Beruflich Dokumente
Kultur Dokumente
PN 7221940 Rev. A
TABLE OF CONTENT
1
1
1
1
1
2. SAFETY PRECAUTIONS
2.1 GENERAL
2.2 LASER SAFETY PRECAUTIONS
2.3 GENERAL LASER PRECAUTIONS
2.4 LS 13 320 SPECIFIC PRECAUTIONS
2.5 RADIATION HAZARDS
2
2
2
2
3
3
5
5
6
4. SYSTEM COMPONENTS
4.1 OPTICAL BENCH OVERVIEW
4.2 LIGHT SOURCE
4.3 SAMPLE MODULES
4.4 COMPUTER SYSTEM
4.5 SOFTWARE
9
9
11
12
12
12
14
14
14
15
16
17
2. PIDS SIZING
2.1 Components
2.2 Functions
2.3 Description
18
18
19
19
PN 7221940 Rev. A
ii
21
21
21
21
22
23
23
24
24
25
25
25
7. GETTING STARTED
7.1 STARTING THE INSTRUMENT AND ITS CONTROL PROGRAM
7.2 SELECTING A MODULE
26
26
27
8. MAKING MEASUREMENTS
8.1 RUNNING A CONTROL
8.2 RUNNING A SAMPLE
29
30
34
36
2. WINDOW
41
3. RUN
42
4. PREFERENCES
46
5. SECURITY
5.1 TYPES OF USERS
5.1.1 ADMINISTRATOR
5.1.2 SUPERVISOR
5.2 NO SECURITY
5.3 LOW SECURITY
5.4 MEDIUM SECURITY
56
58
58
63
65
66
68
69
2. ELECTRONIC RECORDS
69
3. FDA REQUIREMENTS
69
PN 7221940 Rev. A
iii
TABLE OF CONTENT
70
70
71
71
73
75
76
76
78
79
79
80
81
81
82
83
84
84
2. EDIT
2.1 COPY WINDOW
2.2 EDIT SAMPLE INFO
2.3 EDIT SIZE RESULTS
2.4 ADD ELECTRONIC SIGNATURE
85
85
85
85
86
3. VIEW
3.1 GRAPHS
3.2 LISTING
87
87
89
4. ANALYZE
4.1 STATISTICS
4.2 COMPARE TO STANDARD
4.3 COMPUTE SIZES
89
89
90
90
92
96
106
112
117
120
130
150
PN 7221940 Rev. A
iv
CHAPTER 1
INTRODUCTION
_____________________________________________________________________________________
CHAPTER 1
1.
MANUAL DESCRIPTION
1.1. SCOPE
This manual is intended to provide the user with all the information needed to
operate and maintain the LS 13 320 system safely and effectively within the
stated working range and conditions given in the Specifications section.
1.2. ORGANIZATION
This manual is organized into seven chapters covering the description of the
instrument, the theory of laser diffraction, and the major software functions.
Six appendices offer additional information regarding sample preparation,
statistics used in laser diffraction, troubleshooting, optical models, maintenance
of the optical bench, and sieve analysis. Additionally, this manual should be
used together with the sample module manual that you may have purchased
with the optical bench.
1.4. CONVENTIONS
!" The optical bench and sample modules are referred to as the Analytical
Module. The PC, keyboard, monitor and printer, etc., are all referred to
collectively as the computer.
!" Bold type letters like this Enter Sample ID represent menu or button
text appearing on the screen of the computer that can be selected with the
mouse or by keystrokes.
!" #"means click the mouse button. Unless the mouse has been
inverted for left-handed users, this will be the left mouse button.
PN 7221940 Rev. A
CHAPTER 1
INTRODUCTION
_____________________________________________________________________________
2.
SAFETY PRECAUTIONS
2.1. GENERAL
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.
PN 7221940 Rev. A
CHAPTER 1
INTRODUCTION
_____________________________________________________________________________________
!"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.
Never place a mirror or optical surface (other than the sample cell
assembly) into the optical axis of the system.
Do not place your hands or any object inside the optical bench as the
module is docking.
PN 7221940 Rev. A
CHAPTER 1
INTRODUCTION
_____________________________________________________________________________
Figure 4.1 Warning label on front cover of the instrument and on laser
cover
See Figure 4.2 for the certification label which is located on the back cover of
the instrument.
PN 7221940 Rev. A
CHAPTER 1
INTRODUCTION
_____________________________________________________________________________________
3.
3.1.
MECHANICAL
(1)
(2)
(3)
ELECTRICAL
(1)
(2)
CHEMICAL
(1)
Do not use any diluents that are not compatible with the specific
wetted of the sample module. Consult Beckman Coulter Inc. or
its local representative before using any chemicals not listed in
this manual.
(2)
(3)
(4)
FIRE
Many non-aqueous solutions are flammable. Where possible choose less
flammable alternatives.
PN 7221940 Rev. A
CHAPTER 1
INTRODUCTION
_____________________________________________________________________________
CAUTIONS
3.2.
MECHANICAL
(1)
(2)
CHEMICAL
(1)
(2)
WARMING UP
As with all sensitive electronic instruments, the LS 13 320
components achieve best performance once they have reached a
steady working temperature. This may typically take 15 minutes
from power up.
SOURCES OF ERROR
(1)
Sample dispersion
(2)
Air bubbles
(3)
Misalignment
(4)
Incorrect obscuration
(5)
(6)
(7)
PN 7221940 Rev. A
CHAPTER 2
INTRODUCING LS 13 320
_______________________________________________________________________________________
CHAPTER 2
1.
SYSTEM OVERVIEW
The Beckman Coulter LS 13 320, Figure 2.1, measures the size distribution of
particles suspended either in a liquid or in dry powder form by using the principles of
light scattering. This particle size analyzer provides reliable and reproducible results
for researchers, quality control laboratories, product and process control departments,
or anyone with the need to measure particle size distributions. The LS 13 320 consists
of an optical bench and five different sampling modules: the Universal Liquid
Module
Figure 2.1
(ULM), the Aqueous Liquid Module (ALM), the Tornado Dry Powder System (DPS),
the Micro Liquid Module (MLM). In addition, an AutoPrep station can also be used
in conjunction with the ALM. The LS 13 320 incorporates Beckman Coulters
patented PIDS (Polarization Intensity Differential Scattering) technology to provide a
dynamic range that spans from 0.04 to 2000 m. Figure 2.2 shows the PIDS
detectors.
Figure 2.2
PN 7221940 Rev. A
PIDS Detectors
7
CHAPTER 2
INTRODUCING LS 13 320
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The LS 13 320 is designed from conception to be fully compliant with the ISO
standard covering particle sizing by the laser scattering method (ISO/DIN
13320-1 Particle size analysis - Laser scattering methods - Part 1: General
principles). The LS 13 320 includes a sophisticated software package with a
multi-component Standard Operating Procedure (SOP). This multi-component
Standard Operating Procedure (SOP) will assist the operators to ensure their
analyses are the same run-after-run. Every element of the analysis from
method set-up to the final printout can be locked into a user-definable SOP.
The SOP routine is defined into two distinct components; an SOM (Standard
Operating Method) and a Preference file. The SOM covers all those aspects of
the analysis relating to the instrument settings. The Preference file (.prf)
covers data output and format.
2.
Detector
Particles
PN 7221940 Rev. A
CHAPTER 2
INTRODUCING LS 13 320
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The result is that the Fourier lens forms an image of the entire scattering pattern of
each particle, the image being centered at a fixed point on the Fourier plane. This
image is centered at the same fixed point regardless of the position or velocity of the
particle in the scattering sample cell.
The individual scattering patterns from the many moving particles in the sample cell
are superimposed, creating a single composite scattering pattern that represents the
contributions from all the particles in the sample cell. Detectors placed on the Fourier
plane record this composite scattering pattern. Over the course of a measurement, a
running average is created from the flux patterns. When the duration of the
measurement is long enough that the flux pattern accurately represents the
contributions from all particles, an analysis of the resulting pattern will yield the true
particle size distribution of the sample.
3.
4.
SYSTEM COMPONENTS
4.1.
PN 7221940 Rev. A
CHAPTER 2
INTRODUCING LS 13 320
_______________________________________________________________________________________
Figure 2.4
Figure 2.5
PN 7221940 Rev. A
10
CHAPTER 2
INTRODUCING LS 13 320
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Before a module can be docked the sample cell chamber door must be
retracted. This is easily done by pressing the Open button found on the left side
of the optical bench (figure 2.5)
4.2.
LIGHT SOURCE
The LS 13 320 uses a 5 mW laser diode with a wavelength of 750 nm as the
main illumination source and a secondary tungsten-halogen light source for
the PIDS system. The light from the tungsten-halogen lamp is projected
through a set of filters which transmit three wavelengths (450, 600, and 900
nm) through two orthogonally oriented polarizers at each wavelength.
Light from a laser diode is monochromatic, which is required by the
theoretical models that describe a particle's scattering function. However, as
opposed to helium-neon lasers, the light from a laser diode is not focused. The
monochromatic light from a laser diode must also be treated to produce a
'clean' beam. The device that is most often used to condition an illuminating
source is commonly known as a "spatial filter". A spatial filter is a set of
optical elements, - components such as lenses, pinholes, apertures, etc.,
designed to refine the beam to the desired quality. Figure 2.6 depicts a spatial
filter. A feature of the LS 13 320 is that it incorporates a patented fiber optic
spatial filter.
Figure 2.6
4.3.
SAMPLE MODULES
The main function of the sample-handling module is to expose particles in
the sample, without discrimination to their sizes, to the light but not to
introduce any undesirable effects such as air bubbles and/or thermal
PN 7221940 Rev. A
11
CHAPTER 2
INTRODUCING LS 13 320
_______________________________________________________________________________________
turbulence. The sample module is typically composed of the sample cell and
a circulation system. The circulation system may include certain features
such as a circulation pump, an ultrasonic probe, or stirring bars to help better
disperse and circulate the particles. The LS 13 320 operates with sample cells
designed for particles suspended in liquids or in dry powder form. These
modules are the:
In addition the ALM can be used in conjunction with the AutoPrep station.
4.4.
COMPUTER SYSTEM
For operation the LS 13 320 requires of a personal computer (PC) and the
PC-based control and analysis software.
If you are not using a Beckman Coulter-supplied PC, you must provide one
that meets the minimum configuration requirements shown on table 2.1, and
that preferably meets the recommended configuration requirements shown on
the same table.
Item
Microprocessor
RAM
Hard Drive
Monitor
Keyboard
Mouse
MS Windows Version
Minimum
Configuration
Pentium 166
64 Mb
1.2 Gb
800X600
Enhanced 101/102
2 Button
Win 98
Recommended
Configuration
Pentium III
64 Mb
5 Gb
1024X768
Enhanced 101/102
3 Button
Win 98 or better
SOFTWARE
The Microsoft Windows-based LS 13 320 control program provides
both hardware control and data management. Among other functions,
the program allows you to:
PN 7221940 Rev. A
12
CHAPTER 2
INTRODUCING LS 13 320
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PN 7221940 Rev. A
13
CHAPTER 3
OPERATION PRINCIPLES
_______________________________________________________________________________________
CHAPTER 3
1.
THEORETICAL BACKGROUND
1.1.
INTRODUCTION
The scattering of light is one of the most widely used techniques for
measuring the size distribution of particles. In practice, the technique is
fast and flexible, offering precise measurements that can be easily
adapted to samples presented to the analyzer in various forms. The
method involves the analysis (deconvolution) of the patterns of
scattered light produced when particles of different sizes are exposed
to a beam of light. The LS 13 320 series of instruments takes
advantage of these principle to rapidly provide precise and
reproducible particle size distributions.
1.2.
LIGHT SCATTERING
When light illuminates a particle having a dielectric constant different
from unity, depending on the wavelength of the light and the optical
properties of the particle, light will be scattered in a unique way. We
commonly describe scattering phenomena in terms of diffraction,
reflection, refraction, and absorption. When light interacts with the
electrons bound in the material that re-radiate light, scattering is
observed. Because most materials exhibit strong absorption in the
infrared and ultraviolet regions which greatly reduces scattering
intensity, most light scattering measurements are performed using
visible light of wavelengths from 350 nm to 900 nm. The scattering
intensity from a unit volume that is illuminated by a unit flux of light is
a function of the complex refractive index ratio between the material
and its surrounding medium. This intensity falls within the regime of
Rayleigh scattering and is inversely proportional to the fourth order of
the light wavelength, i.e., the shorter the wavelength, the stronger the
scattering. The reason that the sky is blue at midday and red at sunrise
or sunset is that one sees the scattered sunlight during daytime and sees
the transmitted sunlight during dawn and dusk. The blue color of the
ocean can also be attributed in large extent to the strong scattering of
the short wavelength portion in the sunlight. The deeper the water
level, the deeper the blue color becomes because of the reduced
scattering from the longer wavelength portion of the sunlight. Utilizing
this wavelength dependence, we use red as the color for the stoplight
and for all traffic control warning signs because red light has the least
scattering power in the visible light spectrum. This allows the
transmitted light to go through fog, rain, and dust particles and reach
the intended detector: in this case the human eye.
PN 7221940 Rev. A
14
CHAPTER 3
OPERATION PRINCIPLES
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PN 7221940 Rev. A
15
Iv
CHAPTER 3
OPERATION PRINCIPLES
_______________________________________________________________________________________
-9 0
-6 0
-3 0
30
60
90
S c a tte r in g A n g le
PN 7221940 Rev. A
16
CHAPTER 3
OPERATION PRINCIPLES
_______________________________________________________________________________________
sin =
1.22*
d
eq.(3.1)
PN 7221940 Rev. A
17
CHAPTER 3
OPERATION PRINCIPLES
_______________________________________________________________________________________
V E R T IC A L
P O L A R IS A T IO N
H O R IZ O N T A L
P O L A R IS A T IO N
Since the PIDS signal is dependent on particle size relative to the light
wavelength, valuable information about the particle size distribution
can be obtained by measuring the PIDS signal at a variety of
wavelengths.
2.
PIDS SIZING
As mentioned above, with its patented PIDS assembly the LS 13 320 can
provide information about particles smaller than 0.4 microns. Particles in this
range offer limited information in diffraction patterns, so the PIDS
technology is required to accurately measure these small particles.
2.1.
COMPONENTS
The PIDS assembly consists of:
PN 7221940 Rev. A
CHAPTER 3
OPERATION PRINCIPLES
_______________________________________________________________________________________
2.2.
FUNCTIONS
The PIDS assembly functions are:
2.3.
DESCRIPTION
The PIDS assembly provides the primary size information for particles in the
0.04 m to 0.4 m range. It also enhances the resolution of the particle size
distributions up to 0.8 m. This additional measurement is needed because it is
very difficult to distinguish particles of different sizes by diffraction patterns
alone when the particles are smaller than 0.4 m in diameter.
The PIDS assembly in the Optical Module uses an incandescent tungstenhalogen lamp and three sets of vertically and horizontally polarized filters to
provide polarized monochromatic light at three different wavelengths: 450 nm
(blue), 600 nm (orange), and 900 nm (near-infrared, invisible). The light is
focused through a slit and is formed into a narrow, slightly diverging beam
that is projected through the PIDS sample cell.
The PIDS assembly measures the pattern of the difference in scattering of
vertically and horizontally polarized light. To obtain as much information as
possible about the small particles measured by the PIDS assembly, it
illuminates the particles sequentially with vertically and horizontally polarized
light of the three different wavelengths (colors). The three wavelengths of light
permit three independent measurements of the PIDS effect at different ratios of
particle sizes to light wavelength
For each of the three wavelengths, the differential scattering pattern (PIDS
pattern) is observed at six detectors (figure 2.2) centered at a scattering angle
of about 90. In total, the PIDS assembly makes 36 measurements of the light
scattered from the sample: scattered light of two polarizations at three
wavelengths and six scattering angles (2 x 3 x 6 = 36). A seventh detector on
the opposite side of the cell from the light source measures the intensity of the
PN 7221940 Rev. A
19
CHAPTER 3
OPERATION PRINCIPLES
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PN 7221940 Rev. A
20
CHAPTER 4
LS 13 320
INSTALLATION AND VERIFICATION
_______________________________________________________________________________________
CHAPTER 4
1.
INTRODUCTION
2.
ENVIRONMENT
For best performance of the LS 13 320, find a site that is:
Well ventilated.
Smoke free.
2.2.
POWER REQUIREMENTS
21
CHAPTER 4
LS 13 320
INSTALLATION AND VERIFICATION
_______________________________________________________________________________________
Power Category
Requirement
50/60
720 Maximum
Table 4.1
Figure 4.1
2.3.
PN 7221940 Rev. A
22
CHAPTER 4
LS 13 320
INSTALLATION AND VERIFICATION
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2.4. MODULES SPECIFIC REQUIREMENTS
______________________________________________________
!" Be sure that the product being sized and the suspension fluid do not
3.
PN 7221940 Rev. A
23
CHAPTER 4
LS 13 320
INSTALLATION AND VERIFICATION
_______________________________________________________________________________________
Computer
Interface Cable
Figure 4.2
4.
5.
Port - accept the current setting or check the radio button, $, to select a
different communications port.
Baud Rate verify that the speed is set to 19200 Baud. If another speed is
PN 7221940 Rev. A
24
CHAPTER 4
LS 13 320
INSTALLATION AND VERIFICATION
_______________________________________________________________________________________
Figure 4.3
6.
POST-INSTALLATION VERIFICATION
To verify the performance of your LS 13 320, a Beckman Coulter control
sample must be analyzed. The acceptable limits are listed on the assay sheets
enclosed with the control samples.
6.2.
DAILY VERIFICATION
We recommend that a control sample be run daily to verify your instruments
performance. Calibration is determined by the optical design. Therefore, no
calibration is required. Measuring electrical offsets and aligning the laser beam
makes all necessary adjustments.
PN 7221940 Rev. A
25
CHAPTER 4
LS 13 320
INSTALLATION AND VERIFICATION
_______________________________________________________________________________________
7.
GETTING STARTED
The PC software has been designed to control all the operations of the LS 13
320. Once the instrument and its corresponding module have been set up and
the software installed, click on the program icon to launch the program.
When starting up the instrument after it has been shut down, allow the
instrument to warm up for approximately 20 minutes.
7.1.
#%OK launches the control program. Figure 4.4 shows the status
screen after selecting OK from the above screen.
PN 7221940 Rev. A
26
CHAPTER 4
LS 13 320
INSTALLATION AND VERIFICATION
_______________________________________________________________________________________
Figure 4.4
The status screen shown in figure 4.4 allows you to select the security level
you wish to use. For more on security levels refer to Chapter 5.
7.2.
SELECTING A MODULE
The optical module is automatically recognized by the optical bench when the
module is docked into the optical bench.
1.
27
CHAPTER 4
LS 13 320
INSTALLATION AND VERIFICATION
_______________________________________________________________________________________
Figure 4.6
Figure 4.7
PN 7221940 Rev. A
Ready screen
28
CHAPTER 4
LS 13 320
INSTALLATION AND VERIFICATION
_______________________________________________________________________________________
8.
MAKING MEASUREMENTS
In order to obtain the light intensity patterns (diffraction or PIDS) described in
previous chapters, from which the size distribution is calculated, a number of
functions have to be performed by the instrument. These are explained below in the
order they are completed during a complete run cycle.
Measuring Offsets
With the laser off, the offset or bias voltages of the amplifier circuit are measured in
order to 'zero out' (or establish a baseline of any electrical noise) at a detector
channel. This is necessary because the signal at a detector channel (a detector
channel consists of a light sensitive detector surface and the associated amplifying
electronics) does not necessarily go to zero in the absence of light. Therefore, to
accurately measure the light intensity the offset voltage must be measured and
subtracted from the scattering signal from the sample.
Alignment
During this step the laser beam is automatically aligned at the center of the detector
array. In order to accurately measure the light intensity as a function of scattering
angle, the laser beam must be precisely positioned. In the LS 13 320, the laser beam
is aligned within 1-2 microns of the center of the detector array on the horizontal and
vertical axes.
Measure Background
Here the light intensity levels received by the detectors are measured with no sample
in the system, and then subtracted out. This procedure eliminates the signal due to the
outer edges of the Gaussian laser beam, in addition to any light leakage or scattering
from dust on the lenses or any other particulate present in the optical path. The
background should always be measured prior to adding sample to the system.
Measure Loading
This function measures the amount of light scattered out of the beam by the particles
so as to determine an appropriate concentration of sample. Enough sample is needed
to provide an acceptable signal-to-noise level in the detector channels, but if too many
particles are present, light already scattered from one particle will be likely to scatter
from another, blurring the light intensity pattern. The obscuration reported on the title
bar of the run window is the percentage of light scattered out of the beam by the
particles. When sizing particles without using PIDS an obscuration level of 8% to
12% is appropriate, except when using the Dry Powder Module in which case an
obscuration of 4% to 7% is sufficient. When PIDS is used, a PIDS obscuration of
40% to 60% is recommended.
PN 7221940 Rev. A
29
CHAPTER 4
LS 13 320
INSTALLATION AND VERIFICATION
_______________________________________________________________________________________
8.1.
Sample Module
Universal Liquid Module (ULM)
Aqueous Liquid Module (ALM)
Tornado Dry Powder
Micro Liquid Module
Table 4.2
Control
Latron 300LS, G15, GB 500
Latron 300LS, G15, GB 500
G35D
G15
1. #%Run followed
2. #%Run Cycle as shown in figure 4.9
Figure 4.9
3.
#% New Sample and select the PIDS dialog box (see figure 4.10) if your
measurement is to include particles below 0.4 m (ULM and ALM only).
PN 7221940 Rev. A
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CHAPTER 4
LS 13 320
INSTALLATION AND VERIFICATION
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4.
Figure 4.11
PN 7221940 Rev. A
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CHAPTER 4
LS 13 320
INSTALLATION AND VERIFICATION
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Figure 4.12
PN 7221940 Rev. A
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CHAPTER 4
LS 13 320
INSTALLATION AND VERIFICATION
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Figure 4.15
5.
Complete the sample and run information dialog boxes with the pertinent
information.
PN 7221940 Rev. A
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CHAPTER 4
LS 13 320
INSTALLATION AND VERIFICATION
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Figure 4.16
RUNNING A SAMPLE
Once the performance of the instrument has been confirmed to be
correct by an analysis with a control (section 4.8.1), a sample can then
be analyzed. The validity of the results from an unknown sample is
based on the good performance of the instrument, as supported by the
control analysis, and by the correct preparation of the sample in
question. See appendix 2 for more information on sample dispersion
and preparation. The steps to follow to analyze a sample are similar to
those used to analyze a control sample.
1. #% Run followed by #% Run Cycle figure 4.9.
2. Under Run Cycle select New Sample. If PIDS is to be used click
on the Include PIDS data check box to activate this option.
Select Run Settings figure 4.10.
3. In the Run Settings screen (figure 4.16) choose 60 seconds for the
Run Length. When using PIDS select 90 seconds for the Run
Length. Under After each run click on the Compute Sizes and
Save File check boxes. Select the Model (figure 4.17) option and
choose the correct optical model. If the optical model you need is
not found in the list of optical models, you may create a new one
PN 7221940 Rev. A
34
CHAPTER 4
LS 13 320
INSTALLATION AND VERIFICATION
_______________________________________________________________________________________
that will suit your particular sample (See Appendix 3 Optical Models).
4. #% OK
5. #% Start
6. From this point on the sequence of steps is the same as described in the
previous section Running a Control.
Figure 4.17
As with controls, the sample analysis steps can be simplified through the use of
Standard Operating Methods and Procedures (see your specific sample module
manual for more information).
PN 7221940 Rev. A
35
CHAPTER 5
LS 13 320
SOFTWARE MENUS
_______________________________________________________________________________________
CHAPTER 5
INTRODUCTION
The following section will provide a guide to the main menus in the LS 13 320
software.
1. FILE
New
Open
PN 7221940 Rev. A
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CHAPTER 5
LS 13 320
SOFTWARE MENUS
_________________________________________________________________________________________
Open Overlay
Average
Create Size
Trend
PN 7221940 Rev. A
The Create Size Trend command allows you to view and print
sequences or groups of analyses in a single graph. It provides a
graph/listing of a chosen sample statistics across sample files. For
example, the Create Size Trend command allows you to view
37
CHAPTER 5
LS 13 320
SOFTWARE MENUS
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PN 7221940 Rev. A
38
CHAPTER 5
LS 13 320
SOFTWARE MENUS
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In the Size Trend graph, lines may be included to represent the mean
or nominal value, and upper and lower limits, and define lables for
these lines.
Import Size
Data
PN 7221940 Rev. A
Select Import Size Data to import data generated by the software that
is in file format of types txt or XLS. To convert these types of data
files, click on the File menu and then on Import Size Data. Next,
type the file name in the space provided or select the file of interest in
the Open for Import dialog box. Using file names with a 3-character
extension beginning with the symbol $ is recommended when
saving imported data as files that can be automatically recognized by
the LS 13 320 program.
39
CHAPTER 5
LS 13 320
SOFTWARE MENUS
_______________________________________________________________________________________
In the the dialog box (see next figure) select the first and last lines that
include all the data of interest followed by the channel sizes and data.
(Thereafter information can be ignored).
Change
Directory
The Change Directory command can be used to locate data files stored
elsewhere on your computer.
Create
Directory
The Create Directory command displays a dialog box that allows you to
create a blank folder/directory for the storage of new or renamed data files.
Print Reports
PN 7221940 Rev. A
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CHAPTER 5
LS 13 320
SOFTWARE MENUS
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2. WINDOW
Copy Window
Cascade
Tile-Horizontal
Tile-Vertical
Minimize All
Restore All
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LS 13 320
SOFTWARE MENUS
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3. RUN
The Run menus will become active once the the Optical
Module docked into the Optical Bench.
Run Cycle
PN 7221940 Rev. A
The Run Cycle menu allows you to set all the parameters necessary to
perform an analysis on a sample. Within this menu the selection of the
PIDS data option is found as well as Measure Offsets, Align,
Measure Background, and Measure Loading. These options are
explained in detail in section 4.8; Making Measurements.
42
CHAPTER 5
LS 13 320
SOFTWARE MENUS
_________________________________________________________________________________________
Run Cycle
Options
This option allows the user to set up the parameters to perform the
offset, alignment, and background measurements that will be used
under the Run Cycle menu described above.
Create SOM
PN 7221940 Rev. A
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LS 13 320
SOFTWARE MENUS
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Enter Sample
Info
This dialog box allows you to enter all the pertinent information about the
sample to be analyzed. The sample statistics, fluid (diluent), and file name
format can also be edited from this dialog box.
Make Optical
Model
File Name
Generation
The file name generation dialog is used to set the way that file names can be
created and saved. File name generation is used only when creating a new
file. Existing file names cannot be edited using this option.
PN 7221940 Rev. A
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CHAPTER 5
LS 13 320
SOFTWARE MENUS
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4.
PREFERENCES
Preference files define the default settings for data presentation, the appearance of
the program window, the format for reports, etc.
At any time, you may change any of the settings in the dialog boxes accessed by
commands in the Preferences menu. Some of these changes will take effect
immediately, others only when a result file is re-opened. If the preferences file is
saved, all the changes made will become part of that particular preferences file and
will take effect any time that the preferences file is loaded.
Printed
Report
The Printed Report option displays a dialog box that specifies the content of
printed reports. This function allows you to choose any combination of the
following report elements to be included in your printout:
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Size
Provides a graphical display output selected from the Size
Graphs option
Statistics selected in the Size Statistics option or by clicking
the corresponding dialog box under Size Statistics
Averaged Statistics selected statistics computed by the file
averaging function
Compare Statistics comparison with a previously defined
standard data file
Listing data presented in a tabular format
Interpolation analysis using user-selectable channel
boundaries
Trend Graph trend data in a graphical display format
Trend Listing trend data in a tabular format
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Sieve presents the size data (listing or graph) using sieve format by
either mesh size of mesh number.
Auto Print instructs the LS 13 320 program to automatically print
the report elements selected in the Report Preferences dialog box
each time an analysis is completed.
Size Graphs
Size Listings
This option displays the Size Graphs dialog box. Your first selection
determines the default format for the graph display format. Additional
selections determine the other types of graphical presentations to be included in
your report. Up to 12 distribution types may be selected in the desired printing
order. Both the X-axis and Y-axis can be displayed using a log or a linear scale.
The Size Listing Preferences dialog box allows you to customize tabular data
presentations by selecting specific listing information and designating column
sequence for quick output to the printer.
Make your selections by clicking the desired option boxes; click again to
deselect. Up to 7 categories of information may be included in tabular data
output.
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Size Statistics
The Size Statistics option is used to define the distribution and statistic
type used. It is also useful in defining which percentiles and statistics
appear on the size statistics report and when selecting the Analyze
menu followed by the Statistics option from the individual run file
menu.
Size
Interpolation
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activate the Differential (Diff) radio button. This section also determines
whether data are displayed as a cumulative percentage of values either above or
below user-defined percentile values.
Sieve
The sieve dialog offers the option of preseting the size data in a format that
allows comparison of data obtained with that from sieves.
The sieve option allows you to show a Sieve Graph, Sieve Listing, as well as
Define Mesh Sizes. The Sieve Graph option allows you to select up to 12
different graphs by distribution type. Use this function to define which sieve
graphs are printed and their printing order. The first graph type appearing in the
Graph Printing Order list box defines the initial appearance of the sieve data
when it is displayed.
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The Define Mesh Sizes option can be used to define other sets of
sieve sizes, which can be either subsets of one of the provided sets, or
entirely new sets with different diameter values and identifying mesh
numbers. In addition, Mesh Weighting factors can be used to correlate
the LS 13 320 data more closely with the data obtained by sieving. If
the particle size distributions are viewed in sieve format without
weighting factors, the volume distribution is simply interpolated at the
points corresponding to the sieve sizes. The size data obtained,
however, will be slightly different from data obtained with sieves due to
the diffeence in methodologies.
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To meaningfully correlate LS 13 320 size data to sieve data using the mesh
weightings, you must first have a database of LS 13 320 and sieve data for a
given material. A statistically significant number of pairs of data sets, such as 20
or more, should be obtained. That is, you should have an LS 13 320 run and a
sieve run for each of 20 samples of the same material. Then obtain two
averages, one for the sieve data and the other for the LS data (use the LS 13 320
program's file averaging feature for the LS 13 320 data, see Working with Run
Files, Chapter 13). The data set from the LS should be viewed in sieve format,
using the same nominal sieve sizes as they are used in the siever. To create this
sieve set:
1. Select Preferences, Sieve, Define Mesh Sizes.
2. For each sieve used, enter Diameter and Mesh # and select Create.
3. Highlight any meshes not used in your correlation and select
Delete for each one.
4. Select OK.
Note: Do not exit the program before saving a preferences file or the sieve set
just created will be lost.
Trend
Size Trend Analysis allows you to view and print sequences or groups of
analyses in a single graph. A statistical analysis, such as the mean, can be
plotted versus time of analysis, date of analysis, or several other choices.
Two options in the Preferences menu determine what information is included
in the trend reports and listings. The Grpah option allows you to select the
variables to be displayed on the X and Y axes.
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The Listing option allows you to select the column headings for the
Trend Listing report.
Result Options
Averaging and
Size Trend
Result Options will allow you to select the units of measure in which
the data will be reported i.e., m3 for volume. The Default View option
under this menu lets you choose the type of analysis to present (size,
sieve, etc.) in a graph, listing, or interpolation form.
Displays the Averaging and Size Trend dialog box, which may be
used to select the type of measure to use, distribution type, and trend
limits type. It allows file names printed with their full path, and an
option to add data from other averaged or trend files.
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Data Export
Choices in the Data Export dialog allow the user to specify which subsections
of the runfile (e.g., the sample info, statistics, etc.) will be exported. An
extension, such as .xls, may be entered so that another application will
recognize the exported data. Numeric formatting options are also included in
the Data Export dialog.
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Preference
Files
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5.
SECURITY
The Security options allow the software to be configured for 21 CFR part 11 compliance.
This option also permits the operation of the software with some degree of security to be
able to keep the integrity of the data being acquiered by the instrument and stored in
electronic form. This is done by selecting different levels of security, from no security to
high security, from the Security Set-up dialog box shown below.
The Security Set-up box is accessible when the program is first started after installation.
Once a security level is set-up it cannot be changed to a different level. Eventhough the
level cannot be changed, different settings are accessible through the User Priviledges
options which is accessible only by the administrator. These security options can also be
selected at a later time. If you want to set up the security levels at a later time refer to
Chapter 6 for more information.
1.
2.
#%
% OK
3.
The Add a User Account dialog box is displayed. The Full Name, Log-in
Name, and Password are required fields.Select the Type of user.
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4.
5.
After an acoount has been set up, the user must exit the LS 13 320 software
program. Upon re-entering the program and logging-in, the user will be prompted
to change his/her password.
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Note that the Log-in dialog box will automatically close after 60 seconds
of inactivity.
The security set-up scheme on the next page summarizes the steps when setting
up a security level
5.1.
TYPES OF USERS
Under the security options there are different types of users with different levels
of priviledges. Depending on the user type, menu screens will change providing
each user with a range of menu options that can be used to set the operation and
security of the software.
5.1.1. ADMINISTRATOR
The administrator has control over every aspect of the settings of the
software and controls and sets the priviledges for each user. Only the
administrator can set-up accounts as well as user names and passwords.
The figure below shows the menus accessible by the administrator when
logged-in in Administrator Mode.
Select Security
2.
3.
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SECURITY SET-UP
Security
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The following section describes the options under the administrator pull
down menu
User Priviledges
Selecting User Priviledges displays. a dialog box containing all
the options needed to set up the different priviledges for each user.
The options on the left hand side column deal with the creation and
saving of methods (SOMs, SOPs) as well as changing and saving
preferences. The right hand side column deals with file operations.
Under the User Priviledges dialog box you may also select the
User Settings button to access the User Names and Passwords
dialog box. The entire Login process is controlled via the user
names and passwords dialog. This ensures that the system login is
controlled via time dependant metrics, such as password expiry
and dialog inactivity, and has the required password lengths. Select
the options in the dialog box and #%
%OK.
Note that the dialog has a button marked 21 CFR 11. When activated this
ensures all options are set so that the settings meet with the rules as
applicable to 21 CFR part 11. Refer to Chapter 6 for more information.
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5.2.
NO SECURITY
By selecting No Security, there is no need for log-in IDs or passwords.
Any user can make changes to data files without the need for signatures.
The operator may also create Standard Operating Methods (SOMs) and
Standard Operating Procedures (SOPs).
Access to all the administrator options are also available where changes
can be made to any of the options provided, i.e. Audit Trail Settings.
The editing of files will still be tracked with the Audit Trail and reported
in the File History.
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LOW SECURITY
Low security requieres an administrator to set up accounts for other users.
A full name, log-in name and password are required as well as the type of
user.
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Select Security.
2.
3.
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4.
After filling in the dialog boxes with the proper information and
selecting OK, you will be prompted to add a user account. If OK
is selected, the Add a User Account screen is displayed again.
Refer to Chapter 6 for more information on High Security level and 21 CFR Part 11
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5.4.
MEDIUM SECURITY
As with low security, Medium Security requieres an administrator to set
up accounts for other users. The User Priviledges dialog screen default in
the medium security setting is set so that all users are requiered to log in,
but only the administrator and supervisor need a password.
These options can be changed by selecting the option boxes for each user
under the the User Priviledges dialog screen shown below.
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REGULATORY COMPLIANCE
1. 21 CFR PART 11
The Electronic Records and Electronic Signatures Rule (21 CFR Part 11) was
established by the FDA to define the requirements for submitting documentation in
electronic form and the criteria for approved electronic signatures. This rule, which
has been in effect since August 20, 1997, does not stand in isolation; it defines the
standards by which an organization can use electronic records to meet its recordkeeping requirements. Organizations that choose to use electronic records must
comply with 21 CFR Part 11. It is intended to improve an organizations quality
control while preserving the FDAs charter to protect the public. Since analytical
instrument systems such as the LS 13 320 generate electronic records, these systems
must comply with the Electronic Records Rule.
Here are described the relevant portions of the 21 CFR Part 11 regulations and their
implementation using the LS 13 320 control software explained. It is important to
realize that Implementation and compliance of the rule remains the responsibility of
the organization or entity creating and signing the electronic records in question.
Proper procedures and practices, such as GLP and GMP, are as much part of overall
compliance with these regulations as are the features of the LS 13 320 control
software.
2. ELECTRONIC RECORDS
Section 11.3 subpart A of 21 CFR Part 11 deals with the definitions assigned to
electronic records, electronic record means any combination of text, graphics, data,
audio, pictorial, or other information representation in digital form that is created,
modified, maintained, archived, retrieved or distributed by a computer system. In
reality this refers to any digital computer file submitted to the agency, or any
information not submitted but which is necessary to be maintained. Public docket No
92S-0251 of the Federal Register (Vol.62, No 54) identifies the types of documents
acceptable for submission in electronic form and where such submissions may be
made.
3. FDA REQUIREMENTS
In the general comments section of the ruling the following is stated: The agency
emphasizes that these regulations do not require, but rather permit, the use of
electronic records and signatures. In the introduction to the final ruling the following
statement is made The use of electronic records as well as their submissions to FDA
is voluntary.
If electronic submissions are made, Section 11.2 subpart A comes into play: persons
may us electronic records in lieu of paper records or electronic signatures in lieu of
traditional signatures.provided that: (1) The requirements of this part are met; and
(2) The document or parts of a document to be submitted have been identified in
public docket No. 92S-0251.
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The LS 13 320 control software have been designed to allow users to comply
to the electronic records and signatures rule. Any organization deciding to
employ electronic signatures must declare to the FDA their intention to do so.
4. IMPLEMENTATION
OF
ELECTRONIC
ELECTRONIC SIGNATURES
RECORDS
AND
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After all accounts have been set up, exit the LS 13 320 software
program. Upon re-entering the program and logging-in, the user will
be prompted to change his/her password.
6. Select User Privileges.
The User Privileges dialog box is already configured for 21 CFR Part
11 compliance. This dialog box is covered in more detail in Chapter
5 Section 5.1.
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User Privileges dialog box: High Security (21 CFR Part 11)
6.1.1.
The LS 13 320 software also performs data input and "operational checks",
as specified in Subpart B, Section 11.10, "to determine, as appropriate, the
validity of the source of data input or operational instruction", and "to
enforce permitted sequencing of steps and events". These two features
ensure that, as much as possible, valid data are being entered into the
system, and all required steps have been completed to perform the task at
hand.
The purpose of all such data checking and validation is described in Section
11.10, Paragraph (b): "The ability to generate accurate and complete copies
of records in both human readable and electronic form suitable for
inspection, review, and copying by the agency". Consequently, strict
procedures can be enforced within the LS 13 320 software system to record
all changes that are made to data generated from within LS 13 320 software,
as defined in Section 11.10, Paragraph (e).
Any file created by the LS 13 320 software can have a File history or
auditing enabled. Once auditing has been enabled for a file, it cannot be
disabled, nor can it be bypassed. Under these conditions, all changes made
to a file are automatically recorded. These changes consist of "computergenerated, time-stamped audit trails to independently record the date and
time of operator entries and actions that create, modify, or delete electronic
records". When a change to a file is detected, the LS 13 320 software
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automatically records the identity of the user making the change, the
date and timestamp of the change, the parameter that has changed,
the old value and the new value. The user is also required to re-sign
the record electronically and enter a reason for the change, from a
pre-defined list or as free text.
This audit trail is then stored as a File History within the file itself,
such that "record changes shall not obscure previously recorded
information", and in a "form suitable for inspection, review, and
copying by the agency". This ensures that a complete and continuous
record of all changes to the file is maintained. Through the file
protection and archiving capabilities of the LS 13 320 software, it
can be ensured, in compliance with Section 11.10, Paragraph (e),
that "Such audit trail documentation shall be retained for a period at
least as long as that required for the subject electronic records".
To access the File History information:
#%
%Run File and select Get File History
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Open a file
2.
#%Edit
3.
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DATA MIRRORING
The administrator has the option to securely store files in a separate location
and in addition to that specified by a user. This is done by enabling the data
mirroring option that can only be accessed under administrator mode.
1. From the Administrator mode, select User Privileges
2. Select Data Mirroring
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FILE ATTRIBUTES
Files can be protected to varying degrees using the File Attributes
options.
The File Attributes allow you to select a specific file and make it a
read-only file, hide it, etc. You can also show it as a normal file or as
a hidden file only.
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CHAPTER 7
INTRODUCTION
The following section will guide you through the menus that deal with acquired
data.
1. RUNFILE
1.1.
Unlike the File Overlay command, the Open for Overlay command will allow
you to open one file at a time, but you can still overlay up to 30 files.
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1.2. SAVE
If a file has been modified (edited) it has to be saved in order for the
changes to take effect. These changes will be recorded in the File
History and, if working under a high security level, a reason for any
change must be provided. After selecting Save, the following dialog
box is displayed:
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1.3. EXPORT
The Export option allows you to send selected information about a file
to, for example, an Excel spreadsheet, and to any directory using the
file name with a .csv (comma separated value) or other extension.
#%
%RunFile
#%
%Export
Select the options you want to
export
4. Select an option from the
Export to dialog. Make sure
youre exporting to the desire
directory using the .csv
extension
5. #%
%Export
6. If you do not wish to export
your file as a .csv file, select
Settings
1.
2.
3.
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2. EDIT
No security
COPY WINDOW
This command will place the information displayed in the LS 13 320 window
onto the clipboard.
2.2.
Note from the first figure that the edit options change depending on whether
you selected a level of security or not. Under No Security any user can edit the
data file. For Low Security the operator and reviewer may edit data only if the
administrator selects the options under the user privileges dialog. Medium
security does not allow either the operator or reviewer to edit data. For high
security see chapter 6.
2.3.
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Selecting Edit Size Results will lead you to the following dialog
screen:
Select the options you wish to use during the editing and click OK. The
following screen is displayed:
The Edit Size Results option allows you to add or delete data points
from the distribution. The Auto Step option allows you to create size
classes by either adding or multiplying a value entered in the Auto Step
dialog field.
2.4. ADD AN ELECTRONIC SIGNATURE
The addition of an electronic signature is controled by the security level
being used. Under No Security, electronic signatures are not required.
Low Security, offers the option of allowing the administrator to add an
electronic signature. Medium Security permits the administrator and
supervisor to enter an electronic signature. Under High Security every
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user, except for the reviewer, are expected to add an electronic signature
whenever a file is edited. See Chapyer 6, section 6.1.4 for more information on
electronic signatures.
3. VIEW
The View command allows you to
set up different options to set up the
way the data is presented on your
computer screen. This format can
also be printed as it appears on the
screen from the RunFile, Print
commands. The data can be
displayed in graphical form, by
listings, or by showing a set of
interpolation points.
3.1.
GRAPHS
Graphs of data can be diplayed in different formats. The figures below are
examples of a type of graph format, a listing, and interpolation.
The graph options are selected from the Graph menu as shown in the next
figure.
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2.
Point the arrow between two cursors and press the right button of
the mouse.
3.
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3.2. LISTING
The listing options are shown in the following figure.
The options selected will be displayed in tabular form with the first column being the
the first option selected.
4. ANALYZE
4.1. STATISTICS
See Appendix III, Statistics, for definitions of statistics used in the LS 13 320 program.
To view the statistics for the active run file:
1.
2.
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3.
4.
To view the statistics for only part of the size distribution, add
cursors around the distribution, and repeat steps 1 to 3.
2.
Select the optical model needed. If the optical model is not shown
in the list, select New Model. For more on optical models see
Appendix IV.
3.
Select OK.
4.
Wait while the optical model is loaded and the sizes are computed.
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5.
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LS 13 320
SYSTEM SPECIFICATIONS
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APPENDIX I
PHYSICAL SPECIFICATIONS
Power
100 10 V, 120 10 V, 220 20 V, or 240 20 V
50/60 Hz
6A
Temperature
10 to 40C (50 to 104F)
If room temperature varies 2C/hour, perform alignment and
offsets tests more often, at least once an hour.
Humidity
0 to 90% without condensation
Dimensions
Unit
Optical Module
Computer Processor
with Disk Drive
Monitor
Printer
Height
44.5 cm
17.5 in.
13 cm
5 in.
32 cm
12.5 in.
23 cm
9 in.
Width
101 cm
40 in.
36 cm
14 in.
32 cm
12.5 in.
39 cm
15.5 in.
Depth
25.4 cm
10 in.
41 cm
16 in.
41 cm
16 in.
41 cm
16 in.
Altitude
Sea level to 3,000 m (10,000 ft)
Laser
Classification
I for operatior (no access to radiation)
IIIb for service and maintenance (trained Coulter personnel only).
Laser Power
5 mW
4 mW operating power
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Wavelength
750 nm
Life Expectancy
70,000 hours
PIDS Lamp
Type
Tungsten-halogen
Ratings
6.0 V, 1.7 A, 10 W
Output
150 lumens at 2,900 K
Life Expectancy
2,000 hours
Particle Sizing
Range
Aqueous Liquid Module and Universal Liquid Module
0.04 m to 2000 m
Micro Volume Module and Tornado Dry Powder System:
0.4 m to 2000 m
Size Channels
Micro Volume Module and Tornado Dry Powder System: 92
Aqueous Liquid Module and Universal Liquid Module: 116
Repeatability
1% about mean size (repeat runs of the same sample)
Run Time
1 to 999 seconds (30 to 90 seconds typical)
Sample Requirement
All quantities will vary considerably depending on material density and
particle size distribution
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Offset in millivolts
Listings, Size
Graphs, Intensity
Offset in millivolts
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Graphs, Size
Calibration
None
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APPENDIX II
SAMPLE PREPARATION
1. LIQUID AND SOLID MATERIAL HANDLING
The probability of obtaining a sample, which perfectly represents the parent
distribution, is remote. For example, when powder is poured into a heap, size
separation or partitioning occurs with the fine particles located at the center
of the heap. Also, when a container of powder is subjected to vibration the
fine particles percolate through the coarse particles. As a result, it is not a
good practice to just scoop off a small sample and attempt to predict the
properties of the bulk from an examination of that sample. In addition, fine
powders suspended in a liquid medium often tend to partition, meaning that
larger particles will migrate downward while smaller particles remain in
suspension. The viscosity of the liquid plays a key role in the rate that
particles migrate through a medium. Thus, although sample handling is only
one step in the overall process of characterizing the size distribution of a
sample, care in performing this step will lead to a good representative
distribution of the sample when the sizing is performed.
1.1. Liquid Sample Handling
The sampling of powders suspended in a liquid medium that is not
homogenous requires the use of rotational devices such as rollers,
magnetic stirrers, tube rotators and manual inversion, aspiration with a
pipette, etc. These external devices are generally used to keep particles in
suspension while attempting to draw a measurement sample. The most
common method is the use of a magnetic stir bar in a glass beaker
containing the sample and drawing liquid with a pipette as the stir bar
rotates. Even though these techniques are effective in obtaining a good
representative sample from liquid, the overall sampling for powder
samples will be representative only when the solid sampling, which is
performed before the powder is suspended, is performed correctly.
1.2. Solid Sample Handling
The sampling of powders is an important issue because a sample must be
taken through a reduction process from bulk stage down to a
measurement stage, which must be a good representation of the bulk
sample. Clearly before any sampling is performed the bulk material must
be well mixed.
Stationary non-flowing materials, composed of fine cohesive powders,
sticky materials, moist materials, or fibrous solids, do not have a
tendency to segregate but may not be uniform. Hence it is quite necessary
to pass these materials through a mixer before storage. Surface sampling
PN 7221940 Rev. A
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APPENDIX II
LS 13 320
SAMPLE PREPARATION
_______________________________________________________________________________
97
APPENDIX II
LS 13 320
SAMPLE PREPARATION
__________________________________________________________________________________
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APPENDIX II
LS 13 320
SAMPLE PREPARATION
_______________________________________________________________________________
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APPENDIX II
LS 13 320
SAMPLE PREPARATION
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100
APPENDIX II
LS 13 320
SAMPLE PREPARATION
_______________________________________________________________________________
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101
APPENDIX II
LS 13 320
SAMPLE PREPARATION
__________________________________________________________________________________
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102
APPENDIX II
LS 13 320
SAMPLE PREPARATION
_______________________________________________________________________________
Steric Stabilization
Best in organic solutions. Can be anionic, cationic,
or nonionic dispersants or block copolymers.
Optimum structure has anchor region that adsorbs
strongly on the organic solid (example: alkane
chains, aryl groups), and another region that is
highly soluble in the liquid (example:
polyethyleneoxide chains are soluble in water).
PN 7221940 Rev. A
103
APPENDIX II
LS 13 320
SAMPLE PREPARATION
__________________________________________________________________________________
104
APPENDIX II
LS 13 320
SAMPLE PREPARATION
_______________________________________________________________________________
Too high:
Entraining of bubbles
Inadequate sampling of particles due to slow movement
of diluent
Pump may work too hard
2. Too low:
b) Active life:
1. Will the diluent absorb unwanted water?
2. Will the diluent allow growth of bacteria, yeast, etc. (may use
preservatives)?
c) Reactivity:
1. Will the diluent degrade the instruments polyethylene fill and
wastetanks over time?
2. Will the diluent degrade the instruments stainless steel fill and waste
tanks over time?
3. Will the diluent degrade all wetted materials in the instrument?
d) Purity:
1.
Is the diluent chemically pure?
2.
Is the diluent free of interfering particles? (If not,
filtering may be appropriate).
e) Refractive Index:
1. Is the R.I. of the diluent the same or very close to that of the sample? If
so, the instrument may not be able to see the sample.
f) Color:
PN 7221940 Rev. A
105
APPENDIX II
LS 13 320
SAMPLE PREPARATION
__________________________________________________________________________________
1. If the color of the diluent is similar to the color of the laser, the
instrument may not be able to see the sample.
2. If the color of the diluent causes the sample to be too opaque, the
instrument may not be able to see the sample.
PN 7221940 Rev. A
106
APPENDIX III
LS 13 320
OPTICAL MODELS
_____________________________________________________________________________
APPENDIX III
1. INTRODUCTION
The Fraunhofer optical model preprogrammed in your system is a general optical
model that can be used for any sample (and suspension fluid) on the LS 13 320.
The LS 13 320 also lets you make optical models using the complete Mie theory
of the scattering of light by spherical particles. The Mie theory takes into account
the complex refractive indices of both the particles and the suspension fluid. For
particles larger than 100 microns in diameter, the Fraunhofer model will produce
results almost identical to those obtained with an optical model generated for the
material and fluid. Between 10 and 100 microns, the difference will be observable
but slight, and is generally considered negligible. If a sample contains a
significant fraction of material below 10 microns, however, the correct optical
model will produce significantly more accurate size distributions than the
Fraunhofer model.
Please note that for an optical model to be correct, the model must match the
sample. Since the Mie theory assumes spherical particles with a homogeneous
refractive index, if a material deviates significantly from these conditions (for
example needles or rods, or birefringent materials), the resulting size distribution
may not be accurate.
2. REFRACTIVE INDEX
The complex refractive index consists of a real part and an imaginary part. The
real part is what is generally thought of as the refractive index; the imaginary part
represents the absorption coefficient of the material. The real part of the refractive
index of most samples and suspension fluids are listed in reference books such as
the Merck Index or the CRC Handbook of Chemistry and Physics. This number
must be known to within 0.01 to 0.03 units. The real part of the refractive index
for most samples ranges from 1 to 3; the real part for most suspension fluids
ranges from 1 to 2.
The imaginary or absorptive part of the refractive index for a sample is hard to
find in any reference. Use the guidelines below to enter the imaginary part of the
refractive index. This does not affect the results substantially unless the value of
this parameter changes by a factor of greater than approximately 3.
Guidelines to use as an estimation of the imaginary part of the refractive index:
White or transparent powders - 0 to 0.1
&"
PN 7221940 Rev. A
107
APPENDIX III
LS 13 320
OPTICAL MODELS
__________________________________________________________________________________
&"
&"
Clicking on the Dry Powder Module check box will disable the Extended
Optical Model (PIDS) and to switch to the .rff file name extension.
PN 7221940 Rev. A
108
APPENDIX III
LS 13 320
OPTICAL MODELS
_____________________________________________________________________________
2.
Enter a name for the optical model in the File name field.
3.
4.
5.
Enter the real part of the refractive index for the fluid (suspension
fluid). See Table 1. If the Tornado DPS is being used, enter 1 in
this field.
6.
Enter the real and imaginary parts of the refractive index for the
sample to be analyzed.
An optical model can also be created from the RunFile menus or during the creation
of a Standard Operating Method (SOM).
Creating an Optical Model from the RunFile Menu
From the RunFile menus
1. # Analyze
2. # Compute Sizes. The Select Optical Model dialog is displayed
"
3. # the New Model button to display the Make Optical Model dialog. Follow
steps 2 through 6 above under Creating an Optical Model.
PN 7221940 Rev. A
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APPENDIX III
LS 13 320
OPTICAL MODELS
__________________________________________________________________________________
PN 7221940 Rev. A
110
APPENDIX III
LS 13 320
OPTICAL MODELS
_____________________________________________________________________________
Refractive Index
(Real)
Liquid
Refractive Index
(Real)
Acetic acid
1.370
1-Hexanol
1.416
Acetone
1.357
1.395
Acetophenone
1.532
Isopropyl alcohol
1.374
Benzene
1.498
Kerosene
1.440
1-Butyl alcohol
1.398
Methanol
1.326
Carbon
tetrachloride
1.459
1.377
Cyclohexane
1.424
Mineral oil
1.438
Cyclohexanol
1.465
Nitromethane
1.382
Dimethylsulfoxide
1.476
1-Octanol
1.427
Ether (di-ethyl)
1.350
1-Pentanol
1.408
Ethyl alcohol
1.359
Polyethylene glycol
1.460
Ethylene glycol
1.431
1-Propanol
1.383
Formamide
1.446
p-Xylene
1.493
Furfural
1.526
Pyridine
1.507
1-Heptane
1.385
Silicon oil
1.405
1-Heptanol
1.423
Silicone oil
1.399
2-Heptanol
1.418
Styrene
1.545
1-Hexane
1.372
PN 7221940 Rev. A
111
APPENDIX III
LS 13 320
OPTICAL MODELS
__________________________________________________________________________________
Table 2
Refractive Indices for Common Materials
Material
Aluminum657
Refractive Index
Real
Imaginary
1.48
3.9
Material
Refractive Index
Real
Imaginary
Cellulose
1.54
Aluminum Oxide
1.768
Chalk
1.51-1.65
Ammonium
Chloride
1.642
Chromium Oxide
2.55
Anatase
2.49-2.56
Copper729
0.220
Apatite
650
1.63-1.67
Gold
633
2.7
1.8
0.6-0.8
Barite
1.64-1.64
Barium
Fluoride656
1.473
Hematite
2.9-3.2
0.01
Barium Yellow
1.94-1.98
Iron668
1.7
1.8
Boron Oxide
1.63
Iron Oxide
2.32
Cadmium
1.13
Lead Oxide
2.3-2.7
Cadmium Oxide
Calcite
643
Graphite
0.31
756
2.49
Manganese
633
1.66
Platinum
2.7
2.2
Calcium
Carbonate
1.4861.681
Poly(methyl
methacrylate)
1.489
Calcium
Fluoride656
1.432
Poly(styrene
sulfide)
1.657
Calcium
Hydroxide
1.574
Polyvinylchloride
1.52-1.55
Calcium stearate
1.46
Talc
1.54-1.60
Calcium Sulfate
1.521
Teflon
Zinc Oxide
1.35
2.029
633
Carbon Black
1.6-2.0
0.3-0.8
2.1
PN 7221940 Rev. A
112
APPENDIX IV
LS 13 320
STATISTICS
_____________________________________________________________________________
APPENDIX IV
1. INTRODUCTION
The LS13 320 program calculates a number of statistical quantities to characterize
the particle size distribution. The statistics are calculated as they would be for a
frequency distribution, with the volume percent (or surface area percent or number
percent) in a certain size channel being analogous to the frequency of occurrence of
a certain value.
Size channels in the LS 13 320 are spaced logarithmically, and are therefore
progressively wider in span toward larger sizes. Statistical calculations are made
based on the logarithmic center of each channel.
Statistics can be calculated either arithmetically or geometrically (logarithmically);
that is, the statistics are based on either the value of a channel center or the
logarithm of that value. Arithmetic statistics are more appropriate for particle size
distributions that are similar to a Gaussian, or normal distribution. Geometric
statistics are more appropriate for particle size distributions that are closer to lognormal. A log-normal distribution is symmetrical when plotted on a logarithmic
size scale.
The statistical formulas used by the LS 13 320 software, and a brief description of
each, are presented in the next sections.
2.
USER-DEFINED MEAN
The user-defined mean diameter D(p,q) is actually two general formulas, one for
arithmetic means and one for geometric means. These general formulas include the
means defined above as well as others to which the above standard formulas do not
apply. This function allows you to view one type of weighted distribution while
obtaining a mean normally displayed only with another weighting. For example,
the surface-area weighted arithmetic mean diameter can be available when you are
viewing a volume weighted distribution and you have chosen geometric statistics.
You can also define weightings other than the three standard ones, such as
1
n i x ip (p q )
D (p , q ) =
q
n i x i
PN 7221940 Rev. A
113
APPENDIX IV
LS 13 320
STATISTICS
__________________________________________________________________________________
n i x ip ln x i
D (p , p ) = exp
q
n i x i
for p = q (geometric mean),
Where;
xi = the channel center
ni = the percentage of particles in the i'th channel
If D(p,q) is chosen in the Size Statistics Preferences dialog box, and
integers for p and q are entered in the provided entry boxes, D(p,q) will
appear with other statistics when Analyze, Statistics is chosen.
The means represented by some choices of p and q are shown in Table 1,
along with the LS 13 320 program equivalent.
D(p,q)
3.
MEDIAN
The median is the particle diameter at which half of the distribution (half of
the volume percent, surface area percent, or number percent) is larger and
half is smaller.
PN 7221940 Rev. A
114
APPENDIX IV
LS 13 320
STATISTICS
_____________________________________________________________________________
4.
MODE
The mode is the value that occurs most frequently in a set of data. The value of the
mode corresponds to the channel center with the maximum volume percent,
surface area percent, or number percent, depending on the weighting chosen.
5.
6.
VARIANCE
The variance is defined as:
Arithmetic
Va =
[f
(x i
x)
fi
Geometric
Vg = exp2
[f (ln x ln x ) ]
7.
STANDARD DEVIATION
The standard deviation, SD, is the square root of the variance:
Arithmetic
[f (x x ) ]
f
2
SD
Geometric
PN 7221940 Rev. A
115
APPENDIX IV
LS 13 320
STATISTICS
__________________________________________________________________________________
SD g = exp
8.
[f (ln x ln x ) ]
SD * 100 %
x
relative variation as opposed to absolute variation.
CV =
9.
SKEWNESS
Skewness, g1, is the degree of distortion from symmetry of a distribution.
Both the degree and direction of skewness may be determined from the
following formulas:
Arithmetic
g1 =
Geometric
g1 =
[f (x
i
SD
[f (ln x
i
i
3
fi
)]
3
ln x
(ln SD ) f i
)]
3
116
APPENDIX IV
LS 13 320
STATISTICS
_____________________________________________________________________________
10. KURTOSIS
Kurtosis, g2, is a measure of the peakedness of a distribution. It is calculated by
determining moments about the mean from the following equation:
Arithmetic
[f (x x ) ] 3
=
SD f
4
g2
Geometric
g2
[f (ln x
=
i
i
4
ln x
(ln SD ) f i
) ] 3
4
The normal, or Gaussian, distribution is the standard against which the peakedness
of other curves is measured. A normal distribution is referred to as mesokurtic (g2 =
0).
If the distribution has a higher, sharper peak than the normal curve, then it has a
larger degree of kurtosis and is termed leptokurtic (g2 > 0). In a leptokurtic
distribution most of the particle sizes are close to the mean size.
If the distribution has a lower, broader peak than a normal curve, then it has a
smaller degree of kurtosis and is termed platykurtic (g2 < 0). In this type of
distribution, the particle sizes are more widespread.
PN 7221940 Rev. A
117
APPENDIX VI
LS 13 320
MAINTENANCE
__________________________________________________________________________________
APPENDIX V
1. BACKGROUND
The background flux pattern can offer information about the cleanliness and
integrity of the diluent. It is good practice to become familiar with this flux pattern.
Figure 1 is an example of a good background pattern.
Figure 1
Normal Background
If the current background flux pattern is higher in any channel by a factor of two,
the cause should be determined and remedied before running further samples.
Figures 2 and 3 are examples of bad backgrounds and their causes.
To check the background flux pattern on a sample run:
1. # View
2. # Intensity
3. # Graph followed by Background (Flux)
PN 7221940 Rev. A
118
APPENDIX VI
LS 13 320
MAINTENANCE
_____________________________________________________________________________
High background
due to air bubbles
Figure 2
Channel 1
Figure 3
PN 7221940 Rev. A
119
APPENDIX VI
LS 13 320
MAINTENANCE
__________________________________________________________________________________
No
Condensation
on sample cell
windows?
Yes
No
Yes
On sample
cell
windows?
No
Yes
On
projection
windows?
No
Yes
Clean Cell
Windows
Clean Projection
Windows
Yes
Call Service
(800-523-3713)
Scratch on
windows?
No
Yes
PN 7221940 Rev. A
Warm suspension
fluid.
Reduce room
humidity
Scratch on
lenses?
120
APPENDIX VI
LS 13 320
MAINTENANCE
_____________________________________________________________________________
APPENDIX VI
1. CLEANING PROCEDURES
It is important that all glass surfaces in your instrument and sample system are clean,
as dusty or coated optical surfaces can cause erroneous results. Some samples or
suspension fluids may coat the inside of the windows of the sample cell(s). If the
instrument is in a dusty or smoky environment or if vapors are present, the lenses
and outer surfaces of the windows may become coated. Check the optical surfaces
for cleanliness at least every three months, and clean if needed. Depending on the
environment, cleaning may be required more frequently.
1.1. CLEANING FLUIDS
Beckman Coulter recommends the cleaning solution provided with your
instrument to clean the inner surfaces of the sample modules. Beckman
Coulter also recommends LENS CLENS NO. 1 lens cleaner for cleaning the
lenses and sample cell windows.
If a sample module is docked, undock it, if not, open the Optical Module's
door.
________________________________________________________________________
Use lens tissues only once, then discard.
Never use silicone-coated, eyeglass lens tissues to clean lenses. They can
leave a film.
Wash your hands thoroughly before cleaning any lens or sample cell
window. Do not touch optical surfaces with your fingers or skin. Body oils
are difficult to remove from lenses without harming the antireflective
coating.
_______________________________________________________________________
PN 7221940 Rev. A
121
APPENDIX VI
LS 13 320
MAINTENANCE
__________________________________________________________________________________
2.
3.
Squirt lens cleaner onto the creased area of the folded lens tissue.
4.
Place the lens tissues across the upper Fourier lens, holding the tissue in
place with two fingers. See Figure 1.
5.
Wipe down slowly, keeping the tissues about 3 mm (1/8 in.) below the
evaporation line formed.
6.
7.
________________________________________________________________________
If the lens or soft antireflective coating is scratched, the lens must be replaced.
Call your local Beckman Coulter Representative.
_________________________________________________________________________
8.
Carefully inspect the lens' surface for cleanliness by shining a bright light
on it and looking at the surface from all angles.
9.
Upper
Fourier Lens
Lower
Fourier
Figure 1
PN 7221940 Rev. A
122
APPENDIX VI
LS 13 320
MAINTENANCE
_____________________________________________________________________________
________________________________________________________________________
Use lens tissues only once, then discard.
Never use silicone-coated, eyeglass lens tissues to clean lenses. They can
leave a film.
Wash your hands thoroughly before cleaning any lens or sample cell
window. Do not touch optical surfaces with your fingers or skin. Body oils
are difficult to remove from lenses without harming the antireflective
coating.
_______________________________________________________________________
2.
3.
4.
5.
6.
________________________________________________________________________
If the lens or soft antireflective coating is scratched, the lens must be replaced.
Call your local Coulter Representative.
_________________________________________________________________________
7.
Carefully inspect the lens surface for cleanliness by shining a bright light
on it and looking at the surface from all angles.
8.
9.
PN 7221940 Rev. A
123
APPENDIX VI
LS 13 320
MAINTENANCE
__________________________________________________________________________________
Projection Lens
Figure 2
3.1.
2.
Unplug the power cord from the back of the Optical Bench
3.
Insert a screwdriver behind the outer tab and flip out the fuse cartridge.
See figure 3.
4.
Lift the locking tab up and toward you while pulling out the fuse holder.
You might need to use pliers.
5.
6.
7.
8.
9.
PN 7221940 Rev. A
124
APPENDIX VI
LS 13 320
MAINTENANCE
_____________________________________________________________________________
Insert screwdriver
here to lift tab
Figure 3
Fuse Box
_________________________________________________________________________
If a fuse fails shortly after replacement, power down the LS 13 320
optical bench and call your local Beckman Coulter Representative.
________________________________________________________________________
3.2.
A foam gasket from the light shield is blocking the PIDS lamp light path.
If none of these conditions exist, you must replace the PIDS lamp. To replace
the PIDS lamp:
1.
2.
If the ALM is docked into the Optical Bench, Open the Optical Module's
door and remove the sample cell.
3.
4.
Open the left front panel door by inserting a coin into the knob slot and
turning clockwise. See figure 4.
PN 7221940 Rev. A
125
APPENDIX VI
LS 13 320
MAINTENANCE
__________________________________________________________________________________
5.
Unscrew the front two screws on the PIDS lamp assembly cover and
loosen the back two screws. See figure 5.
6.
7.
At the back of the PIDS lamp assembly, loosen the large thumbscrew.
See figure 6.
8.
Push the lever toward the back to expose the PIDS lamp.
_________________________________________________________________________
The PIDS lamp may be very hot if the instrument has just been powered
down. To avoid injury, wait until the lamp cools or wrap some cloth around
the bulb to remove it.
Screws (4)
Figure 5
PN 7221940 Rev. A
126
APPENDIX VI
LS 13 320
MAINTENANCE
_____________________________________________________________________________
2.
3.
Turn the red, gray and black adjustment knobs clockwise as far as they can
go.
PN 7221940 Rev. A
127
APPENDIX VI
LS 13 320
MAINTENANCE
__________________________________________________________________________________
_________________________________________________________________________
Do not look directly at the PIDS lamp when it is on. It emits small amounts of
ultraviolet radiation.
_________________________________________________________________________
4. #% Control, followed by Monitor PIDS Lamp. The PIDS lamp turns on and
the PIDS lamp detector dialog box appears (figure 7).
Figure 7
Note: If the PIDS lamp does not turn on, call your local Beckman Coulter
Representative.
5.
Let the PIDS lamp warm up for 30 seconds before doing the fine alignment. You
can perform step 6 during the warm-up time.
6.
Coarse alignment. Use these steps to align the PIDS lamp filament by centering
its oval beam on the projection slit.
a.
b.
c.
PN 7221940 Rev. A
128
APPENDIX VI
LS 13 320
MAINTENANCE
_____________________________________________________________________________
6. Fine alignment. The goal of the fine alignment is to maximize the beam intensity
at the detector. The red adjustment knob focuses the lamp, and is the primary
control for the fine alignment. If, during focus, the beam location changes, use
the gray and black adjustment knobs to recenter the beam on the slit.
a. Check the PIDS lamp intensity (displayed in %cal) by #% Control,
followed by Monitor PIDS Lamp.
b. Turn the red adjustment knob counterclockwise.
c. Check the PIDS lamp intensity to see if it increased or decreased.
d. Check that the rectangular beam is still centered on the projection slit.
e. Use the gray and black adjustment knobs to again center the
rectangular beam on the projection slit, if needed.
Compare the current PIDS lamp intensity with the one recorded in step 7h.
If they are not within 5%, loosen the locking screws and repeat step 7.
9.
10. Replace the PIDS assembly cover and screw in the four screws.
PN 7221940 Rev. A
129
APPENDIX VI
LS 13 320
MAINTENANCE
__________________________________________________________________________________
PN 7221940 Rev. A
130
LS 13 320
Page
1. Introduction
131
2. System Description
131
132
4. Software
132
4.1 Controls
132
134
134
137
138
138
5. Suspension Fluids
138
141
141
141
144
8. Troubleshooting
148
9. Physical Specifications
149
PN 7221962 Rev. A
131
LS 13 320
________________________________________________________________________________
1. INTRODUCTION
The Universal Liquid Module (ULM) is intended for use with the LS 13 320
Optical Bench. It is capable of suspending samples in the size range 0.04 m to
2000 m.
The ULM measures the entire sample
introduced to the instrument by recirculating the sample. The amount of
sample needed depends on its size and
concentration. Prior sample preparation is
often needed to achieve proper dispersion
(see Appendix II of the Users Manual for
more information on how to disperse
samples) in order to obtain accurate and
valid results. The system is controlled via
software commands that provide ease of
use.
2. SYSTEM DESCRIPTION
The ULM system consists of:
The ULM requires relatively small volumes of sample and dispersing liquid
(total volume 125 ml). It is compatible with both organic and aqueous media.
The set point for the obscuration is user selectable or may be attained
automatically as the sample is added to the vessel.
This sample module has the capability of auto-filling and auto-rinsing using
a self-contained internal pump. The pump allows the unit to be filled and
rinsed automatically, expelling all waste into a waste container (provided
with the module) fitted with an automated level sensor to determine when
the waste container is full.
PN 7221962 Rev. A
132
LS 13 320
4. SOFTWARE
This section covers the controls found in the software program to operate the
ULM. It also covers the parts of the Wizards (Standard Operating Methods
(SOMs)) that deal with the ULM.
4.1. CONTROLS
The ULM system can be operated through a series of manual controls accessed
through the software.
PN 7221962 Rev. A
133
LS 13 320
________________________________________________________________________________
Fill
This option opens the inlet valve to fill the vessel with the diluent. The
drain valve, if open, will be closed. Make sure the fill hose is
completely submerged in the diluent.
Rinse
The rinse settings are found under the Run Cycle Options dialog box.
This dialog box allows you to set the time of drain and the number of
times for the rinse process will take place.
PN 7221962 Rev. A
134
LS 13 320
Pump Speed
This option opens a dialog box that allows you to set the speed of the
pump, by either clicking on the left or right arrow or by dragging the
button to increase or decrease the scale.
PN 7221962 Rev. A
#%Run
Select Create an SOM. A sequence of screens will guide you
through the SOM creation.
135
LS 13 320
________________________________________________________________________________
3.
4.
5.
PN 7221962 Rev. A
136
LS 13 320
6.
PN 7221962 Rev. A
137
LS 13 320
________________________________________________________________________________
The optical model can also be selected during this step. For more on optical
models see Appendix III of the general users manual.
7.
Step 5 provides the user with a summary of the options selected in the
preview steps. The SOM is saved during this step.
SOM files, by default, are saved under the SOP directory, but
they can be saved to the directory of your choice as well.
LS 13 320
4. Select Save. By default the SOP file will be saved under the SOP
directory.
5. SUSPENSION FLUIDS
The materials used in the ULM that come in contact with the suspension fluid
are Teflon, 316 stainless steel, glass, Kal-Rez, and Paralyne Coating.
PN 7221962 Rev. A
139
LS 13 320
________________________________________________________________________________
Only use suspension fluids in the ULM that have Flash Points greater
than 43.3C (110F) and meet the requirements listed below. Examples
of fluids that can be used in the ULM are acetone, weak aqueous-based
acids or bases, mineral oils, ethylene glycol, hexane, etc. The suspension
fluid used depends on the type of sample to be analyzed.
Suspension fluid requirements:
Consistency - no bubbles
Butanol
Carbon Tetrachloride
Ethanol
Glycerol*
Hexanes
Kerosene
Methanol
Mineral Oil*
Petroleum Ether
Propanol
Toluene
Trichloroethylene
Weak acid and base solutions (pH 4-10)
Butanone
Chloroform
Ethylene Glycol*
Heptanes
Jet Fuels
Ketones
Methylene Chloride
Pentanes
Polyethylene Glycol*
Silicone Oil*
Trichloroethane
Water
*These fluids are highly viscous and result in a slower flow rate. Use only when
diluted so that viscosity does not exceed 5 centipoise.
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Note: Before changing from one suspension fluid to another, make sure that the
two fluids are miscible with one another. If the two fluids are not miscible,
replace the current fluid with a suspension fluid with which they are both
miscible and then change to the new suspension fluid. Mixing of immiscible
fluids will form an emulsion that may be very difficult to remove from the
system. Table 1 provides a miscibility guide for some common solvents.
Solvent Miscibility
Acetic acid
Acetone
Acetonitrile
Miscible
Benzene
Immiscible
Butanol
Carbon tetrachloride
Chloroform
Cyclohexane
Cyclopentane
Dichloroethane
Dichloromethane
Dimethylformamide (DMF)
Dimethylsulfoxide (DMSO)
Dioxan
Water
Ethanol
Ethyl acetate
Diethyl ether
n-Heptane
n-Hexane
Methanol
Methyl ethyl ketone
Iso-octane
n-Pentane
2-Propanol
Diisopropyl ether
Tetrachloroethane
Tetrahydrofuran (THF)
Toluene
Trichloroethane
Xylene
Table 1
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________________________________________________________________________________
2.
Select Control.
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3. Select Rinse.
4. Select Open Drain after the Rinse routine has finished.
5. Place the inlet hose into the container containing the cleaning solution
prepared in step 1 above.
6. Select Fill.
7. Let the cleaning solution circulate for 15 minutes to 1 hour,
depending on how dirty the cell is.
8. Select Control, Rinse.
9.
10. After removing the cover you will have access to the inside of the
cell. This will allow you to insert a swab with an extension (provided
with your accessory kit) to clean the inside of the cell windows.
11. Use the same solution prepared in step one to clean the windows
with the swab.
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________________________________________________________________________________
Windows to clean
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Procedure
Use this procedure to replace a diffraction sample cell window that is
scratched or damaged.
To replace a diffraction sample cell window:
1. Drain liquid from module.
________________________________________________________________________
Wear appropriate safety equipment for the suspension fluids being
handled.
_________________________________________________________________________
2. Open the Optical Bench door.
Levers
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________________________________________________________________________________
5. Cup your hand over the loose retaining ring and tilt the sample cell stand
until the retaining ring falls into your hand.
Note: You can now lay down the sample stand so the window to be replaced is facing
up.
6. Stick a piece of masking tape on the window and lift the tape up to remove
the O-ring and window. This may take several tries.
7. Discard the old O-ring, window and nylon screws.
8. Hold the new window by its edge to determine the coated side. Refer to
the figure below to determine which side is the correct one.
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a.
Take the eraser end of a pencil and hold it close to the window,
near its edge. Look at the two reflections, dark- and light-colored,
of the pencil.
b.
c.
The side where the pencil touched the dark-colored reflection is the
coated side.
_________________________________________________________________________
Use lens tissues only once, then discard.
Never use silicone-coated, eyeglass lens tissues to clean lenses or
sample cell windows, as this type of tissue may leave a film.
Wash your hands thoroughly before cleaning any lens or sample cell
window. Do not touch optical surfaces with your fingers or skin. Body
oils are difficult to remove without harming the antireflective coating.
_________________________________________________________________________
9. Lay the window, coated side down, on a piece of lens tissue.
10. Clean the window with lens tissue wetted with lens cleaner.
11. Gently place the window, coated side to the outside, into the sample cell
opening. It must be flat to avoid scratching the other window.
12. Lubricate the O-ring with lens cleaning solution.
13. Carefully place the new O-ring on top of the window.
14. Insert the grooved end of the window-sealing tool into the sample cell.
Push in gently and twist from side to side to seat the O-ring.
15. Remove the tool and check that the O-ring is completely seated down and
around the window.
16. Clean the retaining ring, then gently drop it on top of the window.
17. Screw in the two new nylon screws that hold the retaining ring.
18. Clean the outer surface of the diffraction window as described in step 10.
19. Replace the window on the other side if needed using steps 4 through 18.
20. Insert both hoses into the bottom of the sample cell stand. Make sure they
are tight.
21. Load the ULM into the optical bench and dock it.
22. Perform a leak test.
a.
b.
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________________________________________________________________________________
c.
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8. TROUBLESHOOTING
Problem
No communication with optical
bench
Module wont fill
Module leaking
PN 7221962 Rev. A
Possible Solution
Module docked incorrectly. Undock
module and re-dock. Apply slight
pressure on the front of module while
docking
Check to see if it is already full
Check that connections are air-tight
Check that the fill hose is submerged in
the liquid
The valve should make an audible
sound. If it does not, contact Beckman
Coulter service
Check that the waste container is not
full
Check that the drain hose is clear of
obstructions
Module is not completely full of fluid
Check power to the system
Check belt drive
Check fittings
If leakage is inside, contact Beckman
Coulter service
149
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________________________________________________________________________________
9. PHYSICAL SPECIFICATIONS
Power
The ULM derives its power directly from the optical bench
< 50 W peak-power
Temperature
10 to 40C (50 to 104F)
Humidity
0 to 90% without condensation
Dimensions
Height
49.5 cm
19.5 in
1
2
Width
21.0 cm
8.25 in
Depth1
11.4 cm
4.5 in
Depth2
24.1 cm
9.5 in
Weight
8.85 Kg
19.5 lb.
PN 7221962 Rev. A
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Page
1. Introduction
152
2. System Description
152
2.1 Indicators
3. Connecting the ALM
154
154
154
154
155
4. Software
156
4.1 Contro
156
158
158
161
162
163
7. Suspension Fluids
164
165
165
165
167
10. Troubleshooting
170
171
PN 7221962 Rev. A
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The ALM presents the entire sample to the instrument by re-circulating the
sample. The amount of sample needed depends on its size and concentration. Prior
sample preparation is often needed to achieve proper dispersion (see Appendix II
of the Users Manual for more information on how to disperse samples) in order
to obtain accurate and valid results. The system is controlled via software
commands that provide ease of use.
2. SYSTEM DESCRIPTION
The ALM system consists of:
A Sample cell.
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The ALM requires a total volume of 1250 ml. Using the automatic fill
mode, the system only uses 1100 ml. This module is intended to be used
with water only.
The ALM has the capability of auto-filling and auto-rinsing using a selfcontained internal pump operated through software commands or
manually. The pump fills the vessel to a set point that is controlled by a set
of level sensors (figure 1). If the vessel is manually filled, an alarm will
sound to indicate that the liquid level has reached the top sensor. This is
intended to avoid spillage of fluid.
Liquid
level
Figure 1
2.1.
INDICATORS
A set of LEDs placed in the front panel of the module is used to
provide information about the functioning system when it is operated
in manual mode. Figure 2 shows these LEDs and their function.
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These indicators are active only when used in manual mode and not through
the computer.
Figure 2
Indicators
&"Fill used to fill the vessel. Pressing this button will turn the LED on
to indicate the vessel is being filled.
&"Pump when lit indicates that the pump is on.
&"Sonicate indicates that the sonicator is on.
&"Rinse used to manually rinse the vessel.
Figure 3 shows the Open/Close knob. This knob, found in the front panel
of the module, may be used manually as well as through the computer to
open and close the drain valve.
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RECIRCULATING HOSES
The module is connected to the sample cell by two hoses as shown in figure 4.
Note that each hose is labeled as a line: line 1 takes fluid from the module to
the sample cell while line 2 returns the fluid to the module, making it a
closed-loop system.
Figure 4
3.2.
Two more hoses are used to bring fluid to the vessel and to drain the
entire system. These hoses connect to the back of the instrument
(figure 5), where the inlet hose is also connected to a supplied
pressure regulator and gauge used to maintain the appropriate water
pressure (see specifications for the operating pressures).
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Drain Hose
Pressure
Regulator
Inlet Hose
Pressure
Gauge
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7. When these pins have engaged into the slots on the back of the
Sample Cell, tip the module down to its normal horizontal
position. The Sample Cell should now be resting on the autodock
tray.
8.
Press the Close button and the Sample Cell will be drawn into the
LS 13 320.
4. SOFTWARE
This section covers the controls found in the software program to operate the
ALM. It also covers the parts of the Wizards (Standard Operating Methods
(SOMs)) that deal with the ALM.
4.1.
CONTROL
Fill
This option fills the vessel up to the third level sensor. Note that if
the drain valve is open, it will remain open during the filling
process.
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Rinse
Selecting this option will rinse the vessel by adding, draining and
recirculating fluid throughout the entire module system. During this
process the drain valve knob will automatically open and close. Do not
attempt to stop this action manually. To stop the system from rinsing
select Cancel.
Pump Speed
This option opens a dialog box that allows you to set the speed of the
pump, by either clicking on the left or right arrow or by dragging the
button to increase or decrease the scale.
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Open Drain
Using this option will turn the pump off, if it is on, after the liquid
level drops below the bottom level sensor while draining the
vessel.
Sonicate
Applies sonication to aid in the dispersion of the sample.
Maximum allowable time is 999 seconds. Maximum output power
by the probe is 73 W.
4.2.
4.3.
CREATING SOMS
To create an SOM:
1. #%Run
PN 7221961 Rev. A
2.
3.
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4.
5.
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8.
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maximum (100%) and then reduced to about 50%, air bubbles can be
eliminated. This procedure may need to be repeated two to three
times to eliminate the bubbles. High pump speeds are also useful
when measuring large, dense particles. You can access the manual
speed control from the Control menu, then selecting Pump Speed.
The optical model can also be selected during this step. For more on
optical models see Appendix III of the general users manual.
4.4.
LOADING AN SOM
To load an SOM:
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1. #%Run
2. Select Load an SOM
3. Select the SOM file from the list
4.5.
CREATING SOPS
Standard Operating Procedures (SOPs) are the last step in
setting all the parameters necessary to fully control the operation
of the instrument.
To create an SOP:
1. #%Run
2. Select Create an SOP
3. From the create an SOP dialog box, select an SOM and
preference files
4. Select Save. By default the SOP file will be saved under the
SOP directory.
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4.6.
LOADING AN SOP
To load an SOP:
1. #%Run
2. Select Load an SOP. SOPs can also be loaded from the status bar by
clicking on the Load SOP button
3. Select the SOP file of interest
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5. SUSPENSION FLUIDS
"Be sure that the product being sized and the suspension fluid do not
violate any hazardous waste or clean water discharge regulations.
In normal operation, the materials inside the system that come into contact with
the suspending fluid and the test particles are as follows:
304 stainless steel
borosilicate glass
Teflon tubing
Buna-N rubber
Viton O-rings
Kal-rez O-rings
Brass
Carbon
Kel-F diaphram
Polycarbonate
Titanium
The ALM requires clean, bubble-free liquid for its suspension fluid. Regular tap
water that is filtered and degassed can be used. We recommend that you use a 0.2m, or smaller, prefilter. Only use suspension fluids in the ALM that have Flash
Points greater than 43.3C (110F) and meet the requirements listed below.
Examples of fluids that can be used in the ALM are water, weak aqueous-based
acids or bases, mineral oils, ethylene glycol, hexane, etc. The suspension fluid used
depends on the type of sample to be analyzed.
Suspension fluid requirements:
Consistency - no bubbles
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CLEANING FLUIDS
Beckman Coulter recommends cleaning solution supplied with the module
for cleaning the inner surfaces of the ALM sample system.
Beckman Coulter recommends lens cleaning paper for cleaning the lenses
and sample cell windows.
6.2.
2.
Select Control.
3.
4.
7.
8.
9. After removing the cover you will have access to the inside of the
cell. This will allow you to insert a swab with an extension (provided
with your accessory kit) to clean the inside of the cell windows.
PN 7221961 Rev. A
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10. Use the same solution prepared in step one to clean the windows
with the swab.
Thumbscrews
Figure 6
Make sure you clean both the PIDS and diffraction windows, shown in figure 7.
PIDS Window
Diffraction Window
Figure 7
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7.
Procedure
Use this procedure to replace a diffraction sample cell window that is scratched
or damaged.
To replace a diffraction sample cell window:
1.
________________________________________________________________________
Wear appropriate safety equipment for the suspension fluids being handled.
_________________________________________________________________________
2.
Open the Optical Bench door and remove the sample cell.
3.
Drain remaining liquid in the cell by disconnecting the two hoses from the
line 1 and line 2 ports on the sample cell front.
4.
Loosen the two Nylon screws to remove the windows (figure 8).
Figure 8
PN 7221961 Rev. A
Diffraction Window
168
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5.
Cup your hand over the loose retaining ring and tilt the sample cell stand
until the retaining ring falls into your hand.
Note: You can now lay down the sample stand so the window to be replaced is
facing up.
6.
Stick a piece of masking tape on the window and lift the tape up to remove
the O-ring and window. This may take several tries.
7.
8.
Hold the new window by its edge to determine the coated side. Refer to
the figure below to determine which side is the correct one.
a. Take the eraser end of a pencil and hold it close to the window,
near its edge. Look at the two reflections, dark- and light-colored,
of the pencil.
b. Turn the window over and repeat step a.
c. The side where the pencil touched the dark-colored reflection is the
coated side.
_________________________________________________________________________
Use lens tissues only once, then discard.
Never use silicone-coated, eyeglass lens tissues to clean lenses or
sample cell windows, as this type of tissue may leave a film.
Wash your hands thoroughly before cleaning any lens or sample cell
window. Do not touch optical surfaces with your fingers or skin. Body
oils are difficult to remove without harming the antireflective coating.
_________________________________________________________________________
9.
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10. Clean the window with lens tissue wetted with lens cleaner.
11. Gently place the window, coated side to the outside, into the sample cell
opening. It must be flat to avoid scratching the other window.
12. Lubricate the O-ring with lens cleaning solution.
13. Carefully place the new O-ring on top of the window.
14. Insert the grooved end of the window-sealing tool into the sample cell.
Push in gently and twist from side to side to seat the O-ring.
15. Remove the tool and check that the O-ring is completely seated down and
around the window.
16. Clean the retaining ring, then gently drop it on top of the window.
17. Screw in the two new nylon screws that hold the retaining ring.
18. Clean the outer surface of the diffraction window as described in step 10.
19. Replace the window on the other side if needed using steps 4 through 18.
20. Insert both hoses into the bottom of the sample cell stand. Make sure they
are tight.
21. Load the ALM into the optical bench and dock it.
22. Perform a leak test.
a.
b.
c.
PN 7221961 Rev. A
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8.
TROUBLESHOOTING
Problem
No communication with optical
bench
Module wont fill
Module leaking
PN 7221961 Rev. A
Possible Solution
Module docked incorrectly. Undock
module and re-dock.
Check to see if it is already full
Check that connections are air-tight
Make sure there is enough inlet
pressure
Check that the drain hose is clear of
obstructions
Module is not completely full of fluid
Check power to the system
Sample cell not fully docked
Check fittings
If leakage is inside, contact Beckman
Coulter service
171
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9. PHYSICAL SPECIFICATIONS
Power
The ALM derives its power directly from the optical bench
< 50 W peak-power
TEMPERATURE
10 to 40C (50 to 104F)
Humidity
0 to 90% without condensation
Dimensions
Height
29.85 cm
11.75 in
Width
38.7 cm
15.25 in
Depth
34.9 cm
13.75 in
Weight
15.4 Kg
34.0 lb.
PN 7221961 Rev. A
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