Malvern Mastersizer 3000 User Manual

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MASTERSIZER 3000

USER MANUAL

Mastersizer 3000

User Manual

MAN0474 Issue 2.1 August 2013

Malvern Instruments pursues a policy of continual improvement due to technical development. We therefore reserve the right to deviate from information, descriptions, and specifications in this publication without notice. Malvern Instruments shall not be liable for errors contained herein or for incidental or consequential damages in connection with the furnishing, performance or use of this material. No reproduction or transmission of any part of this publication is allowed without the express written permission of Malvern Instruments Ltd.

Head office:

Malvern Instruments Ltd. Enigma Business Park, Grovewood Road, Malvern, Worcestershire, WR14 1XZ United Kingdom.

Tel + [44] (0)1684-892456 Fax + [44] (0)1684-892789

Mastersizer, Malvern and the 'hills' logo are registered trademarks in the UK and/or other countries, and are owned by Malvern Instruments Ltd.

Windows is a registered trademark of Microsoft Corporation.

Tygon is a registered trademark of Saint-Gobain Corporation.

Kalrez and Viton are registered trademarks of DuPont.

Perlast is a registered trademark of Precision Polymer Engineering Ltd.

PEEK is a registered trademark of Victrex.

Table of contents

Introduction to this manual

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-1

About this manual. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-1

Access to the instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-2

Assumed information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-3

Where to get help . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-4

Introducing the Mastersizer 3000

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-1

About the Mastersizer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-4

Typical systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-5

Optical unit components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-9

End panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-11

Cell components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-13

Software overview

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-1

Powering on and starting the software . . . . . . . . . . . . . . . . . . . . . . . . . . .3-2

Software user interface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-3

Customising the software interface . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-14

Maintenance utilities . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-21

Making measurements

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-1

Measurement types and process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-1

Measurement prerequisites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-2

Making SOP measurements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-3

Making manual measurements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-16

Manual control accessories. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-21

SOP Player . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-22

Measurement settings reference . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-25

Mastersizer 3000 Page 1

Table of Contents

Viewing measurement results

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-1

Working with measurement files. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-2

Analysis report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-11

Fundamental concepts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-14

Optical models . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-21

Sample preparation guidance

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-1

Sample preparation flow chart. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-2

Representative sampling. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-3

Considerations for dry samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-4

Considerations for wet samples. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-5

Symptoms of poor sample preparation. . . . . . . . . . . . . . . . . . . . . . . . . .6-10

Reporting

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-1

About reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-2

Viewing and using reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-3

Copying data from reports. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-9

Creating and editing reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-11

System security

About security . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8-1

Activating security . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8-1

Software licensing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8-3

21 CFR part 11. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8-5

Advanced features

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .9-1

Doing more with SOPs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .9-1

Exporting data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .9-6

Page 2 1

Introduction to this manual

Introduction

This manual covers the operation of the Mastersizer 3000 and Mastersizer 3000E particle characterisation systems. The instrument measures the size of particles contained within a sample, presenting data according to the user’s needs.

This user manual is a companion to the Mastersizer 3000 Basic Guide, which gives Health and Safety, maintenance, troubleshooting and other vital information which all users must read.

Additional user manuals are supplied with both the Hydro and Aero dispersion units.

About this manual

The manual contains the general information required by an operator; as well as supervisor information that concentrates on administration and extension of the system’s functionality.

Topics covered include:

 An overview of the Mastersizer hardware and software.

 A guide to making measurements and how to read the results.

 Sample preparation guidance.

 Reporting - creating and editing reports.

 System security.

 Advanced features.

Mastersizer 3000 Page 1-1

Chapter 1 Introduction to this manual

Warning!

The instrument and the samples to be measured may be hazardous if misused. Users must read the Health and Safety information in the Basic Guide before operating the system.

Access to the instrument

This manual refers to the various people who will have access to the instrument, as follows.

Malvern Instruments personnel

Malvern Instruments personnel (service engineers, representatives etc.) have full access to the instrument and are the only people authorised to perform all service procedures that may require the removal of the covers.

Warning!

Removal of the covers by unauthorized personnel will invalidate the warranty of the instrument. Unless advised within the content of this manual, only Malvern Instruments trained personnel are permitted to remove the main cover of any part.

Supervisor

The supervisor is the person responsible for the management and safety of the instrument and its operation. The supervisor is responsible for the training of the operators. The supervisor can perform all user maintenance routines identified in the Basic Guide and within this manual.

Warning!

Under no circumstances should the supervisor or an operator remove the main cover of the instrument.

Operator

An operator is a person trained in the use of the system. The operator can perform all user maintenance routines identified in the Basic Guide.

Page 1-2 MAN 0474

Introduction to this manual Chapter 1

Warning!

Failure to follow these guidelines could result in the emission of laser radiation. Laser radiation can be harmful to the body and cause permanent eye damage.

Assumed information

To make full use of this manual, the user should understand the following points.

Naming convention

Within this manual:

 The Mastersizer 3000 and 3000E instruments will be referred to as “the optical

unit” or “the instrument”, or simply the Mastersizer.

 The sample dispersion units are referred to as “the Hydro MV” or “the Aero

S”, or as “the dispersion unit”. “Wet dispersion units” refers to the Hydro LV, MV, EV and SM. “Dry dispersion units” refers to the Aero S.

 The combination of the optical unit, one or more dispersion units and the

computer is referred to as “the system”.

Ribbon commands

The control ribbon in the Mastersizer application software is divided into tabs:

The first button on this tab bar is referred to as the Application button and has a similar function to the File menu on older systems.

Ribbon commands are referred to in this manual in the form: ribbon tab selection, followed by option. For example, Home-Manual Measurement describes clicking an option that is found on the Home tab

Whenever a ribbon option also has a sub-item this is shown as by the presence of a down-arrow on the ribbon bar icon; as shown for the Home-Run SOP option shown. Ribbon commands and the names of windows are always shown in bold text.

Mastersizer 3000 Page 1-3

Chapter 1 Introduction to this manual

The SOP Player feature, shown above, is only available with the Mastersizer 3000 / Mastersizer3000E with Extended software option.

Where to get help

This section describes the available sources of information on the system. The primary sources of information on the system are instrument and accessory manuals and the software’s help system. The manuals give an overview of the system as a whole, while the online help system gives more detailed information on the Mas tersizer application software. Some features are described in both the manuals and Help system.

Manuals

The following manuals are available for the Mastersizer:

Basic Guide

A concise yet essential guide that provides an introduction to the system and its usage covering Site requirements, Health and Safety and an instrument and accessory overview. Finally a brief guide to making a measurement and view- ing the results is included.

User Guide

The primary source of information about the Mastersizer hardware and its use. See About this manual earlier in the chapter.

Dispersion unit guides

Separate guides are supplied with both the Hydro and Aero dispersion units. These provide essential information on the connection, operation and maintenance of the dispersion units.

Help System

Each key software window has a Help button giving information specific to it. Additional Info Tips are also available whenever is shown - simply move the

mouse pointer over this icon to see a relevant tip.

Page 1-4 MAN 0474

Introduction to this manual Chapter 1

Technical support

Malvern Instruments offers several methods of technical support, which are described in this section.

Email support

Note

This is the primary support method – only use the other methods if this is not available at your location.

Customers with internet access should use the Contact Malvern feature in the software’s Maintenance window. This is

described fully in the Software overview chapter. This feature ensures that our support team have all the relevant information about your system.

If you do not have internet access from the computer operating the Mastersizer system, contact your local Malvern Instruments representative - details of all local telephone numbers are available at www.malvern.com. Always quote the following information:

 Model and serial number of the instrument. The serial number is shown

on the Mastersizer application software status bar.

 The software and firmware version. To find this select Tools-Mainte-

nance in the software and then examine the System information section alternatively, move the mouse over the instrument status bar icon. The Appli cation Version is the main firmware version number to note.

Additional support

Contact the International Malvern Helpdesk if the local Malvern Instruments representative is not available:

Telephone: +44 (0)1684 891800  Email: helpdesk@malvern.com.

Note

This help line is primarily English speaking.

Mastersizer 3000 Page 1-5

Chapter 1 Introduction to this manual

Remote support

Malvern Instruments offers a remote support service, delivered by an internet connection. Benefits include fast and efficient fault diagnosis, as well as reducing downtime and costs.

Malvern website - www.malvern.com

The Malvern Instruments website offers a comprehensive range of particle characterisation resources for use by customers 24 hours a day, seven days a week.

Page 1-6 MAN 0474

Introducing the Mastersizer 3000

Introduction

This chapter provides information about the Mastersizer 3000 hardware and identifies all major features of the system.

The following topics are covered:

 A description of the purpose of the instrument and its accessories.

 A hardware overview of a typical wet and dry system.

 Detailed reference on the physical parts of the optical unit.

 Information about the parts of the cell, including how to insert and remove it.

Note

Hardware maintenance – for details on how to maintain the hardware, please refer to the Basic Guide and the separate dispersion unit guides.

Mastersizer 3000 and Mastersizer 3000E instruments

There are two core instruments in the Mastersizer 3000 family, these are the Mastersizer 3000 and Mastersizer 3000E. Though identical looking there are some fundamental differences between the two; in terms of their software functionality and operation with the associated dispersion units.

The differences between the two Mastersizer variants are shown in the below table.

Mastersizer 3000 Page 2-1

Chapter 2 Introducing the Mastersizer 3000

Mastersizer 3000E

- Basic software 

feature set

Mastersizer 3000E

- Extended software

feature set

Mastersizer 3000

Hardware

Particle size range 0.1 - 1000μm 0.1 - 1000μm 0.01 - 3500μm

Compatible with Manual Hydro wet dispersion units (Hydro EV / SM)

Compatible with Automated Hydro wet dispersion units (Hydro MV / LV)

Compatible with Aero dry dispersion unit

•••

••

•

Software

SOP operation •••

Customized reporting •••

Entry level legacy system result compatibility tools

Advanced method development and comparison tools

Advanced data quality assessment and reporting tools

Advanced measurement manager functions

Measurement sequencing / SOP player tool

New feature additions and upgrades

Ability to use the software on multiple workstations

User workspace functions ••

•••

••

Page 2-2 MAN 0474

Introducing the Mastersizer 3000 Chapter 2

Mastersizer 3000E

- Basic software 

feature set

IQ/OQ Validation •

CFR21 part 11 ER/ES

(additional Feature key necessary)

Mastersizer 3000E

- Extended software

feature set

Mastersizer 3000

•

The Extended software feature set is detailed later in the Software overview chapter; Customising the software interface section.

To simplify the text throughout the manual, the 3000 and 3000E instruments will be referred to as the Mastersizer (or “the optical unit” or “the instrument”), unless it is necessary to differentiate or highlight any differences; then the instrument will be identified as Mastersizer 3000 or 3000E as appropriate.

Mastersizer 3000 Page 2-3

Chapter 2 Introducing the Mastersizer 3000

About the Mastersizer

The Mastersizer is comprised of the main optical unit, one or more dispersion units and a measurement cell. Commonly, a dispersant such as de-ionised water is also connected directly to the dispersion unit.

Optical unit

The main optical unit, sometimes referred to as the optical bench or just the instrument, is the core of the Mastersizer system. In its simplest terms, its purpose is to transmit red laser light and blue light through a sample and then use its detectors to generate data about the light scattering pattern caused by the particles in the sample. The data is then interpreted by the Mastersizer application software to provide accurate particle size information. The blue light used on MS3000 provides improvements in the measurement resolution below 1 micron in size.

Dispersion units overview

There are two types of dispersion unit: wet and dry. Wet units (Hydro MV/LV/ EV/SM) control the dispersion of a sample suspended within a liquid dispersant.

The function of the dry unit (Aero S) is to ensure that a dry sample is dispersed and evenly fed to the measurement cell within a continuous stream of air.

Measurement cell

The cell is the interface between the dispersion unit and the optical unit. The sample is routed between measurement windows in the cell so that the laser can pass through it in order to make a measurement.

Computer (Mastersizer application software)

At the heart of the system lies the Mastersizer application software, which runs on a computer. This application controls the optical unit and dispersion unit hardware, and also processes the raw data gathered by the system, providing flexible data analysis and reporting features.

Page 2-4 MAN 0474

Introducing the Mastersizer 3000 Chapter 2

Typical systems

Wet dispersion

A wet system consists of the optical unit and either the Hydro LV/MV or EV dispersion unit. These dispersion units are designed to circulate a liquid sample through the Mastersizer's measurement cell. Many materials need to be measured as wet dispersions. Typically these are materials that are used or produced wet in the manufacturing process or need to be dispersed in a liquid in order to achieve reproducible dispersion.

Hydro LV/MV

The Hydro MV and LV units are designed to create a suspension of particles in water or other liquid media. The Hydro LV can handle a liquid volume of 600ml, whereas the Hydro MV unit has a volume of 120ml. Both can be configured to automatically deliver liquid dispersants and also dispose of the sample following a measurement. This enables the cleaning and filling of the units as part of an SOP.

The large capacity of the Hydro LV makes it ideally suited to the measurement of samples which have very broad size distributions or contain large particles. In some cases, sample materials are not plentiful and the MV's smaller volume sample dispersion unit is a sensible choice to minimize sample and dispersant consumption while retaining the benefits of totally automated sample dispersion and measurement.

Hydro EV

In the mineral, chemical, metal powder refining and cement industries, measurements of larger sample volumes are often most appropriate for QC of the manufacturing process and finished product. The large capacity of this unit makes it ideally suited to the measurement of such samples as well as larger materials having broad size distributions.

The Hydro EV is a wet dispersion unit designed to circulate a liquid sample held within a standard laboratory beaker through the Mastersizer's measurement cell. As such the filling and emptying of this unit is a manual process.

Hydro SM

The Hydro SM enables the Mastersizer to be used for particle-in-liquid particle sizing, where the amount of sample available limits the amount of dispersant that can be used to dilute it, or where just a small volume of dispersant is available. This is ideal when the sample or dispersant is toxic or expensive.

Mastersizer 3000 Page 2-5

Chapter 2 Introducing the Mastersizer 3000

The following illustration shows a typical wet dispersion unit installation:

1 2

 

Wet cell

Computer running the Mastersizer application software

Optical unit



Wet dispersion unit





Optical unit (as described in the next section)

Measures the sample using red and blue light wavelengths.

ill 8620

Dispersion unit (in this case the Hydro LV)

Circulates the sample through the cell

Wet cell

Sample flows through the air cell so that it passes through the instrument’s laser path.

Computer running the Mastersizer application software

Controls both the optical unit and the attached dispersion unit, as well as processing and presenting the measured data.

Other wet dispersion units include the Hydro MV, EV and Hydro SM.

Page 2-6 MAN 0474

Introducing the Mastersizer 3000 Chapter 2

4 5

Dry dispersion

The Aero S dry dispersion unit is only compatible with the Mastersizer 3000 optical unit.

A dry system comprises of the main optical unit plus the Aero S dispersion unit. The Aero S is designed for providing an even circulation of dry powder throughout Mastersizer measurement cell.

Direct software control over the feed rate and air pressure is provided, which enables flexible control of both the sample throughput and dispersion. The unit can be controlled either independently of measurement or from within a manual/SOP measurement. The following illustration shows a typical dry dispersion unit instal lation:

ill 8652

Optical unit



Dry dispersion unit



Dry cell



Mastersizer 3000 Page 2-7

Vacuum unit



Ancillary switching unit



Computer running the Master-



sizer application software (not shown)

Chapter 2 Introducing the Mastersizer 3000

Optical unit (as described in the next section)

Measures the sample using red light detection.

Dry dispersion unit (in this case the Aero S)

Disperses the sample and transports it to the measurement cell.

Dry cell

Sample flows through the air cell so that it passes through the instrument’s laser path.

Vacuum unit

Removes the sample from the cell exhaust once it has been measured.

Ancillary switching unit

An external control accessory that is used to switch on the vacuum unit required for the sample extraction during each measurement.

Computer running the Mastersizer application software (not shown)

Controls both the optical unit and the attached dispersion unit, as well as processing and presenting the measured data.

Page 2-8 MAN 0474

Introducing the Mastersizer 3000 Chapter 2

Optical unit components

This diagram shows the optical unit, the main component of the Mastersizer system. The unit directs red and blue light through the sample and then collects the light scattered by the particles within the sample using a set of light-sensitive detec tors. This data enables the system to calculate particle size:

ill 8622

Optical unit



Cell



Instrument status LED



Cell bay



End panel



Mastersizer 3000 Page 2-9

Protection window



Adjustable feet



Drain



Tube/cable routing guide



Chapter 2 Introducing the Mastersizer 3000

Cell

Two types of cell are available:

 Wet - for the Hydro LV, MV, EV and SM units.

Standard and solvent compatible versions of the wet cells are available.

 Dry - for use with the Aero S unit (The dry cell is sometimes known as the air

cell).

Instrument status LED

The instrument status is indicated as follows: Standby (i.e. powered on, but not making a measurement): pulsating dim; Active (i.e. making a measurement) - constant bright; Error - flashing bright.

Cell bay

The interface between the sample dispersion unit and the optical unit. The sample passes between two windows that allow it to be analysed by the optical unit’s laser beam.

End panel

Provides the communication connectors for the optical unit as well as the power connection and switch. Refer to the Mastersizer 3000 Basic guide for further connection reference.

Protection window

Stops dust/dirt entering the system. Clean this window periodically. Refer to the Mastersizer 3000 Basic guide for more information on cleaning the protection window.

Adjustable feet

It is important to ensure that the instrument is levelled on the bench - adjust the feet individually in order to accomplish this.

Drain

Allows any spillages in the cell area to exit onto the laboratory bench.

Tube/cable routing guide

Neatly routes all connection pipes and cables underneath the instrument.

Page 2-10 MAN 0474

Introducing the Mastersizer 3000 Chapter 2

End panel

The end panel of the instrument provides the communications and power connections.

ill 8623

 



Power switch

USB

 

CAN 1-3

Power input

Power switch

Press once to power on the unit, press again to power off.

Mastersizer 3000 Page 2-11

Chapter 2 Introducing the Mastersizer 3000

USB

Provides data communication with the PC. For best performance connect to a high

speed USB port on the PC:

CAN 1-3

Supplies power and data communication to the dispersion unit.

Power input

Input for 24V power supply unit.

Page 2-12 MAN 0474

Introducing the Mastersizer 3000 Chapter 2

Cell components

The following illustration shows the key parts of a wet cell – for a more detailed description of both the wet and dry cells, refer to the Hydro or Aero Dispersion Unit Guides respectively:

Cell release button



Cell handle



Sample output (blue)



Temperature regulator throughput



Sample input (yellow)



Cell windows



ill 8625



Cell eject button

Ejects the cell from the cell bay locking mechanism so that it can be withdrawn from the cell bay.

Mastersizer 3000 Page 2-13

Chapter 2 Introducing the Mastersizer 3000

Cell handle

Only lift the cell by this handle.

Sample output (blue)

Connected to the sample in (blue) on the dispersion unit.

Temperature regulator throughput

Provides throughput connections to a water jacket within the cell. This allows an (optional) heater/chiller to regulate the sample temperature to help minimise the effect of ultrasound heating.

Sample input (yellow)

Connected to the sample out (yellow) on the dispersion unit.

Cell windows

Sample passes through the window and is measured by the system. Cell windows should always be kept clean to ensure accurate measurements - see the Hydro Wet Dispersion Units Guide.

Inserting and removing the cell

Always follow this process when inserting or removing the cell from the instrument. This section assumes that all relevant tubing connections between the dispersion unit and cell have already been made. Refer to the dispersion unit manuals for verification of these connections.

Inserting the cell

1. Lift the cell by its handle .

2. Insert cell into the instrument as shown in the previous Mastersizer optical

unit illustration.

3. Do not force the cell into the instrument - only slide it into the cell holder until

it stops.

4. The cell now automatically locks into place within the cell bay.

Removing the cell

1. Press the cell eject button  to eject the cell from the cell bay.

Caution!

Do not try to remove the cell from the cell bay without first pressing the cell eject button  as this could damage the locking mechanism.

2. Withdraw the cell from the instrument using its handle  in the direction

shown in the previous Mastersizer optical unit illustration.

Page 2-14 MAN 0474

Introducing the Mastersizer 3000 Chapter 2

Note

If the cell is raised and lowered too many times in a short period, the firmware will lock the cell in place for a period of time before it can be ejected again; this is to prevent damage to the locking mechanism.

Mastersizer 3000 Page 2-15

Chapter 2 Introducing the Mastersizer 3000

Page 2-16 MAN 0474



Software overview

Introduction

The Mastersizer application software serves several key functions: it controls both the optical unit and the dispersion unit; it allows users to create and edit measurement files; it enables users to run manual or SOP measurements on both wet and dry samples, and finally it provides access to powerful reporting and data analysis features.

This chapter gives details on the following:

 Powering on and starting the software.

 Description of the software user interface.

 Customising the software interface.

 Maintenance utilities.

This chapter provides a description of the key elements of the software only. For information on how to run a measurement, see the Making measurements chapter. Additional features of the software are also detailed in the Advanced chapter of this manual. Reference information for all features is provided in the Help system.

Note

This section provides a description of the key elements of the software only. For information on how to run a measurement, see the Making measurements chapter. Some advanced features of the software are also detailed in the Supervisor’s section of this guide and reference information for all features is provided in the Help system.

Mastersizer 3000 Page 3-1

Chapter 3 Software overview

Powering on and starting the software

1. Ensure that the optical unit, dispersion unit and computer are connected (con-

nection reference is given in the Mastersizer 3000 Basic guide).

2. Power up the computer and printer (if available) by following the instructions

in the manuals supplied.

3. Connect the optical unit’s power supply to the mains power supply.

4. Press the on/off switch on the instrument’s side panel once to power on.

The blue indicator on the top of the instrument illuminates, together with the blue indicator on the front of the dispersion unit, which pulsates to indicate that standby mode is active.

5. Log in to the computer that is connected to the instrument and start the Mas-

tersizer application software by double clicking on the Mastersizer desktop icon.

6. The main Mastersizer application software window is now displayed. 

A correct connection to the instrument shows both the instrument and accessory name in the status bar:

If the instrument is not connected correctly, the status bar indicates:

If this is the case, check the instrument’s connection to the USB port on the PC and the power connections to the instrument.

If the dispersion unit is not detected, the following is shown:

If this is the case, check the connection from the instrument to the dispersion unit. Also, a blue pulsating power light on the dispersion unit indicates that it is connected correctly to the instrument.

Note

Before using the instrument to measure a sample, wait for 30 minutes for the laser to stabilise.

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Software user interface

The main software window, with a measurement file loaded, is shown as follows:

 Ribbon selector tabs  Reports tabs  Control ribbon  Data Quality tab  Record View panel  Status bar  All files tab  Private/Shared workspace

ill 8811



Ribbon selector tabs

Provides quick access to the different control ribbons. The Application button (leftmost) gives quick access to file, print and software options (including security) as well as software version information.

Control ribbon

Single-click access to key software functions.

Record View panel

Lists all measurements within the active measurement file. Multiple measurement files can be opened simultaneously, which are then accessible by different tabs within the Record View.

All files tab

View all records from all open measurement files in a single tab.

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Chapter 3 Software overview

Reports tabs

Provides access to reports on the currently selected record. The reports shown are a function of the currently selected workspace.

Data Quality tab

Provides guidance on the measurement quality and displays a simple pass/fail data report based on selected models, together with tips on how to improve the measurement. The Data quality tab is not available in the MS3000E basic software.

Status bar

Shows the instrument mode, connected user, 21 CFR status, notifications (see later in this chapter), connected accessory type and the instrument connection status (as well as its serial number when connected).

Private/Shared workspace

The workspace shows the settings and data assigned to the user or users using the instrument at the time. Individual (private) or common (shared) workspaces can be created. Workspaces are not available in the MS3000E basic software.

Control ribbons

Control ribbons provide quick access to key software functions.

 To select an option, click on the appropriate direct-access button, for example

Extract SOP.

If you contract the software window horizontally, the individual ribbon options are grouped under a single icons instead. The ribbon then operates in a similar manner to menus in that the group must be selected initially to reveal the sub-items, for example Result-Extract SOP.

 To select a different control ribbon, click the selector tabs above the ribbon

(Home, View Tools or Audit).

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Record View tab

The Record View allows you to view and edit the records contained in Mastersizer 3000 measurement files. It is also possible to open files that were created by Mastersizer 2000 instruments, but not edit them. Mastersizer measurement files consist of a number of individual measurement records.

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Each open measurement file is given a tab in the Record View: click one of these tabs to show all of the records contained in that measurement file.

Note

You can open as many measurement files as required, and also combine results, using All Files, to view all records within a single tab, making graphical data overlay possible. See Merging records in the Viewing the measurement results chapter for more information.

Each measurement record consists of a set of parameters, one of which is shown in each column. (It is possible to edit the selection of parameters that are displayed if required.) Many parameters contain numerical data measured by the system, but some contain other information, such as Scattering Model, Accessory Name and so on. Some parameters also answer simple yes/no questions, such as Has Background Alarm Triggered? Items like this are checked if affirmative.

Powerful analysis features also allow records to be sorted, grouped and filtered so that users can focus on only those records that are of relevance to their application. See the Viewing the measurement results chapter, and the Help file, for more information on grouping and filtering.

The Parameter filters, grouping and column configuration features are only available with the Mastersizer 3000 / Mastersizer 3000E with Extended software option.

Editing which parameters are displayed

To choose different columns of data to display in the Record View:

1. Right click on a column header and choose Column Configuration.

2. Then, from the Parameter Selection window, select items in the Available

column and add them to the Selected column. Use the Search feature in this window to quickly find a parameter.

3. Click OK to complete the process.

Sorting on a parameter column

Click the column header. Click the header again to reverse-sort based on that selection - sorting is either alphabetical, numeric or boolean, depending on the parameter selected.

Locked measurement files

Any tab indicated with a padlock icon is a read only file that cannot be edited. This is the default status for any Mastersizer 2000 files that are opened with the Mastersizer application software.

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Selected Records Information

At the bottom of the Records view a summary is provided that details the number of records currently selected within each measurement file.

Copying records

Records can be copied in a couple of ways:

 Duplicating records: 

To duplicate records to a new measurement file or within the same measurement file. From the Clipboard group on the Home ribbon, select Copy - this will copy the records to the clipboard. The content can then be pasted back into the Mastersizer application software.

 Copying records into Excel:

To quickly copy records into Excel or similar applications the selected records must be dragged from the Mastersizer application software, and dropped into the chosen application. Alternatively the data export options can be used (refer to the Advanced features chapter).

Reports tab

Reports are displayed automatically whenever you select a record, or number of records, from the Record view (assuming that the selected view is showing the Reports tab).

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Chapter 3 Software overview

Note

For detailed information on the process of viewing, editing or creating new reports, see the Reporting chapter

Data quality tab

The Data Quality tab is only available with the Mastersizer 3000 / Mastersizer 3000E with Extended software option.

The Data quality tab presents a custom analysis of any records selected in the current measurement file.

Select the records for which you wish to view a data quality report.

Click the Data Quality tab (next to the Reports tab).

Select the refresh tab; this will drop-down from the menu bar when a new record is selected)

Alternatively the display can be set to Auto-refresh. Selecting the button will set the display to automatically refresh the data quality view whenever a new record is

selected .  Press again to de-select.

The display is updated to show a quality review of each record selected. Click

to toggle whether items that have passed or failed are displayed.

Items that have passed the quality check are shown .

Items that have failed the quality check are shown .

Results can be shown in a tabular or list format

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The above illustrates the Default data quality selection. Two additional checks are available; these are ISO variability and USP variability.

Illustrations of each are shown below.

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Workspaces

Workspaces are only available with the Mastersizer 3000 / Mastersizer 3000E with Extended software option.

This section describes the purpose of workspaces and the Workspace pane.

Workspaces are a collection of settings that define the information presented in the Reports and Record View, as well as which folders the system uses for accessing SOPs, measurement data and export data.

Each user can access both a Private or Shared workspace, both of which are configurable. This makes it easy for an individual to optimise the software for their own use, with the Private workspace, or to collaborate better across an organisation using a Shared workspace. The latter is particularly useful within quality controlled environments.

The following settings and data are associated with the workspace:

 SOPs and SOP Templates presented to users (i.e. their file locations).

 Record parameters shown in the Record view.

 Reports listed in the Reports view (see the Reporting chapter).

 Measurement data file location.

 Exported data and Export Templates file locations.

 Workspaces also control where the software will look for data quality addins,

macros, user calculations, etc.

Note

Any of these items that are created when the Shared workspace is active will be available to all users of that system (providing their security privileges allow them access to these functions). If the Private workspace is selected, these items are only available to the current user.

Selecting the workspace

Reveal the Workspace pane by clicking the button at the top of the Workspace panel on the left of the window. Clicking the button again will close the Workspace pane. Additionally the panel splitter bar can be dragged left or right to resize the workspace pane.

To select the required workspace click the button at the top of the Work- space panel:

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Any work subsequently performed on the system will now use the selected workspace both to save data and to access settings.

Recent measurement files

This is a simple list of the last five measurement files that have been accessed within the selected workspace.

Measurement files and SOPs within the workspace can be pinned to keep them in the windows indefinitely. To pin an item, hover the mouse over the item and select the pin button.

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Record and reports view selector

The record parameters shown in the Record View, and the reports listed in the Reports view are controlled using the Record and reports view selector to the right of the of the Workspace pane. Additionally the Records and report selector stores (and restores) any selected data quality addins.

You can add as many different views as required – these are stored within either of the currently selected workspaces.

To add a new view:

1. Click Add new view from the Workspace pane.

2. Enter a View name in the Result View Properties window.

3. Click Configure record view columns to show the parameter selection win-

dow. Select the required parameters and then click OK.  Similarly click Configure report selection to display the Report Selection window, select the required reports and tab order, and then click OK.

Refer to the Reporting chapter for details on report selection.

4. Once you have added new views, make them the active view by clicking on

them from the list. The selected view will now be shown as the record and reports view selector title.

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The Reports and the Record View are updated immediately.

5. To edit or remove a view, first select it from the list and then select the Edit or

Remove icons.

Targets

The targets listed are links to Mastersizer system folders and provide quick access to all of your workspaces, reports, SOPs, measurement data, etc. Clicking on a target will open the respective folder within Windows Explorer.

The folders that are linked to from this panel are specific to the selected workspace.

If the Private workspace is selected, the folders all stem from:

C:\Users\YOURNAME\Documents\Malvern Instruments\Mastersizer 3000\Workspace\

If the Shared workspace is selected the folders stem from:

C:\ProgramData\Malvern Instruments\Mastersizer 3000\Workspace\

Shortcuts

Shortcuts are an easy mechanism for users to set-up a set up links to folders, e.g. on a network, that can be shared between all users on that PC.

To create a shortcut: Create new shortcuts to files/folders by dragging them into the Shortcuts panel from Windows Explorer. Shortcuts to web sites can be added by dragging a bookmark from Internet Explorer into the Shortcuts panel.

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Customising the software interface

In addition to the options available as part of the Workspace specification, several further features provide control over how the software is presented to the user.

Options

The options window provides access to various user preferences and allows security to be enabled/disabled. Selection of the options available will enable them for use in the associated software control windows. If they are not selected they will not be available for use.

Note

Some options are only available with a feature key installed. Please contact your Malvern representative for more information.

From the Application button menu choose Options to display the Mas- tersizer 3000 - Options window. Then click the required link on the left to view its corresponding settings.

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General Preferences

Click General from the Options window to choose the following settings:

 Show settings when running manual measurements – this automatically

displays the measurement settings window whenever a manual measurement is initiated. This can be useful during method development where the user needs to switch back into the record view after making each measurement and then make slight alterations to the measurement settings for the subsequent meas urement. If this option is de-selected, the settings are still available to the user

by clicking

 Force saving of records – with this option selected every measurement file

on the Manual Measurement window.

will be saved on creation with temporary measurement files no longer being made. The measurement files will automatically be saved when the software is closed, so there will be no prompting for the user to make changes.

Note that this option is automatically enabled and cannot be changed when the 21 CFR feature is installed.

 Enable Mastersizer 2000 / 2000E Analysis Emulator – Enable this option

to add 3 additional emulated Mastersizer 2000 / 2000E analysis models to the list of analysis models in the Data processing - Analysis SOP and record edi tor.

The emulator converts Mastersizer 3000 results to how it would be analysed on a Mastersizer 2000 instruments, and similarly for a Mastersizer 3000E result the Mastersizer 2000E instruments is emulated.

Refer to Data processing - Analysis SOP description in the Making meas- urements chapter.

 Enable virtual lens ranges – This enables the controls on the advanced anal-

ysis page of the SOP for virtual lens ranges. Virtual lens ranges limit the result analysis range to that of a legacy instrument, such as a 300mm lens used on a Mastersizer X.

Refer to Data processing - Analysis SOP description in the Making meas- urements chapter.

 Display results to same precision as Mastersizer 2000 – this option ena-

bles the software to display results to the same precision as used in the Mastersizer 2000 software. Results will be displayed to 3 decimal places.

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Themes

The Themes option is only available with the Mastersizer 3000 / Mastersizer 3000E with Extended software option.

Several themes are available which modify the colour settings of the user interface. Click Theme from the Options window and then select a scheme that suits your preference by clicking Use this theme.

Graphs

Choose Graphs from the Options menu to access further options that relate to the presentation of graphs:

 Line weight – specify the line weights (Normal, Light or Heavy) to be used in

all graphs.

 Colour scheme – choose from one of several colour schemes. The Master-

sizer 2000 theme emulates the appearance of the Mastersizer 2000 graph colour scheme, Greyscale is optimized for printing on a monochrome printer, High Contrast provides better on-screen visibility.

Folders

Use this option to either view, by clicking on the folder; or edit the workspace folders where the Malvern data is stored.

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Custom layouts (Save/restore layout)

The configurable windows feature is only available with the Mastersizer 3000 / Mastersizer 3000E with Extended software option.

Save layout is a simple feature that allows you to store the exact position of all elements of the Mastersizer interface. This could be useful in situations where you have optimized the interface for your current analysis process.

Positioning elements within the user interface

To reposition items - drag any of the following panels to another position within the main window: Record View, Data Quality, and Reports.

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The following tool is shown on the screen when dragging:

This indicates that pre-set positioning options are available for the element. Whilst still holding down the mouse button, move the mouse pointer over one of the direction arrows in this tool - a shaded box is shown indicating how the element will be placed. Release the mouse button to place the element.

Saving or restoring the window layout

To save commonly used panel and window arrangements for future use:

1. Position any of the panels of the software as desired, for example, the Record

View, Reports etc.

2. Click Save layout on the View ribbon.

3. The New layout file window is displayed – enter a name for the layout (all

layouts have the .mlay file extension) and click Save.

4. To access a previously saved layout, click Restore layout and then locate the

relevant .mlay file.

Note

By default the system initially returns to the window layout that was present when the software was last closed.

Predefined Window Layouts

The Predefined window layouts allow to you quickly select from a number of optimized panel arrangements within the Mastersizer user interface.

 From the Predefined window layouts group in the View ribbon, select the

required layout.

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Quick access toolbar

The Quick access toolbar provides an alternative method for accessing commonlyused functions.

1. To add any ribbon function button to the Quick access toolbar, right-click it

and choose Add to Quick access toolbar. The button is now additionally displayed (in reduced form) in the title bar of the software:

In this example, the Manual measurement, Save and 2-pane tabbed buttons have been added to the Quick Access toolbar.

2. To remove the button, right-click it and choose Remove from Quick Access

toolbar.

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Maintenance utilities

The Maintenance window gives access to various background information about the system that can be useful as part of an ongoing maintenance schedule or in the process of contact with the Malvern Instruments Help Desk.

 Choose Tools-Maintenance from the ribbon to display the Maintenance

window:

The window is broken down into the following sections:

Notifications

Notifications are brief notes that indicate any errors, problems or necessary remedial/investigative action that may be required in order to keep the system functioning correctly. Follow the advice given in any notifications and then remove them by clicking Clear All.

The Status bar also provides a visual reminder that notifications are available:

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Click the Notifications icon on the status bar to view the Maintenance window.

System information

The main purpose of the system information area is to display details about the software, operating system and hardware connected. This information must be passed to the Malvern Instruments Helpdesk whenever you log a support call. To send this information to Malvern Instruments:

If you have email software on the Mastersizer computer:

 Click Contact Malvern to display the contact form. Complete the form and

then click OK. Your default email software then starts and an email is gener ated containing the relevant system information. Additional fields appear in the email where you can input information about the issue you are experiencing with the Mastersizer system.

If you do not have email software on the Mastersizer computer:

 Click Save text report to save a text file containing this information. Then

copy this information onto a data stick and transfer it to a computer that has an email connection in order to attach the file to send to Malvern Instruments.

 Print the information using the Print option and then refer to this information

if you wish to contact the Helpdesk via telephone.

Maintenance reminders

Maintenance reminders can be set up within the software to prompt users to carry out routine maintenance tasks. To configure these, access the Tools-Mainte

nance window. Within the Maintenance window, there is a Maintenance reminders section, where any active reminders are listed.

Click on the Configure icon to open a list of active maintenance tasks, from which existing tasks can be edited, or new ones added:

Click on a maintenance task to show its full details. If the task requires editing select the Modify button.

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To set up a new maintenance task, click the Add button.

The details required include:

 Name: a task name.

 Notifications from: the date when users should start being prompted to carry

out a task.

 Task due by: the date by which the task needs to be completed.

 Repeat interval: how often the task should be done (weekly, monthly, yearly,

etc).

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 Task description: text providing guidance as to what needs to be done by the

user.

 All users can complete task option: Select this checkbox to confirm that

any user can complete the task. If this is left un-ticked then only users who have the Open Maintenance security permission assigned to them can set the task to done. This could, for instance, apply to tasks associated with book

ing a service or OQ visit, where it would be the supervisors responsibility to complete the task.

Users are alerted to tasks which are due to be carried out by a Maintenance icon in the status bar. Clicking on this will display the maintenance detail.

Clicking on the Done? icon clears the task.

If the task is not completed by the due date then a service Notification is gener-

ated and is displayed on the application's status bar.

System health checks

The Mastersizer application software constantly checks the status of the optical system and the dispersion units to ensure it is functioning correctly. If any issues are detected, they will be reported within this section for the maintenance report.

A health check can be performed at any time by selecting the button. The results of the tests will be reported in the System health checks section of the maintenance dialogue.

Note

Connection to a system is required for this option to work.

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System usage

The system usage section provides details on the total Running Time of the instrument and any connected accessory. Additionally details are provided on the running time of the accessory stirrer running time and ultrasound if applicable.

Logs

The Logs section contains links to all the logs generated in the previous 24 hour period. After 24 hours, if no further log files have been generated, only the last log file generated is retained. Log files contain no data that is of direct use to users, but may be requested by the Malvern Helpdesk when trying to resolve any issue.

To send a log file:

 Click on the Save Text Report option on the maintenance report icon bar.

This will record a new system status report.

 Click on the Open folder option within the Logs section of the report. This

will open the directory containing all of the system logs.

 Copy all of the logs, and email these to the Malvern Instruments.

Note

In the case where a software crash has occurred, a series of crash dump files (.dmp) will be stored in the logs directory alongside any maintenance reports and a trace.log file. These files contain detailed information about how any crashes occurred, and should therefore be sent to Malvern Instruments along with any maintenance logs.

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Making measurements

Introduction

The Mastersizer is capable of measuring samples dispersed in a wet or dry medium, either manually as a one-off (or for developing an SOP method) or by utilising pre defined settings stored within an SOP file.

This chapter is the main reference for the measurement making process and includes sections on:

 Measurement types – a brief background on the overall process of making a

Mastersizer measurement.

 Measurement file basics – how to create and open measurement files.

 Making an SOP measurement – includes how to create SOPs as well as the

steps involved in running an SOP.

 Making a manual measurement – the basic steps involved in manual meas-

urement with a wet dispersion unit.

 Measurement settings reference – detailed reference on all measurement

settings available to both SOP and manual measurements.

Measurement types and process

The Mastersizer is capable of making two types of measurement:

 Manual measurements – all of the measurement settings are specified before

the measurement and some further user input is required during the running of the measurement. The measurement process is also split into key stages, which are paused after the completion of each stage.

Manual measurements tend to be used for one-off measurements or as part of method development (i.e. establishing the optimal settings for measuring the

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Chapter 4 Making measurements

 Standard Operating Procedure (SOP) measurements – most of the

measurement settings are stored within an SOP file which has been previously created by the user. Once an SOP has been initiated, the measurement sequence requires less user intervention than a manual measurement.

As SOPs lock-down most of the measurement settings they improve consistency and provide greater repeatability; features that are important in qualitycontrolled environments.

The process of both measurement types is broadly as follows:

1. Power on the system and create a measurement file.

2. Specify the measurement settings for a manual measurement or SOP.

3. Run the measurement.

4. Check the results, looking for any problems.

5. Clean the system.

Measurement prerequisites

Note

The instrument and accessory must have been connected and set up in accordance with the guidance in the Mastersizer Basic Guide and the dry or wet dispersion unit guide. This section assumes all appropriate connections have been made.

Before a measurement can be made, the instrument must be powered up and a measurement file must be created. Measurement files contain all data acquired by the Mastersizer during a measurement. Each measurement file can contain a number of individual records.

1. Switch on the optical unit. The pulsating blue light on the top of the instru-

ment indicates that it is on. Check also that the blue light on the dispersion unit is pulsating - power to the dispersion unit is drawn from the instrument.

Note

Leave the instrument powered on for 30 minutes before making a measurement to allow the laser to stabilise.

2. When 30 minutes has elapsed, switch on the computer, log

in to Windows on clicking on the Mastersizer icon on the desktop:

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Making measurements Chapter 4

Note

If, after successfully starting the Mastersizer application software, any of the functions described in the rest of this section are unavailable to you, this will be due to your login credentials – contact your system Supervisor for assistance.

3. Ensure that the status bar indicates that the instrument is connected correctly:

4. If the instrument is not connected correctly (i.e. if anything else is shown in the

status bar), refer to the Software overview chapter for more information on how to fix this.

5. Create a new measurement file by selecting New-Measurement File from

Home section of the control ribbon:

Alternatively new measurements can be added to an existing measurement file.

6. Choose Save and then name the measurement file, for example Starter sam-

ple.mmes.

Making SOP measurements

SOPs are predefined measurement sequences that can be used to both automate and standardise Mastersizer measurements. Widely used in the pharmaceutical industry to provide traceability, SOPs also provide non-pharmaceutical users with a reliable means of automating measurements, ensuring that a wide selection of personnel can obtain consistent results regardless of familiarity with the instrument.

SOPs can control the configuration of the optical unit and the sample dispersion unit, including the measurement parameters, timings, analysis models and other specific set-up information. They can also be configured to prompt the operator to perform specific tasks such as sample preparation steps.

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The quality and value of an SOP depends on the quality of the method development work on which it is based. A series of manual measurements is required to establish the ideal parameters for use in an SOP. A number of standard SOP templates have been prepared in advance for typical measurements, which may be used unchanged or as the basis for a new SOP.

The Mastersizer application software's powerful SOP editing facility enables users to review and refine SOPs as part of their ongoing quality control process.

Creating or editing an SOP

SOPs need to be created and saved before they can be used. To create a new SOP:

1. Select New-SOP from the Home ribbon. (To edit an existing SOP, choose

Open-SOP instead.)

2. Select an SOP template from the list in the New SOP window or click the

From an existing SOP... button to locate an SOP in the file system that fulfils

(or is close to) your required criteria.

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3. The SOP Editor window is now displayed as illustrated (the Material set-

tings are shown in this example):

4. Step through the SOP Editor by clicking the section titles on the left (Sam-

ple-Identification, Sample-Material etc.) or clicking the Forward / Back

arrows on its toolbar.

Note

Complete each of the sections detailed in the Measurement Settings Reference section in later in this Chapter.

5. When all the required settings have been specified, you can either choose to

save the SOP as a file or as a template. choose File-Save and then give the SOP a logical name.

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Running an SOP (Hydro units)

If you are using a wet dispersion unit (the Hydro LV/MV/EV) work through the steps in the order given here. No manual control of the dispersion units is required after loading the sample; the software controls all settings.

1. Select Run SOP from the Measurements section of the ribbon.

2. The SOP Selector window is shown, which initially presents all SOPs filtered

for the connected accessory (

the Accessory filtered button to show those that are not specific to the

connected accessory.

Accessory filtered). Alternatively, deselect

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Click on an SOP to display its properties in the bottom panel of this window.

3. After selecting an appropriate SOP, click OK.

4. The Measurement Display window is shown. The progress bar at the top of

the window reports both the current status and what to do next.

The Trend view show in the bottom half of the Measurement display illustration is only available with the Mastersizer 3000 / Mastersizer 3000E with Extended software option.

 Result view panel

The Result view panel contains the Laser, Light Scattering and Size Distribution panels. The information shown is either live or, after a measurement

has been completed, relates to the currently selected record (the bold yellow line) - this record number is shown at the top of the Result View panel.

 Laser - the Laser display panel initially provides an indication of the cur-

rent Power output of the laser, and then, during the sample addition phase, with the current obscuration level. When adding sample it is vital that the obscuration falls within the green band - this band is defined by the user in the Measurement obscuration section of the Manual measurement settings window.

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 Light scattering - the light scattering panel provides a live graph

showing the energy plotted against detector number. This is available as a live display before the measurement is initiated. Following the measurement this panel contains the data recorded at the measurement time.

 Size distribution - the size distribution graph plots Volume (%)

against Particle Size (μm) - This is blank until the measurement has been initiated. After a measurement has run, and been selected in the trend view, the data shown is that gathered at measurement time.

 The light scattering and size distribution views can either be shown

separately or tiled next to each other by selecting the split view button.

The split view button is only available with the Mastersizer 3000 / Mastersizer 3000E with Extended software option.

5. Click the Start button to Initialise the instrument. If specified in the

SOP settings, the system prompts the user to enter/confirm sample documentation details. Following this stage. the system automatically moves to the Measure Background stage and measures both the red and blue light values of the background.

Note

To stop both the SOP and the accessory during a measurement, click the

Abort button . This “all stop” command should only be used when a problem is suspected - this is because the sample will stop circulating, which could affect further measurements if the sample is not then refilled.

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6. When the Measure Background stage is complete, the SOP pauses. The sys-

tem now requests that you add sample - do this until the Obscuration bar indicates about 10-20% for a wet dispersion unit. (This is a rough guide only as this setting is highly sample-dependent - refer to the Help system for more guidance.)

7. Click Start again. The measurement now commences, measuring first the red

and then the blue light values. The SOP may make a number of measurements before completion, depending on the Number of measurements specified in the SOP settings. When complete, the Trend view is updated with the new measurement figures:

8. Complete the measurement by closing the SOP Measurement window.

9. The results are now presented in the Record View.

More about the Trend view

The Trend view is only available with the Mastersizer 3000 / Mastersizer 3000E with Extended software option.

The Trend view is a powerful analytical tool that shows record data in a graphical format as soon as it has been measured by the system.

The main purpose of the default view is to indicate that sample measurements are stable. For example, if the sample was slowly dissolving then the apparent sizes may appear to be reducing. In many industries, measurement repeatability is quantified by specifying a maximum Relative Standard Deviation (RSD) over a number of measurements. The Trend view allows you to highlight a number of measurements and display the RSD, and other statistics in real time. Any other parameter

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Chapter 4 Making measurements

can be added to the Trend view, for example to see how Ultrasound Power settings are affecting the measurement.

By default, each measurement’s Dv10, Dv50 and Dv90 figure is shown, so it is very simple to make a quick assessment of the result. The Dv50 category shows the median particle size. Further statistics and measurement parameters can also be viewed on the Trend view.

Once a number of measurements have been performed, it is possible to select multiple records in order to view combined figures for the range. It is also possible to modify the data displayed on the graph, and add entirely new graphs with a different focus of interest if required.

This is an example of the trend view after four measurements have been made. The currently selected range in this example includes just two records: Record Number 2 and 3 - the figures displayed in the coloured boxes relate only to those two records.

Statistics shown in the live trend view

The live trend view identifies each line with a key, which shows statistical information about the measurement:

The data shown relates either to the individual measurement or range of measurements selected by the user. The default view shows particle size statistics. Trend plots can be configured to show any parameter – the statistics shown on a plot line relates to a single parameter only.

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 Main figure – the actual size measurement (μm) for the single base record

that is currently selected (Dv10 - blue, Dv50 - green, Dv90 - red).

 Av – the average particle size (μm) for the selected range.

 RSD – Relative Standard Deviation (%) for the selected range.

 Min – the minimum particle size (μm) for the selected range.

 Max – the maximum particle size (μm) for the selected range.

To modify which figures are shown in the Trend view:

1. Right-click anywhere on the trend graph and choose Statistics.

2. Select or de-select the items required.

Tip

Click anywhere on the graph line to display data points - click again on the line to remove them. Move the mouse pointer over a data point to display its record number and size figure, for example 4, 891.09 indicates that Record 4 has a measured size of 891.09μm.

Selecting a range of records in the trend view

After running several measurements, just one record is selected. Initially this is the last measurement made. This record is shown by a vertical hairline bar with the

record number indicated at the bottom - for example, . The vertical hairline bar always shows the currently selected record.

 To expand the range to incorporate more records, click the left or right

selection arrow buttons at the top of this bar. The bar expands to cover the

records selected:

Click and drag this header bar to the left or right to reposition the selection within the range of records. Alternatively, right-click the trend graph and choose: Statistics range and then select the number of records.

 To contract the range, click and drag the left hairline bar that denotes the

initial record in the selected range. Alternatively, right-click on the trend graph and choose: Statistics range and then select the number of records to include in the selected range. If you have manually dragged the bar to cover a number of records not listed in the Statistics range menu, Custom and the number of records currently selected is displayed.

All numerical data then provided is the arithmetic mean of the currently selected records, with the exception of the initial particle size figure, which is still the figure for the single record.

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Chapter 4 Making measurements

Adding further trend graphs

Add additional plots using the following method (note that the new plot needs to be configured prior to making the measurement in order to display data):

1. Right-click on the trend graph and select Add above or Add below to add a

new plot.

2. Then choose parameters from the Parameter Selection window and click

OK.

To remove the new plot, right-click it and choose Delete.

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Running an SOP (Aero units)

The Aero S dry dispersion unit is only compatible with the Mastersizer 3000 optical unit.

The software controls most of the dispersion unit settings except the hopper height, which is a manual adjustment. Work through the steps in the order given here.

1. Open the Aero S sample area lid and set the hopper flow rate  to an appropri-

ill 8655

ate gap level using the dial (marked from 0-4mm - refer to the Aero Series Dry Dispersion Units Guide for more information).

Mastersizer 3000 Page 4-13

2. Empty the sample into the hopper .

3. The mesh basket and ball bearings may be used on coarser samples to smooth

the flow of sample, breaking up any loose agglomerates before they fall into the hopper.

4. Close the lid of the Aero.

5. Select Run SOP from the Measurements section of the ribbon.

6. The SOP Selector window lists all available SOPs.

Chapter 4 Making measurements

7. Choose an appropriate SOP for the Aero dispersion unit (ensure also that the

SOP is optimized for the venturi type that is fitted to your Aero unit - either stainless steel or ceramic venturi) and then click OK.

The Measurement Display window shown below is displayed:

8. Click Start – the SOP automatically aligns the optical system and then

measures the background using the red light (blue light is not used in dry measurements).

9. After this, the sample tray starts vibrating and the SOP-specified air pressure is

applied. The overall rate at which the sample is fed into the cell is a function of the combination of air pressure, vibration rate and hopper flow-rate setting.

Note

To stop both the SOP and the accessory during a measurement, click the

Abort button .

10. The SOP selected should be optimized for the dry dispersion unit and will

only make a measurement once the obscuration is within the specified range (1-10% obscuration is the rough guide for a dry dispersion unit).

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Making measurements Chapter 4

11. The results are shown immediately in the Trend view as they are gathered.

When all of the measurements have been made, the system pauses - optionally, click Clean System on the top progress bar to initiate a cleaning cycle.

12. Complete the measurement by closing the SOP Measurement window. The

results will now be presented in the Record View.

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Chapter 4 Making measurements

Making manual measurements

In addition to SOP measurements, users can also make manual measurements. This may be useful, for instance, when investigating the most appropriate method for sample dispersion prior to setting up an SOP. This section provides details on how to run a basic manual measurement.

Note

This process description assumes that a wet dispersion unit is connected to the instrument.

The basic procedure is similar to that outlined in the SOP measurement section, but requires the user to set up the measurement settings initially, and then manu ally initiate more stages during the live measurement process:

1. From the Home ribbon click Manual measurement from the Measure-

ments group. The Manual Measurement window is displayed, together

with the Manual Measurement Settings window:

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Making measurements Chapter 4

Note

This section now provides information on how to enter only some of the key measurement settings - for complete details on all settings, see Meas- urement settings reference later in this chapter.

2. Choose the Sample-Identification settings to record both the Sample

Name details and define any further information fields (for example, Notes)

that will help users to repeat the measurement at a later date.

3. Use the Sample-Material section to define the optical properties (the

Refractive index and Absorption index) of the new material. The material

may already be stored in the system’s Materials database. Check this first by clicking Browse database - select the material if it is present to automatically add the RI and Absorption values to the measurement.

4. Use the Measurement-Duration section, shown below, to set up measure-

ment times for the red and blue measurements.

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5. In the Measurement-Obscuration section define the lower and upper

obscuration limits - as a very rough guide, about 10-20% for a wet dispersion unit and 1-10% for a dry dispersion unit.

6. Click OK to close the Manual measurement settings window.

7. From the Initialise Instrument drop down menu, select Auto Alignment.

8. Click the Start button to initialise the instrument - when complete, the

system progresses to the Measure Background stage.

9. Filling and starting the dispersion unit:

Depending on the accessory that is currently connected, the control options (shown in the panel on the right) will vary. For a wet dispersion, a steady circulation of dispersant needs to be in place before adding the sample. To do this, ensure the accessory is filled with dispersant - if using an LV/MV, click Fill in the Dispersant section of the Accessory panel.

Note

See Controlling dispersion units (manual mode) later in this chapter for more information.

The docked accessory control tab in the Measurement display is only available with the Mastersizer 3000 / Mastersizer 3000E with Extended software option. Users with the Basic software feature set should control the dispersion unit using the Accessories option on the Tools ribbon.

10. When the accessory is full, set the Stirrer speed and start the accessory:

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11. Click Start on the measurement progress bar at the top of the window. Both

the red and blue light values for the background are measured.

12. The system now requests the user to Add Sample - add small quantities of

sample to the dispersion unit until the obscuration is within range (10-20% in the case of a wet dispersion). Refer to the Help system for more guidance. With a dry dispersion, the system will skip this step.

Note

With dry dispersions, the whole sample is loaded into the hopper in the Aero before the measurement process is started.

13. Click Start again twice to begin the measurement. First the red and then the

blue light values are measured. When this is complete, the Trend view is updated with the new measurement figures (see Running an SOP in this chapter for more detailed information on the Trend view). The particle Size Distribution graph is shown in the upper right panel. In the example shown here, just a single measurement was specified in the manual measurement set tings.

The Trend view is only available with the Mastersizer 3000 / Mastersizer 3000E with Extended software option.

14. Continue this final Measure Sample process as many times as required by

clicking Start again. To complete the measurement, just close the Manual Measurement window. The new records are now added to the Record View.

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Chapter 4 Making measurements

Manually controlling the dispersion units

Use the Accessory controls panel from the manual measurement mode to configure the currently attached accessory.

Normally, an SOP or Manual measurement controls the accessory's operation within the context of a measurement. Alternatively, the Accessory controls panel allows you initiate the current accessory before the measurement is actually made. This is essential when observing the effects of variation to the accessory's settings on the live Laser and Light Scattering panels, in order to optimise the sample's concentration and circulation prior to making a measurement. This option could also be used as part of a manual cleaning process.

 To access the Accessory control panel: the instrument must be in Manual

Measurement mode, then click the Accessory controls tab on the right of the Manual Measurement window.

Tip

The same controls are also available, when not making a measurement, from the Active accessory control feature (choose Tools-Accessories from the main control ribbon). This option could be useful, for example, if you wanted to keep a sample in circulation whilst undertaking a report analysis.

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The options available on this panel depend on the connected accessory. These are described in the dispersions units respective user manual.

 Hydro series wet dispersion units manual for the Hydro MV, LV, EV and

SM dispersion units

 Aero series dry dispersion units manual for the Aero dispersion units

Manual control accessories

Manually controlled accessories may also be connected to the optical unit. These accessories do not have an automated or manual software control, but will be controlled directly from the control interface on the accessory itself.

Like the automatic controlled dispersion units, manual accessories are selected from the SOP Editor:

 On the Home ribbon, select New-SOP from within the Documents group.

ribbon. (To edit an existing SOP, choose Open-SOP instead.)

 Complete the SOP Editor as described in the Mastersizer 3000 User Manual.

Information on the manually controlled accessories is described in the dispersions units respective user manual.

Refer to the Hydro series wet dispersion units manual for the Hydro SM dis- persion units.

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Chapter 4 Making measurements

SOP Player

The SOP Player is only available with the Mastersizer 3000 / Mastersizer 3000E with Extended software option.

With SOPs created and saved, users are now able to define an SOP playlist sequence where results can be automatically collected for a single sample using different measurement and/or analysis settings - this is done using the SOP player.

In order to set up an SOP playlist, users first need to create a set of SOPs for the dispersion unit they want to use that contain the measurement settings required for the sequence. They then select the SOP Player option from the Home ribbon bar, the SOP Player dialogue will open.

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SOPs available for use in a playlist are shown on the left of the SOP Player window, with the current playlist is shown on the right. The details for any selected SOP are provided in the bottom section of the player, allowing users to confirm the settings the SOP file contains.

To add SOPs to the player, select them from the available SOPs list and drag them

into the SOP playlist, or use the button. SOPs can then be dragged

up and down into the final position or deleted from the list using the button. As the playlist is constructed, messages will appear to help the users organise the finished playlist (e.g.: Drag and drop SOPs here to create a playlist / The SOP does not match the target accessory type).

Changes the currently opened folder

Adds the current folder to the workspace window

Opens the folder browser window

Accessory filter - hides SOPs that do not match the connected dispersion unit

Switches the view between icons or detail view

Name of the playlist and the target dispersion unit

Create a new playlist

Opens a saved playlist

Saves the active playlist.

In the above example:

 The SOP at the top of the playlist (Hydro LV - SOP 1) is used to initialize the

Mastersizer system and request sample details.

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Chapter 4 Making measurements

 The final SOP in the list (Hydro LV - SOP 3) is used to control the clean

sequence. The dispersion unit, measurement and analysis settings for each SOP in the list are applied in sequence when the playlist is run.

 SOP playlists can be opened and saved using the options at the top

of the SOP playlist. Playlist do not have to be saved before they are run, but a prompt will be displayed to ask if saving the playlist.

 Once the list is set up, the sequence can be run by clicking OK.

 The new playlist will be saved into the workspace window.

When the sequence is now playing, the current SOP name is reported in the window bar of the measurement manager:

Apart from the additional playlist bar, the measurement will run in a similar way to standard SOP measurements.

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Measurement settings reference

Note

SOPs and Manual Measurements involve specifying a number of settings before the measurement can be run. This section relates equally to both.

The Measurement settings window is displayed whenever you create a new SOP or manual measurement. This window groups settings into logical sections in which various parameters for the measurement are defined as follows:

 Sample – identify the sample and provide more information to users of the

SOP. Define the physical characteristics of the sample and dispersant.

 Measurement – set both the red and blue light measurement durations, the

number of, and delay duration between, measurements. Specify the obscura tion levels for the measurement.

 Sample Dispersion – control the behaviour of the currently connected acces-

sory.

 Data Processing – specify the scattering model, latex analysis options and

modify the light detectors used in a measurement. Define any Analysis Smoothing, Size Range/Resolution options and set size banding for all meas urement histograms and tables.

Note

When progressing through the settings, any icon next to a field indicates that the user must specify a value for the field before continuing to the next section.

The rest of this section goes through each of the measurement settings in more detail.

Sample - Identification

The Sample Identification settings section allows you to enter details that will both identify the sample and provide more information to users. When the measurement is run, the user is prompted to confirm or alter the fields specified here.

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Chapter 4 Making measurements

Section/option Description

Sample Name

(mandatory)

Adding a Field To add further fields for example, Notes, Batch, Lot, Group

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A descriptive name for the sample, such as "Batch 1A" or "Series 3, Sample 1". This is the only default sample identification field.

etc., click the Add button. The new field is added to the list. Enter a name for the field in the drop down menu to the left of the field. Check Required field if this is mandatory for the operator to enter.

To re-order the list of fields, drag the item up or down by

clicking and dragging the icon next to the item.

To remove unwanted identification fields, click the icon adjacent to the field.

Making measurements Chapter 4

Sample - Particle Type

The Particle Type settings allow you to specify the shape of particles under analysis in order for the software to apply the optimal analysis model.

Section/Option Description

Non-Spherical This analysis mode is applicable for particles which are irreg-

ular in shape, or have a rough surface structure. For example, it should be selected for milled or crushed materials. This mode uses Mie Theory, and therefore requires input of the optical properties of your sample in order to calculate a particle size distribution. The advantage of this is that it provides the possibility of obtaining accurate size distributions for all particle sizes.

Spherical This analysis mode is applicable for particles which are per-

fectly spherical in shape. For example, it should be selected for polymer latex samples or for emulsions.

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Chapter 4 Making measurements

Section/Option Description

Spherical 

(continued)

Opaque Particle (Fraunhofer Approximation)

This mode uses Mie Theory, and therefore requires input of the optical properties of your sample in order to calculate a particle size distribution.

The advantage of this is that it provides the possibility of obtaining accurate size distributions for all particle sizes.

The Fraunhofer Approximation can be used to calculate particle size distributions in cases where the particle size is large and where the particles can be assumed to be completely opaque. It is the easiest mode to use, as you do not have to provide any optical properties in order to calculate a size distribution. However, its use may lead to inaccurate results, particularly for small particles below 50 microns in size or for those which are transparent.

Sample - Material

Use the Material properties section to enter physical characteristics of the material being measured.

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To select a previously added material from the Materials Database, click Browse database, then select an item from the database and click Use these values. See

the Help system for more on the Materials and Dispersants databases. Alternatively, manually complete the fields detailed below.

Section/option Description

Material name Descriptive name for the material.

Refractive index Value of between 0 and 5. This value relates to the speed of

light within the material, which in turn allows the degree of refraction (light bending) to be predicted when light passes from one medium to another.

Absorption index Value between 0 and 10, which is a measure of the quantity

of light absorbed by the particles. Generally, transparent samples will have a low or zero absorption while coloured or black samples will have a higher value.

Density Value of between 0.001 and 25g/cm³.

Different bluelight properties

(Wet dispersion units only)

References and notes

If required, select the check box and add the Refractive index (blue-light) and Absorption index (blue-light). See Help System for more information.

Any further comments that help to describe the material.

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Chapter 4 Making measurements

Sample - Dispersant

This is a unique window for Wet dispersion SOPs.

Use the Sample Dispersant section settings to specify the properties of the dispersant used in the measurement.

It is possible to specify the dispersant details manually or to choose from the Dis-

persants Database. To select a previously added material from the Dispersants Database, click Browse database, then select an item from the database and click Use these values.

Alternatively, manually complete the sections detailed below.

Section/option Description

Dispersant name Descriptive name for the dispersants, for example, Ethanol.

Refractive index Value of between 0 and 5. This value relates to the speed of

light within the material, which in turn allows the degree of refraction (light bending) to be predicted when light passes from one medium to another.

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Section/option Description

level sensor threshold 

(Hydro MV only)

References and notes

A value can be inputted that is suitable for the level sensor to detect the dispersant level when filled. The value will be different depending upon the dispersant used.

The level sensor in the dispersion unit automatically stops the tank being overfilled above a certain level. If the tank fails to fill properly then the level sensor threshold, for the dispersant being used, may need adjusting. This value can be changed either manually (for the current measurement only) or by using the dispersants database, to store the new values for future use.

Configuring this threshold value will be done using the

accessory controls window; this is described in the Hydro series wet dispersion units guide.

Enter any further comments that help to describe the dispersant.

If the newly added dispersant will be used in the future, add it to the Dispersants Database by clicking Add to database.

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Sample - Instructions

Use the Sample Instructions settings to specify pre-measurement and postmeasurement instructions that need to be drawn to the attention of the user.

These are then shown in the Sample Documentation panel/window before and following the measurement respectively. In this example pre-measurement instructions have been specified and are displayed above the Sample Name field in the Sample Documentation window.

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Measurement - Duration

The Measurement Duration settings can be used to separately specify both the red and blue light measurement durations.

Section/option Description

Red measurement duration(s)

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Background measurement duration (seconds) This facility will make a measurement using only clean dispersant – this is then subtracted from the sample measurement by the system in order to ‘clean’ the data. This is often set to the same duration as the sample measurement.

Sample measurement duration (seconds)

The optimum measurement time depends on the size of the sample, its particle size distribution and the dispersion accessory used. If a material is monomodal its essential particle size characteristics can be captured in less time than a material with a broad particle size distribution, which will need to be measured longer to ensure that the coarser particles have been properly represented.

Chapter 4 Making measurements

Section/option Description

Blue measurement duration(s)

(Wet dispersion units only)

Blue light measurement is more effective when measuring particles under approximately 1μm in size. There is a gradual reduction in the effectiveness (and hence significance to the overall measurement result) of the use of blue light on samples containing particles above this size.

Some red and yellow samples (such as pigments) can absorb light in the blue spectrum. This may lead to problems with the validity of the data acquired during the blue light part of the measurement. If you have such a sample, the blue light measurement can be disabled, so limiting the measurement to the main red laser.

Either select Use the durations I specify, or If no blue light measurement is required, select Don't perform blue light measurement. This will speed up the measurement time.

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Measurement - Sequence

The Measurement Sequence settings window allows you to specify the number of measurements and the duration of any delay between measurements.

Section/option Description

Measurements If the material is difficult to disperse, requiring ultrasonica-

tion, surfactant or both to achieve a stable dispersion, several measurements of the same sample may be required in order to determine the ideal dispersion time. In general, repeat measurements are performed until the last measurement obtained agrees closely with the previous one.

Enter the Number of measurements (up to 999) and Delay between measurements (up to 9999 seconds). Specifying several measurements, e.g. 5, allows repeatability to be assessed.

In wet measurements a Pre-measurement delay (s) can be specified. This delay occurs before the very first measurement but after Ultrasound has been stopped, assuming the pre-measurement ultrasound option is selected.

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Measurement - Obscuration

The Measurement Obscuration settings enable you to specify the obscuration levels between which the measurement will be conducted. This is critical for ensuring the correct amount of sample is added to the measurement system.

The optimal obscuration settings for a measurement are both sample and dispersion unit dependent. As a rough guide, use a range of 10-20% for a wet dispersion unit and 1-10% for a dry dispersion unit.

Note

For more advice on obscuration settings see the Help.

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Section/option Description

Measurement obscuration limits

Enable measurement to autostart

Measurement obscuration filtering

Set the following parameters:

Obscuration lower limit (%) - Enter a percentage value from 0.1 to 50 above which the measurement should be run.

Obscuration higher limit (%) - Enter a percentage value from 0.1 to 50 below which the measurement should be run.

This information is subsequently indicated on the Laser pane of the measurement sequence:

If required, select Auto start measurement when obscura-

tion is in range. If selected, it is also necessary to set a Sta- bilisation time delay in seconds - this will then add a delay

before the measurement initiates after the obscuration level is first detected within the specified band.

Select the Enable filtering option to optionally set the software to only record data where the obscuration was within the specified range.

The Time out option forces the measurement to stop if no such data are recorded within the specified number of seconds.

Sample Dispersion - Accessory

The Accessory control settings allows you to set up the behaviour of the currently connected accessory. The options available on this Accessory control depend on the connected accessory. These are described in the dispersions units respective user manual.

 Hydro series wet dispersion units manual for the Hydro MV, LV, EV and

SM dispersion units

 Aero series dry dispersion units manual for the Aero dispersion units

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Chapter 4 Making measurements

Sample Dispersion - Cleaning

The Cleaning options allow you to specify both a clean sequence and whether to use ultrasound as part of the sequence. This ensures that all traces of the sample just measured are removed so that no contamination of the next sample occurs. Cleaning following a measurement is essential to ensure that background noise, consisting of particles agglomerating within the system and forming accumulations, is minimized.

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Section/option Description

Clean Sequence Each Clean type specifies a set number of cycles (nothing

further is changed in the cleaning method). Select a Clean type of either Quick, Normal, Extensive or Custom. If Cus-

tom is selected the user must also manually specify the number of Clean cycles.

If measuring the same sample type in succession a Quick clean may be sufficient.

Clean Sequence

(continued)

Tank fill  behaviour

(Hydro LV/MV only)

If making the last measurement of the session, it is prudent to perform an Extensive clean to ensure that the system is as free as possible from contamination in readiness for the next measurement session.

The tank can be filled with dispersant manually or automatically. When set to Automatic the dispersant is plumbed into the dispersant inlet port at the rear of the accessory and a solenoid valve controls the flow of dispersant into the tank.

However, if a solvent is to be used as a dispersant, it is unlikely that the solvent will be plumbed into the accessory. In these situations the filling of the tank can be set to Man- ual. Under manual filling the solenoid valve is switched off (this will mean that the dispersant inlet does not have to be disconnected during a manual fill) and the tank can be filled by hand.

The software will tell the operator when to fill the tank during an SOP measurement:

Filling the tank manually: Fill the tank slowly until the tank light flashes - this will indicate the correct fluid level for adding sample and running measurements. If the tank is filled higher than this, sample and particles may be lost via the over-flow system (drain), leading to an incorrect particle size distribution being reported.

Degassing

If dispersant is stored under pressure or at low temperature, consider de-gassing before use. The pressure release or temperature rise reduces the solubility of gases, resulting in possible bubble formation in the pipes and tank.

Select the Degas after fill check box to remove bubbles and dissolved gases from the dispersant before use. This pulses the ultrasonics for a period of time after the tank is filled.

Note: It is preferable that all dispersants are degassed before being added to the system. Degas by storing the dispersant at room temperature and pressure before use.

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Chapter 4 Making measurements

Section/option Description

Ultrasonication

(Wet dispersion units only)

Air pressure

(Dry dispersion units only)

Feed rate

(Dry dispersion units only)

Ultrasound can reduce agglomeration, which may help further with cleaning. Select whether to Use ultrasound during the clean sequence or No ultrasound during clean.

Use the slider bar to set the air pressure at which any remaining sample is removed (from 0-4 bar, in 0.1 bar increments).

Use the slider bar to set the rate at which the remaining sample is removed - effectively this controls the vibration speed of the feed tray.

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Data Processing - Analysis

The Analysis settings allow you to specify the scattering model, latex analysis options and modify the light detectors used in a measurement.

Tip

If you are unsure which analysis settings are best suited to your application, try reapplying different analysis settings to the measurement records. To do this, use the Edit Result feature after the first set of measurements has been made – see Viewing the measurement chapter for more information.

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Chapter 4 Making measurements

Analysis model

Section/option Description

Analysis Model standard

Analysis Model Mastersizer 2000/2000E emulator mode

General Purpose – this model is appropriate for most

samples, including naturally occurring and milled materials. You should select this model unless you know that your sample meets more specific requirements stated for the other analysis modes provided for the system.

Narrow Modes – this model is appropriate for sample consisting of one or more narrow modes, where each mode spans much less than a decade in size. It is not intended for use with broad distributions which exhibit more than one peak.

Verification Latex (Wet dispersion units only) – this model is designed to enable the analysis of one or more very narrow Latex size standards, such as those used during verification of the optical unit performance.

Note: For all of the analysis models – use the ‘Keep a single result mode’ option in the Advanced settings to force the analysis to only report the most significant mode present within the sample.

With the Enable Mastersizer 2000 / 2000E Analysis Emu-

lator options enabled (options menu ) 3 additional emulated Mastersizer 2000 / 2000E analysis models are added to the list.

The emulator converts a Mastersizer 3000/3000E results to how it would be analysed on a Mastersier 2000/2000E instruments, The extra analysis modes are:

General Purpose (Emulated MS2000 / MS2000E) – this model is appropriate for the majority of milled and naturally occurring samples.

Multiple modes (Emulated MS2000 / MS2000E) – this model is appropriate for sample consisting of one or more very narrow modes, such as polystyrene lattices.

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Section/option Description

Analysis Model Mastersizer 2000/2000E emulator mode

(continued)

Fine Powder Mode

(Dry dispersion units only)

Single mode (Emulated MS2000 / MS2000E) – this model is appropriate for sample consisting of one very narrow mode, such as polystyrene lattices.

This option should be enabled for samples containing a significant proportion of material below 10 microns in size. It can help improve the result reproducibility, and can be used with any of the Mastersizer 3000 analysis modes.

Advanced button

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Chapter 4 Making measurements

Click the Advanced button to reveal the following additional options:

Section/option Description

Analysis Modes Use Keep a single result mode if you know your sample

has a single mode size distribution. This option eliminates any small modes produced by noise on the measurement.

Disable Detectors

Red Light Only Remove Blue Light from Analysis allows a measurement

Sensitivity

(Wet dispersion units only)

Virtual lens range

Set the number of inner (low scatter-angle) detectors to be ignored by the analysis. Thermal fluctuations in the dispersant can cause signals in the inner channels to be interpreted as large particles. Set the number of detectors to remove the effect of these fluctuations, at the expense of reducing the sensitivity to the presence of genuinely large particles.

made with red and blue light to be analysed as if the blue light was not used. (wet only)

Enhanced sensitivity has maximum sensitivity to any small modes that are separated from the main particle mode; while Normal sensitivity (default) subtracts more of the background and reduces small extra modes.

Virtual lens ranges limit the result analysis range to that of a legacy instrument, such as a 300mm lens used on a Mastersizer X, and are used to help with method transfer from older Malvern laser diffraction systems:

Selecting each lens range will truncate both the detector range and the size range of the Mastersizer 3000 system to match the selected system.

Select this feature for use from the options menu

Mastersizer 3000E

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This option will force a Mastersizer 3000 measurement to be analysed as if it was made on a Mastersizer 3000E.

Selecting the Mastersizer 3000E analysis mode will override some of the other advanced settings. For example, the number of virtual lens ranges available will be reduced.

Making measurements Chapter 4

Data processing - Result

The results settings allow you to specify the displayed size range and the type of distribution that the analysis has used in the measurement.

Section/option Description

Result range Reducing the measurement range is not usually a recom-

mend option, especially when conform to good laboratory practice. This facility is useful though if a sample includes two or more distinct size populations which may need to be monitored individually.

Adjusting the low and high size range will alter the fit applied to the fundamental result, where the intermediate values are then read from the curve allowing interpolation of percentile points. This adjustment will not alter the analysis bands that are used in the measurement.

Mastersizer 3000 Page 4-45

Chapter 4 Making measurements

Result range

(continued)

Result type Set the result type for the particle size distribution - choices

Extend the result Result extension can be used to extend the Mastersizer

Note: The software will automatically flag the use of any

range reduction facility to preserve the integrity and traceability of the results.

are Volume distribution (recommended), Surface area dis- tribution or Number distribution. By default the Mastersizer measurement is fundamentally a measurement of the volume distribution - transforming the result into number distribution is a mathematical process that may amplify any error in the original result. Small volumes of small size particles may be transformed in to significant numbers of particles. Use the size range controls above to limit this effect.

result to sizes beyond 3500μm.

To enable a result extension, first click the Extend with an

External Result option. Then, click the Edit External Result… button to open the External result editor window.

To enter the size band data to add to the Mastersizer result; use the control icons at the top of this Editor window to add or remove size bands, as required.

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Malvern Mastersizer 3000 User Manual

Specifications and Main Features

Frequently Asked Questions

User Manual

Introduction

About this manual

Access to the instrument

Malvern Instruments personnel

Supervisor

Operator

Assumed information

Naming convention

Ribbon commands

Where to get help

Manuals

Help System

Technical support

Malvern website - www.malvern.com

Introducing the Mastersizer 3000

Introduction

Mastersizer 3000 and Mastersizer 3000E instruments

About the Mastersizer

Optical unit

Dispersion units overview

Measurement cell

Computer (Mastersizer application software)

Typical systems

Wet dispersion

Dry dispersion

Optical unit components

End panel

Cell components

Inserting and removing the cell

Software overview

Introduction

Powering on and starting the software

Software user interface

Control ribbons

Record View tab

Reports tab

Data quality tab

Workspaces

Customising the software interface

Options

Custom layouts (Save/restore layout)

Predefined Window Layouts

Quick access toolbar

Maintenance utilities

Making measurements

Introduction

Measurement types and process

Measurement prerequisites

Making SOP measurements

Creating or editing an SOP

Running an SOP (Hydro units)

Running an SOP (Aero units)

Making manual measurements

Manually controlling the dispersion units

Manual control accessories

SOP Player

Measurement settings reference

Sample - Identification

Sample - Particle Type

Sample - Material

Sample - Dispersant

Sample - Instructions

Measurement - Duration

Measurement - Sequence

Measurement - Obscuration

Sample Dispersion - Accessory

Sample Dispersion - Cleaning

Data Processing - Analysis

Data processing - Result