Malvern ZEN3600, ZEN2600, ZEN1500, ZEN2500, ZEN3500 User Manual
...
Zetasizer Nano Series
Zetasizer Nano Series
User Manual
User Manual
MAN0317 Issue 1.0 June 2003
© Malvern Instruments Ltd. 2003
Malvern Instruments makes every effort to ensure that this document is correct. However,
due to Malvern Instruments policy of continual product development we are unable to
guarantee the accuracy of this, or any other document after the date of publication. We
therefore disclaim all liability for any changes, errors or omissions after the date of
publication. No reproduction or transmission of any part of this publication is allowed
without the express written permission of Malvern Instruments Ltd.
Head office:
Malvern Instruments Ltd.
Enigma Business Park,
Grovewood Road,
Malvern,
Worcestershire. WR14 1XZ
United Kingdom.
Tel + [44] (0)1684-892456
Fax + [44] (0)1684-892789
Windows 2000 and XP are registered trademarks of the Microsoft Corporation.
Zetasizer, NIBS and M3-PALS are registered trademarks of Malvern instruments.
Printed in England
Table of Contents
Part 1 - Operators guide
CHAPTER 1 - Introduction to this manual
Introduction to this manual 1-1
How to use this manual 1-2
Access to the Instrument 1-3
Assumed information 1-4
Where to get help 1-4
CHAPTER 2 - What is the Zetasizer Nano?
Introduction 2-1
What does the Zetasizer Nano do? 2-1
The Zetasizer Nano range 2-1
What is Particle Size, Zeta potential and Molecular weight? 2-3
CONTENTS
CHAPTER 3 - How does the Zetasizer Nano work?
Introduction 3-1
How is a Zetasizer measurement performed? 3-1
What does the Zetasizer consist of ?
- Identifying the Hardware 3-4
- Navigating the Software 3-13
CHAPTER 4 - Making measurements - A tutorial
Introduction 4-1
Quick guide to making a measurement 4-2
Powering up the system 4-2
Sample preparation 4-3
Choosing the correct Cell 4-3
Filling the Cell 4-8
Inserting the Cell 4-11
Making an SOP measurement 4-14
Making a manual measurement 4-16
The Measurement display 4-17
Editing the result 4-23
Zetasizer Nano Series Page 1
CONTENTS
Zetasizer Nano Series
CHAPTER 5 - Records and Reports - Viewing the results
Introduction 5-1
Displaying the results 5-1
CHAPTER 6 - Sample Preparation
Introduction 6-1
Preparing the sample
- Size 6-1
- Molecular weight 6-5
- Zeta potential 6-6
CHAPTER 7 - Maintenance
Introduction 7-1
Cleaning the instrument 7-1
Cleaning the Cells 7-2
Replacing the system fuse 7-4
Part 2 - Supervisors guide
CHAPTER 8 - Security
Introduction 8-1
Initial start-up - set up the administrator 8-2
Enabling security 8-3
User groups 8-3
Users 8-5
CHAPTER 9 - Using SOPs
Introduction 9-1
Creating an SOP 9-2
All SOPs 9-4
Size SOPs 9-10
Molecular weight SOPs 9-18
Zeta potential SOPs 9-22
Trend & Protein melting point SOPs 9-27
Extracting an SOP 9-29
Modifying an SOP 9-29
Distributing an SOP 9-30
Page 2 MAN 0317
CONTENTS
CHAPTER 10 - Measurement file window - Workspace management
Introduction 10-1
Measurement file window 10-2
CHAPTER 11 - Exporting results
Introduction 11-1
Exporting results 11-1
Creating an export template 11-3
CHAPTER 12 - Creating custom reports
Introduction 12-1
Overview 12-1
Opening a report 12-2
Creating a report 12-2
Laying out a report 12-2
Customising and editing the report 12-4
A finished report 12-11
Viewing the new report 12-12
CHAPTER 13 - Size theory
Introduction 13-1
What is Dynamic Light Scattering? 13-1
Operation of the Zetasizer Nano
- Size measurements 13-6
CHAPTER 14 - Molecular Weight theory
Introduction 14-1
What is Static light scattering? 14-1
The Debye plot 14-4
CHAPTER 15 - Zeta Potential theory
Introduction 15-1
What is Zeta Potential? 15-1
Laser Doppler Velocimetry 15-5
The M3-PALS technique 15-7
Operation of the Zetasizer Nano
- Zeta potential measurements 15-11
Zetasizer Nano Series Page 3
CONTENTS
Zetasizer Nano Series
Part 3 - Appendices
APPENDIX A - Health and Safety
APPENDIX B - Specification
APPENDIX C - Site requirements
Introduction C-1
Environmental conditions C-1
Space required C-2
Power requirements C-3
Additional services C-3
Computer specification C-4
Laser Safety C-4
APPENDIX D - Unpacking instructions
APPENDIX E - Installation
Introduction E-1
Installing the Zetasizer Nano E-1
Changing the computer E-2
Installing the Titrator E-2
APPENDIX F - Regulatory Statements
CE Declaration of Conformity F-1
Federal Communications Commission (FCC) Notice F-2
Canadian Regulatory Information F-3
Page 4 MAN 0317
Part 1 - Operators guide
Part 1 - Operators guide
Introduction to this manual
Introduction to this manual
CHAPTER 1
Introduction to this manual
This manual covers the operation and maintenance of the Zetasizer Nano particle
analyser series.
CHAPTER 1
Zetasizer Nano
instrument
Nano S (Red badge) ZEN1600 Size measurement particle sizer
Nano S (Green badge) ZEN1500 Size measurement particle sizer
Nano Z (Red badge) ZEN2600 Zeta potential particle sizer
Nano Z (Green badge) ZEN2500 Zeta potential particle sizer
Nano ZS (Red badge) ZEN3600 Size and Zeta potential particle sizer
Nano ZS (Green badge) ZEN3500 Size and Zeta potential particle sizer
Nano S90 (Red badge) ZEN1690 Size measurement particle sizer - 90° optics
Nano S90 (Green badge) ZEN1590 Size measurement particle sizer - 90° optics
Nano ZS90 (Red badge) ZEN3690 Size and Zeta potential particle sizer - 90° optics
Nano ZS90 (Green badge) ZEN3590 Size and Zeta potential particle sizer - 90° optics
Instruments that have a red oval badge fitted to the instrument cover are fitted
with a 633nm ‘red’ laser; instruments that have a green badge are fitted with a
532nm ‘green’ laser.
Model
number
Description
Build options exist for each of the above instruments, these are described in
chapter 2.
Note.The Zetasizer model, Serial number, software and firmware version can
'
The aim of this manual is to:
.
.
be found by left-clicking the Nano icon in the right corner of the status
bar.
Identify what the instrument is.
Explain in simple terms how it works.
Zetasizer Nano Series Page 1.1
CHAPTER 1
How to use this manual
Zetasizer Nano Series
.
Explain how the instrument should be used to make a measurement.
.
Identify the user maintenance procedures.
It is important to read the Health and Safety information in appendix A before
operating the instrument.
It is recommended this manual is read fully before you start your first
measurement, though if more familiar with particle size analysers, jump straight
to chapter 4 - “Making measurements - A tutorial”. This chapter gives practical
details on making measurements.
The manual is divided into 3 sections.
Part 1 – Operators guide
Contains all the information required for the operator to use the Zetasizer Nano
instruments.
Topics covered are: What are the Zetasizer Nano instruments, what are the
components of the Zetasizer Nano and what do they do, instructions on using the
instrument and the software, basic measurement and maintenance procedures.
Part 2 – Supervisors guide
The Supervisors guide concentrates on the administration and creation of the
Zetasizer functionality. It provides a greater insight into the measurement
procedures and results expanding the analysis theories.
Topics covered are: security aspects, use of Standard Operating Procedures
(SOPs), and organising the measurement files, and discussion on each of the
analysis theories used – Zeta potential, Size and Molecular weight.
It is recommended that the supervisor should also read Part 1 – Operators guide
Part 3 - Appendices
Contains supplementary information not necessary for the general operation of
the system.
More detail on the Zetasizer software can be found by using the online Help
within the software.
Page 1.2 MAN 0317
The Zetasizer Nano measures three different particle characteristics; the text
within each chapter has therefore been structured to, detail the instrument
functions as applicable to all measurements types, or individually if the function
only applies to one, i.e. if concerned only with zeta potential measurements
ignore all references to size and molecular weight unless otherwise directed.
Access to the Instrument
Within this manual, reference is made to the various people who will have access
to the instrument.
Malvern personnel
Malvern 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!
#
CHAPTER 1
Removal of the covers by unauthorised personnel will invalidate the
warranty of the instrument.
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. They can perform all user maintenance routines identified in chapter 7.
Under no circumstances, should the supervisor 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 chapter 7, except changing the
fuse.
Under no circumstances, should the operator remove the main cover of the
instrument.
Zetasizer Nano Series Page 1.3
CHAPTER 1
Assumed information
Zetasizer Nano Series
Warning!
#
Failure to follow these guidelines could result in exposure to hazardous
voltages and laser radiation.
Naming convention
The Zetasizer Nano will either be referred to in full, as the Zetasizer, or as the
‘instrument’.
The combination of the Zetasizer Nano instrument, the computer and Zetasizer
software will be referred to as the "System".
Cells and Cuvettes
Any device for holding and measuring the sample in the instrument will generally
be referred to as a “cell”. This includes dip cells and all kinds of cuvettes used (i.e.
glass, small volume, disposable) unless a proper description is more appropriate.
Menu commands
Menu commands from the Zetasizer software are referred to in the form main
menu-menu item. As an example, the command Configure-New SOP refers
to selecting the New SOP item in the Configure menu. Menu commands are
always shown in bold text.
Where to get help
Manual and Help files
The primary source of help for the Zetasizer system is from this manual and the
online help system within the software. This manual is designed to give an
overview of the system as a whole, while the online help system is designed to
give detailed information on the Zetasizer software.
Page 1.4 MAN 0317
CHAPTER 1
Each dialogue within the Zetasizer software has a Help button that gives
information specific to that dialogue. A secondary type of help exists within the
dialogue; this is the Advice button and contains more sample related content.
Help desk
All queries regarding the system should initially be directed to the local Malvern
representative. Please quote the following information:
.
Model and serial number of the instrument (located on the rear panel and
the front of the cuvette holder).
.
The build option fitted: a smaller label attached alongside the model and
serial number labels identifies any options fitted.
.
The Zetasizer software version (select Help-About within the software).
Contact the United Kingdom help desk if the local Malvern representative is not
available. The direct line to the United Kingdom Helpdesk is +44 (0) 1684
891800. It should be noted that this help line is primarily English speaking.
Remote support
Malvern Instruments offers a remote support service, delivered by an Internet
connection. Benefits include fast and efficient fault diagnosis, reducing downtime
and costs.
On-line user training is also available, plus software updates. A direct Internet
connection LAN must be available to make use of this facility.
Zetasizer Nano Series Page 1.5
CHAPTER 1
Zetasizer Nano Series
Page 1.6 MAN 0317
What is the Zetasizer Nano?
What is the Zetasizer Nano?
CHAPTER 2
CHAPTER 2
Introduction
What is the Zetasizer Nano system and what is it supposed to do?
This chapter gives a brief overview of the Zetasizer Nano instrument range: what
the Zetasizer Nano does and simple explanations about the measurement
technique.
What does the Zetasizer Nano do?
The Zetasizer Nano range of instruments provides the ability to measure three
characteristics of particles or molecules in a liquid medium.
These three fundamental parameters are Particle size, Zeta potential and
Molecular weight. By using the unique technology within the Zetasizer system
these parameters can be measured over a wide range of concentrations. The
Zetasizer system also enables determination of the Protein melting point plus
the ability to perform Trend measurements.
The Zetasizer range features pre-aligned optics and programmable measurement
position plus the precise temperature control necessary for reproducible,
repeatable and accurate measurements. In addition facility is included for
measurements of other key parameters such as pH and concentration.
The Zetasizer range has been designed with simplicity in mind, so that a minimal
amount of user interaction is necessary to achieve excellent results. The use of
Standard Operating Procedures (SOPs) and features such as the Folded
capillary cell alleviate the need for constant attention.
The Zetasizer Nano range
There are ten instruments in the Zetasizer Nano particle analyser range: five
different models fitted with either a 633nm ‘red’ or 532nm ‘green’ laser. The
models and their measurement specifications are described in the table below,
with instrument options following.
Zetasizer Nano Series Page 2.1
CHAPTER 2
Zetasizer Nano Series
Zetasizer
Nano S – 3nm to 10µm –
Nano Z 0.6nm to 6µm – 1000 to 2x10
Nano ZS 0.6nm to 6µm 3nm to 10µm 1000 to 2x10
Nano S90 2nm to 3µm – –
Nano ZS90 2nm to 3µm 3nm to 10µm –
Size range
Size range for Zeta
potential
Size range for
Molecular weight
7
Daltons
7
Daltons
Instrument option
(see below)
>?@
>
>?@
>
>?@
Laser fitted
The Zetasizer Nano series is available with either a 633nm ‘red’ laser or a 532nm
‘green’ laser fitted. The laser fitted is identified by the colour of the oval badge on
the cover.
.
The 633nm laser is least suitable for blue samples.
.
The 532nm laser is least suitable for red samples.
90° optics
The instruments above with the suffix 90 indicate the optics have a 90° scattering
angle. These models have been included in the Zetasizer Nano instrument range
to provide continuity with other instruments with ‘classical’ 90° optics.
Instrument options
A range of accessories and options are also available for more advanced
measurement strategies.
Narrow band filter
>
This filter improves the signal for samples that fluoresce at the wavelength
of the laser fitted. If fitted an option label will be attached to the front of the
cuvette holder.
Page 2.2 MAN 0317
CHAPTER 2
Option label Option fitted
ZEN1003 Narrow band filter for all instrument options
Universal ‘Dip’ cell
?
Used to provide repeatable measurements of non-aqueous samples such as
solvents. Also suitable for measurements of valuable aqueous samples
where minimal sample quantity is important.
MPT2 Autotitrator
@
Used to perform sample, pH, conductivity and additive titrations.
What is Particle Size, Zeta potential and
Molecular weight?
This section will describe, “basically”, what Particle Size, Zeta potential and
Molecular weight are and why they are important. Greater detail on the
measurement techniques is given in the theory chapters (13, 14 and 15).
What is Size?
Particle size is the diameter of the sphere that diffuses at the same speed as the
particle being measured.
The Zetasizer system determines the size by first measuring the Brownian
motion of the particles in a sample using Dynamic Light Scattering (DLS) and
then interpreting a size from this using established theories - see chapter 13.
Brownian motion is defined as:
“The random movement of particles in a liquid due to the bombardment
by the molecules that surround them”.
The particles in a liquid move about randomly and their speed of movement is
used to determine the size of the particle.
It is known that small particles move quickly in a liquid and large particles move
slowly. This movement is carrying on all the time, so if we take two ‘pictures’ of
the sample separated by a short interval of time, say 100µS, we can see how much
the particle has moved and therefore work out how big it is.
If there has been a minimal movement and the particle positions are very similar,
then the particles in the sample will be large; similarly if there has been a large
Zetasizer Nano Series Page 2.3
CHAPTER 2
S
Zetasizer Nano Series
amount of movement and the particle positions are quite different, then the
particles in the sample are small.
Using this knowledge and the relationship between diffusion speed and size the
size can be determined.
mall particles moving quickly
1
Time
Large particles moving slowly
Time
10 100 1000
Size nm
1
10 100 1000
Size nm
The above is a very simplistic explanation. A more detailed explanation can be
found in chapter 13 - Size theory.
Why do we use it?
Toners and Liquid inks
Image quality, viscosity and the tendency to aggregate and clog ink delivery
nozzles are all influenced by particle size. Controlling the size of ink and toner
products has a direct effect on image properties, ink permanence and adhesion.
Pigments
Knowledge of Particle size is important in developing stable formulations of
pigments. Pigment colour and hue are highly related to particle size, this has
applications in determining a pigments properties.
ILL 6722
What is Molecular weight?
The molecular weight of a substance is the weight in atomic mass units (amu)of
all the atoms in one molecule of that substance. Mathematically the molecular
weight can be calculated from the molecular formula of the substance; it being
the sum of the atomic weights of all the atoms making up the molecule.
If we take as an example the molecular formula H
molecular weight.
Page 2.4 MAN 0317
O (water) we can work out the
2
CHAPTER 2
In each molecule of water there are two atoms of Hydrogen (H2) and one
atom of Oxygen (O).
Now the atomic weight of hydrogen is 1.008 amu and that of oxygen is
15.999.
Therefore the molecular weight of water is 18.015 i.e.(1.008 x 2)+15.999.
1.0081.008
+
15.999
1.0081.008
=
18.015
This is a calculation using a known molecular formula and applying the values
from the periodic table.
With the Zetasizer Nano series of instruments the molecular weight can now be
determined by use of Static Light Scattering (SLS) measurement techniques.
This technique will be more explained in chapter 14 - Molecular weight theory.
'
Note
.
Malvern uses Daltons to identify the molecular weight.
Why do we want to know it?
We need to know the molecular weight, so we can determine how many grams
there are in 1 mole of a substance. The mole being the chemistry standard term
for ‘1 molecular weight’, e.g. one mole of water is 18.015g).
In an application, knowing the molecular weight of polymer compounds will aid
in determining many of their physical characteristics such as density, flexibility
and strength.
ILL 6721
What is Zeta potential and Electrophoresis?
Most liquids contain Ions; these can be negatively and positively charged atoms
called Cations and Anions respectively. When a charged particle is suspended in
a liquid ions of an opposite charge will be attracted to the surface of the
suspended particle.
i.e. - a negatively charged sample attracts positive ions from the liquid and
conversly a positive charged sample attracts negative ions from the liquid.
Zetasizer Nano Series Page 2.5
CHAPTER 2
p
Zetasizer Nano Series
Ions close to the surface of the particle, will be strongly bound while ions that are
further away will be loosely bound forming what is called a Diffuse layer.
Within the diffuse layer there is a notional boundary and any ions within this
boundary will move with the particle when it moves in the liquid; but any ions
outside the boundary will stay where they are – this boundary is called the
Slipping plane.
Diffuse layer
+
+
+
+
-
Zeta
Ions loosely
attached
+
-
otential
Negatively charged particle
Ions strongly
bound to particle
-
+
+
Slipping plane
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
ILL 6747
A potential exists between the particle surface and the dispersing liquid which
varies according to the distance from the particle surface – this potential at the
slipping plane is called the Zeta potential.
Zeta potential is measured using a combination of the measurement
techniques: Electrophoresis and Laser Doppler Velocimetry, sometimes
called Laser Doppler Electrophoresis. This method measures how fast a
particle moves in a liquid when an electrical field is applied – i.e. its velocity.
Once we know the velocity of the particle and the electrical field applied we can,
by using two other known constants of the sample – viscosity and dielectric
constant, work out the zeta potential.
This technique will be further explained in chapter 15 - Zeta theory.
Why do we use it?
The zeta potential of the sample will determine whether the particles within a
liquid will tend to flocculate (stick together) or not.
Knowledge of zeta potential is therefore useful in many industries such as:
Ceramics:
A high zeta potential is required to ensure the ceramic particles are densely
packed. This gives added strength to the end product.
Page 2.6 MAN 0317
CHAPTER 2
Waste water treatment.
The flocculation state of waste water is altered by changes in pH, the addition of
chemical flocculants, such as charged polymers, and the presence of aluminium
chloride or other highly charged salts. Measurement of zeta potential in
combination with these parameters is fundamental in the development and
maintenance of optimized water treatment protocols.
Emulsions.
Zeta potential is used to study the chemistry involved in determining whether or
not an emulsion will remain stable in the environment where it will be used.
Zetasizer Nano Series Page 2.7
CHAPTER 2
Zetasizer Nano Series
Page 2.8 MAN 0317
How does the Zetasizer
How does the Zetasizer
Nano work?
Nano work?
CHAPTER 3
CHAPTER 3
Introduction
Previously we identified the instrument and described the various measurement
processes that can be performed. This chapter introduces the hardware and
software features, that the instrument incorporates.
The initial section, “How is a Zetasizer measurement performed?”, will briefly
describe what is involved in making a measurement; what the major components
of the system are and how the software performs the task. This is followed by two
sections identifying the major hardware components and the software used.
The complete measurement process for size, zeta potential and molecular weight
measurements will be described in later chapters.
How is a Zetasizer measurement
performed?
A typical system, shown above, comprises the Zetasizer instrument+and a
computer with the Zetasizer software installed,. A cell-is filled with the
sample and loaded into the cell area on the top of the instrument..
1 4 3 2
Zetasizer Nano Series Page 3.1
ILL6744
CHAPTER 3
Zetasizer Nano Series
The software is used to control the measurement of the sample, there are two
basic ways to make a measurement:
.
SOP measurements. A Standard Operating Procedure (SOP) is like a
template that pre-defines all the measurement settings. This ensures that
measurements made on the same type of sample are made in a consistent
way. SOPs are ideal if the same type of sample is regularly measured,
inputting the same parameters each time a measurement is made is tedious
and runs the risk of making errors.
SOPs can be created or modified as required.
To perform an SOP measurement, select Measure-Start SOP from the
menu bar and select an SOP to use. With an SOP chosen the
Measurement display will appear (below). The measurement will begin
by pressing the Start ($) button.
.
Manual Measurement. A manual measurement is where all the measure
ment parameters are set immediately before the measurement is performed.
This is ideal if measuring many different types of sample, or experimenting
with the measurement parameters.
To perform a manual measurement, select Measure-Manual from the
menu bar. A manual measurement dialogue window will appear where the
measurement settings can be chosen, and if required saved as an SOP.
Once chosen the measurement can begin by simply pressing the Start ($)
button on the Measurement display.
Page 3.2 MAN 0317
ILL 6601
-
Loading...