MAN0494-1 (Zetasizer APS Basic Guide).book Page i Friday, August 9, 2013 2:08 PM
Zetasizer APS
Basic Guide
MAN0494 Issue 1.0 July 2013
English
MAN0494-1 (Zetasizer APS Basic Guide).book Page ii Friday, August 9, 2013 2:08 PM
Copyright © 2008, 2013 Malvern Instruments Ltd.
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
Zetasizer, 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.
MAN0494-1 (Zetasizer APS Basic Guide).book Page i Friday, August 9, 2013 2:08 PM
Table of contents
Introduction to this manual
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1
Using this manual. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1
Access to the instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-2
Where to get help. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-2
Site requirements
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
Environmental conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
Space required. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-2
Power requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Computer specification. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-4
Additional services . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-4
Laser safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
Health and safety
General warnings and Safety regulations . . . . . . . . . . . . . . . . . . . . 3-1
Electrical warnings and Safety regulations . . . . . . . . . . . . . . . . . . . 3-2
PAT testing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2
Power cords and Power safety . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2
Laser safety regulations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-4
Temperature warnings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-5
Sample handling warnings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6
Moving the system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-7
Disposal of the instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-8
Making a measurement
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1
Switching on & starting the software . . . . . . . . . . . . . . . . . . . . . . . 4-1
Making a measurement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-2
Viewing the results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-7
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Table of Contents Zetasizer APS Basic Guide
Maintenance
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1
Transit locks. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1
Cleaning the instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3
Replacing the system fuse . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-8
Replacing the tubing and needle . . . . . . . . . . . . . . . . . . . . . . . . . . 5-8
Installing the Zetasizer APS. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-19
Changing the computer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-21
Appendix
Specification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-1
Chemical compatibility . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-2
Disposal of Electrical & Electronic Equipment . . . . . . . . . . . . . . . . . A-3
Regulatory statements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-4
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Introduction
to this manual
Introduction
This manual covers the operation and maintenance of the Zetasizer APS particle
analyser.
Zetasizer
instrument
Zetasizer APS APS2000 Particle size
Zetasizer APS +
PTC-1000
Note
For the Zetasizer serial number double-click the APS icon in the status
bar.
Model
number Measurement types
APS5000 Particle size
Using this manual
Read the Health and Safety information in Chapter 3 before using the instrument.
For more detail on the Zetasizer software, use its Help system. Each window has a
Help button giving information about it. Advice buttons present sample-related
content.
Menu commands
Software menu commands are referred to in the form main menu-menu item.
As an example, the command Measure-Plate Scheduler refers to selecting the
Plate Scheduler item from the Measure menu. Menu commands are shown in
bold text.
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Chapter 1 Introduction to this manual
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 main covers.
Warning!
Removal of the main covers by unauthorized personnel, even a supervisor,
will invalidate the warranty of the instrument. It is however permissible to
lift off the front cover, which provides internal access to the user-serviceable tubes and needle. Refer to Chapter 5 for more information on this.
Supervisor
The supervisor is responsible for the management and safety of the instrument and
its operation. The supervisor also trains the operators. They can perform all user
maintenance routines identified in Chapter 5.
The supervisor has access to a more detailed manual in English.
Operator
An operator is a person trained in the use of the system. The operator can perform
all user maintenance routines identified in Chapter 5, except changing the fuse.
Warning!
Failure to follow these guidelines could result in exposure to hazardous
voltages and laser radiation.
Where to get help
Help desk
Direct all queries regarding the system to the local Malvern representative initially.
Please quote the following information:
Model and serial number of the instrument (located on the rear panel).
The Zetasizer software version (select Help-About within the software).
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Introduction to this manual Chapter 1
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.
This help line is primarily English speaking.
Remote support
Malvern Instruments offers a remote support service over the Internet. (A direct
Internet connection must be available.)
Benefits include fast and efficient fault diagnosis, reducing downtime and costs.
Online user training is also available, plus software updates.
Malvern website - www.malvern.com
The Malvern website offers a comprehensive range of particle characterization
resources for use by customers 24 hours a day, seven days a week.
Resources include software downloads, frequently asked questions, a knowledge
base and Application Notes, plus information on other particle characterization
solutions that Malvern can provide.
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Chapter 1 Introduction to this manual
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Site requirements
Introduction
This document outlines site requirements for a Zetasizer APS. Ensure all these are
met before the instrument is delivered.
Environmental conditions
The site must be:
Indoors and away from strong light (windows).
Away from heat sources like radiators.
Well ventilated (for noxious materials).
On a horizontal vibration-free bench.
We recommend that the computer is positioned to the right of the instrument.
Zetasizer APS Basic Guide Page 2-1
2
800mm
500mm
100mm
150mm
200mm
200mm
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Chapter 2 Site requirements
Space required
Provide enough space to allow easy access to all components and connections. This
diagram shows the recommended space for a system. Always place the (optional)
PTC-1000 to the left of the instrument as the heat output is from the left side of
the PTC-1000 and this will prevent hot air being directed towards the APS.
Allow at least 800mm above the bench surface for access to the plate holder area.
The system dimensions are given below:
Component Width Depth Height
Zetasizer APS 500mm 410mm 420mm
PTC-1000 195mm 351mm 304mm
Computer Refer to manufacturer’s literature.
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Site requirements Chapter 2
Power requirements
The mains power supply must be clean and filtered. If necessary, fit an Un-interruptible Power Supply (UPS) to remove any spikes or noise. The power requirements are:
Component Power requirement Power sockets required
Zetasizer APS 90-260V AC, 50-60Hz,
150W
PTC-1000 115-230V AC, 50-60Hz,
294W
Computer See manufacturer’s documentation
Computer monitor See manufacturer’s documentation
Printer See manufacturer’s documentation
1
1
Power cords and Power safety
The notes in this section indicate best practice. Adhere to these when connecting
the instrument to the power supply.
Warning!
Do not operate this product with a damaged power cord set. If the power
cord set is damaged in any way, replace it immediately.
Warning!
Do not use the power cord supplied with this product on any other
products.
Power cord set requirements
Power cord sets must meet the requirements of the country where the product is
used. For more information, contact a Malvern representative.
General requirements
The following requirements apply to all countries:
The power cord must be approved by an acceptable accredited agency respon-
sible for evaluation in the country where the power cord set will be installed.
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Chapter 2 Site requirements
The power cord set must have a minimum current capacity of 10A (7A in Japan
only) and a nominal voltage rating of 125 or 250 volts AC, as required by each
country's power system.
The area of the wire must be a minimum of 0.75mm
length of the cord must be less than 3m.
The power cord must be routed so it will not be walked on, pinched by items
placed on or against it, or become wet. Pay particular attention to the plug, the
electrical outlet and the point where the cord exits the product.
Computer specification
As with any software, running other applications at the same time may affect the
speed of the Zetasizer software.
Minimum recommended specification
Contact the Malvern Helpdesk or website for the recommended computer specification, otherwise consult the Software update notification document supplied on
the software CD.
Note:
A laptop computer must have a free USB port to operate with the system.
2
or 18AWG, and the
Networks
The PC running the Zetasizer software can be connected to a network, but the
Zetasizer software must be run locally.
Additional services
Purge specification
If measuring samples at low temperatures there is a risk of condensation occurring
on the cell; this occurs when the measurement temperature is less than the ‘dew
point’ of the ambient air surrounding the cell being measured. This is particularly
likely in humid climates.
If this may be a problem the purge inlet port can be used to connect a dry air supply
i.e. a supply with a dew point below the target temperature. This removes any
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Site requirements Chapter 2
moisture in the air immediately surrounding the cell and prevents condensation. If
using the purge inlet connector, the air or Nitrogen supply must conform to the
following specification:
Compressed air to DIN 8573-1
Oil = Class 1
Water = Class 3
Particulate = Class 3
Pressure = 100 kPa
Caution!
The purge air line supply must conform to the above specification. Failure
to meet this specification may result in permanent damage to the instrument and invalidate the warranty.
Telephone socket specification
The telephone socket for remote support needs a direct Internet connection.
Laser safety
Zetasizer APS instruments are Class 1 laser products and as such, require no special
laser safety considerations during normal operation. However, during servicing
(which must be performed by a qualified Malvern representative), the servicing
engineer may be exposed to class 3b or above laser radiation. We therefore recommend that the administrative controls recommendations of the Laser Safety Regulations (IEC 60825-1(1993) +A1(1997)+A2(2001) are implemented.
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Chapter 2 Site requirements
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Health and safety
General warnings and Safety regulations
Warning!
The instrument or samples to be measured may be hazardous if misused.
Read and fully understand this section before operating the system.
Warning!
Use of the system in a manner not specified by Malvern Instruments Ltd
may impair the protection provided by the system.
The instrument must only be stored or operated in environmental conditions conforming to Chapter 2.
Positioning the Instrument
Warning!
Do not position the instrument such that the power cord, where it exits the
product, is unreachable for disconnection.
Zetasizer APS Basic Guide Page 3-1
Warning!
Do not obstruct the ventilation slots underneath the instrument, nor the
fans on the rear panel. Restricting airflow can damage the instrument or
cause overheating.
3
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Chapter 3 Health and safety
Electrical warnings and Safety
regulations
Warning!
The Zetasizer APS contains high voltage components. Only Malvern
trained personnel are permitted to remove its main cover.
The instrument is mains powered and all power cables and electrical sockets should
be treated accordingly. Do not place cables where they may become wet.
Should the instrument become wet (e.g. sample or dispersant is spilt), switch it off
and disconnect it from the mains power supply immediately. Scrupulously clean
and dry the instrument before re-applying power.
Warning!
This product must be connected to a protective earth.
The metal parts of the optical unit and the accessories are earthed via a
protective earth connection.
PAT testing
If PAT testing is required, connect the earth lead to the earth stud underneath the
rear right-hand corner of the instrument. We recommend that the product is PAT
tested annually, or if it is suspected that its electrical safety has been compromised.
Power cords and Power safety
The notes in this section indicate best practice. Follow these when connecting the
instrument to the power supply.
Warning!
Do not operate this product with a damaged power cord set. Replace a
damaged power cord set immediately.
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Health and safety Chapter 3
Warning!
Do not use the supplied power cord on any other products.
Power cord set requirements
Power cord sets must meet the requirements of the country where the product is
used. For further information on the requirements, contact a Malvern
representative.
General requirements
These requirements apply to all countries:
The power cord must be approved by an acceptable accredited agency respon-
sible for evaluation in the country where the power cord set will be installed.
The power cord set must have a minimum current capacity of 10A (7A in Japan
only) and a nominal voltage rating of 125 or 250 volts AC, as required by each
country's power system.
The area of the wire must be a minimum of 0.75mm
2
or 18AWG, and the
length of the cord must be less than 3m.
The power cord must be routed so it will not be walked on, pinched by items
placed on or against it, or become wet. Pay particular attention to the plug, the
electrical outlet, and the point where the cord exits the product.
Power safety information
The following notes are guidelines for connecting the Malvern Instruments power
supply using single and multiple extension leads, connection via AC Adapters and
use of Uninterruptible Power Supplies (UPS).
Warning!
To prevent electric shock, plug the instrument or accessory into correctly
earthed electrical outlets.
The power cord supplied is equipped with a grounding connection to
ensure grounding integrity is maintained.
Advice on use of Extension leads
Follow this advice when using single or multiple socket extension leads. These
are also called ‘trailing sockets’.
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Chapter 3 Health and safety
Ensure the lead is connected to a wall power outlet and not to another
extension lead. The extension lead must be designed for grounding plugs and
plugged into a grounded wall outlet.
Ensure that the total ampere rating of the products being plugged into the
extension lead does not exceed the ampere rating of the extension lead.
Use caution when plugging a power cord into a multiple socket extension
lead. Some extension leads may allow a plug to be inserted incorrectly.
Incorrect insertion of the power plug could result in permanent damage to the
instrument or accessory, as well as risk of electric shock and/or fire. Ensure that
the ground connection (prong/pin) of the power cord plug is inserted into the
mating ground contact of the extension lead
Advice on use of AC adapters (when used)
Warning!
Do not use adapter plugs that bypass the grounding feature, or remove the
grounding feature from the plug or adapter.
Place the AC adapter in a ventilated area, such as a desk top or on the floor.
The AC adapter may become hot during normal operation. Take care when
handling the adapter during or immediately after operation.
Use only the Malvern-provided AC adapter approved for use with the instru-
ment and/or accessory. Using another AC adapter may cause a fire or explosion.
Advice on use of Uninterruptible Power Supplies (UPS)
To help protect the instrument and/or accessory from sudden, transient
increases/decreases in electrical power, use a surge suppressor, line conditioner
or UPS.
Laser safety regulations
The Zetasizer APS is a Class 1 laser product. As such, there is no exposure to laser
radiation in normal operation of the instrument. The standard laser has a maximum cw-power of 60mW at 830nm (invisible, near infrared).
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Health and safety Chapter 3
Caution!
The use of controls or adjustments or performance of procedures other
than those specified in this document may result in hazardous exposure to
laser radiation.
This diagram shows the location of the laser warning labels
:
Temperature warnings
Zetasizer APS Basic Guide Page 3-5
ill 8768
Warning!
The temperature range of the measurement area is 2°C to 90°C. The
optional PTC-1000 Plate Temperature Control unit can control the plate
holder in the range 2°C to 40°C.
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Chapter 3 Health and safety
Sample handling warnings
Always handle all substances in accordance with the COSHH (Control Of
Substances Hazardous to Health) regulations (UK) or any local regula-
tions concerning sample handling safety.
Before using any substance, check the Material Safety Data Sheets for safe
handling information.
Use the instrument in a well ventilated room, or preferably a fume cupboard, if
fumes from the sample or dispersant are toxic or noxious.
Wear personal protective equipment as recommended by the Material Safety
Data Sheets if toxic or hazardous samples are being handled, particularly dur-
ing sample preparation and measurement.
Wear protective gloves when handling hazardous materials, or those that cause
skin infections or irritations.
Do not smoke during measurement procedures, particularly where inflamma-
ble samples are used or stored.
Do not eat or drink during measurement procedures, particularly where haz-
ardous samples are used or stored.
Take care when handling glass (e.g. beakers). Hazardous materials may enter a
wound caused by broken glass.
Always test a new sample or solvent for chemical compatibility before use.
After measuring hazardous samples, scrupulously clean the system to remove
any contaminants before making another measurement.
Always label samples for analysis using industry standard labelling, 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 system
for protection of service and maintenance personnel.
Always adopt responsible procedures for the disposal of waste samples. Most
local laws forbid the disposal of many chemicals 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. For recommendations see the Materials Safety Data Sheets.
The surfaces of the system may be permanently damaged if samples are spilt
onto them. If a spillage occurs, disconnect the system from the power supply
before scrupulously cleaning it up.
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Health and safety Chapter 3
Moving the system
If it is necessary to move the system, follow these guidelines:
Always disconnect the computer and power supply before attempting to move
the system.
Always adopt proper lifting techniques to avoid back injury.
Always lift the instrument by holding the under its base. Never lift an instru-
ment by its covers. Refer to the Unpacking instructions provided.
If the system is moved large distances, we recommend that it is repacked in its
original packaging.
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Chapter 3 Health and safety
Disposal of the instrument
Dispose of the system responsibly. Follow these guidelines:
Disable the laser in such a way as to make it impossible for it to be powered up.
Ask the local Malvern representative for advice.
Decontaminate the instrument if hazardous materials have been used in the
system.
Refer to any local regulations on disposal of equipment.
European Union and other European countries
This regulation applies in the European Union and other European countries with
separate collection systems.
Here the system must be disposed of in accordance with the European Disposal of
Electrical & Electronic Equipment regulations.
This symbol on the product or on its packaging indicates that when the last user
wishes to discard this product it must not be treated as general waste. Instead it
shall be handed over to the appropriate facility for the recovery and recycling of
electrical and electronic equipment.
By not discarding this product along with other household-type waste, the volume
of waste sent to incinerators or landfills will be reduced and natural resources will
be conserved.
ill 7610
For more detailed information about recycling of this product, please contact the
local city office, a waste disposal service, or the Malvern representative.
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Making a
measurement
Introduction
This chapter provides a quick overview of how to get started with making measurements, and covers the following:
Switching on and starting the software
Making a measurement
Viewing the results
For more detailed information on how to make measurements, refer to the Zetasizer APS User Manual and software help system.
Switching on & starting the software
1. Turn on the instrument by pressing the power switch on the back of the
instrument.
2. Double-click the
icon on the
desktop.
3. If this dialogue
appears, it will
show your Windows login name.
Click OK.
4. The instrument
must be powered up for 30 minutes before a measurement is made to
ensure its temperature has stabilized
Zetasizer APS Basic Guide Page 4-1
4
Instrument connected correctly
Instrument not connected
(or malfunction)
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Chapter 4 Making a measurement
The icon in the lower right corner of the
Zetasizer software’s main screen is displayed as shown (right) if the instrument
has been connected correctly.
If the icon is greyed out, re-check all connections, ensure that the power supply to
the instrument is turned on and that the
power switch on the instrument is in the
On position. Then close and re-start the
software. If the icon is still greyed out,
contact Malvern Instruments.
Making a measurement
This section provides simple overview information on how to fill and insert a plate,
and then run a measurement by using a plate schedule and an SOP.
1. Load a plate with sample:
Prepare a sample, for example 60nm latex or BSA 2-3 mg/ml. Fill the wells with a
minimum sample volume of 20μL for a 384 well plate and 50μL for a 96
well plate.
Caution!
Do not overfill the wells - this could lead to cross-contamination or spillage.
2. Create a new measurement file:
It is necessary to create a new measurement file into which measurement data can
be saved. To do this, choose File-New from the menu and type a name for the new
measurement file - in this example the file has been named “Test 2.dts” (measurement files all use the “.dts” file extension).
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Making a measurement Chapter 4
3. Start the Plate Scheduler:
Once the instrument is set up, measurements are made by creating a plate schedule
that identifies which wells to measure with which SOP. Malvern Instruments supplies a number of default SOPs, but you can also create your own.
Select Measure-Plate Scheduler from the menu bar. The Plate Scheduler is
displayed:
.
4. Set up the Schedule Settings:
1. Click the Schedule Settings button on the lower toolbar to display the
Schedule Settings window:
2. Enter any identifying text, such as barcode or plate label etc. in the Plate ID
field. This information is then visible in the Records View as long as Plate ID
has been enabled as a parameter for that view (listed under the Measurement–
Details section).
3. Click OK when the Schedule Settings have been completed.
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Chapter 4 Making a measurement
5. Create plate schedule - allocate SOPs to wells:
1. Click the Add existing SOPs button and then select the “Typical Protein -
general purpose.sop” from the Protein folder.
2. Select the well(s) containing the sample by clicking on them. A red outline
shows that the well is selected.
3. Click on the name of the SOP in the left panel to allocate that SOP to the
selected well(s). The well(s) will change colour to that of the SOP.
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Making a measurement Chapter 4
6. Load the plate into the instrument:
1. If the plate holder is not in the ejected position, click Eject on the
toolbar.
2. Load the plate into the plate holder using the illustration for reference.
ill 8334
3. Ensure that the plate is oriented correctly in the plate holder, with the top-left
of the plate (i.e. the origin of the plate’s well identification markings) closest to
the instrument. This is critical and ensures that the instrument measures the
correct wells.
4. There is a little play in the plate when seated in the plate holder. This is normal
- the plate holder clamps it securely when it retracts into the instrument.
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Chapter 4 Making a measurement
7. Start the measurement:
1. Click Start on the toolbar.
2. The system asks for the plate schedule to be saved. Select Yes,
enter a file name and click Save.
3. The plate holder withdraws into the instrument and the measurement process
begins. As the SOP analysis runs the results are displayed:
4. Further messages in the status bar show the progress of the measurement.
5. When the measurement has finished, close the window .
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Making a measurement Chapter 4
Viewing the results
1. The results are stored as the latest record in the currently open measurement
file. To view the result, select this record and then click one of the Report tabs.
The following example shows the Aggregation Point (M) report.
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Chapter 4 Making a measurement
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Maintenance
Introduction
Warning!
Although the front cover lid may be removed to service the needle and
tube areas of the instrument, no one except a qualified Malvern representative must remove the main casing which extends down the back of the
machine.
This instrument has been designed so that supervisor/operator maintenance is kept
to a minimum. This chapter explains the routine user maintenance procedures that
can be performed. These procedures are:
Removing (or replacing) the transit locks.
Cleaning the instrument.
Replacing the system fuse.
Cleaning and replacement of the tubing, needle and measurement block.
Transit locks
Before initial use of the system, remove the transit locks from the instrument.
These locks prevent movement of the internal parts of the instrument during shipping.
Zetasizer APS Basic Guide Page 5-1
Caution!
The transit locks should be re-fitted if the machine is shipped to another
destination. Failure to do so could damage the instrument.
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Chapter 5 Maintenance
Refer to the following illustration for confirmation.
ill 8587
1. Use an allen key to remove all four bolts and from the transit locks, pic-
tured above, then remove the angle brackets.
2. Move the needle holder approximately 80mm left, to the centre of the tray, by
applying light finger pressure.
3. Switch on the instrument and then start the software. The needle will move to
the wash station.
4. Restart the software to initialise the needle to its correct position.
5. Retain all bolts and brackets for future shipment of the instrument.
Contact the Malven Helpdesk for guidance on the procedure of refitting the
transit locks.
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Maintenance Chapter 5
Cleaning the instrument
The instrument should be regularly cleaned externally to remove any sample spillages, plus regular cleaning of the measurement components to ensure optimum
performance.
Warning!
Before cleaning, always disconnect the instrument from the power supply
and disconnect all electrical cables.
Caution!
The surfaces of the instrument may be permanently damaged if samples or
solvents are spilt onto them. If a spillage occurs, disconnect the system
from the power supply before cleaning it up.
Clean the covers periodically using a mild soap solution.
Never use excessive liquid to clean the instrument and always avoid electrical
components (connectors, etc.).
Always ensure that the instrument is completely dry before applying power.
The paint has a solvent resistant finish, but it is good practice never to use a sol-
vent based solution as this may damage the painted surfaces.
Never use an abrasive cleaner to clean the instrument as this may damage the
painted surfaces.
Never use compressed air.
Cleaning the internal measurement components
During and after each measurement session, it is important that the internal measurement components (tubing, measurement block and needle) are rinsed out and
cleaned sufficiently. This is necessary to ensure consistent and accurate measurement results. Use the APS Wash Controls as described below.
The wash controls are used as part of the SOP sequence (refer to the Zetasizer
APS User manual for details) and can also be accessed separately as good practice
for reducing contaminants in the system. It is recommended to occasionally clean
the system without initially making a measurement. This has the effect of flushing
the tubing, measurement block and sample needle to ensure that any residual sample is completely removed.
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Chapter 5 Maintenance
The APS wash controls can be accessed by selecting Tools-Instrument-APSWash controls.
There are three Clean sequence options that can be used for general washing
either as a separate cleaning routine, or for in between well measurement (that is
set up in the SOP). Wash fluid - red inlet. Solvent - black inlet.
Standard wash:
Step 1: 600ul of DI water
Step 2: 1250 uL (1 full syringe) of 0.1M NaOH
Step 3: 2500uL (2 full syringes) of DI water
Vigorous wash:
Step 1: 1250uL of DI water
Step 2: 3750 uL of 0.1M NaOH
Step 3: 5000uL of DI water
Custom wash:
Where the volumes for the rinse and wash fluids can be set as a rinse protocol;
recommendations and examples are described below.
Select to execute the selected clean sequence, and to cancel.
After a clean sequence it is recommended to check cleanliness using the count rate
meter - refer to Monitoring the instrument cleanliness later in this section.
Recommended cleaning Protocols for the Zetasizer APS
The cleaning protocol necessary will depend on the type of sample, the sample
concentration and the type of measurement that is performed.
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Maintenance Chapter 5
In general, a size measurement of a sample requires less cleaning afterwards than a
thermal trend measurement of the same sample (as the thermal trend denatures the
protein which exposes hydrophobic parts which can give it a tendency to stick to
the cell and tubing). The user providing the samples should be in the best position
to know what could be an efficient cleaner for their sample, however the following
protocols have been shown to be effective for a variety of proteins.
The rinse fluid scattering (a parameter selected in the schedule settings) should be
monitored to make sure there is no build up of contamination in the optical cell.
For most protein samples tested (albumins, lysozyme, antibodies), the washing
protocols outlined below have worked well for concentrations up to 200mg/ml:
For standard size measurements:
Select Custom Wash
Activate all three steps by clicking on them
Choose 600µl of rinse fluid/solvent, then 1250µl of wash fluid, and finally
µl of rinse fluid
5000
Deionised water is suggested as the rinse fluid and 0.1M NaOH as the
wash fluid
For thermal trend measurements:
Use either use vigorous wash or select custom wash for concentrations of
proteins <10mg/ml
Activate all three steps by clicking on them
Choose 1250µl of rinse fluid/solvent, then 3750µl of wash fluid, and finally
µl of rinse fluid
7500
Deionised water is suggested as the rinse fluid and 0.1M NaOH as the
wash fluid. Higher concentrations up to 1M might be needed to keep the
system clean.
After a longer period of non-use or as a procedure to use if the system will
not be used for a long period:
Rinse the system with 10ml of deionised water through each inlet.
If the instrument is to be left unused for a very long period, rinse through
Extensive cleaning
If the rinse fluid scattering has increased to greater than 50-60kcps, it is recommended that a thorough wash with 1M NaOH and 1M HCl is performed using
the Wash control tools.
Zetasizer APS Basic Guide Page 5-5
the system extensively with water and then with 20% ethanol in water to
prevent anything growing in the system.
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Chapter 5 Maintenance
Select Custom Wash.
Activate all three steps by clicking on them.
Choose 1250μl of rinse fluid/solvent (water), then 10000μl of wash fluid
(1M NaOH), and finally 20000μl of rinse fluid (water).
Exchange the wash fluid bottle for1M HCL and repeat the same settings.
Choose 1250μl of rinse fluid/solvent (water), then 10000μl of wash fluid
(1M HCL), and finally 20000μl of rinse fluid (water).
Monitoring the instrument cleanliness
Note:
It is recommended that a stable count rate no greater than 500kcps is
achieved before any measurements are performed.
The cleanliness of the instrument can be monitored using the Count rate meter.
This check should be done routinely and, if required a clean sequence performed,
as described above.
When checking the cleanliness of the system, first perform a clean sequence
using filtered deionised water.
Monitor the count rate select Tools-Count rate meter from the main menu;
this will open the Count rate meter window.
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Maintenance Chapter 5
Within the attenuation section:
Set the top (attenuator) slider to 0%, by selecting and dragging to the left.
Set the lower (laser power) slider to 100%, by selecting and dragging to the
right.
Monitor the count rate in the top graph of the count rate window - the current
count rate will be displayed.
With a clean instrument you should see no correlation and the count rate
should be more or less a straight line with random fluctuations of less than
10kcps. The count rate should be stable and less than 120kcps. For a reasonably
clean system this should be less than 50kcps.
If this is not the case check the connections, the cleanliness of the wash fluid,
and finally repeat the cleaning of the flow cell itself.
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Chapter 5 Maintenance
Replacing the system fuse
Warning!
Fuses must not be replaced by the operator. Only the supervisor or a
Malvern representative should attempt to change the fuse.
If the instrument does not power up, check the system fuses. These are located in
the mains power switch on the rear panel.
Before changing a fuse, disconnect the instrument from the mains power.
Pull the fuse holders out and replace any faulty fuses with ones of the following
specification:
Rating:
Size:
T 4A HRC 250V (T = Time delay)
5mm x 20mm
Replacing the tubing and needle
General safety
Warning!
Before replacing parts, always disconnect the instrument from the power
supply and disconnect all electrical cables.
Warning!
A small volume of residual solvent or sample may remain in the tubing and
spill when the tube is disconnected. Always ensure that protective gloves
are worn.
Internal instrument parts
The following internal parts are all user replaceable:
Sample needle.
Sample needle tubing - to measurement block.
(Includes tubing and pre-fitted ferrule connectors for connection to measurement block)
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Maintenance Chapter 5
Sample tubing - from measurement block to syringe pump.
(Includes tubing and pre-fitted ferrule connectors for connection to measurement block)
Rinse tubes and ferrule connectors.
Rinse inlet filters and ferrule connectors.
Measurement block flowcell.
The following parts can be ordered from your local Malvern Instruments distributor.
Part No. Description
APS4000 Needle and tubing spares kit
APS4002 Consumable kit
APS0007 Flow cell
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Chapter 5 Maintenance
Removing the lid
To access the user-replaceable internal parts of the system remove the cover by lifting it vertically off the instrument, as shown in the illustration below:
On removing the lid, a laser safety interlock is activated which prevents the
machine being used whilst open.
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Maintenance Chapter 5
The following image identifies the internal parts of the instrument:
ill 8584
Measurement block
Needle and tube
Needle holder
Rinse well
Syringe pump
Well plate holder (shown with plate in situ)
Measurement block tubing and connections
The tubing and respective connection to the measurement block are manufactured as one assembly. The assembly is not user-serviceable and must be replaced
as a complete item.
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Chapter 5 Maintenance
The ferrule connections to the syringe and sample needle are re-usable between
tube changes, unless they have become damaged - refer to their respective sections.
Measurement block flowcell cleaning
With the measurement block tubing connections removed, the flowcell can then be
removed for cleaning. Follow the process below:
Note:
The measurement block flowcell is a critical optical component. Utmost
care must be taken on all aspects of the cleaning procedure.
1. Unscrew the sample needle (bottom ) connection first, followed by the
syringe (top
) connection.
ill 8704
2. Loosen screw , then with an M3 Allen key, remove the two screws , and
remove the measurement block top plate
3. Insert a clean 0.45mm interdental brush into the central channel of the flow-
cell.
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Maintenance Chapter 5
4. Holding onto the interdental brush, use a clean cotton bud to push the flowcell
up out of the measurement block from below. As the flowcell exits the block,
angle the brush so the flowcell does not fall off.
5. Place the flowcell onto a clean lint free cloth.
6. If sample build up is suspected inside the flowcell a wetted interdental brush
can be used to gently clean the internal channel. Take great care when performing this operation as the central core of the brush is metal and could
potentially damage the flowcell.
7. Remove any sample or grease by lightly dragging a clean lint free cloth over
the flowcell; if desired the cloth can wetted with ethanol or propan-2-ol.
Repeat this action for each optical side of the cell.
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Chapter 5 Maintenance
8. Re-insert the cell back into the measurement block. As with removing, angle
the cell when re-inserting.
Note:
Ensure that the flowcell is replaced with the matt black side (side without
any windows) facing the rear of the instrument and chamfered corner to
the right hand side.
9. Fit lid - tighten screw first to push lid into corer, then tighten both lid
screws
10. Screw in the tubing connections. Attach the syringe (top) connection first, fol-
.
lowed by the sample needle (bottom) connection. Screw each connection in
until they ‘click’ - once clicked the connection is complete.
11. Using filtered deionised water, perform a basic clean sequence and check
the resultant count rate. This will test the block for any leakages and check that
the cell is sufficiently clean for performing measurements.
The count rate should be stable and less than 120kcps. For a reasonably clean
system, this should be less than 50kcps. If this is not the case, check the connections, the cleanliness of the wash fluid, and finally repeat the cleaning of the
flow cell itself. Refer to Cleaning the internal measurement components
and Monitoring the instrument cleanliness for instructions.
Syringe pump connections
Note:
Connectors are re-usable between tube changes, unless they have become
damaged. Ferrules are not re-usable and should be discarded whenever the
tubing is replaced.
All rinse tubes that terminate at the syringe pump, and the rinse inlet filters, are fitted with a standard ferrule and screw connection; if these need to be replaced or
removed for tubing changes, follow the process below:
1. Insert the tube through the connector (via the large, non-threaded end).
2. Thread the ferrule onto the tube (i.e. the end of the tube that has just been
passed through the connector). The end of the tube should be positioned flush
with the end of the ferrule. See illustration below:
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Maintenance Chapter 5
3. Push the tube and ferrule into the threaded end of the connector so that it is
seated flush in the connector.
When the connector is screwed into the instrument, the tube is clamped securely.
Rinse inlet filters
ill 8589
The two rinse inlet filters are of microporous structure to prevent foreign particles
entering the system and causing inaccurate measurements. Both external rinse
tubes terminate with an inlet filter that screws onto the connector. The filters
then rest inside the fluid within each rinse bottle:
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Chapter 5 Maintenance
Note
Rinse inlet filters have a working life of approximately one year. Contact
Malvern Instruments to order replacement parts.
Replacing the needle
When to replace the needle
The needle will need to be replaced periodically when it can no longer be cleaned
sufficiently. Additionally, the needle can be replaced to suit the kind of plate that is
currently being used. The piercing needle (included) is more suited to piercing the
membrane used to cover some plates, whereas a flat-tipped needle (included) could
be more effective in plates with flat well bases filled with a very low sample volume.
Removing and replacing the needle
1. Remove the lid from the Zetasizer APS instrument.
2. Completely loosen the existing needle in its holder using a 2.5mm allen key in
the securing bolt
3. Carefully withdraw the needle from the holder.
.
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Maintenance Chapter 5
4. Unscrew the tube connector from the underside of the measurement block.
The needle assembly
consists of:
A needle housing
Sample needle
Two ferrules
Two connectors
Tubing
ill8590
5. Unscrew both connectors from the needle housing . One end is con-
nected to the tube, the other to the needle.
6. Remove the ferrule from the end of the needle and also withdraw it from
the connector.
7. Pull the ferrule off the end of the tube and remove the connector from the tube
.
8. To re-fit the needle, reverse the process described. When seating the needle in
the needle holder, ensure that the exposed needle length is precisely
50mm ± 1mm. Failure to do this could result in damage to the needle. Do not
over tighten the securing bolt as this also may damage the needle.
9. Referring to the Measurement block tubing and connections section, refit
the needle tubing to the measurement block.
Discard used needle and any tubing following the correct local waste disposal
Zetasizer APS Basic Guide Page 5-17
procedures.
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Chapter 5 Maintenance
Replacing the rinse tubing
Note:
For this section, please refer to the illustrations earlier in this chapter.
There are three rinse tubes inside the machine and two located externally.
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Maintenance Chapter 5
All tubes have connectors at both ends.
+
This tube connects the syringe pump to the measurement block.
+ These two external tubes connect to ports on the outside of the instru-
1. Remove the lid from the Zetasizer APS instrument.
2. Unscrew all rinse tube connectors as previously described and then remove the
These two internal tubes connect the syringe pump to the inside of the
external casing and are of equal length.
Refer to the Syringe pump connections section earlier in this chapter.
Refer to the Syringe pump connections and Measurement block
tubing and connections sections earlier in this chapter.
ment - their tubes terminate in connectors that are attached to the rinse
inlet filters.
Refer to the Syringe pump connections and Rinse inlet filters sections earlier in this chapter.
tubes.
3. Re-fit the tubes by reversing the removal procedure.
4. Discard used tubes, following the correct local waste disposal procedures.
Installing the Zetasizer APS
The Zetasizer APS system should initially be installed and commissioned by
Malvern trained personnel. This appendix shows how to re-install the system,
typically required under the following circumstances:
Moving the instrument.
Should it become necessary to move the system from one laboratory to
another, read the information in this appendix to correctly reconnect the
system.
Changing the computer.
It may be company policy to periodically upgrade computers. Detail is given on
actions required.
Only install the system in a suitable environment as detailed in Site Requirements
section of this document.
Warning!
Do not obstruct the ventilation slots underneath the instrument, nor the
fans on the rear panel.
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Chapter 5 Maintenance
To install the system:
Caution!
Remove the transit locks from the instrument - refer to the Transit Locks
section of this document. These locks should be re-fitted if the machine is
shipped to another destination.
Connect the USB cable to the connector marked USB on the rear panel of the
Zetasizer APS instrument
connection on the computer.
Connect the power cable to the power socket on the rear panel of the
instrument
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. Connect the other end of the cable to the USB
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Maintenance Chapter 5
Warning!
This product must be connected to a protective earth
Make all computer connections (mouse, keyboard, power, etc) by following
the instructions provided with your computer.
Rinse fluid: connect a bottle containing solvent to the black port on the side of
the instrument. Connect a bottle containing a wash fluid to the red port on the
side of the instrument.
Place a beaker below the waste outlet.
Installation options
If purge air is required connect to the purge air port at the base of the rear panel
. Refer to the specification in Appendix A.
If using the optional Plate Temperature Control unit, connect to input .
Changing the computer
If, at some point in the future, the computer used with the instrument is changed,
the following actions will be required.
To install the system:
1. Insert the Zetasizer Software CD into the CD drive.
2. If Autorun is enabled on the computer, the software will start to install auto-
matically. Follow all on-screen instructions to complete the installation.
3. If Autorun is not enabled, browse to the CD drive using Windows Explorer
and double click on the file named Malvern Zetasizer Software...exe. Note: this
file name changes with the version number of the software released.
Note
If the software is subsequently updated with a new version, any custom
reports, parameter settings, SOPs, etc. will be preserved.
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Chapter 5 Maintenance
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Appendix
Specification
Parameter Specification
Size range maximum (radius) * 0.15nm to 1μm
Molecular weight range **
(est from hydrodynamic diameter)
Molecular weight range **
(calculated using Debye plot)
Minimum sample volume 20μL
Sensitivity at minimum volume 0.1mg/ml of 15kDa protein
High concentration Yes - optically clear samples
Laser 60mW, 830nm
Temperature control 2-90°C
Temperature control accuracy 0.1°C@25°C, 0.2°C@2°C, 0.5°C@90°C
Weight 22.5kg
Dimensions W:D:H, 500mm x 410mm x 420mm
Power 90V-260V AC, 50/60Hz ,150W
Dry air 100kPa (1bar), 4mm o.d. tubing
Computer interface USB
Measurement technique Dynamic light scattering (90 degrees)
Detector Avalanche photodiode, Q.E. >50% at 830nm
Product laser class Class 1 compliant,
Condensation control Purge facility using dry air
Ambient operating conditions
- Humidity
342Da to 2x10
980Da to 2x10
IEC 60825-1(1993)+A1(1997)+A2(2001)
+15 to +30 °C (+59 to 86 °F)
10 to 90% (non-condensing)
7
Da
7
Da
* Peak mode range (radius), 0.3nm - 0.5 microns, sample and sample preparation dependent
** Sample and sample preparation dependent
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Appendix A Appendix
PTC-1000 Thermoelectric temperature control
unit (optional)
This device is referred to throughout this manual as the Plate Temperature Controller.
Parameter Specification
Temperature range 4ºC to 40ºC +/- 0.1ºC*
Weight 12.2kg
Dimensions W:D:H, 195mm x 351mm x 304mm
Power 115V-230V AC, 50/60 Hz, 294W
*Although the PTC-1000 is capable of maintaining its coolant within +/-0.16ºC, the
plate itself is controllable within +/-2ºC.
Chemical compatibility
Components of the Zetasizer APS that may come into contact with the sample are
manufactured from materials that are considered to give the widest protection from
chemical attack. However, it is important to check that any sample used is chemically compatible with the materials mentioned.
Warning!
It is advisable that the chemical compatibility is checked against the materials identified below before inserting a sample. It is also recommended that
a test is performed on the material with the sample before more permanent
usage is undertaken.
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Appendix Appendix A
Materials used
The materials list below details all components that may come into contact with the
sample or solvent.
Component Materials
Rinse tubing FEP
Waste tubing FEP
Wash station Acetal
Drain tube Tygon
Needle PTFE coated stainless steel
Union to hold needle PEEK
Plate retention Acetal and stainless steel
Plate holder Black anodised aluminium
PTC tubing Tygon
Microtiter plates Variable composition
Disposal of Electrical & Electronic
Equipment
This regulation is applicable in the European Union and other European countries
with separate collection systems.
This symbol on the product or on its packaging indicates that when the last user
wishes to discard this product it must not be treated as general waste. Instead it
shall be handed over to the appropriate facility for the recovery and recycling of
electrical and electronic equipment.
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Appendix A Appendix
By not discarding this product along with other household-type waste, the volume
of waste sent to incinerators or landfills will be reduced and natural resources will
be conserved.
For more detailed information about recycling of this product, please contact your
local city office, your waste disposal service, or your Malvern representative.
Regulatory statements
FCC Notice (US only)
The Federal Communications Commission (FCC) mark on this product signifies
conformance to FCC regulations relating to Radio Frequency Devices. These have
been satisfied by testing the product against, and being found to be compliant with:
FCC CFR 47 Part 15:March 2003.Class A digital device.
The device complies with part 15 of the FCC Rules. Operation is subject to the
following two conditions:
1) This device may not cause harmful interference, and
2) this device must accept any interference received, including interference that
may cause undesired operation.
Note
This equipment has been tested and found to comply with the limits for a
Class A digital device, pursuant to part 15 of the FCC rules. These limits
are designed to provide reasonable protection against harmful interference
when the equipment is operated in a commercial environment. This
equipment generates, uses, and can radiate radio frequency energy and, if
not installed and used in accordance with the instruction manual, may
cause harmful interference to radio communications. Operation of this
equipment in a residential area is likely to cause harmful interference in
which case the user will be required to correct the interference at his own
expense.
Page A-4 MAN 0494
Note
Changes or modifications not expressly approved by Malvern Instruments
Limited could void the user’s authority to operate the equipment.
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Appendix Appendix A
Canadian Regulatory Information
(This applies to Canada Only.)
This digital apparatus does not exceed the Class A limits for radio noise emissions
from digital apparatus set out in the Radio Interference Regulations of the
Canadian Department of Communications.
Note that Canadian Department of Communications (DOC) regulations provide,
that changes or modifications not expressly approved by Malvern Instruments
Limited could void your authority to operate this equipment.
This Class A digital apparatus complies with Canadian ICES-003.
Cet appareil numérique de la classe A est conforme à la norme NMB-003 du
Canada.
VCCI acceptance (Japan only)
The Voluntary Control Council for Interference (VCCI) mark on this product
signifies compliance to Japanese EMC regulations as specified by VCCI.
ill 6793
Transl at ion:
This is a Class A product based on the standard of the Voluntary Control Council
for Interference by Information Technology Equipment (VCCI). If this equipment
is used in a domestic environment, radio disturbance may occur, in which case the
user may be required to take corrective actions.
Zetasizer APS Page A-5
MAN0494-1 (Zetasizer APS Basic Guide).book Page 6 Friday, August 9, 2013 2:08 PM
Appendix A Appendix
Page A-6 MAN 0494
www.malvern.com
Malvern Instruments Limited
Grovewood Road, Malvern
Worcestershire, WR14 1XZ, UK
Tel +44 1684 892456
Fax +44 1684 892789
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