Beckman Coulter LS 13 320 User manual

PN B05577AC
July 2017
User’s Manual
LS 13 320 Laser Diffraction Particle Size Analyzer
Beckman Coulter, Inc.
250 S. Kraemer Blvd.
Brea, CA 92821 U.S.A.

LS 13 320 Laser Diffraction
Particle Size Analyzer
User’s Manual
PN B05577AC (July 2017)
Copyright © 2017 Beckman Coulter, Inc.
All rights reserved.
Beckman Coulter, the stylized logo, and the Beckman
Coulter product and service marks mentioned herein are
trademarks or registered trademarks of Beckman Coulter,
Inc. in the United States and other countries.
All other trademarks, service marks, products, or services
are trademarks or registered trademarks of their
respective holders.
Contact Us
If you have any questions, contact our Customer Support
Center.
• Worldwide, find us via our website at
www.beckmancoulter.com/customersupport/support.
• Outside of the USA and Canada, contact your local
Beckman Coulter Representative.

PN B05577AC iii
Revision History
This document applies to the latest software listed and higher versions. When a subsequent software
version affects the information in this document, a new issue will be released to the Beckman Coulter Web
site. For labeling updates, go to www.beckmancoulter.com and download the latest version of the manual
or system help for your instrument.
Initial Issue, B05577AA, 2009
Issue AB, September 2011
Updates were made to the following sections:
• Updated corporate address
• Revised Figure 1.2 Certification Label (Instrument Back Cover)
• Other minor edits and deletions
• Revision page added
• Added the Beckman Coulter, Inc. Customer End User License Agreement
• Trademarks page added
Issue AC, July 2017
Updates were made to the following sections:
• Alerts for Danger, Warning, Caution, Important, and Note
• RoHS Notice
• Safety Labels

PN B05577AC
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Revision History

PN B05577AC v
Safety Notice
Read all product manuals and consult with Beckman Coulter-trained personnel before attempting
to operate instrument. Do not attempt to perform any procedure before carefully reading all
instructions. Always follow product labeling and manufacturer’s recommendations. If in doubt as to
how to proceed in any situation, contact your Beckman Coulter Representative.
Alerts for Danger, Warning, Caution, Important, and Note
DANGER
DANGER indicates an imminently hazardous situation which, if not avoided, will
result in death or serious injury.
WARNING
WARNING indicates a potentially hazardous situation which, if not avoided, could
result in death or serious injury. May be used to indicate the possibility of
erroneous data that could result in an incorrect diagnosis.
CAUTION
CAUTION indicates a potentially hazardous situation, which, if not avoided, may
result in minor or moderate injury. It may also be used to alert against unsafe
practices. May be used to indicate the possibility of erroneous data that could
result in an incorrect diagnosis.
IMPORTANT IMPORTANT is used for comments that add value to the step or procedure being performed.
Following the advice in the Important adds benefit to the performance of a piece of equipment or to a
process.
NOTE NOTE is used to call attention to notable information that should be followed during installation, use,
or servicing of this equipment.

PN B05577AC
vi
Safety Notice
RoHS Notice
WARNING
California Proposition 65: This product can expose you to chemicals including
phthalates, which are known to the State of California to cause cancer and birth
defects or other reproductive harm. For more information go to
www.P65warnings.ca.gov.
Information
CAUTION
Read all product manuals and consult with Beckman Coulter-trained personnel
before attempting to operate instrument. Do not attempt to perform any
procedure before carefully reading all instructions. Always follow product labeling
and manufacturer’s recommendations. If in doubt as to how to proceed in any
situation, contact your Beckman Coulter Representative.
RoHS Notice
These labels and materials declaration table (the Table of Hazardous Substance's Name and
Concentration) are to meet People’s Republic of China Electronic Industry Standard SJ/T11364-2006
“Marking for Control of Pollution Caused by Electronic Information Products” requirements.
RoHS Caution Label
This label indicates that the electronic information product contains certain toxic or hazardous
substances. The center number is the Environmentally Friendly Use Period (EFUP) date, and
indicates the number of calendar years the product can be in operation. Upon the expiration of the
EFUP, the product must be immediately recycled. The circling arrows indicate the product is
recyclable. The date code on the label or product indicates the date of manufacture.
RoHS Environmental Label

PN B05577AC vii
Safety Notice
Laser Safety
This label indicates that the electronic information product does not contain any toxic or hazardous
substances. The center ‘e’ indicates the product is environmentally safe and does not have an
Environmentally Friendly Use Period (EFUP) date. Therefore, it can safely be used indefinitely. The
circling arrows indicate the product is recyclable. The date code on the label or product indicates
the date of manufacture.
Laser Safety
The LS 13 320 contains a 5 mW diode laser. The instrument therefore may pose certain hazards
associated with low-power lasers if misused. You should be aware of these possible hazards as
described in the next paragraph. Additionally, misuse of diluents for sample dispersion can also
create hazardous situations.
Laser Safety Precautions
CAUTION
Diode laser power of up to 5 mW at 750 nm or 780 nm could be accessible in the
interior if the safety interlocks are defeated.
To comply with Federal Regulations (21CFR Subchapter J) as administered by the Food and Drug
Administration's (FDA) Center for Devices and Radiological Health (CDRH), defeatable
microswitches are located on the right and left of the door panel. Because the system contains a
laser, it should be isolated from non-laser instruments. Users are advised to keep a copy of ANSI
standard 2136.1, SAFE USE OF LASERS, near the instrument for ready reference. Copies are available
from:
American National Standards Institute
1430 Broadway
New York, NY 10018
General Laser Precautions
WARNING
The laser beam can cause eye damage if viewed either directly or indirectly from
reflective surfaces (such as a mirror or shiny metal surface). Avoid direct exposure
to beam. Do not view directly or with optical instruments.
A laser is a unique light source that exhibits characteristics different from conventional light
sources. The safe use of any laser depends upon familiarity with the instrument and the properties
of coherent, intense beams of light. The beam can cause eye damage. The beam might cause damage
if viewed indirectly from reflective surfaces such as a mirror or shiny metal surface.

PN B05577AC
viii
Safety Notice
Safety Labels
WARNING
Use of controls or adjustments or performance of procedures other than those
specified herein may result in hazardous radiation exposure.
Follow these precautions:
• Advise all those using the instrument of these precautions.
• Limit access to the instrument to those trained in the use of the equipment.
• Post warning signs in the area of the laser beam to alert those present.
• Never look directly into the laser light source or at scattered laser light from any reflective
surface.
• Stop viewing if:
—you see an unusually bright spot that makes you uncomfortable (similar to looking at the
sun).
—you get a headache (a symptom of overexposure).
• Do not tamper with or attempt to defeat the safety interlock switches.
LS 13 320 Specific Precautions
• Never place a mirror or optical surface (other than the sample cell assembly) into the optical
axis of the system.
WARNING
Do not place your hands in the pathway of the door as it closes.
WARNING
Do not place your hands or any object inside the optical bench as the module is
docking.
Safety Labels
Radiation Hazards
In the design and manufacture of the BECKMAN COULTER LS 13 320, Beckman Coulter Inc., Particle
Characterization Group, has complied with the requirements governing the use and application of
a laser as stipulated in regulatory documents issued by the U.S. Department of Health and Human
Services and the Center for Devices and Radiological Health (CDRH). In compliance with these
regulatory documents, every measure has been taken to ensure the health and safety of users and
laboratory personnel from the possible dangers of laser use. CDRH-required labels are placed near

PN B05577AC ix
Safety Notice
Safety Labels
or on those covers that, when removed, might expose laser radiation. Refer to the figure titled
Warning labels - Instrument Front Cover And Laser Cover for the warning labels and their locations.
Warning labels - Instrument Front Cover And Laser Cover
Certification Label (Instrument Back Cover)

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Safety Notice
Mechanical, Electrical, Chemical, and Fire Safety Notices
Mechanical, Electrical, Chemical, and Fire Safety Notices
Mechanical Safety
DANGER
For safe operation of the equipment, observe the following:
• Do not place fingers inside bench as automatic sliding door closes.
• Do not place fingers inside bench as module docks into bench.
• Do not interfere with or attempt to disable the interlocks incorporated in the
left and right doors.
Electrical Safety
DANGER
To reduce the risk of electrical shock, observe the following:
• High voltages are present inside the instrument. Always disconnect the
instrument from the main power supply before removing any cover.
• The instrument must be grounded correctly.
Chemical Safety
DANGER
Normal operation may involve the use of diluents and reagents that are
pathogenic, or toxic. Such materials require that you take all necessary safety
precautions.
• Do not use any diluents that are not compatible with the specific wetted
surface of the sample module. Consult Beckman Coulter or its local
representative before using any chemicals not listed in this manual.
• Proper handling procedures for diluents and reagents used in particle analysis
should be adhered to at all times. Consult appropriate safety manuals and
Material Safety Data Sheets for all samples, diluents and reagents used.
• Care should be taken when mixing or exchanging diluents. Reactions can
occur between incompatible solvents that may be violent.
• Flammable solutions should be prepared for use in an appropriate
environment and brought to the instrument only when required for analysis.

PN B05577AC xi
Safety Notice
Scope of Manual
CAUTION
To reduce the risk of instrument damage, observe the following:
• Take care disconnecting diluent lines. Open-ended tubing may allow liquid to
spill out of the vessel.
• Never place containers of liquids on top of the LS 13 320. Repair of
instruments damaged or affected by spilled liquids will not be covered by any
warranty.
Fire Safety
WARNING
Many non-aqueous solutions are flammable. Where possible choose less
flammable alternatives.
Warming Up
Many non-aqueous solutions are flammable. Where possible choose less flammable alternatives.
Sources of Error
• Sample dispersion
• Air bubbles
• Misalignment
• Incorrect obscuration
• External mechanical vibration, if present, may cause misalignment of the laser. (Automatic
alignment should be performed more often.)
• Electrical interference. (Use of an uninterruptible power supply (UPS) is recommended.)
• Sudden changes in temperature can cause misalignment as well as changes to the measured
electrical offsets.
Scope of Manual
This manual is designed to familiarize you with the Optima XE, its functions, specifications,
operation, and routine operator care and maintenance. Read this entire manual, especially the
safety notices and all safety-related information, before operating the instrument or performing
maintenance.
NOTE If the instrument is used in a manner other than specified in this manual, the safety and performance
of this equipment could be impaired. Further, the use of any equipment other than that recommended
by Beckman Coulter has not been evaluated for safety. Use of any equipment not specifically
recommended in this manual and/or the appropriate rotor manual is the sole responsibility of the user.

PN B05577AC
xii
Safety Notice
Scope of Manual

xiii
Contents
Revision History,iii
Safety Notice,v
LS 13 320 Introduction,xxiii
CHAPTER 1: Theory,1-1
Theoretical Background,1-1
Light Scattering,1-1
Mie Theory,1-2
3.1.2 Fraunhofer Theory,1-2
Polarization Intensity Differential Scattering (PIDS),1-3
3.1.4 Particle Non-Sphericity & Light Scattering,1-4
Laser Diffraction Measurement for Non-spherical Particles,1-4
PIDS Sizing,1-5
Components,1-5
Functions,1-5
Description,1-6
CHAPTER 2: Installation,2-1
Installation Requirements,2-1
Environment,2-1
Power Requirements,2-1
Temperature and Humidity Requirements,2-2
Sample Modules Specific Requirements,2-2
Suspension Fluid for Aqueous and Universal Liquid Modules,2-2
Drain for Aqueous Liquid Module,2-3
Drain for Universal Liquid Module,2-3
Vacuum for Tornado Dry Powder System,2-3
Hardware Connections,2-3
Software Installation,2-4
Installing and Starting the Software,2-4
Configuring Software Parameters,2-4
Instrument Verification,2-5
Post-Installation Verification,2-5
Daily Verification,2-5
Getting Started,2-5
Starting the Instrument and its Control Program,2-5

xiv
Contents
Setting Up For Compliance,2-7
Selecting a Module,2-10
Making Measurements,2-12
Measuring Offsets,2-12
Alignment,2-12
Measure Background,2-12
Measure Loading,2-12
Running a Control,2-13
Running a Sample,2-18
Reference Background,2-19
CHAPTER 3: LS 13 320 Software,3-1
File Menu Options,3-2
Window Menu Options,3-11
Run Menu Options,3-12
Preference Options,3-17
Printed Report,3-17
Preference Files...,3-30
Security Options,3-32
Security Setup,3-34
5.5.2 Types of Users,3-35
5.5.2.1 Administrator,3-35
Add a User Account,3-38
Edit a User Account,3-39
View User Account Info,3-39
Supervisor,3-40
Customize Main Menu,3-40
Customize Run Menus,3-41
Customize Sample Info Names,3-41
Recent Files and Directories,3-42
No Security,3-42
Low Security,3-43
Medium Security,3-45
High Security,3-46
Logging Out,3-48
CHAPTER 4: Regulatory Compliance - 21 CFR Part 11,4-1
Electronic Record Control - 21 CFR Part 11,4-1
File Historyand Tracking,4-1
Audit Trail,4-3
Electronic Signatures,4-4
Generating Electronic Signatures,4-5
Applying Electronic Signatures,4-7

xv
Contents
Additional Security Features,4-8
Data Mirroring,4-8
File Attributes,4-8
Starting Security-Enabled Software,4-9
CHAPTER 5: Data File Menus,5-1
RunFile Menu,5-1
Open for Overlay,5-1
Save,5-3
Export,5-3
Get Info,5-6
Get File History,5-6
Edit Menu,5-7
View Menu,5-9
Graphs,5-9
Display Values on One Channel,5-10
Display Multiple Channel Values,5-10
Expand Part of a Graph,5-10
Listing,5-11
Analyze Menu,5-12
Statistics,5-12
Compare to Standard,5-13
Compute Sizes,5-13
CHAPTER 6: Sample Modules,6-1
Aqueous Liquid Module,6-1
ALM Description,6-2
System Description,6-2
Indicators,6-2
Connecting the ALM,6-4
Recirculation Lines,6-4
Inlet and Drain Hoses,6-4
Loading the Sample Cell Into the Optical Bench,6-5
Software,6-6
8.1.3.1 Control Menu,6-7
8.1.3.2 Standard Operating Methods (SOM),6-8
8.1.3.3 Loading an SOM,6-12
8.1.3.4 Standard Operating Procedures (SOP),6-13
Suspension Fluids,6-14
Cleaning the ALM,6-15
Replacing the Diffraction Cell Window,6-17
ALM Troubleshooting,6-21
ALM Specifications,6-21
Auto-Prep Station,6-21
APS Description,6-22
Connecting the APS,6-22

xvi
Contents
Software,6-24
Run Menu,6-24
File Menu,6-25
Edit Menu,6-26
8.2.3.1 APS Run Menu,6-26
Auto-Prep Station Settings,6-27
8.2.3.2 APS Select Menu,6-29
8.2.4 APS Troubleshooting,6-30
Micro Liquid Module,6-30
MLM Description,6-31
Loading the MLM,6-32
Software,6-32
Control Menu,6-32
Stirrer Speed,6-33
Stirrer On/Off,6-33
Standard Operating Methods (SOM),6-33
Creating SOMs,6-33
Loading an SOM,6-38
Standard Operating Procedures (SOP),6-40
Creating an SOP,6-40
Loading an SOP,6-41
Suspension Fluids,6-42
MLM System Preparation,6-44
Placing the Cell on the Sample Stand,6-44
Filling Micro Liquid Module with Diluent,6-45
Adding Sample,6-46
Setting the Stirring Motor,6-46
Cleaning the MLM,6-47
Clean the cell components,6-47
MLM Troubleshooting,6-49
Tornado Dry Powder System,6-49
Tornado Description,6-50
Indicators,6-50
Docking the Tornado DPS,6-51
Software,6-51
8.4.3.1 Control Menu,6-52
8.4.3.2 Standard Operating Methods (SOM),6-53
Creating SOMs,6-53
8.4.3.3 Loading an SOM,6-56
8.4.3.4 Standard Operating Procedures (SOP),6-57
Creating SOPs,6-57
Loading an SOP,6-58
Cleaning the Tornado DPS,6-58
Using the Cleaning Sample,6-58
Cleaning the Cell Windows,6-59
Cleaning the Sample Tubing,6-61
Cleaning the Sheath Flow Filter,6-63
Tornado DPS Troubleshooting,6-64
Tornado DPS Specifications,6-66

xvii
Contents
Universal Liquid Module,6-66
ULM Description,6-67
Loading the ULM,6-67
ULM Software,6-68
8.5.3.1 Control Menu,6-68
8.5.3.2 Standard Operating Methods (SOM),6-70
8.5.3.3 Loading an SOM,6-74
8.5.3.4 Standard Operating Procedures (SOP),6-75
Suspension Fluids,6-76
Cleaning the ULM,6-78
Cleaning Fluids,6-78
Cleaning the Cell,6-79
Replacing the Diffraction Cell Window,6-81
ULM Troubleshooting,6-85
ULM Specifications,6-85
APPENDIX A: LS 13 320 Specifications,A-1
Specifications,A-1
APPENDIX B: Sample Handling,B-1
Material Handling,B-1
Liquid Sampling,B-1
Solid Sampling,B-1
Spinning Riffler,B-2
Chute splitter,B-2
Table sampling,B-3
Scoop sampling,B-4
Cone and quartering,B-4
Liquid Sample Dispersion,B-4
Liquid Sample Dispersion,B-5
Physical Methods of Liquid Dispersion,B-5
Chemical Methods of Liquid Dispersion,B-6
Stabilization by surface charge,B-6
Steric Stabilization,B-7
Physical and Chemical Methods of Liquid Dispersion,B-7
Special cases,B-7
A Practical Recipe For Liquid Sample Dispersion,B-7
Solid Sample Dispersion,B-8
Diluent Selection,B-8
Consider Solvation Effects,B-8
Consider Other Effects,B-8
Consider the Effects the Diluent Has on the Sample's Suspension
Fluid,B-8
Consider Characteristics of the Diluent,B-9
Viscosity:,B-9
Active life:,B-9
Reactivity:,B-9

xviii
Contents
Purity:,B-9
Refractive Index:,B-9
Color:,B-9
APPENDIX C: Optical Models,C-1
Introduction,C-1
Refractive Index,C-1
Extended Optical Model,C-2
Creating an Optical Model,C-2
Creating an Optical Model from the RunFile Menu,C-3
Statistics,C-5
User-Defined Mean,C-5
Median and Mode,C-6
Median,C-6
Mode,C-6
Characterizing the Distribution,C-6
Variance,C-6
Standard Deviation,C-7
Coefficient of Variation,C-7
Skewness,C-7
Kurtosis,C-8
APPENDIX D: Troubleshooting,D-1
Background,D-1
Troubleshooting High Backgrounds,D-3
Reference Background Set-Up,D-3
Part 1 - Setting Up a Reference Background,D-4
Part 2 - Using the Reference Background,D-8
APPENDIX E: Maintenance,E-1
Cleaning Procedures,E-1
Cleaning Fluids,E-1
Cleaning the Lens,E-1
Fourier Lenses,E-2
Projection Lens,E-3
Beckman Coulter, Inc.
Customer End User License Agreement
Related Documents

xix
Illustrations
Illustrations
1.1 Scattering Patterns for Spheres,1-2
1.2 Scattering From Different Polarizations,1-4
2.1 Electrical Specification Labels,2-2
2.2 Location of Interunit Connections,2-3
2.3 Connections Dialog Box,2-4
2.4 Security Level Options,2-6
2.5 User Set-up Flowchart,2-7
2.6 Selecting An Optical Module,2-11
2.7 Message When An Optical Module Is Not Found,2-11
2.8 Ready Screen,2-11
2.9 Run Menu,2-13
2.10 Run Menu,2-14
2.11 Measuring Offsets Screen,2-15
2.12 Auto Align Screen,2-15
2.13 Measuring Offsets Screen,2-16
2.14 Measuring Obscuration (Loading) Screen,2-16
2.15 Sample Info Dialog,2-17
2.16 Run Settings Dialog,2-17
2.17 Optical Model Dialog Screen,2-19
2.18 Run Cycle Options Dialog,2-21
2.19 Reference Background File Selection,2-22
3.1 LS 13 320 Software,3-1
3.2 User Privileges Dialog: No Security,3-43
3.3 User Privileges Dialog: Low Security,3-45
3.4 User Privileges Dialog: Medium Security,3-46
3.5 User Privileges Dialog: High Security,3-47
5.1 Export Data Dialog Box,5-4
5.2 Preferences Data Dialog Box Exporting Data,5-5
5.3 No Security,5-7
5.4 Statistics information,5-12
5.5 Select Optical Model Dialog Box,5-13
6.1 Aqueous Liquid Module (ALM) with Sample Cell,6-1
6.2 Liquid Level Sensors,6-2
6.3 Indicators,6-3

xx
Illustrations
6.4 Drain Valve Knob,6-3
6.5 Figure 4 Line Locations and Connections,6-4
6.6 Inlet and Drain Lines,6-5
6.7 Sample Cell,6-5
6.8 PIDS Windows Thumbscrews,6-16
6.9 Diffraction and PIDS Windows,6-16
6.10 Diffraction Window,6-18
6.11 Pencil Reflections Test,6-19
6.12 Auto-Prep Station with Aqueous Liquid Module,6-22
6.13 Connecting the APS,6-23
6.14 Electrical and Communications Connections,6-23
6.15 Micro Liquid Module,6-31
6.16 Micro Liquid Module,6-31
6.17 Figure 1 Control Menu,6-33
6.18 Figure 2 Stirrer Speed,6-33
6.19 Figure 3 Step 1 of SOM development,6-34
6.20 Figure 4 Select Fluid Dialog,6-34
6.21 Figure 5 Edit Fluid List Dialog,6-35
6.22 Step 2 of SOM Development,6-35
6.23 Figure 7 Step 3 of SOM Development,6-36
6.24 Figure 8 Run Cycle Options Dialog,6-36
6.25 Figure 9 Step 4 of SOM Development,6-37
6.26 SOM Summary,6-38
6.27 SOM List Dialog,6-39
6.28 Create an SOP Dialog,6-41
6.29 Figure 13 SOP List Dialog,6-42
6.30 Miscibility Guide,6-44
6.31 Locator Notch,6-45
6.32 Cell Diluent / Sample Entry,6-45
6.33 Sample Cell Components,6-48
6.34 Figure 17 Cleaning the Cell With a Swab,6-49
6.35 Tornado DPS LED Indicators,6-50
6.36 Bracket Screws,6-59
6.37 Sample Cell Latches,6-60
6.38 Sample Cell Windows,6-61
6.39 Cover Latches,6-62
6.40 Wall Impact Plate,6-62
6.41 Suction and Sheath Flow Tubes,6-63