Malvern Instruments Mastersizer X User manual

QS Small Volume Sample
Dispersion Unit
QS Small Volume Sample
Dispersion Unit
MAN 0161 Issue1.1 April 1997

©Malvern Instruments Ltd. 1995, 1997
Malvern Instruments makes every effort to ensure that this document is correct. However, due to
Malvern Instruments policy of continual product development we are unable to guarantee the accuracy
of this, or any other document after the date of publication. We therefore disclaim all liability for any
changes, errors or omissions after the date of publication.
No reproduction or transmission of any part of this publication is allowed without the express written
permission of Malvern Instruments Ltd.
Head Office:
Malvern Instruments Ltd.
Spring Lane South,
Malvern.
Worcestershire.
WR14 1XZ U.K.
Tel + [44] (0) 1684-892456
Fax + [44] (0) 1684-892789
Printed in England

Contents
Chapter 1 - Introduction to this manual
Access to the Accessory 1.1
Malvern personnel 1.1
Supervisor 1.1
Operator 1.1
Systems covered by this manual 1.1
Assumed information 1.2
Windows terms 1.2
Menu Commands 1.2
Where to find information 1.3
Other reading 1.5
Chpater 2 - Health & safety
Introduction 2.1
Site requirements 2.1
Laser safety 2.2
General laser safety 2.2
Laser Warnings 2.2
Electrical safety warnings 2.3
Sample handling 2.3
Moving the Accessory 2.5
Repackaging the Accessory 2.5
Disposing of the Accessory 2.6
Chapter 3 - Installation
Introduction 3.1
Site requirements 3.1
CONTENTS
QS SMALL VOLUME SAMPLE DISPERSION UNIT Page i

Unpacking the Accessory 3.2
Checking the contents 3.3
Connecting up your Accessory 3.4
Mastersizer S and X 3.4
Mastersizer Micro and Microplus 3.6
Power up the Accessory 3.8
Installation check 3.9
Chapter 4 - Getting to know your Dispersion Unit
Introduction 4.1
Features of the Accessory 4.1
Controller Unit rear panel 4.3
The Malvern software 4.4
Qspec MS1 macro 4.4
Chapter 5 - How the Accessory works
Introduction 5.1
What does the Accessory do? 5.1
How does the Accessory do it? 5.1
Operating principle 5.1
How to make a measurement using the Accessory 5.2
Chapter 6 - Making a measurement using the Accessory
Introduction 6.1
System and Accessory preparation 6.1
Making a measurement 6.1
CONTENTS QS Small Volume Sample Dispersion Unit
Page ii MAN 0161

Chapter 7 - Creating and changing SOP’s
Creating a new SOP 7.1
Editing and deleting a SOP 7.5
Chapter 8 - Sample preparation
Introduction 8.1
Trapped air/bubbles 8.1
Using a slurry 8.2
The use of ultrasonics 8.2
Chapter 9 - Maintenance
Introduction 9.1
Replacing the sample tubing 9.1
Replacing the fuse 9.2
Cleaning the Accessory 9.2
Disassembly 9.3
Cleaning 9.4
‘O’ ring seals 9.4
Reassembly 9.4
Cleaning the cell windows 9.5
Appendix A - Specification
Introduction A.1
Appendix B - Chemical compatability
Introduction B.1
Components in contact with
sample and dispersant B.1
CONTENTS
QS SMALL VOLUME SAMPLE DISPERSION UNIT Page iii

Appendix C - Simple fault finding
Introduction C.1
Fault diagnosis and correction C.1
Appendix D - Installing the Qspec MS1 macro
Introduction D.1
Appendix E - Statement of EMC performance
Statement of EMC performance E.1
CONTENTS QS Small Volume Sample Dispersion Unit
Page iv MAN 0161

CHAPTER1
Introduction to this manual
Introduction to this manual

Access to the Accessory
Within this manual reference is made to the various people that will have access to
the Accessory. Below is a list of these people and their responsibility:
Malvern personnel
Malvern personnel (service engineers, representatives etc.) have full access
to the Accessory and are authorised to perform all service procedures that
may be required.
Supervisor
The supervisor is the person responsible for the management/safety of the
System and of its operation. The supervisor is responsible for the training
of the operators. The supervisor can perform all user maintenance routines
identified in chapter 9, including changing the fuses.
Operator
An operator is a person trained in the use of the system. The operator can
perform all user maintenance routines identified in chapter 9, except
changing the fuses.
Systems covered by this manual
This manual covers the installation, operation and maintenance for the QS Small
Volume Sample Dispersion Unit. This accessory is used in association with
various Mastersizer optical units.
Mastersizer is a generic name given to a family of systems. Each system within the
family uses the same principles of operation and only vary in operation in small
areas. For this reason the manual has been written to cover more than one
instrument.
CHAPTER 1
QS SMALL VOLUME SAMPLE DISPERSION UNIT Page 1.1

This manual covers the Accessory in association with the following Mastersizer
family members:
Instrument. Ref. Number.
Mastersizer X standard bench. MAM 5000
Mastersizer X long bench. MAM 5002
Mastersizer S standard bench. MAM 5004
Mastersizer S long bench. MAM 5005
Mastersizer Micro. MAF 5000
Mastersizer Microplus. MAF 5001
Assumed information
For clarity this manual will assume that you are using your Accessory in
association with a standard bench Mastersizer S. If there are any operational
procedures that differ when in use with another Mastersizer family member, the
alternative information will be given.
Within this manual the QS Small Volume Sample Dispersion Unit will be
referred to as the “Small Volume Sample Dispersion Unit”, or as the “Accessory”.
Throughout this manual the Small Volume Sample Dispersion Unit refers to the
Dispersion Unit & the Controller Unit.
Within this manual the Mastersizer system will be referred to as the “Mastersizer”
or the “system” unless the information given is for a particular instrument.
Windows terms
It is important that you understand some windows terms before reading further.
Refer to chapter 1 of the Getting Started manual.
Menu Commands
Menu commands from the Malvern software are referred to in the form main
menu-menu item. As an example, the command Setup-Hardware refers to
selecting the Hardware item in the Setup menu. The same rules apply for
sub-menus of sub-menus. Menu commands are always shown in bold text.
CHAPTER 1 QS Small Volume Sample Dispersion Unit
Page 1.2 MAN 0161

Where to find information
As stated above, this manual is designed to give a brief overview of what the
Accessory can do and how it is used in association with the system. In other
words it is a quick guide that allows you to understand how the Accessory
operates and runs you through how the Accessory is used when making a
measurement, hopefully steering you around the main pitfalls and directing you
to more information if needed.
The following is a list of the contents and objectives of the chapters within this
manual.
Chapter 2 - Health and Safety
This chapter covers health and safety guidelines that should ensure the safe
installation, operation and maintenance of the Accessory. You should read this
chapter in conjunction with the Health and Safety manual for your Mastersizer
system.
You are provided with information on:
.Laser safety.
.Electrical safety.
.Sample handling.
.Moving the Accessory.
.Disposing of the Accessory.
Chapter 3 - Installation
This chapter provides you with all information required to install the Accessory
and includes information on:
.Positioning the Accessory.
.Unpacking the Accessory.
.Checking the contents.
.Connecting the Accessory.
.Powering up the Accessory.
Chapter 4 - Getting to know your Accessory
This chapter is designed to enable you to identify the physical features of the
Accessory and is divided into two parts.
CHAPTER 1
QS SMALL VOLUME SAMPLE DISPERSION UNIT Page 1.3

The first part identifies the features of the Accessory, for example the function
controls, connectors and indicators etc. The second part identifies the areas of the
Malvern software, which are pertinent to the Accessory.
Chapter 5 - How the Accessory works
After reading this chapter you will have a basic understanding of the operating
procedures of the Accessory and in particular:
.Know the basic operating principle.
.Know the simple steps involved in using the Accessory when making a
measurement.
Chapter 6 - Making a measurement using the Accessory
This chapter will guide you through the practical steps involved when making a
measurement using the Accessory. Reference is made to the Getting Started
manual which provides detailed information regarding the system.
Chapter 7 - Creating & changing SOP’s
This chapter will give details on how you can create and maintain your own
Standard Operating Procedures.
Chapter 8 - Sample preparation
This chapter, in conjunction with chapter 9 of the Getting Started manual,
provides you with information on one of the most important stages in making a
measurement. It provides you with specific sample preparation requirements
pertinent to the Accessory.
Chapter 9 - Maintenance
This chapter provides information on certain maintenance routines that can be
carried out by the user. These include cleaning the Accessory, changing the fuses
etc. After reading the “Access to the Accessory” section earlier in this chapter, you
should now be aware of what the Supervisor and the Operator are allowed to do.
Appendices
At the rear of the manual is a series of appendices that cover some of the technical
aspects of the Accessory, including the technical specification.
CHAPTER 1 QS Small Volume Sample Dispersion Unit
Page 1.4 MAN 0161

Other reading
More detail on the subjects within this manual can be found in the following
manuals:
Title Ref. Number
Getting Started system manual (Mastersizer S and X). MAN 0101
Getting Started system manual (Mastersizer Micro and Microplus). MAN 0106
The Malvern Software reference manual. MAN 0102
The Malvern BASIC reference manual. MAN 0103
Health and Safety (Mastersizer S and X). MAN 0104
Health and Safety (Mastersizer Micro and Microplus). MAN 0107
Installation Guide (Mastersizer S and X). MAN 0100
Installation Guide (Mastersizer Micro and Microplus). MAN 0105
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QS SMALL VOLUME SAMPLE DISPERSION UNIT Page 1.5

CHAPTER 1 QS Small Volume Sample Dispersion Unit
Page 1.6 MAN 0161

CHAPTER2
Health and safety
Health and safety

Introduction
This chapter covers health and safety guidelines that should ensure the safe
installation, operation and maintenance of the Accessory. You should read this
chapter in conjunction with the Health and Safety manual for your system.
#
Warning
Site requirements
The Mastersizer and its accessories have specific site requirements that must be
enforced to ensure the safe operation of the instrument. Information on site
requirements can be found in section A of the Mastersizer Installation Guide for
your system.
For information on the space required by your Accessory, refer to chapter 3 of
this manual.
#
Warning
Failure to follow these guidelines, particularly when making a measurement,
could result in the emission of laser radiation. Laser radiation can be harmful to
the body and can cause permanent eye damage.
If the System and Accessory is used in an environment not conforming to the site
requirements, safety may be compromised.
CHAPTER 2
QS SMALL VOLUME SAMPLE DISPERSION UNIT Page 2.1

Laser safety
It should be noted that the Accessory does not contain a laser, but is connected to
the Mastersizer optical unit that does. The information given below is general
advice that refers to the Mastersizer system as a whole.
#
Warning
General laser safety
The following general laser safety guidelines should be followed at all times
.Never look into the direct path of a laser beam or its reflections.
.Never look into the expected path of a laser beam without ensuring by posi-
tive means that the laser cannot be excited.
.While carrying out any operations in which the laser can be exposed, wear
protective goggles, ensuring that they are suitable for the power output and
wavelength of the laser in use and avoid, even when wearing such goggles,
direct viewing along the paths of the laser beam.
.Only authorised personnel should be allowed to enter the area where serv-
icing of the instrument is taking place.
.Avoid traversing the laser beam with any reflective object.
.Warning signs of the presence or potential presence of laser radiation
should be posted at the entrance to the hazard area.
Laser Warnings
For specific laser warnings pertinent to your Mastersizer system, refer to the
Health and Safety manual.
Laser radiation can be harmful to the body and can cause permanent eye
damage. Read this section of the manual carefully before installing or operating
the equipment.
CHAPTER 2 QS Small Volume Sample Dispersion Unit
Page 2.2 MAN 0161

Electrical safety warnings
The Accessory is mains powered and input power cables should be treated
accordingly.
The metal parts of the instrument are earthed via the protective earth connection.
Never run the equipment without a protective earth connection.
Exert care when measuring samples to avoid liquid or powder spillages over the
Controller Unit. Conducting materials or liquids can break down insulation and
cause dangerous conditions within the Accessory. Should such spillages occur,
disconnect the power and scrupulously clean up before re-applying power to the
Accessory.
'Note
.
The operator should under no circumstances remove the covers of the
Controller Unit. If it is suspected that liquid or powder has entered the
Controller Unit call your Malvern representative to arrange for a service
call.
Opening the covers of the Controller Unit will render its calibration
void.
Sample handling
#
Warning
Always handle all substances in accordance with the COSHH regulations (UK)
or any local regulations concerning sample handling safety.
Use the Accessory in a well ventilated room if noxious samples or dispersants are
to be analysed.
Highly flammable and volatile solvents such as Methanol, Ethanol, Acetone and
Benzene may be used in the Dispersion Unit with care. It should, however, be
noted that the Dispersion Unit contains a brushed DC motor which is not vapor
protected.
Always consult the Materials Safety Data Sheets of all samples that are to be
measured.
CHAPTER 2
QS SMALL VOLUME SAMPLE DISPERSION UNIT Page 2.3

Wear a protective respiratory mask if noxious samples or dispersants are being
handled, particularly in their dry state during sample preparation or measurement.
Do not smoke during measurement procedures, particularly where inflammable
samples or dispersants are used or stored.
Do not eat or drink during measurement procedures, particularly where
poisonous samples or dispersants are used or stored.
Wear protective gloves when handling hazardous materials, or those that cause
skin infections or irritations.
Take care when handling glass (e.g. beakers). Hazardous materials may enter a
wound caused by broken glass.
Use of the Accessory involves the use of a flow cell. Always replace tubing and
“O” rings with items of an equivalent or better specification in order to retain
chemical compatibility, see Appendix B.
Always test a new sample or dispersant for chemical compatibility before use.
Appendix B of this manual provides a list of the material in contact with the
sample and dispersant.
After measuring hazardous samples or dispersants, scrupulously clean the system
(including Dispersion Unit) to remove any contaminants before making another
measurement.
Always label samples for analysis using industry standard labeling, particularly if
they are handled by a number of staff or stored for long periods. Clearly mark any
operator hazard and associated safety precautions that are required for the
handling of dangerous materials. It is important to keep a record of all hazardous
substances used in the instrument for protection of service and maintenance
personnel.
Always adopt responsible procedures for the disposal of waste dispersant and
sample mixtures. Many chemicals are forbidden by law to be disposed of in such a
manner as to allow their entry into the water system. The user is advised to seek
local advice as to the means available for disposal of chemical wastes in the area of
use. Recommendations can be found within the Materials Safety Data Sheets.
The surfaces of the Mastersizer system and Accessory may be permanently
damaged if samples or dispersants are spilt onto them. If spillages should occur
then the system should be disconnected from the power supply before
scrupulously cleaning up the spillage.
CHAPTER 2 QS Small Volume Sample Dispersion Unit
Page 2.4 MAN 0161