhofer analysis. The Fraunhofer model is applicable with reasonable
accuracy down to approximately 10microns. Below this it becomes systematically
in error, to a degree which of course depends on the actual optical properties of
the sample, with a tendency to overestimate the volume of fine particles. For this
reason it is advisable to use one of the Standard model unless the measurement
is specifically intended to be compared with other equipment which uses
Fraunhofer scattering theory.
A special presentation, 3$$1, is provided for use with the Malvern Diffraction
Reference Reticle. Contact your Malvern Instruments representative, or see the
Reticle manual, for more information.
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ILL 1927
. Select Calculate Result from the Measure menu. The Calculate Result
dialogue box will appear. This dialogue is shown below.
The Calculate Result dialogue shows the progress of the analysis by displaying
the residual. The residual is an indication of how well the presentation data is
fitted to the measurement data and is given as a percentage. A final residual of
under 1% shows a good fit.
Once the calculation is complete the graph and table panes update to show the
new result data. The final result can be displayed in many ways. You will now
need to view the result to gauge whether the result is acceptable.
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Introduction
Now that you have measured your sample you can display and print reports of the
results and data generated.
This chapter runs through the options you have for displaying and printing the
results. This chapter should be read in conjunction with the next chapter that
gives advice on understanding the information within the results.
By the end of this chapter you will be able to change the way the result is viewed
and printed using the standard reports supplied with the Mastersizer.
A detailed description of each of the views is given within the Software Reference
manual.
Views
ILL 1934
The first five views display the result data in different ways, for example some
views display the data in a % under format (i.e. 15% of the sample is under 1.5
microns etc) and other views display the data in a % within size band format
(i.e. 5% of the sample is between 1.2 and 1.6 microns etc). Other views arrange
the data to be displayed within custom size bands so that the information
measured on the Mastersizer can be compared to various standards. The ASTM
E11:61 and BS410:1986 views for sieves, for example, display the data in a format
that can be compared directly with these two sieve standards.
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'
Note:
S t a r t e d
The sixth result view shows the current shape correction table. See chapter 10 for
details on shape correction.
As well as these first six standard views there are five other views available within
the view menu. These last five views help you to inspect and compare the data
and results. For example the Data view displays the measurement data before it
has been analysed. The Fit view allows you to view how well the analysed data has
been fitted to the measurement data. The Statistics and Difference views allow
you to compare one result with another etc.
The Parameters view shows the current settings of the instrument. There is no
graph associated with this table.
NOTE'
An alternative to
selecting the Graph
option from the Setup
Most (but not all) views are separated into a table and a graph. The graph can be
made to display the information in different ways by altering the settings within
the Setup-Graph dialogue box. This dialogue gives you options on the way the
graph is drawn. The Graph setup dialogue is shown below.
ILL 1847
The Plot Types section of the dialogue allows you to plot the graph in various
formats. For example the data can be plotted as a frequency curve, histogram
undersize or an oversize plot. It is possible to select more than one plot type
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so, for example, you could have the data plotted as undersize, oversize and as a
histogram on the same graph.
Other options within the dialogue allow you to change the format of the axis.
Any changes made to the graph is reflected in the table pane. For example, if the
graph is changed from plotting an undersize plot to a histogram plot then the
table pane will change from displaying the data in an % under to % in band
format automatically. If the result is modified by using some of the advanced
analysis features discussed later in chapter 10 the results in the table pane are
colour coded to highlight the data that is affected. The colours used are:
Colour
Represents
Black
Dark Red
Green
Blended results
Magenta
Dark Blue
Extended results
Light Blue
Transformed results
Each view is produced using the Malvern page description language which is a
sub-set of the Mastersizer Basic language. It is possible for the advanced user to
create their own views to display the information in a format specific to their own
requirement. New views can be assigned to the View menu - see Setup-Table
in the software reference manual for details.
Reports
Each of the standard views that is provided by Malvern has a corresponding print
report that will allow you to print the data within the view. Each report is
designed to suit A4 size paper. The report contains the same information as in the
table and graph panes except that up to 4 lines of sample documentation are also
included in the report.
As with the table pane above, any result modification will be colour coded on the
printed report using the same colour codes as above.
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G e t t i n g
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If you are an advanced user you can also customise the report to display the
information to suit you own needs using the Mastersizer Basic language. See the
Malvern Basic Reference manual (MAN 0103) for more information.
$ To print a report
ILL 1866
. To print a report of the view you are currently in select the Print item in
the File menu. When selected the dialogue below will appear.
NOTE'
An alternative to using
the File-Print menu item
is to select the Print
button.
The dialogue gives you the option to print either one or more from the choice of;
a report, graph, table or a view of the whole screen. If you wish to print a graph
you will have further options on whether the graph is printed on a full page, half
page or third of a page.
Further information on printing is given at the end of this chapter in the section
Understanding printing. This section will go into more detail on how to
optimise the print out and how to install and setup a printer. If you are reading
this manual for the first time you may feel that this information will not be of
much benefit at present. If, however, you are experiencing difficulties with
printing you may find this section useful.
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not require your data to be presented in a format that can be compared to sieve
measurements then you will never use the three standard views on sieve
standards.
The following section gives an overview of the views available. Take time to read
through the section - you should be able to quickly identify the views that are not
applicable to your type of analysis.
View - Result 1 Analysis Sizes.
This shows the result of the analysis in terms of the measurement size bands.
This range is increased if the result is extended or blended.
View - Result 2 Histogram Sizes.
This shows a higher resolution than the analysis size bands. You can change the
number and range of the size intervals. This range is increased if the result is
extended or blended.
View - Result 3 Derived Diameters.
This shows various derived diameters, the distribution moments of volume,
surface, length and number, the distribution percentiles and result modes.
View - Result 4 ASTM E11:61 Sieves.
This shows the standard ASTM sieve size bands. Size bands outside of the
instrument range are shown in red.
View - Result 5 BS 410:1986 / ISO 565:1990 Sieves.
As Result 4 but for the BS 410 / ISO 565 sieve size bands.
View - Result 6 Shape Factor.
The shape factor correction terms for the current result.
View - Data
This view shows the light energy data as measured by the instrument. There are
three columns, background signal (light without any sample added), signal
(sample added) and data (signal minus the obscuration corrected background).
View - Fit
This shows the analysis fit to the data and the difference between them.
View - Parameters
This view shows various system parameters such as current file name, record
number and measurement details etc - a graph is not shown.
View - Difference
This view shows the difference between the current result and a result set as the
reference. An information message appears if no reference record has been set.
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Understanding printing
This section goes into more detail on the subject of printing. If you are reading
this manual for the first time you may feel that the information within this section
will not be beneficial at this point. If so, go onto the next chapter.
Printing in Windows is page based. That is, a page must be complete before
printing will start. Because of the Multi-tasking nature of Windows the printing
can take place in the background, that is, at the same time as the user is doing
something else. However, before printing can start the page must be made up
and, because of Windows extensive use of graphics, this can take some time. To
find out more about printing from Windows read about Print Manager in the
Microsoft manual or start Print Manager from the Main group and use the Help
system.
To optimise printing requires a compromise between print quality and speed. To
improve printing speed:
. Choose Draft Table Quality from the File-Print... dialogue box. This
disables the drawing of lines and boxes in Tables and Reports. Pictures,
such as Logos, are also disabled but the system graphs will still appear in Reports. All text information in tables will use the Draft font set up in Setup Table....
. Choose a printer-resident font. The Draft font is usually a printer resident
font. From the Setup -Table... dialogue box check the Draft Font radiobutton then select the Setup Font... button. The list of fonts include symbols to the left of the font name will appear. Printer-resident fonts have a
picture of a printer. If you select a printer-resident font but still have
graphic lines and boxes in the same area of the page then the printing may
actually be slower, because the printer has to make one pass to do the graphics and another to do the text.
. Choose a lower resolution for graphics printing. Use the Microsoft Control Panel to change the resolution. With a lower resolution there is less information to print and hence it is faster.
. Disable colour printing. Dot-matrix printers with coloured ribbons require
one pass of the print head for each of the 4 colours and hence are very slow.
Change to a black ribbon and remove the check from the Use Colour
checkbox in the File-Print dialogue box. Note that the Hewlett-Packard
colour DeskJets are not substantially faster in monochrome.
Once printing has started you have some control of the printing speed by altering
the priority in Print Manager. The Priority setting is done from the Options
menu. With high priority the printing will complete sooner, but other
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applications, such as the Mastersizer software, will become less responsive to the
keyboard and mouse.
If you have sufficient memory installed you might consider installing a ramdrive.
The Print Manager is able to use this area of memory for temporary spooling
instead of writing files to the hard disc. To install a ramdrive please consult the
DOS manual provided with your system.
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G e t t i n g
S t a r t e d
See the Table Font dialogue in the software reference manual for details on
changing a font.
When selecting the Draft font you can choose a printer resident font (ones with a
small picture of a printer beside their names in the font list box). These
sometimes print faster and do not have to be represented on the screen.
Note that the font size will have an effect on the size of the table. All the tables
provided by Malvern use a line spacing set by the font in use. If the font size is
increased the table will increase in length and may not fit on the screen or the
printed page. A font size for Font 1 of 10 points or smaller should be used.
$ To install a printer:
. Start the Microsoft Control Panel. This is in the Main window group.
. Select the Printer icon by double-clicking with the mouse or moving the
highlight with the cursor keys and pressing the Enter key.
. Select the Add >> option. A list box is produced.
. Select your printer from the list and press Install.... The Control Panel
then gives you instructions on how to install the driver.
$ To set up a printer:
. From the Control Panel Printer dialogue box select the Connect.. button.
. Select the port for the printer. This will generally be LPT1. If you have a serial printer remember that COM1 is used by default for the Mastersizer interface.
. To set other options such as time-out and re-try times refer to the Control
Panel Help system.
. Select OK to return to the main screen.
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. Select the Setup... button. A dialogue box is produced that allows printer
options to be changed. Refer to the Help system by selecting the Help button on this dialogue. Pay particular attention to the resolution setting.
If you have installed more than one printer make the one you will use most of the
time the default.
ILL 1848
Using the File-Print... menu item or the Print Easy button will produce the
print dialogue:-
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CHAPTER 7
Introduction
This chapter sets out to give you guide-lines on the interpretation of the results
that the Mastersizer generates. The first section explains some important concepts
that you have to understand before proceeding.
The second section runs through some of the terms and expressions that are used
in the standard views.
Fundamental concepts
To understand the meaning of the results from the Mastersizer there are a
number of fundamental concepts which may require explanation. These are:
. The results are volume based.
. The result is expressed in terms of equivalent spheres.
. The derivation of distribution parameters.
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G e t t i n g
S t a r t e d
%
30
20
1
10
2
0
1.0
10.0
100.0 1000.010000.0
ILL 1874
0.1
Equivalent spheres
The Mie theory presumes that the particles you are measuring are perfect spheres.
In practice they are very rarely so. This causes a problem in the definition of the
term measure the particles size - if the particle is an irregular shape which
particular dimension do you measure?
As an example, imagine that I give you a matchbox and a ruler and ask you to tell
me the size of it. You may reply by saying that the matchbox is 50mm x 25mm x
10mm. You cannot say that the matchbox is 25mm as this is only one aspect of
its size. It is not possible to describe the three dimensional matchbox with one
unique dimension. Obviously the situation is even more complex for irregular
shaped particles such as grains of sand or the pigment particles in paint.
Most people want a single measurement to describe their sample i.e. they wish to
say that their sample is made up of 50 micron particles for example. What is
required is a unique number that describes the particle. There is only one shape
that can be described by one unique number and that is a sphere. If we say we
have a sphere of 50 microns, this describes it exactly. We cannot do the same even
for a cube as 50 microns can refer to its edge or to a diagonal.
One way to get a single unique number to describe your irregular shaped particle
is to compare some feature of the actual particle to an imaginary spherical particle.
Some typical methods of doing this are:
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. Equivalent surface area. You can calculate the diameter of a theoretical
sphere that has the same surface area of the original particle.
. Equivalent maximum length. This is where the diameter of a theoretical
sphere is the same as the maximum dimension of the original particle.
. Equivalent minimum length. This is where the diameter of a theoretical
sphere is the same as the minimum dimension of the original particle.
There are many other methods available to do this. This technique is known as
equivalent spheres.
The Mastersizer uses the volume of the particle to measure its size. In the
example above the matchbox has a volume of 50x25x10mm = 13750mm3. If the
Mastersizer was able to measure this size of particle it will take this volume and
calculate the diameter of an imaginary particle that is equivalent in volume - in
this case it will be a sphere of 30mm diameter.
Obviously you will get a different answer if you where using the surface area or
maximum dimension of the matchbox to calculate an equivalent sphere. All of
these answers are correct but each is measuring a different aspect of the matchbox.
We can therefore only seriously compare measurements that have been measured
using the same technique.
di l di
This number will be slightly different to the arithmetic mean:
di l + di
2
For example the size band 404.21 - 492.47 microns has a geometric mean of
446.16 microns and arithmetic mean of 448.34 microns. In most cases the
difference is small but the geometric mean is chosen in these calculations as more
appropriate to the logarithmic spacing of the fundamental size classes.
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100
90
80
70
60
10
50
40
30
20
10
0
0
10.0
ILL 1869
100.0
Particle Diameter ( m.)
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The undersize curve takes the form of the percentage below a certain size for
example 20% (reading the figures from the right hand scale) of the sample is
under 40 microns etc.
The oversize curve takes the form of the percentage above a certain size for
example 80% of the sample is over 40 microns etc. Again the oversize plot uses
the right hand scale to take its percentage scales.
The frequency curve is obtained by differentiating the cumulative undersize
curve. The peak of the frequency curve gives the modal diameter - the most
commonly occurring particle diameter. Note that the frequency curve is scaled to
be approximately the same height as the analysis size band histogram.
The histogram plot shows the percentage of the volume of the sample that is
within a particular size band (% in). Histogram plots use the left hand scale. It is
the height of the histogram bars that are of interest, not the area under the bar.
Each bar represents a size band of particles - on the initial analysis the size bands
are determined by the physical design of the detector. Once analysed the user can
set the number of size bands.
A typical report is shown below, followed by a brief description of the key features.
3
Result: Analysis Table
Run No:
Rec. No:
1
3
Range: 1000 mm
Beam: 2.40 mm Sampler: None
Presentation:3$$D
Analysis: Polydisperse
Modifications: None
Obs': 10.3 %
Residual: 0.617 %
10
6
7
5
Volume
In %
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
Size
(um)
22.49
26.20
30.53
35.56
41.43
48.27
56.23
65.51
76.32
88.91
103.58
120.67
Volume
In %
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
Size
(um)
120.67
140.58
163.77
190.80
222.28
258.95
301.68
351.46
409.45
477.01
555.71
647.41
8
1
4
2
9
Volume
In %
0.07
0.47
2.71
14.15
38.71
29.50
9.89
3.39
0.96
0.15
0.00
Size
Volume
In %
(um)
647.41
0.00
754.23
0.00
878.67
0.00
1023.66
0.00
1192.56
0.00
1389.33
0.00
1618.57
0.00
1885.64
0.00
2196.77
0.00
2559.23
0.00
2981.51
0.00
3473.45
ILL 2063
ID: Sample D
File: MSSTEST
Path: C:\SIZERS\DATA\
The residual, as stated earlier, is an indication on how well the analysis data
was fitted to the measurement data. A good fit is indicated by a residual of under
1%. If the residual is over 1% then this may be an indication that you have not
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used the correct presentation. Try re-analysing the measurement data with a new
presentation.
The statistics of the distribution are calculated from the results using the
derived diameters D[m,n] - an internationally agreed method of defining the
mean and other moments of particle size. See British standards BS2955:1993 for
more details.
D(v, 0.5), D(v, 0.1) and D(v, 0.9) are standard percentile readings from the
analysis.
. D(v, 0.5) is the size of particle at which 50% of the sample is smaller and
50% is larger than this size. This value is also known as the Mass median diameter (MMD).
. D(v, 0.1) is the size of particle for which 10% of the sample is below this
size.
. D(v, 0.9) gives a size of particle for which 90% of the sample is below this
size.
D[4,3] is the volume mean diameter.
D[3,2] is the surface area mean diameter. Also known as the Sauter mean.
Span is the measurement of the width of the distribution. The smaller the
value the narrower the distribution. The width is calculated as:
b g b g
b g
d 0.9 d 01
.
d 0.5
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SSA (Specific Surface Area) The specific surface area is defined as the total area
of the particles divided by the total weight. If you are using this value then it is
important to set the density of the sample from the Setup-Analysis dialogue.
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CHAPTER 8
Introduction
The manual so far has taken you through the individual steps of making a
measurement and processing the data. This has allowed you to understand the
individual processes involved. In practice however you would most probably set
up the whole measurement sequence as a semi-automatic process.
Setting up a sequence
NOTE'
Measurement
Sequence
Setup
Sequence
The
dialogue can
also be selected by
pressing the
button.
ILL 1876
From this dialogue you can select the measurement procedures you require. You
have the option of running more than one measurement by increasing the
Number of Measurements edit box. A delay can also be set in between the
measurements. This is useful, for example, if you wish to automatically measure
the same sample over a period of time.
Once you have set up the measurement details you can set the way the
measurement data will be analysed by pressing the Process Sequence Setup
button . The dialogue below will appear.
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ILL 2015
CHAPTER 8
The options within this dialogue allow you to analyse the measurement data
(using the analysis model and presentation currently selected in the Setup Analysis and Setup - Presentation menu items) and save the results for each
measurement that the sequence makes. Other options allow you to perform
various statistical calculations.
NOTE
'
An alternative to
selecting
Measure-Start
is to press
the Start Sequence
sequence
ILL 2016
button.
Once set up the whole sequence can be started by selecting the Measure-Start
Sequence menu item.
Clicking the Close button will terminate the sequence and display the message:
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ILL 2018
If a delay has been set between cycles of the sequence and the time of the
measurement is less than the delay time then a window appears to count down
the remaining time.
Click the Cancel Timer button to continue directly with the next cycle or
Abort Sequence to return to manual control.
More details on setting a sequence can be found in the software reference manual.
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Sample preparation
CHAPTER 9
Introduction
Now that you have successfully made a measurement and analysed the result, we
shall return to the important subject of sample preparation.
The preparation of the sample before it is added to the system can be critical.
Over half the problems encountered when measuring a sample are caused by bad
sample preparation. If your sample is sticking together, dissolving, floating on the
surface or if you have failed to get a representative sample you will not get a
correct result.
There are many techniques available to ensure that the sample is prepared
successfully. Once you have found a suitable dispersion technique for your
sample you can standardise the procedure so that comparisons can be made
between samples.
The information given in this chapter does not assume you are using an
Automated Sample Dispersion Unit - information is given on wet and dry
measurements.
Representative sampling
When taking a sample for a measurement it is most important to ensure that the
sample you are using is representative of the whole sample. If the sample is taken
from a bottle or container then care must be taken to ensure that the sample is
thoroughly mixed. When the sample is a powder large particles tend to rise to the
top of the container, as smaller ones fall to the bottom (as can be seen in the
diagram below).
ILL 2064
The large particles in the bottle of powder migrate to the top in transit .
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As the bottle vibrates in transit , large particles part to allow fine particles to fall
through and then close together over the fine particles - being lifted in the
process.
In most samples there are some large particles and some small, but the majority
fall in-between these two. If a sample is taken from the top of the container, then
only the large particles will be measured. If this is then compared to a
measurement with the sample taken from the centre of the container then the
results will be different.
If the sample is stored in a container then mix the sample thoroughly. Do not
shake the container as this often increases the separation of the particles. Instead,
hold the container in both hands and gently roll the container, continually
changing its orientation.
If the distribution of particles within a sample is particularly broad, then
representative sampling can be difficult. If you are experiencing problems then the
use of a spinning riffler may be beneficial. A spinning riffler uses the same
principle that causes the sample to separate when it is kept in a container. The
riffler comprises of a vibrating hopper which vibrates the sample down a shute.
The act of vibrating the sample causes the larger particles to separate out and
travel down the shute first. At the end of the shute is a collection of rotating plates
that collect the sample evenly. When all of the sample has passed down the shute
then each collecting plate will contain a representative sample.
Liquid samples can also separate out if stored in containers, with larger particles
sinking to the bottom. Again the sample should be thoroughly mixed if you are to
get a representative sample. Sample splitters/rifflers are also available for liquid
samples.
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measurement. Obviously care should be taken with delicate materials where
drying in the oven may damage the sample.
A fresh sample that has not had time to absorb moisture from the atmosphere is
always preferable and will usually give better results.
Some samples can only be measured in a dry state as they react with all wet
dispersants, for example they may dissolve or the particles may swell when in
contact with a liquid.
G E T T I N G
S T A R T E D
Page 9.3
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G e t t i n g
S t a r t e d
tank will be suitable. Filter this water prior to use. Another solution is to warm
the dispersant (for water typically to 60 - 80oC) and then allow to cool before use.
Warning
The practice of warming dispersants to allow de-gassing should not be
attempted on volatile dispersants. Never allow dispersants to reach their
boiling points.
Dispersant
Refractive index
Water
1.33
Ethanol
1.36
Propan-2-ol (Isopropyl-alcohol)
1.39
Acetone
1.36
Butanone
1.38
Hexane
1.38
Dimethyl Digol
1.41
The cost of some of the organic dispersants may limit its use to the Small Volume
Sample Dispersion Unit that typically only uses 100ml of dipersant. Also the
problem of the safe disposal of the sample after measurement must also be
considered. Always adopt the correct procedures for disposing of the sample and
dispersant, following any local guidelines. Most local regulations forbid hazardous
samples and dispersants to be tipped down the drain, allowing it to enter the
water system.
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CHAPTER 9
Surfactants
The addition of a surfactant may assist the preparation of the sample by removing
the surface charge effects on the sample that cause it to float on the surface or
clump together.
Surfactants have to be added in minute quantities, typically one drop per litre of
dispersant. If too much surfactant is added to the dispersion tank then the action
of stirring and pumping the sample may cause it to froth, entering bubbles into
the system. Bubbles are measured by the system as particles which can bias the
results. Anti-foaming agents may be added to prevent the formation of bubbles.
Try adding a drop of surfactant to a quantity of sample and dispersant mixed in a
small beaker. If the sample sinks to the bottom of the beaker in large clumps then
discard the sample and start again. Try again, this time adding the sample to a dry
beaker and adding a drop of surfactant and mixing thoroughly. Add the dispersant
and mix well. This usually avoids the agglomeration caused by adding the
dispersant first.
A list of recommended surfactants in order of common use is given below:
Surfactant
Nature
Nonidet P40
Non-ionic
Teepol L
Non-ionic
Synperonic N
Non-ionic
Aerosol OT
Anionic (solid)
Anionic
Hyamine 2389
Cationic
G E T T I N G
S T A R T E D
Page 9.5
CHAPTER 9
G e t t i n g
S t a r t e d
Admixtures
Admixtures also aid dispersion by modifying the properties of the dispersant itself
that are responsible for the problem. Admixtures are added in larger quantities,
typically 1g/l. A list of commonly used admixtures is given below:
Sodium Hexametaphosphate
Sodium Pyrophosphate
Trisodium Phosphate
Ammonia
Sodium Oxalate
Calgon
Calcium Chloride
As these are solid materials dissolved into the dispersant the solution should be
filtered after preparation to remove impurities.
Slurries
The act of mixing up a small quantity of concentrated sample, dispersant and
additives before it is added to the instrument tank is known as preparing a slurry.
Once the particles have been successfully dispersed into a slurry, then the sample
may be added to the instrument without any further additions of surfactants etc.
to the instrument dispersion unit. The problem of the sample settling out within
the beaker can be solved by using a pipette to continually stir the sample. At the
same time as stirring you can continually fill and empty the pipette. Use the
pipette to add the sample to the dispersion tank.
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ultrasonics by placing the slurry and its beaker into an ultrasonic bath. It will be
apparent if this has been effective. Further ultrasonics can be applied when the
sample is added to the tank, if necessary. This will often prevent
re-agglomeration, but is not always necessary.
Caution
Be wary of using ultrasonics with fragile particles as the ultrasonic action may
actually break up the particles themselves. If in any doubt, microscopic
observation before and after ultrasonics should establish whether it has been
beneficial or not.
Bubbles
Bubbles have been mentioned earlier in this chapter. To the Mastersizer optics all
bubbles are seen as particles and are therefore measured. You should always be
wary of bubbles within the system.
G E T T I N G
S T A R T E D
Page 9.7
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G e t t i n g
S t a r t e d
Bubbles can be tested for by circulating the dispersant with appropriate additives
through the cell using the dispersion unit, and turning on the ultrasonics. Should
bubbles pass through the cell and scatter light then you have a problem. The
solution is to use the ultrasonics for one or two minutes, then turn them off and
wait for several minutes with the sample continually circulating.
Bubbles will vary in size but will typically be in the region of 100 microns in size.
In many cases these bubbles can be clearly seen as a second and separate peak
when the measurement data is analysed.
SAMPLE
For Dry Analysis
Representative Sample
(riffle if necessary)
No
Yes
Representative Sample
(mix well or riffle if dry powder)
Try Solvent
Analyse
e.g. Ethanol
Propan-2-ol (IPA)
Methanol
Acetone
Butanone (Methyl Ethyl Ketone)
Hexane
Toluene
Dimethyl
Digol
Analyse
Yes
No
Ultrasound If
Necessary
Does It Float ?
Ultrasound If Necessary
Analyse
Yes
No
Analyse
Try Surfactant
Page 9.8
No
ILL 2019
Yes
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CHAPTER 10
Modifying results
The result produced by the analysis may be modified in a number of ways before
it is presented in the graph or table.
The modifications are controlled from the Setup-Result Modifications
dialogue. In this dialogue you have the option of setting the modifications so they
are applied to the current result only, or to the subsequent measurement results.
The modification setup is saved with each result record and can be loaded for
alteration.
The modifications to the standard result are:
Blend Results - two results of the same sample measured with different
range lenses can be blended to produce a result across two size ranges.
Shape Correction - the Mastersizer size range can be modified to make
the result comparable with that from other sizing methods.
Extend Result - results from other sizing methods can be added to the
Mastersizer result to extend the result range.
Transform Result - the default volume distribution result is transformed
to surface area, length or number distributions.
Kill Result - one or more result channels can be removed to isolate a result
or remove the effects of noise.
Kill Data - One or more data channels can be removed from the analysis,
limiting the effects of bubbles and other contaminants, such as propellant
gasses during spray measurements. This modification is carried out as part
of the result calculation.
Each of these modifications will now be discussed in detail.
Killing channels
Killing data channels
The analysis normally uses all the data channels. There are, however, some types
of measurement in which it is inherently impossible to obtain all channels
measured accurately. These channels are removed from the analysis by setting the
kill data ranges to exclude a few channels at the lower or upper end of the range.
G E T T I N G
S T A R T E D
Page 10.1
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G e t t i n g
S t a r t e d
It is important to realise that if these parameters are set unnecessarily the accuracy
and resolution of the analysis will be reduced. Do not set kill channels at the
lower end of the range to exclude data routinely unless you have good reason.
For example in some spray measurements the presence of a propellant material
imposes on the signal a scattering pattern of its own. This signal is only present at
the same time as the sample and so cannot be compensated for by the background
subtraction. In such cases the effects are frequently confined to a small angular
range and it is desirable to exclude that range from the analysis. Unexpectedly
large signals in these channels are more likely to be due to excessive bubbles in
the dispersion, bad alignment or dirty optics.
Large signals in the outer channels may well result from allowing high levels of
daylight or artificial light to fall on the receiver optics during spray measurements.
If spray measurements have to be conducted at a distance from the range lens
such that the one or more outer rings of the detector are cut off then you should
kill these rings to stop possible bias in the results. See Avoiding lens cut off in
chapter 4 for more details.
Up to ten data channels may be removed from the inner (lower numbered) and
outer (higher numbered) data channels. The channels are counted from each end
of the range so it is not possible to kill a lower numbered channel without also
killing the channels below it, or a higher numbered channel without killing the
channels above it. Killing a channel is not the same as putting the value to zero the killed channel is actually excluded from the analysis.
Below is an example of how killing data channels affects the result. The left hand
display shows the measured data and on the right is the corresponding result. The
data from the 50 microns particle distribution has been corrupted by scattering
from bubbles - showing up as high readings in the first three channels. This
produces the peak at 220 microns in the result. The lower displays show what
happens if the first three channels are killed . The result display now shows the
expected distribution.
Page 10.2
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CHAPTER 10
30
20
10
0
1000.
10.0
30
20
10
ILL 1879
0
1000.
10.0
Particle Diameter (m.)
The data channels may be killed by either using the Setup-Analysis dialogue or
by adding kill cursors to the data graph, as shown below. Both of these methods
create a new result with the channels killed. Alternatively you can set the killed
channels during the inspect phase of the measurement, as shown in the section on
Measure-Inspect in the Software reference manual.
G E T T I N G
S T A R T E D
Page 10.3
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G e t t i n g
S t a r t e d
ILL 2020
The kill cursors are produced by depressing the left mouse button with the cursor
in the left or right margin of the graph and then dragging the mouse towards the
centre of the graph. You will have to be in the Data view to use the kill data
cursors. When the grey cursor is at the correct position release the mouse button.
A small dialogue appears on the screen. At this point you can choose to either;
move the other cursor onto the graph, click the Apply button or Cancel the
operation.
For the kill data option the Apply button starts an analysis to produce a new
result with the required data channels removed. For the kill result option a new,
modified result is produced.
Page 10.4
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The Shape Correction works by modifying the size boundaries of each
measurement class, which are originally defined by scattering theory and the
geometry of the optics and detector. The action of the shape correction is to
change these size values - in effect changing the calibration of the Mastersizer.
To simplify the calculation of the terms the shape correction is limited to a linear
transform between size classes:
d 'i = Ai di + Bi
where di is the corrected size of class i and di is the original size value. Ai and Bi
are the shape correction terms.
The Ai and Bi terms can be calculated by using the following method:
1. Draw a cumulative undersize curve on graph paper of the results of the
alternative particle sizing method.
2. From the Mastersizer result list the size and cumulative result under that
size.
3. From the list of Mastersizer result values find the corresponding size
values from the graph of the alternative sizing method.
4. Draw a graph, an example of which is shown below, of the normal
Mastersizer sizes d against d, the sizes found in stage 3.
5. Draw the best straight lines through one or more points. The slope of
these lines are the shape terms A and the intercepts at zero d are the shape
terms B.
Below is an example of the graph drawn in stage 4. The dotted line shows an
un-corrected result (A = 1, B = 0). The points are sizes read from the result of
the other sizing method. Two lines have been drawn through these points of
slopes A1 and A2 and with intercepts at zero d of B1 and B2. When applying the
generated shape correction terms to the Mastersizer size range values, A2 and B2
would be used for the upper 4 size values, and A1 and B1 for the lower 10 sizes.
You can also see that there are two points, near the middle of the graph, that
require a third line to be drawn with intermediary values.
G E T T I N G
S T A R T E D
Page 10.5
CHAPTER 10
G e t t i n g
S t a r t e d
12
10
A2
Slope = A1
d' m
Slope = A2
A1
4
0
B1
10
12
ILL 2021
B2
d m
The shape correction factors are stored as a shape file. The shape file can be
created and edited using the Edit-Shape Factors dialogue. As the shape
correction factors are generated for a specific Mastersizer size range, the correct
range must be selected when creating and editing the shape file. The selected size
range is also saved with the shape file. When a shape correction is required a shape
file is selected and loaded during the process of modification. All shape files have
extension .SHA.
Details of creating and editing shape files and selecting shape file for the result
modification are described under Edit-Shape Factors and Setup-Result
Modification in the Software reference manual.
Page 10.6
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CHAPTER 10
. At least one result within the range of the Mastersizer. The Mastersizer result will be scaled to be the percentage below the smallest of these sizes.
The lower end of the Mastersizer may also be extended by entering manually a
value in the smallest size band of the Mastersizer in place of the value calculated
from the analysis.
See the Setup-Result Modification command and the Extended Result
dialogue in the Software reference manual for details of entering the extended
result.
Xi =
100Vi / din
Vi / din
G E T T I N G
S T A R T E D
Page 10.7
CHAPTER 10
G e t t i n g
S t a r t e d
%
30
20
1
10
2
0
1.0
10.0
100.0 1000.010000.0
ILL 1874
0.1
Blending results
In some cases the sample size range may be so broad that it cannot be covered by a
single range lens but can be covered by the combination of two range lenses. The
results measured by the two range lenses can be blended to produce a result with
a broader size range.
The blending takes place within the overlapped region of the two size ranges. The
two results within this region are combined to give a smooth transaction of result
from one size range to the other.
In the following example the sample has a size ranging from 1 micron to about
3000 microns. When measured with the 300mm range lens of the Mastersizer S
the results above 900 microns are cut off; whereas with a 1000mm lens the results
below 4 microns are cut off. To get a result covering the entire sample size range,
the results measured with the two range lenses are blended.
Volume%
10
100
90
80
70
60
50
2
40
30
20
10
0
0
10.0
100.0
1000.0
10000.0
ILL 2798
1.0
Page 10.8
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CHAPTER 10
Of the two selected records the record with a smaller size range will be loaded as
the current result ( in the graph above) and the one with a larger size range is
marked as the blend record ( in the graph above). The blended result will have
the smallest size of the first record and the largest size of the second record as its
size range boundaries ( in the graph above).
The number of results channels for the blended result is the same as the result
with the smaller size range.
Unlike other result modifications result blending is operated from the Open
Sample File and Load Record dialogue. For details see the Software reference
manual.
Multiple modifications
Sometimes you may want to apply more than one modification to a single result.
This is achieved by setting up the required modifications from the Setup Result Modification dialogue. The result is always modified in the order of Kill
Results, Shape Correction, Extend Result and Transform Result.
For a blended result only the extending and transforming modifications can be
applied.
G E T T I N G
S T A R T E D
Page 10.9
CHAPTER 10
Page 10.10
G e t t i n g
S t a r t e d
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Maintenance
CHAPTER 11
Introduction
The Mastersizer has been designed so that supervisor/operator maintenance is
kept to a minimum. It should be fully understood that no one, except a qualified
Malvern representative, should remove the transmitter or receiver covers of the
instrument. The supervisor should only remove the sample area cover if spray
measurements are to be performed and should only do so after reading the Health
and Safety manual and the instruction manual for the spray accessories.
Warning!
Failure to follow these guidelines correctly could result in the emission of laser
radiation. Laser radiation can be harmful to the body and can cause permanent
eye damage.
This section explains the routine maintenance procedures that the supervisor can
perform. These procedures are:
. Replacing the sample tubes to and from the flow cell.
. Replacing the fuses.
. Cleaning and replacing the cell windows and window O rings.
. Cleaning the range lenses and beam expander.
. Cleaning the covers.
An operator may perform all the above procedures except replacing the fuses.
G E T T I N G
S T A R T E D
Page 11.1
CHAPTER 11
G e t t i n g
S t a r t e d
Caution!
When changing the tubing do not allow any dispersant or sample to come in
contact with the instrument. Some dispersants and samples can cause
permanent damage to the surfaces.
The specification of the tubing is:
Internal diameter - 3/16".
External diameter - 5/16".
Flexible - to allow the cell to be removed without having to remove the
pipes.
Replacing fuses
Warning!
Fuses must not be replaced by the operator. Only the supervisor or a
Malvern representative should attempt to replace the fuses.
If the Mastersizer system does not power-up, check the fuse. The fuse holder is
located on the transmitter end panel next to the power input socket. Disconnect
the mains power supply before unscrewing the fuse holder using a flat bladed
screwdriver. The fuse and fuse holder can now be withdrawn. If the fuse requires
Page 11.2
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CHAPTER 11
replacing simply pull the fuse out of its holder and replace with the appropriate
fuse from the list below.
The fuse required is:
CSA applications (USA, Canada etc).
240V/110V, 1.25" 5A AS UL/CSA
Rest of the world.
240V/110V, 20mm 2A AS
Warning!
Failure to replace the fuses with the correct size and value may result in
hazardous operation.
Caution!
The surfaces of the system may be permanently damaged if samples or
dispersants are spilt onto them. If a spillage should occur then the system
should be disconnected from the power supply before scrupulously cleaning
up the spillage.
Periodically the covers and sample area should be thoroughly cleaned using a mild
soap solution. Always ensure that the instrument is disconnected from the power
supply and computer.
. Never use excess liquid to clean the instrument and always avoid electrical
components (Connectors etc.).
. Always ensure that the instrument is completely dry before applying power.
. Never use a solvent based solution to clean the instrument as damage to the
painted surface may result.
G E T T I N G
S T A R T E D
Page 11.3
CHAPTER 11
G e t t i n g
S t a r t e d
Caution!
Always remove the lenses from the optical unit before cleaning. Do not
however remove the actual lens from the lens holder as these are precisely
set at manufacture.
. Locate the two pegs on the window tool into the two holes on the retaining ring.
. Rotate the window tool anti-clockwise and remove the ring .
Page 11.4
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. If the O ring did not come out with the ring then carefully remove it
with a pair of tweezers.
. Tip the window out of the cell onto a clean paper towel.
The window assembly is shown in the diagram below.
5
5
3
4
ILL 2983
2
1
Inspect both sides of the cell window. If there are any signs of scratches the
windows should be replaced. Spare windows may be obtained through your
Malvern representative.
At this point any dust on the surfaces of the window can be removed using a
compressed gas duster can. Keep the can upright while in use to prevent liquid
emerging.
Caution!
Do not wipe the windows with an ordinary dry cloth as this will cause
scratches. Always use the procedure below to clean the surfaces.
Inspect the windows by reflected light and see if there are any smears or prints on
it. If so then you must wipe the lens surface using the following guidelines.
Use a good quality lens tissue and gently wipe it over the surface once. Do not put
your fingers on the lens during this wipe. Re-inspect the window and if still
marked then repeat with another clean tissue.
G E T T I N G
S T A R T E D
Page 11.5
CHAPTER 11
G e t t i n g
S t a r t e d
If this does not eliminate the mark then consider the use of a liquid cleaner such
as Ethanol Absolute or Propan-2-ol. This can be soaked on a cotton wool bud and
wiped across the window gently. Use one pass over the window and then discard
to avoid scratching. Re-inspect the window and repeat until clean.
The outer faces of the windows have an anti-reflective coating and are more
prone to scratching than the inner surfaces. Be careful not to touch the faces of
the windows or put them down on dirty surfaces.
If the O rings shows any sign of damage they should be replaced.
Re-assemble the windows by first fitting the O-ring to the retaining ring then
pushing the window into position. (Place a piece of tissue over the window to
prevent finger marks getting onto the surface.) The window has a chamfered edge
and the side with the widest diameter must face outward. The diagram above
shows this orientation .
Screw the window ring back in place. Ensure the window is fully home in the
mount and not held by the O-ring, otherwise the window will move when the
pump speed is changed, causing the system to mis-align.
Replace the cell onto the Mastersizer and reconnect the sample tubes. To check
the integrity of the cell, pump dispersant through it. Check that no dispersant
leaks from the cell or sample tube connectors.
'
Note:
The cell windows are part of the optical system and removing them for
cleaning will change their position. Remember to add an Align stage to
your next measurement sequence or click the Align Easy button.
Page 11.6
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Caution!
Never remove the lens from the lens holder. The lens is precisely set at
manufacture.
Store the lens with lens caps on to avoid the need to repeat this procedure often.
Caution!
Read the following instructions fully before starting to clean the beam
expander. Failure to follow the procedure correctly may result in the improper
functioning of the instrument.
To clean the lens the aperture plate must be removed. This plate is a beam stop
aperture that fits exactly around the emergent laser beam, helping to clean up
stray light. It is precisely located and will need to be re-fitted in the exactly the
same position on re-assembly.
A simple means to achieve this is to mark the orientation of the plate with a pencil
so that a line is drawn on the aperture plate and the beam expander body as shown
in the figure below . Then loosen one locking screw only to release the plate
. The front face of the lens may be cleaned by the same procedures used for the
range lenses.
G E T T I N G
S T A R T E D
Page 11.7
CHAPTER 11
G e t t i n g
S t a r t e d
ILL 2073
When replacing the aperture plate, rotate the plate until the two pencil lines
match up. Once in position tighten up the locking screw. Do not tighten any
other locking screws.
Caution!
Failure to align the aperture plate in the exact original position will result in
clipping of the laser. This will require a visit from one of Malverns qualified
service engineers or representative to rectify. The user should on no account
attempt to re-align the aperture plate.
Page 11.8
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CHAPTER 11
G E T T I N G
S T A R T E D
Page 11.9
Specification
APPENDIX A
Introduction
This specification covers the Mastersizer in its most basic form i.e. without any
details of the sampling accessories. Details on the specification of the accessories
can be found in their individual accessory manuals. This specification covers both
the Mastersizer X and Mastersizer S - any information that is specific to a
particular model is given separately.
Mastersizer X
Mastersizer S
Lens
Size range
Lens
Size range
45mm
0.1 - 80 m
300RF
0.05 - 900m
100mm
0.5 - 180 m
300mm
0.5 - 900m
300mm
1.2 - 600 m
1000mm*
4.2 - 3500m
1000mm*
4.0 - 2000 m
* The 1000mm lens is only available on the long bench Mastersizers only.
It should be noted that accessories may have individual size range limits that are
more restrictive.
Dynamic range.
17600:1 maximum for the Mastersizer S, and 800:1 for the Mastersizer X
on a single measurement.
Accuracy.
Measurement
data.
G E T T I N G
S T A R T E D
Page A.1
APPENDIX A
G e t t i n g
S t a r t e d
Scattering angle
range.
Number of size
classes.
Primary output.
Relative volume size distribution, diffraction energy data and laser beam
obscuration.
Secondary
output.
Volume distribution on sieve size classes.
Tabulated on screen.
Plotted on screen.
Stored/recalled to disc.
Transferred over RS232.
Printed reports.
Laser transmitter.
Page A.2
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APPENDIX A
Receiver for the
Mastersizer S.
Range lenses of 300RF (reverse Fourier), 300mm and 1000mm (1000mm
for long bench Mastersizer only).
Composite detector array measuring a large angle range and two back
scatter detectors in the 300RF range lens assembly.
Detector carriage with motorised X-Y positioning under computer control for
automatic alignment.
Detector electronics.
Receiver for the
Mastersizer X.
Range lenses with 45mm (reverse fourier), 100mm, 300mm focal lengths
and 1000mm for long bench Mastersizer X only.
Detector carriage with motorised X-Y positioning under computer control for
auto alignment.
Detector electronics.
Detector for the
Mastersizer S.
Mastersizer X.
G E T T I N G
S T A R T E D
Page A.3
APPENDIX A
G e t t i n g
S t a r t e d
Detector
electronics.
requirements.
Dimensions.
Weights.
Data Capacities.
Keyboard.
Mouse.
Ports.
1 serial port (COM 1) for use with the Mastersizer. A second serial port is
required if you need to use a serial mouse or to control the Mastersizer and
software by a remote computer.
Page A.4
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APPENDIX A
Screen.
Printer.
Software.
MS-DOS
Microsoft Windows
A graphical interface software that allows control of the computer and data
using simple visual metaphors. Version 3.1 or later, running in enhanced
mode is required.
Mastersizer software
Utilities
Presentation generator.
The Malvern instruments warranty over the computer configuration only extends
to those supplied by Malvern Instruments. Users should be aware that not all
hardware sold as Microsoft Windows compatible is fully so. If you wish to operate
your own configuration it should be fully tested before purchase.
Malvern Instruments does not provide any warranty of software performance on
user selected computer configurations.
G E T T I N G
S T A R T E D
Page A.5
APPENDIX A
G e t t i n g
S t a r t e d
After use the system writes the configuration to disc and on subsequent use will
automatically configure the Mastersizer to this last used mode. Recall also
includes last data, results, programmes, key functions, etc.
Easy mode
Measurements made using buttons to select from a limited range of operations.
These allow safe step by step operations to perform the measurement. User
intervention is minimised.
Guidance and help are given using; menus, advice and error messages during
execution.
Menu mode
The system is operated by a selection of menu and sub-menu choices which may
be made using the mouse or from the keyboard. Many sub-menu items which are
frequently used may be selected by single key (accelerator) operations.
Programme Mode
Measurements are made using a command language (Sizer BASIC). These
programmes may be stored and recalled from disc, automatically or manually run
and allow fully automatic operations with little or no user interaction.
Help features
There is an extensive on-line help system available.
Page A.6
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Chemical compatibility
APPENDIX B
Introduction
The Mastersizer and its accessories have be manufactured from materials that are
considered to give the widest protection from chemical attack. However, it is
important to check that any sample or dispersant you may use is chemically
compatible with the materials that they will come in contact with the system.
This appendix will list all materials that come in contact with the sample and
dispersant in the normal operation of the optical unit only. The sample and
dispersant mostly come in contact with the sample accessories and the cells. See
the accessory manuals of the accessories you have to check for chemical
compatibility.
Location
Materials
Stainless steel.
Location
Materials
External covers.
When using the Free Fall Dry powder Feeder it is possible to spill sample onto
the covers. This should be avoided at all times. All spillages should be cleaned up
immediately.
G E T T I N G
S T A R T E D
Page B.1
APPENDIX B
G e t t i n g
S t a r t e d
Spray measurements
Component
Location
Materials
Sample area
Internal surfaces.
Glass (lenses).
Anodised aluminum.
Two-pack polyester paint.
Stainless steel.
Page B.2
MAN
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Remote interlock
APPENDIX C
Remote interlock
The Mastersizer does not require an external interlock switch to comply with
CDRH or EC laser safety regulations. However, some company safety regulations
may require the room in which the Mastersizer is installed to be protected so that
if the door to the room is opened then the laser in the optical unit is disabled.
ILL 3211
The Mastersizer allows you to do this by using the Remote connector socket on
the transmitter end panel. This socket is shown in the diagram below .
G E T T I N G
S T A R T E D
Page C.1
APPENDIX C
'
G e t t i n g
Note
S t a r t e d
The second switch must be of the spring return type that will
automatically return the switch to the open position when the switch is
released.
INTERLOCK
L
OFF/
REMOTE
2
1
ILL 3630
12V
Page C.2
MAN
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APPENDIX D
Introduction
When choosing the presentation for an analysis you will be required to enter a
value for the imaginary refractive index (this is effectively the absorption) of the
sample you are measuring. This can be difficult as the value has to be calculated
by performing an experiment. However, in most cases the value can be guessed
with very little effect on the result. In practice you will probably only use two
values; if the sample in transparent (glass beads for example) then there will be no
absorption so the value will be 0 (A on the grid), otherwise use 0.1 (H on the
grid) as the absorption value. If you feel you need a more accurate value then it
can be estimated by following the procedure below.
C=
k
VQ
id i
i
where k is a constant (for fixed beam length and obscuration), Vi and Qi are the
relative volume concentration and extinction efficiency for particles of diameter di.
Qi is sensitive to the optical properties and so, also, will be the concentration. The
technique then is first to determine the refractive indices of the particle and
medium either from tabulated values or by direct measurement using a
refractometer. A sample of known concentration is then prepared by mixing
weighed amounts of the materials and a measurement made. The data is analysed
using a range of presentations for the correct particle and medium refractive
indices and a range of absorptions. The presentation which gives the closest
agreement with the known volume concentration is then used as a good
approximation to the correct absorption value.
This technique has been used successfully with oil/water emulsions. It should be
noted that, a good estimate of the real refractive indices is necessary and the beam
length must be correctly entered (using the Setup - Hardware dialogue box),
therefore the method is difficult to apply with spray measurements.
G E T T I N G
S T A R T E D
Page D.1
APPENDIX D
Getting Started
As an example consider the measurements shown below.
A sample of material was suspended in water at a volume concentration of 0.032
%.
The differential refractive index is low and the size around 1m so that
presentation is important.
The analysis was performed with presentations GAD, GDD, GFD and GHD.
A plot of the log of reported volume concentration against absorption gives:-
Volume Concentration %
0.1
1
0.01
GAD
GFD
GDD
GHD
0.001
0.01
ILL 1885
0.001
0.1
The horizontal line at 0.032% indicates that the closest approximation to the
presentation is GFD with absorption 0.01.
Presentation
Absorption
Volume
Concentration
Residual
GAD
GDD
GFD
GHD
0
0.001
0.01
0.1
0.421%
0.157%
0.025%
0.004%
0.099%
0.119%
0.049%
0.531%
The table shows that, in this case, the volume concentration match is a much
more sensitive indicator of the absorption than the residual.
Page D.2
MAN
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APPENDIX E
Introduction
The measurement of a continuous stable spray is the simplest that can be made
with your instrument, requiring no essential extra accessories. Malvern offer an
Aerosol Mounting Unit which you may find useful for repeatably positioning the
nozzles and directing the spray.
G E T T I N G
S T A R T E D
Page E.1
APPENDIX E
G e t t i n g
S t a r t e d
ligaments that will later divide into stable droplets. Thus the limiting minimum
distance may not be set by concentration considerations alone.
In other sprays the droplets themselves may be volatile and evaporate rapidly
causing size distributions that will change with distance from the nozzle.
For all of the above reasons it is important to choose carefully the distance
between the nozzle and the analyser beam. Having set a suitable distance satisfied
by measurements, continue to use this configuration every time.
It is most common for measurements to be made with the analyser beam
intersecting the centre of the expanding spray cone. The result reported is the
average size distribution in the volume of spray in the beam. By moving the beam
off the spray axis it is possible to obtain the average size distribution in a different
part of the spray. By this means it is possible to probe the spatial variation of size
distribution and hence obtain further diagnostic information about the nozzle
characteristics.
Page E.2
MAN
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Malvern addresses
APPENDIX F
Malvern subsidiaries
If you purchased your Malvern Mastersizer from an agent for Malvern
Instruments Ltd. products please contact them for servicing and sales
information. If you purchased your Malvern Mastersizer from Malvern
Instruments direct please use the following information to contact us.
Head Office:
Malvern Instruments Limited
Spring Lane South
Malvern
Worcs
WR14 1AT
Tel: +44 (0) 1684 892456
Fax: +44 (0) 1684 892789
Malvern Instruments Inc
10 Southville Road
Southborough
MA 01772
U.S.A.
Tel: +1 508 480 0200
Fax: +1 508 460 9692
Malvern Instruments SA
Parc Club De LUniversit
30 Rue Jean Rostand
91893 Orsay Cedex
France
Tel: +33 (1) 69 35 18 00
Fax: + 33 (1) 60 19 13 26
Malvern Instruments GmbH
Rigipstrae 19
71083 Herrenberg
Germany
Tel: +49 (0) 7032 97770
Fax: +49 (0) 7032 77854
G E T T I N G
S T A R T E D
Page F.1
APPENDIX F
G e t t i n g
S t a r t e d
Page F.2
MAN
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Regulatory compliance
statements
APPENDIX G
Model
Mastersizer S
MSS
Support equipment:
NEC PowerMate 386/33i
PM-530-2421
VDU
APC-H5340
Kbd
APC-HH122
Mouse
M\N M-SE9-6MD
Test conditions
The Mastersizer S is a particle size measurement instrument, controlled and
operated from a computer. The particles are presented in a suitable medium
within a test cell through which a laser beam is focused. The diffraction pattern
produced by the particles is measured and from the result the size of the particles
is calculated.
G E T T I N G
S T A R T E D
Page G.1
APPENDIX G
G e t t i n g
S t a r t e d
EMC performance
The equipment under test, when subjected to the following tests was found to be
compliant.
. Complies with EN50081-2 (1995), generic emission standard (industrial
environments).
. Complies with EN55022 (1995), class B, radiated and conducted emissions.
. Complies with EN50082-2 (1995), generic immunity standard (industrial
environments).
. Complies with EN61000-4-2 (1995), Electrostatic discharge, to severity
level 4, with performance criteria A, ie. no loss of function or performance.
. Complies with DDENV50140, (1994), Radiated electromagnetic field, to
10V/m, with performance criteria A, ie. no loss of function or performance.
. Complies with DDENV50204, (1995), Radiated electromagnetic field, to
10V/m, with performance criteria A, ie. no loss of function or performance.
. Complies with EN61000-4-8 (1995), Fast transient burst, to severity level 4
with performance criteria A, ie. no loss of function or performance.
. Complies with DDENV54141 (1994), Conducted RF susceptibility, to 10V
with performance criteria A, ie. no loss of function or performance.
Page G.2
M A N
0 1 0 1
APPENDIX G
Model
Mastersizer X
Support equipment:
NEC PowerMate 386/33i
PM-1222-2431 31154UB
VDU
JC-1521HMP-EE 2YT01803A
Kbd
APC-H4122 2800578M
Mouse
Test conditions
The equipment under test measures the size of particles by means of laser
diffraction. An optical reticle was placed in the path of the beam to simulate a
given particle size. The computer is polled to the Mastersizer, and calculated the
particle size result. The computer program was instructed to signal an alarm
condition if the measured particle size fell outside the acceptability band. This
represented the EUT failure criteria. This also represented the equipment under
test activity for emissions.
EMC performance
The equipment under test, when subjected to the following tests was found to be
compliant.
. Complies with BS EN50081-2 (1994), generic emission standard (industrial environments).
G E T T I N G
S T A R T E D
Page G.3
APPENDIX G
G e t t i n g
S t a r t e d
Page G.4
M A N
0 1 0 1
Index
INDEX
A
Abort connector
Access to the instrument
Malvern personnel
Operator
Supervisor
Accessory panels
Adding the sample
Admixtures
Align button
Alignment
Intelligent Align
Analysis
Analysis model
Calculating the result
Choosing the correct
analysis mode
Compressed range
Monomodal
Multimodal
Presentation
Selecting
Sequence
Very polydisperse
Automated Sample
Dispersion Unit
Aux. Comms connector
B
Back scatter connector
Background
Background measurement
Bitmap Editor
Blending results
Bubbles
Button bar
Buttons
Align button
Background
Document
Inspect button
Next
Previous
2-9
1-2
1-2
1-2
1-2
2-6
4-11
9-5
4-10
3-4, 4-10
4-10
3-6
3-7, 5-8
5-1
3-6
3-6, 5-1
5-1
3-6
5-2
8-2
3-6, 5-1
1-3, 2-1
2-9
2-7
3-5
4-11
2-10
10-8
9-3
2-12
4-10
4-11
4-8
4-13
4-9
4-9
Print
Setup sequence
Start/stop
6-4
8-1
4-9
C
Calculating the result
Cells
Air
Flow
Pipe connectors
Stirred
Choosing a presentation
Cleaning the beam expander
Cleaning the cell windows
Cleaning the covers
Cleaning the range lenses
Colours
Table
Compressed range
Computer
Computer Comms connector
Cursors
Kill
Help jump
Query
Splitter bar
Cut off
10-4
2-19
2-14
2-15
4-3, 4-5
D
Derived distribution
parameters
Detector
Digital I/O connector
Dispersant
Dispersion method
Document button
Document the measurement
Dry sample preparation
7-3
3-2
2-9
9-3
4-5
4-8
3-5, 4-8
9-2
E
Easy buttons
SEE Button bar
Easy mode
Equivalent spheres
G E T T I N G
3-7
2-6
2-6
2-6
2-6
2-6
5-3
11-7
11-4
11-3
11-6
6-3
3-6
2-2
2-8
2-15
7-2
S T A R T E D
Page 1
INDEX
G e t t i n g
S t a r t e d
D-1
10-6
F
Finding your way around the screen
2-11
Flow cell
1-3
Fonts
Graph fonts
6-7
Table fonts
6-7
Fraunhofer
3-1
Frequency curve
3-3, 7-5
Fuse holder
2-3
Fuses
11-2
G
Graph dialogue
Graph fonts
Graph pane
Graphs
H
Hardware setup
Help
F1 Function key
Help jump cursor
Help menu
Help window
Jumps and Popups
On-line help
Status line
Histograms
I
Identifying a range lens
In-band
Inspect
Inspect button
Intelligent Align
Interlock connector
6-2
6-7
2-14
7-4
4-7
2-16
2-17
2-19
2-17
2-17
2-18
2-16
2-19
3-3, 7-5
4-3
3-3
3-5
4-13
4-10
2-3
K
Kill cursors
Killing channels
Page 2
10-4
10-1
L
Laser interlock connector
Laser interlock switch
Laser power indicator
Lens
Changing
Cut off
SEE Range lens
Live display
Long bench Mastersizers
LV out connector
2-7
2-7
2-4
4-7
4-5
4-10
2-9
2-3
M
Maintenance
Cleaning the beam expander
11-7
Cleaning the cell windows
11-4
Cleaning the covers
11-3
Cleaning the range lenses
11-6
Fuses
11-2
Replacing the sample tubing
11-1
Malvern personnel
1-2
Malvern presentation grid
5-4
Mastersizer program group
2-10
Bitmap Editor
2-10
Mastersizer program icon
2-10
Presentation generator
2-10
Measure windows
4-8
Measurement
3-2
Add the sample
3-5
Align the optics
3-4, 4-10
Background
3-5, 4-6, 4-11
Inspect
3-5, 4-12
Instrument preparation
4-6
Making a measurement
3-4
Measure
3-5, 4-13
Measure windows
4-8
Obscuration
3-5, 4-12
Setup the hardware
4-7
Menu bar
2-11
Menu commands
1-5
Menu mode
2-15
Mie theory
3-1
Modes of operation
2-15
MAN
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INDEX
Easy mode
Menu mode
Program mode
Modifying results
Blending results
Extending the result
Kill cursors
Killing channels
Multiple modifications
Shape correction
Transforming result type
Tromp curve analysis
Monomodal model
Multimodal mode
N
Next
2-15
2-15
2-16
10-1
10-8
10-6
10-4
10-1
10-9
10-4
10-7
10-9
3-6, 5-1
3-6, 5-1
4-9
O
Obscuration
Operator
Optical unit
Optical unit power switch
Other reading
Oversize plot
3-5, 4-12
1-2
2-1, 2-2
2-4
1-7
3-3, 7-5
P
Polydisperse model
Power input socket
Power switch
Presentation
3$$1
3$$A
3$$D
Choosing
Fraunhofer (3$$D)
Grid
Methods of selecting
Reference Reticle (3$$1)
Special
Standard - Dry (3RHA)
Standard - Wet (3OHD)
Presentation grid
Previous button
3-6, 5-1
2-3
2-4
3-2, 3-6
5-8
5-8
5-8
5-3
3-7
5-3
5-5
3-7
5-8
3-7
3-7
5-4
4-9
Printing
Graph
Installing a printer
Print button
Report
Table
Understanding printing
Window
Program mode
6-4
6-10
6-8
6-4
6-10
6-10
6-6
6-10
2-16
Q
Query Cursor
2-14
R
Range lens
SEE Cut off
SEE Choosing
SEE Identifying
Receiver
Abort connector
Aux. Comms
Computer Comms
Detector
Digital I/O
Exp. trigger
L.V. In
Sweep trigger
Records
Remote connector
Replacing the sample tubing
Reports
Representative sampling
Residual
Riffler
Run number
2-2, 2-7
2-9
2-9
2-8
2-8
2-9
2-9
2-9
2-9
3-8
2-3, C-1
11-1
6-3, 7-5
9-1
3-7, 5-9
9-2
3-8
S
Sample area
Back scatter connector
Beam expander
Cell pipe connectors
Laser interlock connector
Laser interlock switch
Range lens
2-2, 2-4
2-7
2-5
2-6
2-7
2-7
2-5
G E T T I N G
2-5
S T A R T E D
Page 3
INDEX
G e t t i n g
S t a r t e d
Page 4
2-6
2-5
2-6
2-5
2-6
3-8
4-2, 9-1
9-2
9-3, 9-7
9-3
9-2
9-6
9-6
9-3
2-1
3-8
3-2
8-1
8-1
3-4
10-4
4-12, 9-6
2-10
2-9
2-12
2-14
2-11
2-15
2-15
2-14
2-11
2-15
2-15
4-9
2-15
9-5
2-9
3-2
1-1
Tables
Theory
Derived distribution
parameters
Equivalent spheres
Fraunhofer
Mie theory
Volume based results
Transforming result type
Transmitter
Fuse holder
Interlock connector
Laser power indicator
Laser power key
LV out connector
Optical unit power switch
Power input socket
Remote connector
Tromp curve analysis
Typical system
7-4
3-1
7-3
7-2
3-1
3-1
7-1
10-7
2-2
2-3
2-3
2-4
2-4
2-3
2-4
2-3
2-3
10-9
2-1
U
Ultrasonics
Undersize plot
Unstable concentrations
9-6
3-3, 7-5
9-7
V
Very polydisperse model
Viewing the result
Views
Graph
Overview
Vignetting
Volume based results
3-6, 5-1
3-8
6-1
6-2
6-4
4-5
7-1
W
Wet sample considerations
Where to find information
Windows terms
9-3
1-5
1-3
6-7
2-14
MAN
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