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Getting Started

MAN 0101

Issue1.3

August 1997

Malvern Instruments Ltd. 1995, 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

Windows is a registered trademark of Microsoft Corporation.


Tygon is a registered trademark of Cole Parmer Instruments Company Limited.

Printed in England

CONTENTS

Contents
Chapter 1 - Introduction to this manual
Welcome

1-1

Systems covered by this manual

1-1

Access to the instrument

1-2

Assumed information

1-3

Windows terms

1-3

Menu commands

1-5

Where to find information

1-5

Other reading

1-7

Chapter 2 - Getting to know your system


Introduction

2-1

A typical system

2-1

The optical unit

2-2

The transmitter

2-2

The sample area

2-4

The receiver

2-7

Differences between the long and standard bench Mastersizers 2-9


The Malvern software

2-10

The Mastersizer program group

2-10

Finding your way around the screen

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

The F1 Function key

2-17

The Help menu

2-17

The Help window

2-17

Jumps and Popups

2-18

Status line

2-19

Reporting Problems

2-19

Chapter 3 - How the Mastersizer works


Introduction

3-1

What does the Mastersizer do?

3-1

How does the Mastersizer do it?

3-2

How to make a measurement

3-4

How to analyse the measurement data

3-6

The analysis model

3-6

The presentation

3-6

Calculating the result

3-7

Viewing the result

3-8

Saving the result

3-8

Chapter 4 - Making a measurement

Page ii

Introduction

4-1

General measurement advice

4-1

Sample preparation

4-2

Cleanliness of the optical system

4-2

Choosing a range lens

4-3

Size range of your sample

4-3

Sample dispersion method

4-5

As general advice

4-5

M A N

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CONTENTS
Avoiding lens cut off (Vignetting)

4-5

Always measure a background

4-6

Making a measurement

4-6

Instrument preparation

4-6

Document the measurement

4-8

An introduction to the measure windows

4-8

Align the system

4-10

Take a background measurement

4-11

Add the sample

4-11

Measure the sample

4-13

Chapter 5 - Analysing the measurement data


Introduction

5-1

Choosing the correct analysis mode

5-1

Choosing the correct presentation

5-3

The Malvern presentation grid

5-3

Methods of selecting a presentation

5-5

When is the presentation important?

5-6

Selecting a presentation

5-7

Special Presentations

5-8

Calculating the result

5-8

Chapter 6 - Viewing and printing the results


Introduction

6-1

Views

6-1

Reports

6-3

Overview of the standard views and reports

6-4

Understanding printing

6-6

Selecting fonts for graphs and tables

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

The Graph fonts

6-7

The Table fonts

6-7

Installing and selecting a printer

6-8

Changing print settings

6-9

Printing from the Mastersizer

6-9

Chapter 7 - Interpreting the results


Introduction

7-1

Fundamental concepts

7-1

Results are volume based

7-1

Equivalent spheres

7-2

Derived distribution parameters

7-3

Understanding the tables and graphs

7-4

Chapter 8 - Automating the process


Introduction

8-1

Setting up a sequence

8-1

Chapter 9 - Sample preparation


Introduction

9-1

Representative sampling

9-1

Considerations for dry samples

9-2

Considerations for wet samples

9-3

Choice and preparation of the dispersant


Surfactants and admixtures

Page iv

9-3
9-5

Surfactants

9-5

Admixtures

9-6

Slurries

9-6

The use of ultrasonics

9-6

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CONTENTS
Samples with unstable concentrations

9-7

Bubbles

9-7

Summary of sample preparation

9-8

Chapter 10 - Advanced result processing


Modifying results

10-1

Killing channels

10-1

Killing data channels

10-1

Killing result channels

10-3

Using the Kill cursors

10-4

Shape correction - Changing the size calibration

10-4

Extending the result

10-6

Transforming result type

10-7

Blending results

10-8

Multiple modifications

10-9

Tromp curve analysis

10-9

Chapter 11 - Maintenance
Introduction

11-1

Replacing the sample tubing

11-1

Replacing fuses

11-2

Cleaning the covers

11-3

Cleaning the optics

11-4

Cleaning the cell windows

11-4

Cleaning the range lenses

11-6

Cleaning the beam expander

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

Particle sizing specification

A-1

Optical unit specification

A-2

Computer requirements (minimum)

A-4

Mastersizer programme specification

A-5

Software Revision Level

A-6

Appendix B - Chemical compatibility


Introduction

B-1

Components in contact with sample and dispersant

B-1

Wet sample measurements

B-1

Dry sample measurements

B-1

Spray measurements

B-2

Appendix C - Remote interlock


Remote interlock

C-1

Appendix D - Estimating the absorption


Introduction

D-1

Estimating the absorption using concentration measurements

D-1

Appendix E - Advice for continuous sprays

Page vi

Introduction

E-1

Arrange for the spray to be extracted

E-1

Use the correct optical configuration

E-1

Positioning the spray nozzle

E-1

Dont spray the optical unit

E-2

Ensure the spray is stable during measurement

E-2

M A N

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CONTENTS
Appendix F - Malvern addresses
Malvern subsidiaries

F-1

Appendix G - EMC performance


Statement of EMC performance

G-1

Statement of EMC performance for the Mastersizer S

G-1

Equipment under test

G-1

Test conditions

G-1

EMC performance

G-2

Statement of EMC performance for the Mastersizer X

G-3

Equipment under test

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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Introduction to this manual

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.

Systems covered by this manual


Mastersizer is a generic name given to a family of systems. Each system within the
family uses the same principles of operation and only vary in operation in small
areas. For this reason this manual has been written to cover more than one
instrument.
This manual covers the operation of the long and standard bench versions of the
Mastersizer X and the Mastersizer S i.e.

Instrument.

Ref. Number.

Mastersizer X standard bench.

MAM 5000

Mastersizer X long bench.

MAM 5002

Mastersizer S standard bench.

MAM 5004

Mastersizer S long bench.

MAM 5005

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Access to the instrument


Within this manual reference is made to the various people that will have access to
the instrument. Below is a list of these people and their responsibility:

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.

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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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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

Option Button or Radio Button - A series of buttons in a group, selecting one


button cancels the others in the group. A radio button is shown below.

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

Combination List Box or Combo Box - A combination of a list box with a


text box. A button beside the text box displays or hides the list part of the
control. In some cases you can type new values into the text box part, in others
the text box just shows the current selection from the list.

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.

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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.

Where to find information


As stated above this manual is designed to give a brief overview of what the
Mastersizer can do and how to do it. In other words it is a quick guide that allows
you to understand how the Mastersizer gets a result and runs you through a
simple measurement procedure, hopefully steering you around the main pitfalls
and directing you to more information if needed.
If you have used a Malvern particle analyser before you may wish to go straight to
chapters 4 and 5 where you can find practical information on making a
measurement and analysing the data. However, it is recommended that you read
this manual fully before you start a measurement.
On-line help can be gained at any point when using the Malvern software. See
chapter 2 for more details.
The following is a list of the contents and objectives of the chapters within this
manual.
Chapter 2 - Features of the Mastersizer system.
This chapter is designed to enable you to identify the physical features of the
system and is divided into two parts.
The first part identifies the features of the optical unit, for example the function
of the connectors on the end panels or the purpose of the lenses etc. The second
section does the same for the Malvern software, identifying the key areas of the
screen.
Chapter 3 - How the Mastersizer works.
After reading chapter 3 you will have a basic idea of the operating procedures of
the Mastersizer and in particular be able to:
. Know the basic operating principles.
. Know the simple steps involved in making a measurement and analysing
the data.

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CHAPTER 1

Chapter 4 - Making a measurement.


Chapter 4 will guide you through the practical steps needed to make a
measurement to obtain the raw data.
Chapter 5 - Analysing the measurement data.
This chapter will show you how to take the raw measurement data and analyse it,
using the Malvern software, to get a final result. Advice is given on the choice of
optical model and the presentation.
Chapter 6 - Viewing the results.
The Mastersizer software has several standard viewing formats that allow you to
display and print the results in different ways. This chapter explains the standard
views and how to print them.
Chapter 7 - Interpreting the results.
This chapter gives some essential advice on understanding the results given by the
software.
Chapter 8 - Automating the procedure.
This chapter gives a brief overview of the procedures involved in measuring and
analysing a sample by setting up a semi-automatic sequence.
Chapter 9 - Sample preparation.
Sample preparation is one of the most important stages in making a measurement
on the Mastersizer. This chapter gives additional advice to that covered in the
chapter 4.
Chapter 10 - Advanced result processing.
The Mastersizer software gives the option to perform some advanced result
manipulation. This chapter gives an overview on some of the options.
Chapter 11 - Routine maintenance.
The Mastersizer has no user serviceable parts but there are certain maintenance
routines that can be carried out by the user. These include cleaning the optics etc.
This chapter gives advice on these routines.
Appendices.
At the rear of the manual is a series of appendices that cover some of the technical
aspects of the Mastersizer, including the technical specification.

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

The Malvern Software reference manual.

MAN 0102

The Malvern BASIC reference manual.

MAN 0103

Health and safety.

MAN 0104

G E T T I N G

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Getting to know your system

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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CHAPTER 2

G e t t i n g

S t a r t e d

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.

The optical unit


The optical unit consists of three components; the transmitter , the receiver
and the sample area . Each of these components are identified in the diagram
below.
The purpose of the optical unit is to collect the information from the scattered
light when a laser is passed through the sample to be measured.
3

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.

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CHAPTER 2

FUSE

5 10
5A
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260V~
~

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rkin

g Th

ay
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ILL 3209

Ma

LV out connector
Connector that carries the low voltage power supply to the receiver.

Power input socket


Main power input socket to the optical unit.

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.

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G e t t i n g

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Laser power key


The laser has to be turned on by turning the laser power key. This is an additional
safety feature, allowing the key to be removed to stop unauthorised use of the
system.

Laser power indicator


A visual indicator to warn the operator that the laser has been powered up by
turning the laser power key.

Optical unit power switch


The main on/off power switch for the optical unit.

The QSpec logo


If your company operates within the pharmaceutical industry, you will be pleased
to know that the Qspec sticker means that the instrument is eligible for coverage
by a Malvern QSpec Validation contract which can help you to meet the
requirements of the Food and Drug Administration (FDA). For further details
contact your local Malvern Distributor.

The sample area


The area between the transmitter and receiver is the sample area. This is where
the sample to be measured is passed through the laser.
Use the diagram below to identify the main features of the sample area.

Page 2.4

ILL 3210

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Sample area cover


Protective cover over the sample area. Designed to protect the operator from laser
radiation and to keep the amount of background light to a minimum during a
measurement.

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.

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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.

See Choosing a range lens in chapter 4.

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.

Cell pipe connectors


If a flow cell is used then the connecting pipes from the cell to the sample
preparation accessory are passed through the covers via the pipe connectors.

Removable accessory panels


Certain accessories, e.g. the Free Fall Dry Powder Feeder or the air cells, protrude
outside the sample area cover. To facilitate this there are three removable
accessory panels where one or more are removed to fit the accessory.

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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.

Back scatter connector


Mastersizer S only. The 300RF range lens has a back scatter detector which is
connected to the back scatter connector on the receiver bulkhead. No other lens
uses the back scatter connector.

Laser interlock connector


On the rear of the sample area cover is the laser interlock connector. This
connection must be made if the laser is to work.
The long bench versions of the Mastersizer have two interlock connections - one
on the rear of each sample area cover.

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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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.

Computer Comms connector


Communication cable that is connected to the computer. Data from the receiver
and control commands from the computer are transmitted down this cable.

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Aux. Comms connector


Auxiliary communications connector. Some sample preparation accessories (e.g.
Automated Sample Dispersion unit) are capable of controlling the optical unit.
When this is the case they are connected to this connector.

L.V. In connector
Connector that carries the low voltage power supply into the receiver.
Features to are usually used when performing spray measurements.

Digital I/O connector


The digital I/O connector is a general purpose user programmable I/O port. A
particular use for the port is to connect the spray synchroniser accessory.

Sweep trigger connector


The sweep trigger is used to start a measurement sweep when using the spray
accessories.

Exp. trigger connector


The Exp. trigger is the experiment trigger. The experiment trigger is used to
start an experiment when using the spray accessories.

Abort connector
The abort connector is used to stop the experiment triggered using the Exp.
trigger above.

Differences between the long and


standard bench Mastersizers
The long bench Mastersizer is able to measure a larger range of particle sizes. To
do this the long bench version has an extra sample area cover and an extra lens
(the 1000mm lens). When the 1000mm lens is used it is mounted in the
additional sample area. All other functions and features are the same as the
standard bench.
The following section gives an overview of the Malvern software.

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The Malvern software


The Malvern software controls all the functions of the optical unit during a
measurement and then uses the data collected to calculate the result.
The software is Windows based, requiring version 3.1 or greater and has been
designed to follow the guidelines laid down by Microsoft regarding the way in
which the software is operated and how it co-operates with other Windows
programs. Remember that, although the software is often operated using the
mouse, all of the measurement functions are accessible by using the keyboard
alone.
If you are unfamiliar with using the Microsoft Windows environment you should
read the Microsoft Windows manual. Running the Microsoft Windows tutorial
will allow you to practice your mouse skills.

The Mastersizer program group

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.

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Finding your way around the screen


Before we explain how the software works you should familiarise yourself with
some of the key features of the screen by using the diagram below.

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The main features are:

Title bar (or Caption)


This shows the name of the program (Malvern Mastersizer) and, among other
things, tells you the name of the current sample file.

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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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

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The default button bar set when the Mastersizer software is first installed is:

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A - Setup

B - Open Sample File

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

N - Graph Scale Down

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.:

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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

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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.

The F1 Function key


You can get help on using the Mastersizer software at any point by pressing the F1
function key. If the main Mastersizer window is active then the Help Contents
page will be shown. If a dialogue box or other Mastersizer window is active then
help on using that window will appear. This ability to give help on the operation
being carried out is known as context-sensitive help.
To get help on the main Mastersizer window hold down the Shift key and press
F1. The mouse cursor then changes from the normal arrow to the Help cursor.
Help Cursor

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.

The Help menu


The far right menu in the Mastersizer menu bar is for Help. This allows you to
go direct to specific parts of the Help system. The Help menu items are:
Contents - The main list of contents in the Help system.
Menu Command - The list of menu commands.
Program Language - The contents of the help on using the built-in
Mastersizer Basic language (program mode).
Keyboard - How to use the keyboard for; commands, moving the splitter
bar of the window and changing the scale the graph etc.
Window - The list of Mastersizer window components.
Help - This command displays the Microsoft Help information on using
the Help system.
For more information on the commands in the Help menu see the software
reference manual.

The Help window


The Help window is an independent window with its own menu and sizing
border. If you have the Mastersizer window maximised (filling the whole screen)

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you may find it useful to make the help window always stay on top of the
Mastersizer window.

$ To set the Help window to be always on top:

. Select the Help menu item from the Help window.


. If the Always on Top item does not have a check mark against it then click
this item (or press the Enter key with this item highlighted).

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.

$ To search for the required information:

. 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.

Jumps and Popups


In the Help window you will see text which is underlined with a solid line for
example Diffraction. Click this to move to another topic. This is known as a jump.
Text that is underlined with a dotted line will show a popup window with extra
information when it is clicked with the mouse. Click the mouse in the window to
make it disappear. This is known as a popup.
When the mouse cursor moves over a jump or popup item it changes to the help
jump cursor.

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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.

$ To print a data report:

. Change the View to Data.


. Select a report print in the File - Print dialogue.

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How the Mastersizer works

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.

What does the Mastersizer do?


Scientists have for centuries tried to predict the way particles scatter and absorb
light. There are many theories and models that the modern particle analyst can
use.
One of the simplest theories used is the Fraunhofer model. This model can
predict the scattering pattern that is created when a solid, opaque disc of a known
size is passed through a laser beam.
This model is fine for a lot of particles but it does not describe the scattering
exactly. Very few particles are disc shaped and a lot of particles are transparent.
The Mie theory was developed to predict the way light is scattered by spherical
particles and deals with the way light passes through, or is adsorbed by, the
particle. This theory is more accurate but it does assume you know some specific
information about your particle, such as its refractive index and its absorption.
The key fact about these theories is that if you know the size of the particle and
other details about its structure, you can accurately predict the way it will scatter
light. Each size of particle will have its own characteristic scattering pattern, like a
fingerprint that is unlike any other size of particle.
So how does the Mastersizer measure the size of particles? The Mastersizer works
backwards from the above theories by using the Mastersizers optical unit to
capture the actual scattering pattern from a field of particles. Then using the
theories above it can predict the size of particles that created that pattern.

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How does the Mastersizer do it?


There are two distinct procedures involved in measuring a sample on the
Mastersizer.
. Firstly there is the capturing of the scattering pattern from the sample - this
is known as the measurement. This is the purpose of the optical unit.
The detector within the optical unit is made up of many individual
detectors. Each detector will collect the light scattering from a particular
range of angles. A typical light scattering pattern is shown below.
5000

Obscuration = 10.3 %

Data

Background

4500
4000
3500
3000
2500
2000
1500
1000
500

16

24

32

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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.

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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.)

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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

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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

How to make a measurement


It is vitally important that the measurement is carried out correctly. It should be
obvious that if you make a poor measurement then no amount of analyzing of the
data can give you a good result.
A brief note on each stage of the measurement follows. The practical procedures
for making the measurement is covered in chapter 4.

Setup for the measurement


The Malvern software will need to know some of the physical parameters
of the system, i.e. which lens is fitted or the type of sample preparation
accessory is attached.
Obviously this will only be done once and will only have to change if you
alter the physical setup, by changing a lens for example.

Align the optics


If the instrument has just been switched on or any of the optics have been
moved (removing and cleaning the cell for example) you will have to align
the laser so that it hits the centre of the detector. This is a totally automatic
procedure with the Mastersizer and only requires the pressing of a single
button.

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Document the measurement


It is always good practice to document your measurement so that you will
be able to identify what was measured and how it was measured. A short
sample identifier and notes can be saved with the measurement.

Measure the background


The scattering pattern from your sample is contaminated by light scattered
by impurities within the dispersant, on the windows and lenses and also
electrical noise. To remove this contamination a background
measurement is made that measures the scattering pattern with no sample
in the analyser beam. This background measurement is then subtracted
from the scattering pattern with the sample present to leave only the
information from the particles.

Add the sample and inspect the concentration


The correct amount of sample has to be passed through the laser beam to
allow a good measurement to take place. Too little sample and there will
not be enough scattered light to be detected. Too much sample and the
light scattered from an individual particle will itself be scattered by other
particles - this is known as multiple scattering.
The Mastersizer determines the correct concentration of the sample by
measuring the amount of laser light that has been lost by passing it through
the sample. This is known as the obscuration and is given as a percentage.
For example if 30% of the laser light is lost when it passes through the
sample it is said to have an obscuration of 30%.
Sample is added to the system until the obscuration is within an acceptable
range.

'

Note

The preparation of the sample before it is added to the system can be


critical. Over half of 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. Read chapter 9
for details on sample preparation.

Measure the sample


Once all the steps above are completed the scattering pattern is then
measured.

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It is usual at this point to go on and analyse the measurement but it can be


saved on the computer so that it can be analysed at a later date if you wish.

How to analyse the measurement data


There are three steps required to analyse the measurement data:
. Choose the analysis model to be used.
. Choose the presentation to be used.
. Tell the computer to calculate the result.

The analysis model


The analysis model tells the computer what the expected shape of the result graph
will be. There are four choices available; polydisperse, multimodal, monomodal
or very polydisperse.
Polydisperse model does not assume anything about the shape of the
result graph.
Multimodal model assumes that there will be one or more distinct peaks
in the results graph - indicating that there are several distinct sizes of
particles.
The monomodal model assumes that there will only be one peak in the
result graph - indicating that there is only one size of particle.
Very polydisperse is similar to polydisperse but is only used for one or
two special circumstances. (For Mastersizer X only.) See chapter 5 for more
information.
Compressed range analysis has a reduced upper size limit and is meant
for use with dry powder and spray measurements. (For Mastersizer S only.)
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.

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

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(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.

Calculating the result


Once the analysis and presentation have been selected, the result is calculated by
simply pressing the calculate button. The progress of the calculation of the result

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is shown on the screen by the Residual. The residual is an indication of how


closely the calculated data has been fitted to the measurement data and is
expressed as a percentage. By examining the residual you will be able to determine
if the correct analysis mode or presentation has been chosen.

Viewing the result


Once the software has finished calculating the result, the graph pane and table
pane of the screen are updated to show the new result, using the present settings
for the displays. The result data can be shown in different forms by loading in a
different view. There are several standard views available or you can create your
own.
Details of the views available are described in chapter 6.

Saving the result


It is important to have a structured way to save all of your data so that in can be
locatedeasily in the future. There are three items you need to understand to
successfully file your data. These are:
. Records.
. Run number.
. Sample file.
A record contains all the data that has been collected for a particular experiment.
A record will contain the measurement data, the analysis data, notes on the
experiment and the run number. A record is identified by a sequential record
number.
If you run a number of experiments, on the same sample for example, the run
number can identify the sequence of results. The run number can either
increment after analysis or after saving.
A sample file is a file that contains a collection of records. The sample file takes
the form of a file name with a .SAM extension.
It is probably easier to understand these terms by following a practical example.
Suppose you had to measure some samples from a production line that operated 5
days a week and 4 hours a day. Every hour you have to take 3 samples from the
production line and measure these samples. One way to store these results is to
have a separate sample file for each day of the week. A typical structure of the
sample file for one day (Monday) is shown on the next page.

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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.

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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.

General measurement advice


Before we make a measurement there is some important general advice that
should always be noted.

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.

Cleanliness of the optical system


Laser scattering is a high resolution optical method in which the lenses and cell
windows are an integral part of the measurement zone. Dust or smears on the
lenses will scatter light that will be measured with the sample scattering. In
general the process of measuring both a background and a sample and then
subtracting the two corrects for such contributions. However this correction is
first order only and excessive dirt on the optics degrades the instruments
sensitivity.
You are recommended to ensure at all times that your lenses and cell windows are
clean. Use the procedures described in chapter 11 for advice on cleaning the
system.
If you are in doubt about the optical cleanliness then you can use the live display
of scattered light to view the background measurement. By viewing this screen
you will be able to judge if the optics are clean or not. This procedure is described
in chapter 11.

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CHAPTER 4

Choosing a range lens


The Mastersizer has several range lenses available. For this initial measurement
you will be using the 300RF lens on the Mastersizer S or the 45mm lens on the
Mastersizer X. If you have followed the installation manual successfully then one
of these lens will already be installed, if not go back to the installation manual and
add the appropriate lens.
In future though you will have to know which lens to choose. There are two
main things to consider - the size range of your sample and the method of
dispersing your sample.

Size range of your sample


The choice of lens will depend on the size of the particles within the sample. Each
range lens covers a different size range of particles. The table below gives these
ranges.

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

(* Used on the long bench Mastersizers only.)


You will have to use a lens that covers the size range of particles in your sample.
For example if you have a sample with particles in the range of 2 microns to 10
microns, using the 1000mm lens will not allow you to measure the bottom range
of the sample. Using the 300RF lens though will give you the correct range.
You may have noticed a problem with the above statement. How do you know
the size range of the sample before you have measured it? If you do not know the
size range of your sample you will have to perform a test measurement. If the
range lens you are using is cutting off the results then the result has a
characteristic look.
The measurement below shows a sample measured on the 0.5-900m range lens
(300mm lens on the Mastersizer S).

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

Particle Diameter (m.)

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

Particle Diameter (m.)

Page 4.4

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CHAPTER 4

Sample dispersion method


The second thing to consider when choosing a lens is the way the sample is
dispersed. Because of the physical arrangement of the 45mm and 300RF lenses it
is not possible to measure samples dispersed in air (i.e. using one of the dry
powder feeder accessories or performing spray measurements) using these lenses.
Due to lens cut off (discussed next) the 100mm lens on the Mastersizer X is
also unlikely to be used for spray measurements.

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.

Avoiding lens cut off (Vignetting)


Care should be taken when measuring spray samples. It should be noted that
there is a physical measurement zone - an area in front of the range lens that the
spray must be confined to. If you spray outside this area then the scattering
information will not be picked up by the detector.
This measurement zone is defined by the cut off point, a distance from the face
of the range lens along the analyser beam.
The chart below gives the cut off point for the lenses. (The 45mm and 300RF
lens have not been included as it is not possible to measure spray samples with
these lenses).

Mastersizer X

Mastersizer S

Lens

Cut off. (mm)

Lens

Cut off. (mm)

100mm
300mm
1000mm*

24
84
290

300mm
1000mm*

36
290

(* Used on the long bench Mastersizers only.)

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

It should be noted that spray measurements can be made with the


sample beyond the cut-off point but the outer detector elements must
be removed from the analysis using Kill data.

Always measure a background


The background measurement is used to subtract the ambient light signals from
the total scattering received from your sample. This allows the instrument to
differentiate stray light from sample scattered light and is important for accurate
results. The background should ideally be freshly taken for every sample that you
analyse. It is advisable to measure the background as near as possible to the time at
which your sample is to be measured, to avoid changes in ambient lighting
conditions.
Exceptions to this rule occur when you wish to run a series of measurements on
the same sample. Here the one background measurement is applied to all the
measurements. This is necessary to allow them to proceed without operator
intervention. In such circumstances the user is advised to operate under stable
lighting conditions if the sample area cover is removed from the instrument (i.e.
when measuring sprays).

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.

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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.

$ To setup the hardware:

. 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!

unit selected here is printed


in the result reports.

GETTING STARTED

Page 4.7

CHAPTER 4

Getting Started

Document the measurement


It is good practice to document the measurement so that you will be able to
identify what you where measuring and how you measured it at a later date. The
Malvern software has a document dialogue that allows you to enter a name for the
sample and enter details that will allow you to recreate the measurement in the
future - such as how much sample you added, what dispersant you used, the
pump speed etc.

$ To document the measurement:


NOTE'

. Select Document from the Measure menu. The document dialogue


shown below will appear.

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.

An introduction to the measure windows


The rest of the measurement procedures, align the system, measure a
background, add the sample and measure the sample are controlled by the
measure windows; measure-align, measure-background, measure-inspect and
measure-sample. The four windows all look very similar and have common
features. A typical window is shown below.

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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.

Align the system


NOTE

'

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.

$ To align the Mastersizer:

. 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.

Take a background measurement


A background measurement is taken to measure the background electrical noise
and the laser scattering from contaminants on the optics and within the dispersant.
It is important that the cell is full of clean dispersant. If you have followed the
installation instructions correctly the dispersion unit will already be pumping a
dispersant around the cell at a pump speed of about 40%. If not follow the
instructions within the Automated Sample Dispersion Unit to fill the unit with
water and pump with the correct pump speed.

$ To take a background measurement:


NOTE'

. From the Measure-align dialogue press the Next button. The Measurebackground dialogue shown below will appear.

If you are not in the


Measure-align
dialogue you can
select the
Measure-background
dialogue by selecting
Background from the
Measure menu or
alternatively you can
select the background

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.

Add the sample


The correct amount of sample has to be added to the system.

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

Too low. Add more sample.


Low but usable with a good sample measurement to
background measurement ratio. Add more sample if possible.
Ideal.
There is a possibility of multiple scattering. Usable but try to
add more dispersant.
Too high.

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.

$ To add the sample:

. From the Measure-background dialogue press the Next button. The


Measure-inspect dialogue shown below will appear.

Page 4.12

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CHAPTER 4
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

the Inspect button.

. 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.

Measure the sample


The final stage of the measurement procedure is to measure the sample.

$ To measure the sample:

. From the Measure-Inspect dialogue press the Next button. The dialogue
below will appear.

GETTING STARTED

Page 4.13

CHAPTER 4
NOTE

Getting Started

'

If you are not in the


Measure-Inspect
dialogue then you can
select the
Measure-Sample
dialogue by selecting
Sample from the

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.

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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.

Choosing the correct analysis mode


The analysis model tells the computer what the expected shape of the result graph
will be. There are five choices available; polydisperse, multimodal, monomodal,
very polydisperse, and compressed range.
. Polydisperse model does not assume anything about the shape of the result graph.
. Multimodal model assumes that there will be one or more distinct peaks
in the results graph - indicating that there are several distinct sizes of particles.
. The monomodal model assumes that there will only be one peak in the result graph - indicating that there is only one size of particle.
. Very polydisperse is similar to polydisperse but is used for a few special
circumstances. (Mastersizer X only).
. Compressed range analysis has a reduced upper size limit and is meant
for use with dry powder and spray measurements. (For Mastersizer S only).

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.

$ To select an analysis mode:

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.

Page 5.2

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CHAPTER 5
Remember - unless you definitely know that the result graph will be of a
particular shape always use the polydisperse model.

Choosing the correct presentation


As stated in earlier chapters the Mastersizer uses the Mie theory to calculate the
size of your sample. The Mie theory requires some knowledge of the optical
characteristics of the sample and the medium it is dispersed in - in particular their
refractive indices. This information is used to calculate a predicted scattering
pattern that the sample would generate when the analyser beam is passed through
it. This predicted scattering pattern is known as a presentation.
The choice of presentation can be one of the most difficult decisions to make
when using the Mastersizer. Saying this, if you are in any doubt you can use one
of the default presentations as these have been chosen to give a middle of the
road setting and in most situations this is more than adequate. It should be noted
that even if you only use the default presentations you would still get more
accurate results when measuring small particles than using an instrument that
only uses the Fraunhofer theory.
If however you decide you need a more accurate result then you can use a
presentation that is more closely matched to your sample. The Mastersizer system
is supplied with many pre-calculated presentations based on the Malvern
presentation grid.

The Malvern presentation grid


The Malvern presentation grid is a convenient method of labeling presentations.
The presentation is labeled by a four character code of the form 3OHD.
The presentation grid is shown on the next page - refer to this grid when reading
the next section, which which discuses its contents.
The first character is a number representing the instrument you are using. If you
have a Mastersizer X then all your presentations will begin with 2 (for example
2OHD) or, if you have a Mastersizer S then all presentations will begin with 3
(for example 3OHD). In the following section the codes for the Mastersizer S (3)
will be used in the examples.
The second character represents the real refractive index of the particle relative to
that of the dispersant. If your particle and dispersant has a relative real refractive
index of 1.45 then the second character will be R, if it has a value of 1.005 then
the second character will be F etc. The values within the grid have been carefully

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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CHAPTER 5
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.

Methods of selecting a presentation


There are several ways to select a presentation. A presentation is always selected
through the Setup presentation dialogue shown below.

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.

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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.

When is the presentation important?


This is a difficult question to answer and usually depends on your own
requirements. Creating a more accurate presentation can be very time consuming
and the extra amount of accuracy may be minimal. If you are unsure of the
benefit of using a different presentation it is best to try using two presentations
close to the one required and see if the difference is acceptable. For example if you
required a presentation that has not been generated, the software will tell you the
closest presentation available. If you make an analysis using this presentation and
then made a second analysis using the next available presentation (effectively
making an analysis using a presentation from both sides of the actual presentation
required) you can then examine the difference in the result. If the difference is
minimal then you should use the closest presentation available.
Remember that you can select an existing presentation and analyse the
measurement data in a few seconds - it may take over an hour to calculate a new
presentation for each lens! It is always best to check if neighboring available
presentations are acceptable before generating a new one.
There are two instances when the presentation becomes important.
Firstly, when the size of the particles within your sample are under 10 microns.
As the particles get smaller then the choice of presentation becomes more
important. In general, if the particles are over 10 microns, then one of the system
presentations will be adequate.
Secondly the presentation becomes more important as the value of the refractive
index of the sample and the dispersant become closer. In general if the refractive
index of the sample divided by the refractive index of the dispersant is greater
than 1.2 then the choice of presentation is not important - the system presentation
should be adequate.

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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.

Calculating the result


Once the optical model and presentation has been chosen the final procedure is to
calculate the result.

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$ To calculate the result

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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Viewing and printing the results

CHAPTER 6

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 information you have generated by analysing the measurement data is


displayed on the screen. The data can be displayed in various formats - each
format is known as a view. Malvern provides 11 standard views that can be
quickly selected by opening the View menu. The View menu is shown below.

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

It should be noted that the result data is never changed - it is only


displayed in a different way.

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.

menu is to press the


right mouse button
when the cursor is over

ILL 1847

the graph pane.

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

Normal data and results

Dark Red

Killed data and results

Green

Blended results

Magenta

Shape corrected results

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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S t a r t e d

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.

Overview of the standard views and


reports
This section describes the contents of the standard views and reports. More detail
on understanding the information is described in the next chapter. For a detailed
description of the Views see the Software Reference manual.
It should be noted that these standard views are there for your convenience. They
have been designed to give a wide choice of common methods of displaying the
result data. You may never have to use some of the views, for example, if you do

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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.

Selecting fonts for graphs and tables


The Graph fonts
The graphs all use the same font for axes, labels and key table. The font is selected
from the Setup - Graph dialogue box. Select the Font... button to produce the
font selection dialogue box. Select a font name, style and size. Note that the title
at the top of the graph is always a bold version of the font. Choose a True Type
font as these give the best reproduction on most printers.
If Scale Size with Graph is selected the size in the font size list box is ignored
and the text size scales as a proportion of the height of the graph frame. This
option is automatically used when transferring a graph to the clipboard, but it may
also be of use if you reduce the size of the Mastersizer window while working in
another application.

The Table fonts


To change the fonts for tables, the text part of reports and the footer of each
printed page select Setup-Table. The section at the bottom of the dialogue box
shows the font information. Up to four fonts may be used in a table or report.
The recommended use for these font styles are:
. Normal font for table entries.
. Same size but bold, for headings.
. Same size and bold but italic or underlined, for showing values that are out
of limits etc.
. Larger size for titles.
Besides each font radio-button is an example of the current font style, but not the
correct font size. The fifth font is marked Draft and is used for the footer of each
printed page and replaces the other four fonts if Draft mode is selected when
printing.

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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.

Installing and selecting a printer


If you want to print from the Mastersizer you must have a printer installed. If
Malvern supplies the computer and printer then the printer will be already
installed. If you are supplying your own printer then you must install a Windows
printer driver compatible with your printer.

$ 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.

Setting up a printer involves:. Selecting the Port.


. Setting resolution and paper size.
. Setting time-outs.

$ 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.

Changing print settings


Using the print options from the Mastersizer software has already been discussed
briefly earlier in this chapter. That information is expanded upon within this
section.
By selecting the Printer Setup dialogue box using File - Printer Setup... you can
change which printer to use and many printer options may be changed without
returning to the Windows Control Panel. In particular:Page Orientation. Tables and Reports look best if Portrait orientation is
used. Full page graphs look best in a Landscape orientation. Changing the
page orientation may have an effect on how tables look in the Table pane.
Page Size. If your printer has more than one paper bin then the page size
may be changed. Remember you may also have to adjust the Margins set in
File - Print... Changing the page size has an effect on how tables look in
the Table pane.

Printing from the Mastersizer

ILL 1848

Using the File-Print... menu item or the Print Easy button will produce the
print dialogue:-

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S t a r t e d

From this you can select the content of the print.


A Report is a single page summary of the result as a table of values, a graph and a
summary of measurement conditions and sample details. The contents and style
of this report are controlled by your choice in the Setup-Table menu item.
The Graph print will be the graph for the currently selected View. The contents
and appearance of this graph depend on your choice in the Setup-Graph menu
item.
The Table print will be the table for the currently selected View. The contents of
this table depend on your choice in the Setup-Table menu item.
The Window option allows you to print a copy of the currently active window.

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Interpreting the results

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.

Results are volume based


The first, and probably most important point to remember in interpreting results
from a laser diffraction instrument is that the fundamental size distribution
derived by this technique is volume based. This means that when the result lists,
for example 11% of the distribution is in the size category 6.97-7.75 microns this
means that the total volume of all particles with diameters in this range
represents 11% of the total volume of all particles in the distribution.
It is useful to consider a numerical example on this point. Suppose, for simplicity,
that a sample consists of only two sizes of particle. 50% by number having a
diameter of 1 micron and 50% by number 10 microns. Assuming spherical
particles, the volume of each of the larger particles is 1000 times the volume of
one of the smaller ones. Thus, as a volume distribution, the larger particles
represent 99.9% of the total volume.
The graph below illustrates this for a more realistic distribution. The example
below shows the result of transforming a skewed volume distribution to
number . Of course, for a mono-size distribution such as a latex, 100% of
particles of a particular diameter will still be 100% whether expressed by number
or volume.

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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

Particle Diameter (m.)

The Malvern software allows the result to be converted to other distribution


forms such as a number distribution for example, but it should be remembered
that the initial measurement is volume based and any subsequent conversions are
liable to introduce systematic errors.

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.

Derived distribution parameters


The third point is that the analysed distribution is expressed in a set of size classes
which are optimised to match the detector geometry and optical configuration
giving the best resolution. All parameters are derived from this fundamental
distribution.
Distribution parameters and derived diameters are calculated from the
fundamental distribution using the summation of the contributions from each
size band. In performing this calculation the representative diameter for each
band is taken to be the geometric mean of the size band limits:

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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The same principle of calculation applies to the distribution statistics standard


deviation, skewness and kurtosis.
For mono-size distributions such as latex the distribution mean is reported as
the geometric mean of the size class and standard deviation, skewness and kurtosis
are reported as zero.
The procedure used for other parameters of the distribution is to create a spline fit
to the fundamental result. Intermediate values are then read off this curve
allowing interpolation of percentile points which do not coincide with the
measurement size band boundaries.

Understanding the tables and graphs


When you have finally completed your analysis you will probably print out a
report from one of the standard views described in the previous chapter. Many of
the measurement statistics and information given are common to most of the
views. Within this section we will explain in simple terms the meaning of these
items, and where possible, give advice on the ideal values they should be reporting
if your analysis is correct.
The result from the analysis is the distribution of particles using the set of size
classes that have been determined by the design of the detector. The detector has
been designed for the optimum arrangement of size classes. It is from this basic
distribution that other statistics are calculated. As stated above, a spline curve is
also fitted to the basic result that allows a result from in-between the size classes
to be determined. The various graphs and report types such as oversize,
undersize, frequency curve and histograms are obtained from this fitted curve.
Volume %
20

100
90

80

70
60
10

50

40
30

20
10
0

0
10.0

ILL 1869

100.0
Particle Diameter ( m.)

The graph above shows the various graph types available.

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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

Measured: 9/08/94 14:52


Analysed: 9/08/94 14:54
Source: Analysed

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

Conc. = 0.3827 %Vol


Distribution: Volume
D(v, 0.1) = 211.47 um
Span = 0.43
Size
(um)
4.19
4.88
5.69
6.63
7.72
9.00
10.48
12.21
14.22
16.57
19.31
22.49

Volume
In %
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00

Density = 1.000 g/cm^3


D[4, 3] = 260.14 um
D(v, 0.5) = 253.18 um
Uniformity = 0.14

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

S.S.A.= 0.0238 m^2/g


D[3, 2] = 252.31 um
D(v, 0.9) = 319.36 um

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

Concentration. This is the volume concentration. It is calculated from the


Beer-Lambert law and is expressed as a percentage.
Distribution. This tells you the type of distribution the analysis has used. The
options for this is set in the Result modification dialogue in the Setup menu.
Options include change from volume to surface area, length or number. It must
be remembered that the Mastersizer measurement is fundamentally a volume
distribution - transforming the result into a surface, length or number
distribution is a mathematical process that may amplify any error in the original
result.
Obscuration. The obscuration helps set the concentration of the sample when
it is added to the dispersant. It is a measure of the amount of laser light lost due to
the introduction of the sample within the analyser beam. An ideal range is
between 10 and 30%.
Uniformity. The uniformity is a measure of the absolute deviation from the
median.

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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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Automating the process

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

A sequence is set up through the Setup-Measurement Sequence menu item.


The Measurement sequence dialogue is shown below.

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

The measurement window during the sequence is similar to that when a


measurement is carried out manually. The Previous button is removed because
you cannot move backwards through the sequence. If the Pause between Stages
checkbox is set in the Setup-Measure Sequence dialogue ( in the diagram at
the beginning of this section) then clicking the Next button will move the
measurement on to the next stage, otherwise the progress through the stages
happens automatically. The figure below shows part of the Measure Window
during a sequence. (Note that the pause status can not be changed after the
sequence has started)

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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CHAPTER 8

Click No if you want to stop the sequence.

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.

Considerations for dry samples


The first step when analysing a sample for the first time is to decide whether to
analyse the sample in a wet or dry state. This is usually determined by the nature
of the end use of the sample. If the product is to be used and stored in a dry form,
for example sand, then perhaps a dry analysis is preferred. Another consideration
is whether the material in its dry state is free flowing. Good pouring
characteristics indicate a non-cohesive powder which will usually disperse well in
a dry powder feeder without any difficulties, whereas a highly cohesive material
tends to stick and clump together giving biased readings.
The sample clumping together can often be overcome by drying the sample in an
oven or by placing in a desiccator until dry and then continuing with the

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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.

Considerations for wet samples


The above are considerations to make when analysing a dry sample. Even more
care should be taken when analysing a sample in a wet medium as there are more
choices to be made.

Choice and preparation of the dispersant


The first choice to consider when measuring a wet sample is the choice of
suspension medium (dispersant). When analysing a sample for the first time, it is
always best to check the dispersion before hand. Add the selected dispersant (for
an initial measurement it is usual to use water) to a little of the sample in a beaker
and visually note the result. The sample may dissolve, this can usually be seen
visually, or if unsure, analyse the sample and observe the obscuration figure. If the
obscuration figure is seen to decrease then the sample is probably dissolving.
The dispersant may itself contain impurities or particles that could be significant.
You are recommended to filter your dispersant before use either with an in-line
pipe filter or, for small quantities, a syringe based disposable type. Filtration to 1
micron is generally adequate with 0.22 microns being commonly available and an
ideal size.
If your dispersant is stored under pressure, or low temperature then you may also
have to consider degassing before use. The pressure release, or temperature rise
will reduce the solubility of gasses resulting in the formation of bubbles in the
pipes and tanks etc. Bubbles are a problem as they are measured with the sample
and are counted as particles - biasing the results. This is particularly a problem
with some mains water supplies. The simple answer is to store sufficient
dispersant at room temperature and pressure for several hours before use to allow
the de-gassing to occur. It should also be noted that the use of cold dispersant in a
warmer environment can also give rise to condensation on the outside surfaces of
the cell windows. For systems plumbed into the mains supplies a small header

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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.

When analysing particles suspended in a liquid dispersant, one of the most


important decisions is which liquid to use. The dispersant can be any clear (at
633nm wavelength) optically uniform liquid that does not interact with the
sample causing it to change its size. Clearly you wish to use the safest, lowest cost
solutions that are effective. Particles that give problems in one medium, such as
dissolution, may be quite suitable in another. In all instances where difficulties in
dispersion are experienced consider the option of another dispersant. The list
below gives the commonly used dispersants (together with their refractive index
for presentation calculations).

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 and admixtures


If you are experiencing problems such as the sample floating on the surface of the
dispersant then the addition of a surfactant or an admixture may be helpful. The
next section briefly explains the use of these additives.

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)

Sodium dodecyl sulphate

Anionic

Hyamine 2389

Cationic

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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.

The use of ultrasonics


In addition to the processes above ultrasonics can be applied to help the
dispersion whether or not it contains a surfactant.
When mixing the sample in the suspension medium, a visual inspection will often
indicate whether ultrasonics are necessary. If there are large agglomerates of
particles which sink to the bottom of the beaker, then try applying two minutes of

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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.

Samples with unstable concentrations


When adding the sample to the tank using the measure-inspect facility of the
software you will occasionally experience obscurations that change during the
dispersion period. Most samples will disperse very quickly so you will not notice
the obscuration value rising. With some samples however the slow dispersion of
the sample can be clearly seen. A measurement should not be made until the
obscuration has stabilised - indicating that the sample has properly dispersed.
The obscuration and its behaviour during the dispersion of the sample can also
warn of other potential problems.
If the obscuration decreases then the size of the particles within the sample may
be increasing, either the sample is sticking together or the particles are actually
swelling due to the dispersant. Other causes could be the larger particles settling
out due to inadequate pumping and stirring or even the particles dissolving.
If the obscuration increases rapidly it could be that particles are attaching
themselves to the cell windows due to surface charges. The material is therefore
in the analyser beam continuously and the obscuration appears to increase. To
solve this problem use an appropriate admixture.

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.

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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.

Summary of sample preparation


The flow diagram below shows the route taken to prepare an unknown sample.
Does Ultrasound
Work ?

SAMPLE
For Dry Analysis
Representative Sample
(riffle if necessary)

For Wet Analysis

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

Does It disperse In Water ?

Analyse

Yes

No

Ultrasound If
Necessary

Does It Float ?
Ultrasound If Necessary

Analyse
Yes

No

Analyse

Try Surfactant

Does This Disperse It ?

Page 9.8

No

ILL 2019

Yes

MAN

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Advanced result processing

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.

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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.

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30

20

10

0
1000.

10.0
30

Particle Diameter (m.)


%

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.

Killing result channels


If it is not possible to remove the effects of contaminants and bubbles by killing
data channels then the alternative is to kill the result channels. These
contaminants form extra modes or peaks in the result after the analysis. By killing
result channels the characteristics of the expected result distribution are isolated.
In a similar manner to killing data channels, only channels at either end of the size
range may be killed. Any number of channels may be killed as long as at least one
channel remains unmodified. Unlike killing data channels the killed result
channels are simply zeroed and the remaining distribution re-normalised.
An alternative use for the kill result facility is to isolate a mode of the distribution
so that the characteristics of that mode may be obtained separately from the
complete distribution. This is particularly important if you are also transforming
the result, where small modes, caused by errors, in the volume distribution are
magnified and can become dominant when transformed to a number distribution.
See Transforming Result Type later in this chapter.
The result channels may be killed by either using the Setup - Result
Modifications dialogue or by adding kill result cursors to the result graph.

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S t a r t e d

Using the Kill cursors

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.

Shape correction - Changing the size


calibration
Each method of particle size measurement is likely to produce different results
when measuring the same sample. This is because different particle sizing
methods measure different physical characteristics of the particle. The particle
diameter is then implied by using some theoretical connection to the measured
parameters. Even image analysis can only produce an indisputable diameter for a
particle if it is spherical and every particle in the sample must be spherical for the
distribution parameters to be correct.
If you have measurements on a sample from an alternative particle sizing method
and wish to compare these with the results of the Mastersizer then you can use
Shape Correction to modify the characteristics of the Mastersizer so it measures
the same as the alternative method.
The modification method is called Shape Correction because the Mastersizer uses
a light scattering theory to convert measured data to a size distribution result and
the theory depends on the particles being near spherical. For non-spherical
particles a correction can be applied.

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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

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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.

Extending the result


If you want to measure samples with a broad range of sizes, some of which are
above the size limit of the Mastersizer, then you may consider using the range
extend facility. The Extend Result modification adds results measured by
another method, usually by sieving, to those of the Mastersizer.
To extend the result at least one measurement by the other method must lie
within the measurement range of the Mastersizer. You need to calculate the
cumulative result distribution using the other method ready for entering into the
Mastersizer software. The values you will need are:
. The size for which 100% of the result is smaller.
. Up to 8 results, consisting of size and cumulative percent smaller, at sizes
above the range of the Mastersizer.

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. 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.

Transforming result type


The basic result produced by the analysis is a volume distribution which is the
volume proportion in each size class of the total volume of the particles. It is
possible to convert the distribution to a different type. Probably the next most
useful distribution type after volume is that of number, where the number
proportion of particle in each size class is the tabulated quantity. The other two
types are surface and length distributions.
The transformation can be expressed mathematically as:

Xi =

100Vi / din
Vi / din

where Xi is the transformed percentage distribution, Vi is the volume distribution


result, di is the mean size of class i and n is the required distribution type: 1 for
surface, 2 for length and 3 for number.
Note that a small volume of particles of small sizes can be transformed to a
significant part of a number distribution. If this small volume is just due to noise,
or other errors in the measurement, then it may swamp the actual desired
distribution. These small errors in the measurement are, in effect, magnified by
the transformation. You may consider using the Kill Result facility to isolate the
significant part of the volume distribution before doing the transformation.
See the Setup-Result Modification menu item in the Software reference
manual for details on setting up a result transformation.

G E T T I N G

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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

Particle Diameter (m.)

The example above shows the result of transforming a skewed volume


distribution to number .

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

Diameter of particles (m)

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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.

Tromp curve analysis


This technique is popular in the cement and mining industries for gauging the
efficiency of classifiers and separators.
View and report files MTROMP.PAG and MTROMP.REP are available in the
Pages sub-directory which display the tromp curve. The analysis is done in
program MTROMP.BSC which also assigns the page to View Result 8. Use the
Control-Run Program command to load and run this program.
When the program is run the current result should be the measurement taken at
the output of the classifier. A result representing the feed distribution will be
asked for by the program along with values for the feed rate input and product
rate input in tons per hour.
For more information on Tromp analysis ask your Malvern representative for the
paper The Importance of Particle Size in the Cement Industry by Dr Alan
Rawle.

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

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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.

Replacing the sample tubing


If organic solvents are regularly used as a dispersant you may find that the plastic
tubing that connects the flow cell becomes hard and discoloured. To change the
tubing simply pull it off the connecting pipes and replace with new tubing.

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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.

The tubing originally supplied by Malvern is Tygon R-3603 available from


Cole-Parmer Instrument Company. Tygon is chemically compatible with a
large range of materials. Contact the manufacturers for specific information on
compatibility.
If the tubing is to be replaced always replace with tubing of the same or better
grade, in order to retain chemical compatibility. Always check the compatibility of
new tubing with the dispersants and samples you are using before connecting and
using the instrument.

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

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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.

Cleaning the covers

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

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Page 11.3

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G e t t i n g

S t a r t e d

Cleaning the optics


The Mastersizer is a precision optical device. Cleanliness of the optics are
fundamental to ensuring good measurements. It will occasionally be required to
clean the cell windows, range lenses and the beam expander.
One guideline for determining when the optics require cleaning is to observe the
live display when making a background measurement. The display shows the
values for each of the data channels. If any channel gives a value of more than 400
divisions then you are recommended to clean the optics.

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.

Cleaning the cell windows


The flow cell is used as an example in this cleaning procedure. The removal and
cleaning of the cell windows are similar on most cells used on the Mastersizer.
Cleaning the system by rinsing through with fresh dispersant a couple of times is
usually sufficient to prepare for a new measurement. Over time you will notice
you cannot achieve such a good background measurement. That is the time to
clean the cell windows.
Make sure that the cell has been drained of dispersant then remove the cell
assembly from the Mastersizer bulkhead. Disconnecting the two sample tubes
from the cell.
The windows are held in place by a metal retaining ring that can be unscrewed by
using the window tool that is found in the accessory case. The cell windows are
sealed by O rings.

$ To remove a cell window:

. 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 .

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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.

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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.

Cleaning the range lenses


The range lenses should not require cleaning often. If you find that you are
getting poor background measurements then the lenses may require cleaning.
The range lenses may be cleaned when removed from the optical unit. First
remove dust from the lens without rubbing. An aerosol clean air duster or a
camera blower brush are both suitable ways to achieve this.
Inspect the lens by reflected light and see if there are smears or prints on it. If so
then you must wipe the lens surface using the guidelines described in the section
Cleaning the cell windows above.

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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.

Cleaning the beam expander


The beam expander will not require cleaning as often as the range lenses. Every
12 weeks however the lens should be carefully inspected for signs of dust. Always
remove the beam expander for cleaning.

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

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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.

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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.

Particle sizing specification


The Mastersizer X has an overall size range of 0.1 - 2000 micron covered in four
ranges. The Mastersizer S has an overall size range of 0.05 - 3500 microns covered
in three ranges.
The table below gives these ranges.

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.

2% on Volume Median Diameter (measured by an approved technique


using a diffraction reference reticle).

Measurement

Up to 45 light energy measurements for the Mastersizer S and 31 for the

data.

Mastersizer X from a custom design semiconductor detector optimised for


light scattering measurement. In addition a centre ring reading measures
the unscattered light energy for determination of the obscuration.

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

0.01 - 135 degrees (over the 3 ranges of Mastersizer S).

range.

0.03-50 degrees (over the 3 ranges of Mastersizer X ).


0.01-50 degrees (over the 4 ranges of long bench Mastersizer X).

Number of size

Up to 100 uniformly spaced on logarithmic or linear plot or user selectable.

classes.
Primary output.

Relative volume size distribution, diffraction energy data and laser beam
obscuration.

Secondary

Relative volume concentration.

output.
Volume distribution on sieve size classes.

Transformation of volume distributions to surface area, length and number


distributions and reverse transformations.

Derived diameters (D[4,3] to D[1,0]) which include volume, surface and


number mean diameters.

Sauter Mean Diameter.

Volume distribution percentiles (user selectable).

Moments of the volume, surface and number distributions, up to 4th


(kurtosis).
Documentation.

Tabulated on screen.
Plotted on screen.
Stored/recalled to disc.
Transferred over RS232.
Printed reports.

Optical unit specification


Description.

Transmitter and receiver units mounted on a rigid optical bed, with


provision for mounting sample presentation cells & accessories.

Laser transmitter.

Minimum 2mW He-Ne Laser (633nm wavelength) with 18mm beam


diameter, collimated and spatially filtered to a single transverse mode.

Page A.2

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APPENDIX A
Receiver for the

Fourier transform lens mount.

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.

Laser safety covers.

Detector electronics.
Receiver for the

Fourier transform lens mount.

Mastersizer X.
Range lenses with 45mm (reverse fourier), 100mm, 300mm focal lengths
and 1000mm for long bench Mastersizer X only.

Detector on sliding rail carriage with automatic positioning at preset optical


positions.

Detector carriage with motorised X-Y positioning under computer control for
auto alignment.

Laser safety covers.

Detector electronics.
Detector for the

42 element composite solid state detector array - optimised for light

Mastersizer S.

scattering measurement, 1 centre detector, 2 alignment detectors, 2


backscatter detectors and 1 laser monitor.

Detector for the

31 element solid state detector array - optimised for light scattering

Mastersizer X.

measurement, 1 centre detector.

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

48, (31 for the Mastersizer X) amplifier parallel sample/hold construction,

electronics.

A/D conversion and on board digital storage.

Sampling time 10 s for all 48 detectors of the Mastersizer S, and the 31


detectors for the Mastersizer X.

Read in time to computer approximately 2ms.

Sampling from internal/external trigger source.

On board storage for 100 experiments.

Digital I/O interface. 12 output, 16 input lines.


Power

110/240V, 50/60Hz, 1200VA

requirements.
Dimensions.

Standard Mastersizer 1200(L) x 335(H) x 290mm (W).


Long bench Mastersizer 1853(L) x 335(H) x 290mm (W).

Weights.

Standard Mastersizer optical unit - 47 Kg.


Long bench Mastersizer optical unit - 66 Kg.

Computer requirements (minimum)


Description.

IBM-PC/AT compatible 486DX/33 or SX with Overdrive chip fitted


(minimum).

Data Capacities.

4 Mbytes total RAM Memory, (minimum).


60 Mbyte (minimum) integral hard drive, (7.1 Mbytes required for
Mastersizer software).
3.5" high density floppy disc drive.

Keyboard.
Mouse.

102 key standard layout with 12 function keys.


Microsoft Windows compatible. If a serial mouse is used note that the
Mastersizer software, by default, expects the instrument to be connected to
the COM 1 port.

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.

Parallel port for for a printer.

Page A.4

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APPENDIX A
Screen.

Enhanced VGA monitor supporting a resolution of 800 x 600 or greater is


recommended. (The Malvern software is compatible with VGA resolution.)

Printer.

High resolution printer - 300dpi or greater. Microsoft Windows compatible.


Laser or Bubble / Ink Jet type preferred. Colour printer is optional.

Software.

MS-DOS

Disc Operating System - all commands for; configuration of system,


peripherals, disc management and batch operation capabilities. Version 5.0
or later required.

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

All files needed to operate Mastersizer, presented as an integrated suite


with installation procedures. All Mastersizer files are contained in one
directory named by the user, further sub-directories being automatically
created.

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.

Mastersizer programme specification


Loading
Fully automatic with optional self starting of preprogrammed activities.
Copying
Copying restricted to end user use only. Passing on to others contravenes the
software license.
Configuration
User tells system the optical configuration which is used to scale results correctly.

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.

Software Revision Level


Malvern is engaged in a continuing programme of development, both in
measurement capabilities and software features. Thus, during the lifetime of a
product a number of software versions will exist, in general increasing in
capability as they become more current. In general users of older versions will be
able to purchase updates to these later versions if they are significant. Seek advice
regarding costs from your local representative.

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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.

Components in contact with sample


and dispersant
Wet sample measurements
Component

Location

Materials

Cell pipe connectors.

Sample area cover.

Stainless steel.

Dry sample measurements


Component

Location

Materials

Sample area cover.

External covers.

Two-pack polyester paint.

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.

All spray measurements should be extracted to the outside of the building.


However, some material may settle out onto the surfaces of the sample area. If
this happens the area should be cleaned immediately.
As an additional caution the paint finish of the external covers may be
permanently damaged if samples or dispersants are spilt onto them. Any spillage
must be scrupulously cleaned up immediately.
Remember to check the chemical compatibility of your sample accessories before
using a new sample and dispersant.

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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 .

If no remote interlock is to be used then the connector is fitted with a shorting


plug that will enable the laser to be switched on.
It should be noted that the continual interruption of the power supply to the laser
will reduce the life of the laser. To solve this problem an interlock switch system
similar to the circuit diagram below is recommended.
In this system there are two switches. The first is a normal interlock switch that
is attached to the door of the room that will disable the laser when the door is
opened. The second switch is a spring return type manual override switch
that allows the user of the Mastersizer to keep the laser power on if they know
that someone is going to enter the room. Using this configuration will reduce the
number of times the laser is switched off by only disabling the laser when
someone unexpectedly enters the room. The circuit is connected to the remote
socket using a standard 3 pin DIN plug.

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

0 1 01

Estimating the absorption

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.

Estimating the absorption using


concentration measurements
The following technique may be useful in estimating the absorption in certain
cases. For a given measurement, the volume concentration is calculated using the
equation:-

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

Particle Imaginary Refractive Index

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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Advice for continuous sprays

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.

Arrange for the spray to be extracted


Sprays are not contained within a cell and if there is nowhere for them to go after
they have passed through the beam they can back circulate and possibly deposit
out onto the optics. Remember therefore to consider where your spray goes after
measurement and ensure that nothing prevents it. Avoid operating against walls
or other equipment that prevent air circulation. Ideally arrange for an extraction
air flow. Also consider any health risks when spraying hazardous materials.

Use the correct optical configuration


Because all normal sprays will occupy a long illuminated beam length it is not
feasible to measure sprays using the 300RF lens and the Mastersizer S or the
45mm lens on the Mastersizer X. In addition, the short lens cut-off distance of
the 300mm range restricts the usefulness of this range for sprays. The most
suitable range is the 1000mm range (long bench users only) but the 300mm range
may also be used if you pay attention to the possibility of the large angle scattering
being cut-off (vignetting) by the lens aperture.

Positioning the spray nozzle


A spray invariably expands in extent as it travels away from the nozzle. If no
evaporation occurs then this means that the concentration of particles that will lie
at any time in the Mastersizer analyser beam will reduce as the distance from
beam to nozzle increases. Close to the nozzle there will be a limit caused by the
concentration being too high for accurate measurement. Downstream a limit will
also occur where the spray concentration has become so low as not to be reliably
detectable. Between these extremes an acceptable range of measurements can be
made.
In some types of spray the droplets do not reach a stable size until some distance
away from the nozzle. Close to the nozzle the liquid may be in the form of

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.

Dont spray the optical unit


Care is required to avoid the spray settling on the lenses. The droplets formed
will scatter light and distort the size distribution accordingly.

Ensure the spray is stable during


measurement
Variations or inconsistent spray performance during the measurement can lead to
fluctuating results. Try to ensure that the spray conditions are stable and if
fluctuations are inherent remember to increase the measurement interval so that
averaging increases the result stability. If you wish to probe time variations in the
size distributions then you must use the Spray Synchroniser accessory which
allow accurate time resolution of the size measurement. For advice on making
pulsed spray measurements please see Spray Measurements in the Software
Reference manual.

Page E.2

MAN

0 1 01

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

Malvern Instruments (Asia Pacific)


38 Jalan Bangkung
Bukit Bandaraya
59100 Kuala Lumpur
Malaysia
Tel: +60 (0) 3 252 1973
Fax: +60 (0) 3 253 0542
Malvern Instruments Nordic AB
Vallongatan 1
750 15 Uppsala
Sweden
Tel: +46 (0) 18 55 24 55
Fax: +46 (0) 18 55 11 14

Page F.2

MAN

0 1 01

Regulatory compliance
statements

APPENDIX G

Statement of LVD compliance


The CE badge on this product signifies conformance to European Commission
Directive 72/23/EEC the Low-Voltage Directive as amended by Directive
93/68/EEC the CE Marking Directive. The directive has been satisfied for
Malvern equipment by applying BS EN 61010-1 :1993 Safety requirements for
electrical equipment for measurement, control, and laboratory use Part 1 General requirements.

Statement of EMC performance for the


Mastersizer S
The CE-badge on this product signifies conformance with the protection
requirements of the European EMC directive, (89/336/EEC).
The following statement of EMC performance refers to the Mastersizer S system
as defined below operating under the following test conditions.

Equipment under test


Equipment

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

During emission tests the equipment was under control of a Mastersizer S


Version 2.11 Software Automated Sequence. This repeatedly measured a known
sample.
For immunity tests the operator checked that the measurement was within the
determined experimental error, and if outside this pre-set tolerance flagged or
noted an error. The susceptibility pass/fail criteria was that the equipment repeats
the measurement within the norm of experimental error.

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

Statement of EMC performance for the


Mastersizer X
The CE-badge on this product signifies conformance with the protection
requirements of the European EMC directive, (89/336/EEC).
The following statement of EMC performance refers to the Mastersizer X system
as defined below operating under the following test conditions.

Equipment under test


Equipment

Model

Mastersizer X

MSX build version 036226. Feb 93

Support equipment:
NEC PowerMate 386/33i

PM-1222-2431 31154UB

VDU

JC-1521HMP-EE 2YT01803A

Kbd

APC-H4122 2800578M

Mouse

M\N M-5E9-6MD A1019300200

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

. Complies with BS EN55022 (1995), class B, radiated and conducted emissions.


. Complies with BS EN50082-2 (1995), generic immunity standard (industrial environments).
. Complies with BS EN61000-4-2 (1995), Electrostatic discharge, to severity
level 4, using 8kV contact discharge and 15kV air discharge, with performance criteria 1, i.e. normal performance within specified limits, i.e. generic
performance criteria A
. Complies with DDENV50140, (1994), Immunity to radiated electromagnetic energy to severity level 3 (10V/m 1kHz 80% AM 80MHz - 1GHz and
200Hz 1000PM at 900Hz) with performance criteria 1 i.e. normal performance within performance criteria 1. i.e. generic performance criteria A.
. Complies with BS ENV61000-4-4, immunity to electrical fast transient/bursts, to severity level 4 using 2kV on signal lines and 4kV on power
supplies, with performance criteria 1, i.e. normal performance within specified limits , i.e. exceeds specified requirements to generic performance criteria A.
. Complies with BS ENV50141 (1995), Immunity to conducted RF disturbances to severity level (10Vrms 1KHz 80% AM 150KHz - 80MHz) with
performance criteria 1 i.e. normal performance within specified limits, i.e.
generic performance criteria A.

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

Estimating the absorption


Extending the result

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

0 1 01

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

Removable accessory panels


Sample area cover
Sample cell
Sample area cover
Sample cell
Sample file
Sample preparation
Riffler
Bubbles
Dispersant
Dry samples
Slurries
Ultrasonics
Wet samples
Sample preparation accessory
Saving the result
Scattering pattern
Sequence
Setup sequence button.
Setup measurement
Shape correction
Slurry
Software
Software screen
Button bar
Graph pane
Menu bar
Splitter bar
Status bar
Table pane
Title bar
Splitter bar
Splitter bar cursor
Start/stop buttons
Status bar
Surfactants and admixtures
Sweep trigger connector
Sweeps
Systems covered by this manual
T
Table fonts
Table pane

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

0 1 01